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n\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg1}{\bkmkend Pg1}\par\pard
\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\
ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\
f2\fs20 Materiales y mtodos \par\pard\ql \li4352\sb0\sl-322\slmult0 \par\pard\ql\
li4352\sb152\sl-322\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf2\f3
\fs28 3- MATERIALES Y MTODOS \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql
\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb24\sl-276\slmult0 \up0 \expndtw
-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 3.1. DISOLVENTES Y REACTIVOS \par\p
ard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pa
rd\ql\li1418\sb12\sl-276\slmult0 \up0 \expndtw-2\charscalex100 Los disolventes y
reactivos, normalmente de calidad PA-ACS, se utilizaron sin purificacin previa.
\par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb268\sl-276\slmult0
\up0 \expndtw-3\charscalex100 Los disolventes deuterados utilizados para RMN so
n: \par\pard\li1418\sb147\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex10
0 -\tab \up0 \expndtw-3\charscalex100 CDCl\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\
cf3\f4\fs24 -d, grado de deuteracin mnimo 99,8% (Merck).\par\pard\li1418\sb137\sl276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\chars
calex100 TFA-d, grado de deuteracin mnimo 99,8% (Aldrich).\par\pard\li1418\sb138\s
l-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\cha
rscalex100 TFA, grado de pureza 99,8% (Aldrich).\par\pard\li1418\sb136\sl-276\sl
mult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\charscalex1
00 cido frmico-d, grado de deuteracin mnimo 98% (Aldrich).\par\pard\li1418\sb0\sl-27
6\slmult0\par\pard\li1418\sb274\sl-276\slmult0\fi0 \up0 \expndtw-3\charscalex100
Los enzimas utilizados en los ensayos de biodegradacin son:\par\pard\li1418\sb13
8\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0 \expndtw-3\
charscalex100 Papana (Carica papaya), 30,000 unidades/mg, N 7144 (Merck).\par\pard
\li1418\sb137\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscalex100 -\tab \up0
\expndtw-3\charscalex100 Proteinasa K (Tritirachium album), 11.3 unidades/mg (S
igma).\par\pard\li1418\sb136\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\charscale
x100 -\tab \up0 \expndtw-3\charscalex100 Lipasa (Pseudomonas cepacea), 40 unidad
es/mg (Fluka).\par\pard\li1418\sb137\sl-276\slmult0\fi0\tx1778 \up0 \expndtw-3\c
harscalex100 -\tab \up0 \expndtw-3\charscalex100 Lipasa (Candida cylindracea), 9
43 unidades/mg (Sigma).\par\pard\li1418\sb138\sl-276\slmult0\fi0\tx1778 \up0 \ex
pndtw-3\charscalex100 -\tab \up0 \expndtw-3\charscalex100 Lipasa (Rizophus delem

ar), 0.4 unidades/mg (Fluka)\par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql


\li1418\sb254\sl-276\slmult0 \up0 \expndtw-3\charscalex100 3.2. SNTESIS \par\pard
\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\
ql\li1418\sb12\sl-276\slmult0 \up0 \expndtw0\charscalex103 3.2.1. Sntesis de comp
uestos modelo. \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri122
0\sb20\sl-412\slmult0 \up0 \expndtw0\charscalex105 La sntesis de los compuestos m
odelo se llev a cabo segn los procedimientos empleados en la \line \up0 \expndtw0\
charscalex100 preparacin de retro-pptidos.\ul0\super\cf5\f6\fs23 76 \ul0\nosupersu
b\cf3\f4\fs24 Para los dos compuestos con estructura: MeO-OC-R-NH-OC-R-CO-\line \
up0 \expndtw0\charscalex103 NH-R-CO-OMe, donde R es un grupo metileno para el ca
so del aminocido glicina y R\u8217? es el grupo \line \up0 \expndtw0\charscalex10
5 tereftlico (C\ul0\sub\cf5\f6\fs24 6\ul0\nosupersub\cf3\f4\fs24 H\ul0\sub\cf5\f6
\fs24 4\ul0\nosupersub\cf3\f4\fs24 ) u oxlico (CO-CO), el mtodo consisti en hacer r
eaccionar dos moles del ster \line \up0 \expndtw-1\charscalex100 metlico del aminoc
ido con un mol del dicloruro del cido correspondiente en presencia de trietilamin
a \line \up0 \expndtw-3\charscalex100 como base. \par\pard\qj \li1418\sb0\sl-413
\slmult0 \par\pard\qj\li1418\ri1219\sb15\sl-413\slmult0 \up0 \expndtw0\charscale
x100 El modelo: CH\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 C\ul0\sub\cf
5\f6\fs24 6\ul0\nosupersub\cf3\f4\fs24 H\ul0\sub\cf5\f6\fs24 4\ul0\nosupersub\cf
3\f4\fs24 CO-NHCH\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 CO-O(CH\ul0\s
ub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 )\ul0\sub\cf5\f6\fs24 6\ul0\nosupers
ub\cf3\f4\fs24 O-OCCH\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 NH-COC\ul
0\sub\cf5\f6\fs24 6\ul0\nosupersub\cf3\f4\fs24 H\ul0\sub\cf5\f6\fs24 4\ul0\nosup
ersub\cf3\f4\fs24 CH\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 , se prepa
r en dos etapas. La \up0 \expndtw0\charscalex109 primera es una esterificacin con c
ido p-toluenosulfnico de dos moles de glicina con uno de \up0 \expndtw0\charscale
x107 1,6-hexanodiol. A continuacin, un mol del trmero anterior se trat con dos mole
s de cloruro de \up0 \expndtw-3\charscalex100 4-metilbenzoilo en presencia de tr
ietilamina como base. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10
287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb19\sl-230\slmult0 \up0 \expndtw-4\
charscalex100 \ul0\nosupersub\cf1\f2\fs20 33
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}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g2}{\bkmkend Pg2}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0
\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscal
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\ql \li1418\sb0\sl
-276\slmult0 \par\pard\ql\li1418\sb216\sl-276\slmult0 \up0 \expndtw0\charscalex1
03 \ul0\nosupersub\cf3\f4\fs24 3.2.2. Sntesis de polmeros. \par\pard\qj \li1418\sb
0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb24\sl-410\slmult0 \up0 \expndtw0\c
harscalex100 El mtodo de polimerizacin empleado se eligi en funcin del tipo de polmer
o. Las poliesteramidas y \up0 \expndtw0\charscalex104 poliamidas fueron sintet
izadas por polimerizacin interfacial o trmica, y los polisteres por \up0 \
expndtw-3\charscalex100 polimerizacin trmica. \par\pard\ql \li1418\sb0\sl-276\slmu
lt0 \par\pard\ql\li1418\sb265\sl-276\slmult0 \up0 \expndtw-3\charscalex100 3.2.2
.1. POLIMERIZACIN INTERFACIAL \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\pard\q
j\li1418\ri1221\sb20\sl-412\slmult0 \up0 \expndtw-2\charscalex100 Se trata de un
a reaccin bimolecular que tiene lugar en la interfase entre dos lquidos inmiscible
s. En la \up0 \expndtw-1\charscalex100 fase orgnica se encuentra disuelto el diha
luro de cido, y en la fase acuosa la diamina o el diol segn \up0 \expndtw0\charsca
lex106 se trate de poliamidacin o poliesterificacin, respectivamente. Esta tcnica a

provecha la mayor \up0 \expndtw0\charscalex104 reactividad de los dihaluros de ci


do frente a sus correspondientes disteres o dicidos.\ul0\super\cf5\f6\fs23 77 \ul0
\nosupersub\cf3\f4\fs24 Algunos \up0 \expndtw0\charscalex100 factores como la co
nversin de la reaccin pueden verse afectados por la agitacin del sistema. Dos \up0
\expndtw0\charscalex100 tipos de sistemas pueden ser empleados: sin agitacin y co
n agitacin. \par\pard\qj \li1418\ri1220\sb402\sl-420\slmult0 \up0 \expndtw0\chars
calex102 En los sistemas sin agitacin el polmero no es soluble en la interfase y a
l poner en contacto ambas \up0 \expndtw0\charscalex103 soluciones se observa la
formacin de un film o filamento, l cual puede tener resistencia mecnica \up0 \expnd
tw-2\charscalex100 suficiente para ir estirndose y eliminndose de forma contnua del
medio de reaccin. \par\pard\qj \li1418\ri1220\sb400\sl-420\slmult0 \up0 \expndtw
0\charscalex103 Los sistemas con agitacin se aplican a polmeros que precipitan rpid
amente y no es necesaria la \up0 \expndtw-2\charscalex100 formacin de un film par
a eliminarlo del medio de reaccin, el polmero es aislado por filtracin. \par\pard\q
j \li1418\ri1220\sb405\sl-414\slmult0 \up0 \expndtw0\charscalex103 Algunos facto
res que influyen en el rendimiento y peso molecular de los polmeros obtenidos por
el \up0 \expndtw0\charscalex109 mtodo de polimerizacin interfacial deben ser cons
iderados. En primer lugar, es necesaria la \up0 \expndtw-2\charscalex100 presenc
ia en la fase acuosa de una base inorgnica que neutralice el subproducto cido proc
edente de \up0 \expndtw0\charscalex107 la reaccin de condensacin, en caso contraro s
te reaccionara con la diamina para dar la sal \up0 \expndtw-1\charscalex100 hidro
clrica y se reducira sustancialmente el peso molecular resultante. Aunque las base
s fuertes son \up0 \expndtw0\charscalex100 mejores aceptores de subproductos cido
s y deben emplearse en la sntesis de poliamidas,\ul0\super\cf5\f6\fs23 78 \ul0\no
supersub\cf3\f4\fs24 deber \up0 \expndtw0\charscalex100 considerarse su eleccin en
el caso de monmeros con enlaces fcilmente hidrolizables a pH bsico. \up0 \expndtw2\charscalex100 En stos casos se escogen bases ms dbiles como el carbonato de sdio.
\par\pard\qj \li1418\ri1222\sb402\sl-420\slmult0 \up0 \expndtw-2\charscalex100 E
l dihaluro de cido puede sufrir hidrlisis dando lugar al dicido a concentraciones e
levadas de base y \line \up0 \expndtw-2\charscalex100 a bajas velocidades de pol
imerizacin. La hidrlisis no slo reduce la velocidad de polimerizacin, sino \par\pard
\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\
ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql
\li1418\sb37\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2
\fs20 34
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p{\sn fBehindDocument}{\sv 1}}{\sp{\sn lineColor}{\sv 0}}
}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g3}{\bkmkend Pg3}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0
\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscal
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1220
\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 t
ambin limita en gran medida el peso molecular del polmero debido a que el dicido re
sultante no \up0 \expndtw-2\charscalex100 resulta reactivo a las temperaturas
en que tiene lugar la polimerizacin interfacial. \par\pard\qj \li1418\sb0\sl-412\
slmult0 \par\pard\qj\li1418\ri1220\sb19\sl-412\slmult0 \up0 \expndtw-1\charscale
x100 La eleccin del disolvente en la fase orgnica tambin juega un papel importante
en el control del peso \line \up0 \expndtw0\charscalex107 molecular, ya que la r
eaccin parece tener lugar en este lado de la interfase. El disolvente debe \line
\up0 \expndtw0\charscalex106 mantener disuelto el polmero en crecimiento hasta qu
e ste alcance un tamao suficientemente \line \up0 \expndtw-2\charscalex100 grande

como para precipitar. Disolventes como xileno y tetracloruro de carbono tienden


a dar polmeros \line \up0 \expndtw0\charscalex103 de peso molecular ms bajo que cl
oroformo o diclorometano porque precipitan todas las fracciones \line \up0 \expn
dtw-3\charscalex100 polimricas. \par\pard\qj \li1418\ri1219\sb408\sl-413\slmult0
\up0 \expndtw-2\charscalex100 A pesar de las ventajas que el mtodo representa, ex
isten ciertos inconvenientes que limitan su utilidad \line \up0 \expndtw0\charsc
alex100 industrial como el elevado coste de los reactivos y la grande cantidad d
e disolvente que es necesario \line \up0 \expndtw0\charscalex100 utilizar y recu
perar posteriormente. La polimerizacin interfacial puede utilizarse para obtener
diversos \line \up0 \expndtw-2\charscalex100 polmeros, aunque los policarbonatos
son los nicos que se obtienen actualmente a escala industrial. \par\pard\ql \li14
18\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw-3\c
harscalex100 3.2.2.2. POLIMERIZACIN TRMICA \par\pard\qj \li1418\sb0\sl-410\slmult0
\par\pard\qj\li1418\ri1220\sb44\sl-410\slmult0 \up0 \expndtw0\charscalex105 El
mtodo de polimerizacin trmica es ventajoso respecto al de polimerizacin interfacial
para la \up0 \expndtw0\charscalex106 produccin industrial debido a que no es nece
saria la recuperacin de reactivos o cualquier otro \up0 \expndtw-3\charscalex100
tratamiento posterior a la polimerizacin. \par\pard\qj \li1418\ri1220\sb402\sl-42
0\slmult0 \up0 \expndtw0\charscalex104 Este proceso tiene un inters particular en
la preparacin industrial de polisteres. Concretamente \up0 \expndtw0\charscalex10
0 podemos ilustrar el proceso caracterstico seguido en la sntesis de los polisteres
relacionados con el \up0 \expndtw-3\charscalex100 presente trabajo. \par\pard\q
j \li1418\ri1221\sb407\sl-412\slmult0 \up0 \expndtw0\charscalex110 Los component
es, dicidos o sus steres y dioles, son aadidos en un recipiente provisto de \line \
up0 \expndtw0\charscalex109 condensador, una entrada de gas, un termmetro y agita
cin. En general se utiliza un exceso \line \up0 \expndtw-2\charscalex100 estequio
mtrico de diol debido a su mayor volatibilidad. Un flujo constante de nitrgeno es
suministrado \line \up0 \expndtw0\charscalex100 para eliminar el aire, mantenien
do la atmsfera inerte. Los componentes son calentados y agitados a \line \up0 \ex
pndtw-1\charscalex100 una temperatura cercana a 140-160\ul0\super\cf5\f6\fs23 \ul
0\nosupersub\cf3\f4\fs24 C para eliminar por destilacin el agua o alcohol, subpro
ductos de \line \up0 \expndtw-1\charscalex100 la reaccin de esterificacin segn si e
l reactivo empleado es un dicido o un dister. La viscosidad de \line \up0 \expndtw
0\charscalex102 la mezcla fundida aumenta conforme lo hace el peso molecular pro
medio del polmero, por lo que la \line \up0 \expndtw-1\charscalex100 agitacin es c
ada vez ms difcil. El polmero puede resultar de bajo peso molecular debido a la men
or \line \up0 \expndtw-1\charscalex100 difusin de los reactivos. El problema se e
vita elevando poco a poco la temperatura del sistema, la cual \par\pard\ql \li10
287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10
287\sb99\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs2
0 35
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}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g4}{\bkmkend Pg4}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0
\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscal
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1221
\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex104 \ul0\nosupersub\cf3\f4\fs24 d
epender de la estabilidad trmica del polmero. En una segunda fase se prosigue la re
accin de \up0 \expndtw-2\charscalex100 condensacin sobre alto vaco para eliminar el
exceso de diol empleado en la polimerizacin. \par\pard\li1418\sb0\sl-276\slmult0

\par\pard\li1418\sb0\sl-276\slmult0\par\pard\li1418\sb7\sl-276\slmult0\fi0\tx282
8 \up0 \expndtw0\charscalex104 (1)\tab \up0 \expndtw0\charscalex104 HO\ul0\nosup
ersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\ul0\nosupersub\cf6\f7\fs
24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OH + HOOC\ul0\nosupersub\cf6\f7\fs24 \u-1
817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0
\nosupersub\cf3\f4\fs24 COOH \ul0\nosupersub\cf6\f7\fs24 \u8594?\ul0\nosupersub\
cf3\f4\fs24 HO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R
\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OCO\ul0\nosupers
ub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f
7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 COOH + H\ul0\sub\cf5\f6\fs24 2\ul0\no
supersub\cf3\f4\fs24 O\par\pard\li1418\sb165\sl-276\slmult0\fi0\tx2834 \up0 \exp
ndtw0\charscalex104 (2)\tab \up0 \expndtw0\charscalex104 HO\ul0\nosupersub\cf6\f
7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\ul0\nosupersub\cf6\f7\fs24 \u-1817?
\ul0\nosupersub\cf3\f4\fs24 OCO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupers
ub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f
4\fs24 COOH + n HO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs2
4 R\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OH + n HOOC\u
l0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosup
ersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 COOH \ul0\nosupersub\cf6\f
7\fs24 \u8594?\par\pard\ql \li2834\sb147\sl-276\slmult0 \up0 \expndtw0\charscale
x105 \ul0\nosupersub\cf3\f4\fs24 H\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosup
ersub\cf4\f5\fs24 [\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs
24 O\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\ul0\nosupe
rsub\cf6\f7\fs24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 OCO\ul0\nosupersub\cf6\f7\f
s24 \u-1817?\ul0\nosupersub\cf3\f4\fs24 R\u8217?\ul0\nosupersub\cf6\f7\fs24 \u-1
817?\ul0\nosupersub\cf3\f4\fs24 CO\ul0\nosupersub\cf6\f7\fs24 \u-1817?\ul0\nosup
ersub\cf4\f5\fs24 ]\ul0\sub\cf7\f8\fs24 n+1\ul0\nosupersub\cf6\f7\fs24 \u-1817?\
ul0\nosupersub\cf3\f4\fs24 OH + 2n H\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4
\fs24 O \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1222\sb38\
sl-413\slmult0 \up0 \expndtw0\charscalex100 Cada una de las sucesivas esterifica
ciones que conducen a la formacin del polister constituye un \up0 \expndtw0\charsc
alex107 verdadero equilibrio qumico. As pues, para obtener un polmero de alto peso
molecular debe \up0 \expndtw-4\charscalex100 desplazarse, tanto como sea posible
, el equilibrio de las reacciones hacia la derecha, o sea, eliminando \up0 \expn
dtw-5\charscalex100 el subproducto que se va formando por aplicacin de alto vaco.
\par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1221\sb14\sl-413\s
lmult0 \up0 \expndtw-1\charscalex100 La velocidad de la reaccin puede ser conside
rablemente aumentada por la accin de catalizadores. \up0 \expndtw0\charscalex100
Algunos trabajos de investigacin demuestran que cidos y varios compuestos organome
tlicos son \up0 \expndtw0\charscalex106 capaces de catalizar estas reacciones.\ul
0\super\cf5\f6\fs23 79\ul0\nosupersub\cf3\f4\fs24 Actualmente, los catalizadore
s de titanio son los ms \up0 \expndtw-3\charscalex100 empleados para la sntesis de
polisteres.\ul0\super\cf5\f6\fs23 80 \par\pard\ql \li1418\sb0\sl-276\slmult0 \pa
r\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosuper
sub\cf3\f4\fs24 3.3. CARACTERIZACIN FISICOQUMICA \par\pard\qj \li1418\sb0\sl-420\s
lmult0 \par\pard\qj\li1418\ri1221\sb6\sl-420\slmult0 \up0 \expndtw-1\charscalex1
00 Los compuestos modelo se han caracterizado por espectroscopa de infrarrojo (IR
), espectroscopa de \up0 \expndtw0\charscalex100 resonancia magntica nuclear de pr
otn (\ul0\super\cf5\f6\fs23 1\ul0\nosupersub\cf3\f4\fs24 H-RMN) y carbono 13 (\ul
0\super\cf5\f6\fs23 13\ul0\nosupersub\cf3\f4\fs24 C-RMN) y determinacin del punto
\up0 \expndtw-3\charscalex100 de fusin (p.f.). \par\pard\qj \li1418\ri1220\sb409
\sl-410\slmult0 \up0 \expndtw0\charscalex109 La caracterizacin de los polmeros se
ha realizado mediante viscosimetra, cromatografa de \line \up0 \expndtw-2\charscal
ex100 permeabilidad en gel (GPC), espectroscopa de infrarrojo (IR), espectroscopa
de resonancia magntica \line \up0 \expndtw-2\charscalex100 nuclear de protn (\ul0\
super\cf5\f6\fs23 1\ul0\nosupersub\cf3\f4\fs24 H-RMN) y carbono 13 (\ul0\super\c
f5\f6\fs23 13\ul0\nosupersub\cf3\f4\fs24 C-RMN), calorimetra diferencial de barri
do \up0 \expndtw-3\charscalex100 (DSC), \par\pard\qj \li1418\ri1220\sb2\sl-420\s
lmult0 \up0 \expndtw0\charscalex100 termogravimetra (TGA), ensayos termodinamomecn
icos (DMTA), ensayos de solubilidad y ensayos \up0 \expndtw-3\charscalex100 de t

ensin-deformacin. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb24


3\sl-276\slmult0 \up0 \expndtw0\charscalex103 3.3.1. Evaluacin del peso molecular
. \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb24\sl-410
\slmult0 \up0 \expndtw0\charscalex107 Las reacciones de polimerizacin pueden prod
ucir cadenas polimricas con distinto nmero de \up0 \expndtw0\charscalex102 unidade
s repetitivas. La mayor parte de los polmeros sintticos son mezclas de macromolcula
s de \up0 \expndtw-2\charscalex100 distintos tamaos, por lo que el peso molecular
proporciona siempre un valor promedio. \par\pard\ql \li1418\sb0\sl-230\slmult0
\par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb19\sl-230\slmult0 \
up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 36 \par\pard\sect\sectd
\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg5}{\bkmkend Pg5}\par\
pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\p
ard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\
cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\sb0\sl-414\slmult0 \par\pard
\qj\li1418\ri1221\sb364\sl-414\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosuper
sub\cf3\f4\fs24 Son muchas las tcnicas existentes para la determinacin del peso mo
lecular medio de un polmero. \up0 \expndtw0\charscalex108 Por tanto, segn el mtodo
experimental utilizado se definen varios valores promedio del peso \up0 \expndtw
0\charscalex103 molecular: en nmero (M\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf3\f
4\fs24 ), en peso (M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 ) o viscos
imtrico (M\ul0\sub\cf5\f6\fs24 v\ul0\nosupersub\cf3\f4\fs24 ). La relacin entre lo
s valores de los \up0 \expndtw0\charscalex102 distintos promedios (M\ul0\sub\cf5
\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 /M\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf
3\f4\fs24 ) se conoce como polidispersidad (D) y se utiliza a menudo para dar un
a \up0 \expndtw-2\charscalex100 idea de la heterogeneidad del peso molecular en
las muestras de polmeros, o lo que es lo mismo, para \up0 \expndtw0\charscalex109
evaluar la anchura de la curva de distribucin de los pesos moleculares. Entre la
s tcnicas de \up0 \expndtw0\charscalex107 determinacin del peso molecular podemos
citar: la dispersin de luz, ebulloscopa, crioscopa, \up0 \expndtw-3\charscalex100 u
ltracentrifugacin, anlisis de grupos terminales y viscosimetra. \par\pard\qj \li141
8\ri1221\sb402\sl-420\slmult0 \up0 \expndtw0\charscalex106 Sin duda, una de las
tcnicas ms utilizadas es la viscosimetra. Esta tcnica para medir el peso \line \up0
\expndtw0\charscalex100 molecular de un polmero fue desarrollada por Staudinger e
n 1930.\ul0\super\cf5\f6\fs23 81\ul0\nosupersub\cf3\f4\fs24 Es una tcnica fcil y
rpida que \line \up0 \expndtw-1\charscalex100 permite conocer el peso molecular p
romedio viscosimtrico \up0 \expndtw-1\charscalex100 (M\ul0\sub\cf5\f6\fs24 v\ul0\
nosupersub\cf3\f4\fs24 ). Cuando el polmero es poco \par\pard\ql \li1418\sb99\sl276\slmult0 \up0 \expndtw-3\charscalex100 polidisperso, M\ul0\sub\cf5\f6\fs24 v\
ul0\nosupersub\cf3\f4\fs24 corresponde aproximadamente a M\ul0\sub\cf5\f6\fs24
w\ul0\nosupersub\cf3\f4\fs24 . \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard
\qj\li1418\ri1219\sb18\sl-413\slmult0 \up0 \expndtw-2\charscalex100 Por otro lad
o, la tcnica que proporciona mayor informacin sobre los pesos moleculares es la GP
C. La \line \up0 \expndtw0\charscalex102 determinacin de la polidispersidad a par
tir de la determinacin de M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 y M
\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf3\f4\fs24 se realiza habitualmente \lin
e \up0 \expndtw0\charscalex106 mediante esta tcnica basada en los principios del
fraccionamiento en funcin del tamao de las \line \up0 \expndtw-3\charscalex100 mac
romolculas. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb265\sl276\slmult0 \up0 \expndtw-3\charscalex100 3.3.1.1. DETERMINACIN DE LA VISCOSIDAD
INTRNSECA [\ul0\nosupersub\cf6\f7\fs24 \u951?\ul0\nosupersub\cf3\f4\fs24 ] \par\p
ard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1219\sb38\sl-413\slmult0
\up0 \expndtw0\charscalex100 La viscosidad de un polmero en solucin depende de la
naturaleza del polmero, del disolvente, de la \line \up0 \expndtw0\charscalex100
distribucin de pesos moleculares, de la concentracin y de la temperatura. Al elim
inar el efecto de la \line \up0 \expndtw-2\charscalex100 concentracin por medidas
a dilucin creciente se obtiene la viscosidad intrnseca que est relacionada \line \
up0 \expndtw0\charscalex104 con el peso molecular promedio de la distribucin deno
minado viscosimtrico, y que para un buen \line \up0 \expndtw0\charscalex103 solve
nte es prximo al promedio en peso. Para cuantificar la relacin viscosidad/peso mol
ecular se \line \up0 \expndtw0\charscalex102 requiere un calibrado con muestras

de peso molecular conocido, normalmente el promedio en peso \line \up0 \expndtw0


\charscalex100 determinado por dispersin de luz. En ausencia de patrones se utili
za la correlacin existente para un \line \up0 \expndtw0\charscalex109 polmero de n
aturaleza similar en el mismo solvente y temperatura. De este modo, se ignoran \
line \up0 \expndtw0\charscalex104 interacciones especficas del polmero en estudio
y el valor que se obtiene es slo orientativo pero \line \up0 \expndtw-3\charscale
x100 adecuado a efectos comparativos. \par\pard\ql \li10287\sb0\sl-230\slmult0 \
par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \
par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \
par\pard\ql\li10287\sb209\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosu
persub\cf1\f2\fs20 37
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{\sp{\sn fFillOK}{\sv 1}}{\sp{\sn fFilled}{\sv 1}}{\sp{\sn fillColor}{\sv 0}}{\s
p{\sn fLine}{\sv 0}}{\sp{\sn lineType}{\sv 0}}{\sp{\sn fArrowheadsOK}{\sv 1}}{\s
p{\sn fBehindDocument}{\sv 1}}{\sp{\sn lineColor}{\sv 0}}
}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g6}{\bkmkend Pg6}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0
\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscal
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1221
\sb374\sl-420\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 M
ediante la ecuacin de Hagen-Poiseuille para lquidos con movimiento en flujo lamina
r, se puede \up0 \expndtw0\charscalex102 relacionar el tiempo que tarda en pasar
un fluido por un capilar con la viscosidad del mismo, por lo \up0 \expndtw0\cha
rscalex100 tanto, la viscosidad de una solucin puede definirse como el tiempo que
tarda la disolucin en pasar \up0 \expndtw0\charscalex106 por un capilar fino por
efecto de la gravedad. La viscosidad intrnseca [\ul0\nosupersub\cf6\f7\fs24 \u95
1?\ul0\nosupersub\cf3\f4\fs24 ] es la extrapolacin a \up0 \expndtw-4\charscalex10
0 concentracin cero de la viscosidad reducida (\ul0\nosupersub\cf6\f7\fs24 \u951?
\ul0\sub\cf5\f6\fs24 red\ul0\nosupersub\cf3\f4\fs24 ), segn la expresin:\par\pard\
sect\sectd\sbknone\cols2\colno1\colw5760\colsr60\colno2\colw5940\colsr160\ql \li
4935\sb0\sl-276\slmult0 \par\pard\ql \li4935\sb79\sl-276\slmult0 \up0 \expndtw0\
charscalex100 [\ul0\nosupersub\cf6\f7\fs24 \u951?\ul0\nosupersub\cf3\f4\fs24 ] =
lm\par\pard\column \ql \li20\sb189\sl-276\slmult0\tx680 \up0 \expndtw0\charscale
x80 \ul0\nosupersub\cf6\f7\fs24 \u-1813? \up0 \expndtw-3\charscalex100 t\tab \up
0 \expndtw0\charscalex80 \u-1802?\par\pard\ql \li401\sb0\sl-192\slmult0\tx1200 \
up0 \expndtw0\charscalex104 \u8722?1\tab \up0 \expndtw-3\charscalex100 c\par\par
d\sect\sectd\sbknone\cols3\colno1\colw5780\colsr40\colno2\colw505\colsr160\colno
3\colw5285\colsr160\ql \li5361\sb1\sl-204\slmult0 \up0 \expndtw-3\charscalex100
\ul0\nosupersub\cf9\f10\fs20 c\u8594?0\par\pard\column \ql \li20\sb0\sl-216\slmu
lt0 \up0 \expndtw0\charscalex80 \ul0\nosupersub\cf6\f7\fs24 \u-1812? \up0 \expnd
tw-3\charscalex100 t\par\pard\ql \li20\sb0\sl-152\slmult0\tx237 \up0 \expndtw0\c
harscalex80 \u-1811? \tab \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf8\f9\f
s14 0\par\pard\column \qj \li20\ri5094\sb0\sl-192\slmult0 \up0 \expndtw0\charsca
lex80 \ul0\nosupersub\cf6\f7\fs24 \u-1801? \line \up0 \expndtw0\charscalex80 \u1800? \par\pard\sect\sectd\sbknone \ql \li1418\sb26\sl-255\slmult0 \up0 \expndtw
0\charscalex106 \ul0\nosupersub\cf3\f4\fs24 donde t y t\ul0\sub\cf5\f6\fs24 0\ul
0\nosupersub\cf3\f4\fs24 son los tiempos de cada de la disolucin y el disolvente;
c es la concentracin de la \par\pard\qj \li1418\ri1222\sb46\sl-400\slmult0 \up0
\expndtw0\charscalex102 disolucin en g.dL\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub
\cf3\f4\fs24 . Los tiempos son proporcionales a la viscosidad si son suficientem
ente grandes \up0 \expndtw-3\charscalex100 para lo cual debe elegirse adecuadame
nte el dimetro del capilar. \par\pard\qj \li1418\sb0\sl-400\slmult0 \par\pard\qj\
li1418\ri1220\sb40\sl-400\slmult0 \up0 \expndtw0\charscalex100 Una vez calculada

la viscosidad intrnseca, se puede determinar el peso molecular viscosimtrico (M\u


l0\sub\cf5\f6\fs24 v\ul0\nosupersub\cf3\f4\fs24 ) \up0 \expndtw-3\charscalex100
de un polmero a partir de la ecuacin de Mark-Houwink: \par\pard\ql \li5559\sb202\s
l-253\slmult0 \up0 \expndtw-3\charscalex100 [\ul0\nosupersub\cf6\f7\fs24 \u951?\
ul0\nosupersub\cf3\f4\fs24 ] = K.M\ul0\sub\cf5\f6\fs24 va \par\pard\qj \li1418\r
i1221\sb106\sl-400\slmult0 \up0 \expndtw0\charscalex104 \ul0\nosupersub\cf3\f4\f
s24 donde K (dL.g\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 ) y a so
n constantes tabuladas que dependen de la naturaleza del polmero, del \up0 \expnd
tw-5\charscalex100 disolvente y de la temperatura. \par\pard\ql \li1418\sb0\sl-2
76\slmult0 \par\pard\ql\li1418\sb267\sl-276\slmult0 \up0 \expndtw-2\charscalex10
0 Experimentalmente la determinacin de la viscosidad intrnseca se realiza midiendo
el tiempo de flujo \par\pard\qj \li1418\ri1222\sb6\sl-420\slmult0 \up0 \expndtw
0\charscalex100 (t) requerido para que un volumen determinado de disolucin polimri
ca atraviese el tubo capilar por \line \up0 \expndtw-4\charscalex100 efecto de l
a gravedad y el tiempo que tarda en hacerlo un volumen equivalente de disolvente
puro (t\ul0\sub\cf5\f6\fs24 0\ul0\nosupersub\cf3\f4\fs24 ). \par\pard\qj \li141
8\ri1219\sb400\sl-420\slmult0 \up0 \expndtw-2\charscalex100 Las medidas se efect
uaron en un viscosmetro capilar Cannon-Ubbelhode tipo semi-micro (modelo 150) \up
0 \expndtw-2\charscalex100 termostatizado a 25\ul0\nosupersub\cf6\f7\fs24 \ul0\no
supersub\cf3\f4\fs24 0.1\ul0\super\cf5\f6\fs23 o\ul0\nosupersub\cf3\f4\fs24 C en
un bao de agua. Se utiliz cido dicloroactico como disolvente, en el \up0 \expndtw-3
\charscalex100 rango de concentraciones 0.1 a 0.035 g/dL. \par\pard\ql \li1418\s
b0\sl-276\slmult0 \par\pard\ql\li1418\sb243\sl-276\slmult0 \up0 \expndtw-5\chars
calex100 3.3.1.2. CROMATOGRAFA DE PERMEACIN EN GEL (GPC) \par\pard\qj \li1418\sb0\
sl-412\slmult0 \par\pard\qj\li1418\ri1221\sb20\sl-412\slmult0 \up0 \expndtw0\cha
rscalex104 La cromatografa de permeacin en gel es una potente tcnica de separacin qu
e encontr gran \line \up0 \expndtw-3\charscalex100 aplicacin en el campo de los po
lmeros despus de su desarrollo en 1961.\ul0\super\cf5\f6\fs23 82 \ul0\nosupersub\c
f3\f4\fs24 Actualmente es la tcnica \line \up0 \expndtw0\charscalex100 ms utilizad
a para la separacin de las molculas de una muestra polimrica en funcin del tamao \lin
e \up0 \expndtw-3\charscalex100 molecular. Se produce como consecuencia de la di
ferente penetracin de las macromolculas a travs \line \up0 \expndtw0\charscalex103
de los poros de un gel dispuesto en el interior de una columna cromatogrfica. Los
materiales de \line \up0 \expndtw-4\charscalex100 relleno de la columna son pri
ncipalmente poliestireno poroso (entrecruzado e hinchado) y vidrio poroso. \par\
pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\p
ard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb29\sl-230\slmult0 \up0 \e
xpndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 38
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}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P

g7}{\bkmkend Pg7}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0


\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscal
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1220
\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 L
os cromatgrafos utilizados son similares a los de HPLC, siendo la columna y el de
tector las partes \up0 \expndtw-3\charscalex100 ms importantes del instrumento. \
par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1221\sb17\sl-413\sl
mult0 \up0 \expndtw0\charscalex100 Cuando una disolucin polimrica, con diferentes
tamaos moleculares es introducida en el interior de \line \up0 \expndtw0\charscal
ex102 la columna cromatogrfica tiene lugar un fraccionamento en funcin de su tamao
molecular y de la \line \up0 \expndtw0\charscalex100 distribucin de tamao de poro
del gel polimrico. Las molculas de mayor tamao se arrastran con el \line \up0 \expn
dtw-1\charscalex100 disolvente, tardan menos tiempo en atravesar la columna y so
n las primeras en abandonarla, mientras \line \up0 \expndtw0\charscalex106 que l
as de tamao menor son retenidas durante un tiempo superior. A la salida de la col
umna se \line \up0 \expndtw0\charscalex107 registra la variacin entre el ndice de
refraccin del disolvente puro y la fraccin recogida. Para \line \up0 \expndtw-2\ch
arscalex100 conocer los valores de los pesos moleculares se requiere un calibrad
o con patrones. \par\pard\qj \li1418\ri1221\sb399\sl-423\slmult0 \up0 \expndtw0\
charscalex105 En este trabajo las medidas se realizaron en un cromatgrafo Waters
(modelo 510) equipado con \line \up0 \expndtw0\charscalex100 columnas \ul0\nosup
ersub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 -Stiragel (Polymer Lab.) de 10000 y
1000 \ul0\nosupersub\cf4\f5\fs24 \ul0\nosupersub\cf3\f4\fs24 de estireno-divini
lbenceno termostatizadas a \line \up0 \expndtw0\charscalex105 35\ul0\super\cf5\f
6\fs23 o\ul0\nosupersub\cf3\f4\fs24 C, con un detector de ndice de refraccin (RI
410) y un programa para tratamiento de datos \line \up0 \expndtw-1\charscalex10
0 (Mxima 820). El calibrado se realiz con muestras de poliestireno (Polysciences)
de baja dispersidad. \line \up0 \expndtw-1\charscalex100 El eluyente consisti en
una mezcla de cloroformo/ortoclorofenol (90/10, v/v) y su velocidad de flujo fue
\line \up0 \expndtw0\charscalex103 de 0.5 mL/min. El volumen inyectado fue de 1
00 \ul0\nosupersub\cf6\f7\fs24 \ul0\nosupersub\cf3\f4\fs24 L y la concentracin d
e las muestras fue de 2.5 \line \up0 \expndtw-3\charscalex100 mg/mL. \par\pard\q
j \li1418\ri1219\sb408\sl-410\slmult0 \up0 \expndtw0\charscalex100 En este traba
jo solamente se efectu el anlisis cromatogrfico con los polisteres. En los nylons y
en \up0 \expndtw0\charscalex104 las poliesteramidas no fue posible su realizacin
debido a los problemas de insolubilidad de estos \up0 \expndtw-3\charscalex100 m
ateriales en los disolventes orgnicos comunes. \par\pard\ql \li1418\sb0\sl-276\sl
mult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmu
lt0 \par\pard\ql\li1418\sb113\sl-276\slmult0 \up0 \expndtw0\charscalex103 3.3.2.
Espectroscopa infrarroja (IR) \par\pard\qj \li1418\sb0\sl-420\slmult0 \par\pard\
qj\li1418\ri1220\sb6\sl-420\slmult0 \up0 \expndtw-1\charscalex100 Constituye una
tcnica espectroscpica de amplio uso que se basa en la excitacin de los modos de \u
p0 \expndtw0\charscalex107 vibracin de las molculas por la absorcin de la radiacin i
nfrarroja. Aunque esta comprende \up0 \expndtw-4\charscalex100 longitudes de ond
a (\ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 ) entre el visi
ble y el microondas, la regin de infrarrojo medio entre 4000-300cm\ul0\super\cf5\
f6\fs23 -1 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\f4\fs24 es la ms emp
leada desde un punto de vista prctico. Durante la excitacin es necesaria una varia
cin \up0 \expndtw-3\charscalex100 del momento dipolar de la molcula para que se pr
oduzca una absorcin en el IR que puede asociarse \up0 \expndtw0\charscalex106 a v
ibraciones de tensin (simtrica o asimtrica) o de deformacin. La deteccin de los grupo
s \up0 \expndtw-3\charscalex100 funcionales presentes es la principal aplicacin d
e la tcnica. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl
-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb187\
sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 39 \par
\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg8}{\b
kmkend Pg8}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-23
0\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100
\ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri2139\sb390
\sl-400\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Las ba

ndas de mayor importancia para los materiales estudiados se resumen a continuacin


: \up0 \expndtw-3\charscalex100 Metilenos \par\pard\ql \li2126\sb123\sl-276\slmu
lt0 \up0 \expndtw-3\charscalex100 2940 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersu
b\cf3\f4\fs24 : tensin asimtrica del C-H. \par\pard\ql \li2126\sb144\sl-276\slmult
0 \up0 \expndtw-3\charscalex100 2860 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\
cf3\f4\fs24 : tensin simtrica del C-H. \par\pard\ql \li1418\ri2990\sb6\sl-420\slmu
lt0\fi708\tx2126 \up0 \expndtw-3\charscalex100 1460 cm\ul0\super\cf5\f6\fs23 -1\
ul0\nosupersub\cf3\f4\fs24 : deformacin asimtrica del C-H. \line\tab \up0 \expndtw
-3\charscalex100 725 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : de
formacin simtrica del C-H. \line \up0 \expndtw-3\charscalex100 Amida \par\pard\ql
\li2126\ri5080\sb0\sl-420\slmult0 \up0 \expndtw-3\charscalex100 3300 cm\ul0\sup
er\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibracin de tensin del N-H (AMIDA A
). \line \up0 \expndtw-3\charscalex100 3100 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosu
persub\cf3\f4\fs24 : sobretono de la amida II (AMIDA B). \line \up0 \expndtw-3\c
harscalex100 1650 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibra
cin de tensin del C=O (AMIDA I). \par\pard\ql \li2126\sb79\sl-276\slmult0 \up0 \ex
pndtw-3\charscalex100 1550 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs2
4 : vibracin de torsin del N-H y tensin del C-N (AMIDA II). \par\pard\qj \li2126\ri
1222\sb34\sl-410\slmult0 \up0 \expndtw-2\charscalex100 1300-1250 cm\ul0\super\cf
5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : interacciones entre las vibraciones de
tensin del C-N y las de torsin del N-H. \up0 \expndtw0\charscalex100 Adems en esta
zona aparecen las vibraciones de tensin del C-C y de torsin de los grupos \up0 \e
xpndtw-3\charscalex100 CH\ul0\sub\cf5\f6\fs24 2\ul0\nosupersub\cf3\f4\fs24 y CH
(AMIDA III). \par\pard\ql \li2126\sb121\sl-276\slmult0 \up0 \expndtw-3\charscal
ex100 627 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibracin de to
rsin de N-C=0 (AMIDA IV). \par\pard\ql \li1418\ri3802\sb6\sl-420\slmult0\fi708\tx
2126 \up0 \expndtw-3\charscalex100 700 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersu
b\cf3\f4\fs24 : vibracin de torsin fuera del plano de N-H (AMIDA V). \line\tab \up
0 \expndtw-3\charscalex100 600 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4
\fs24 : vibracin de torsin fuera del plano de C=O (AMIDA VI). \line \up0 \expndtw
-3\charscalex100 ster \par\pard\ql \li2126\sb99\sl-276\slmult0 \up0 \expndtw-3\ch
arscalex100 1740 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibrac
in de tensin del C=O. \par\pard\ql \li2126\sb144\sl-276\slmult0 \up0 \expndtw-3\ch
arscalex100 1100 cm\ul0\super\cf5\f6\fs23 -1\ul0\nosupersub\cf3\f4\fs24 : vibrac
iones de tensin (simtrica y asimtrica) del C-O. \par\pard\qj \li1418\sb0\sl-420\slm
ult0 \par\pard\qj\li1418\ri1218\sb6\sl-420\slmult0 \up0 \expndtw-1\charscalex100
Los espectros fueron registrados en espectrofotmetros de transformada de Fourier
Perkin-Elmer 1600 \up0 \expndtw0\charscalex106 y Perkin-Elmer 2000 a partir de
muestras slidas dispersas en pastillas de KBr o como pelculas \up0 \expndtw-3\char
scalex100 preparadas por evaporacin lenta del disolvente sobre ventana de NaCl. \
par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \p
ar\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb111\sl-276\slmult0 \u
p0 \expndtw0\charscalex103 3.3.3. Espectroscopa de resonancia magntica nuclear (RM
N) \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1222\sb18\sl-41
3\slmult0 \up0 \expndtw0\charscalex109 La tcnica de RMN se utiliza como complemen
taria a la espectroscopa infrarroja y constituye \line \up0 \expndtw0\charscalex1
09 actualmente una de las ms tiles y empleadas para conocer la estructura de los c
ompuestos \line \up0 \expndtw0\charscalex102 orgnicos. Su papel en el campo de lo
s polmeros se destaca especialmente por proporcionar datos \line \up0 \expndtw-2\
charscalex100 sobre su constitucin, organizacin y dinmica, que difcilmente podran obt
enerse por otros medios. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li
1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li14
18\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418
\sb229\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20
40 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart
Pg9}{\bkmkend Pg9}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb
0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charsca
lex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri122
1\sb379\sl-413\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24
La tcnica analiza la interaccin entre los niveles de energa de los espines de cier

tos ncleos atmicos \up0 \expndtw0\charscalex104 con la radiacin electromagntica. nica


mente los ncleos con momento magntico nuclear sern \up0 \expndtw0\charscalex105 obs
ervables. Los ncleos de sustancias orgnicas ms usuales en RMN, son los de protn (\ul
0\super\cf5\f6\fs23 1\ul0\nosupersub\cf3\f4\fs24 H) y \up0 \expndtw0\charscalex1
09 carbono 13 (\ul0\super\cf5\f6\fs23 13\ul0\nosupersub\cf3\f4\fs24 C). La posic
in de las seales obtenidas depende en los dos casos del entorno \up0 \expndtw0\cha
rscalex105 electrnico. Los espectros de \ul0\super\cf5\f6\fs23 1\ul0\nosupersub\c
f3\f4\fs24 H-RMN consisten en un registro de las seales de resonancia que \up0 \e
xpndtw0\charscalex104 corresponden a los diferentes tipos de hidrgeno presentes e
n la muestra en forma de picos cuya \up0 \expndtw0\charscalex104 posicin, anchura
, rea y subestructura permiten la potente caracterizacin arriba mencionada. La \up
0 \expndtw0\charscalex104 posicin est asociada a la identidad de los diferentes gr
upos vecinos a los protones y se expresa \up0 \expndtw0\charscalex106 como despl
azamiento qumico en ppm respecto a la seal de un grupo de referencia. El rea es \up
0 \expndtw-3\charscalex100 proporcional al nmero de protones presentes en la mues
tra. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\sl
mult0 \up0 \expndtw0\charscalex100 Los espectros de RMN se realizaron con un esp
ectrofotmetro Bruker AMX-300 que opera a 300.13 y \par\pard\qj \li1418\ri1221\sb3
7\sl-406\slmult0 \up0 \expndtw-1\charscalex100 75.4 MHz para \ul0\super\cf5\f6\f
s23 1\ul0\nosupersub\cf3\f4\fs24 H y \ul0\super\cf5\f6\fs23 13\ul0\nosupersub\cf
3\f4\fs24 C, respectivamente. Experimentalmente estos espectros se obtienen diso
lviendo \line \up0 \expndtw0\charscalex100 la muestra en disolvente deuterados c
omo son el cloroformo (CDCl\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 ), c
ido trifluoroactico (TFA-d) y \line \up0 \expndtw0\charscalex106 cido frmico. La di
solucin resultante se introduce en un tubo de vdrio especial de 5-10 mm de \line \
up0 \expndtw0\charscalex106 dimetro, se aade una gota de la substancia de referenc
ia \up0 \expndtw0\charscalex106 (TMS) y se introduce en el imn \par\pard\ql \li14
18\sb122\sl-276\slmult0 \up0 \expndtw-3\charscalex100 superconductor del aparato
. \par\pard\qj \li1418\sb0\sl-415\slmult0 \par\pard\qj\li1418\ri1220\sb15\sl-415
\slmult0 \up0 \expndtw0\charscalex106 En el caso de los polmeros se pueden determ
inar su estructura qumica, la presencia de grupos \line \up0 \expndtw0\charscalex
100 terminales y posibles ramificaciones. La presencia de grupos terminales en e
l espectro se utiliza para \line \up0 \expndtw0\charscalex100 determinar el peso
molecular (M\ul0\sub\cf5\f6\fs24 n\ul0\nosupersub\cf3\f4\fs24 ) de los polmeros.
Por ltimo, tambin resulta til en el seguimiento \line \up0 \expndtw0\charscalex100
de la degradacin de polmeros. La aparicin de nuevas seales o la disminucin de la int
ensidad de \line \up0 \expndtw-2\charscalex100 otras existentes en el espectro i
nicial del polmero sirve para conocer el avance de la degradacin. \par\pard\ql \li
1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li14
18\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb112\sl-276\slmult0 \up0 \expndtw0\ch
arscalex104 3.3.4. Anlisis trmico \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\par
d\qj\li1418\ri1221\sb18\sl-413\slmult0 \up0 \expndtw0\charscalex111 El anlisis trm
ico comprende un conjunto de tcnicas cuyo objetivo es la determinacin del \line \u
p0 \expndtw0\charscalex100 comportamiento trmico de un material en funcin de la te
mperatura o del tiempo. En el campo de los \line \up0 \expndtw0\charscalex100 po
lmeros las tcnicas ms usuales son: anlisis trmico diferencial (DTA), calorimetra difer
encial de \line \up0 \expndtw-2\charscalex100 barrido (DSC), anlisis termogravimtr
ico (TGA) y el anlisis trmico dinamomecnico (DMTA). \par\pard\ql \li10287\sb0\sl-23
0\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-23
0\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-23
0\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-23
0\slmult0 \par\pard\ql\li10287\sb189\sl-230\slmult0 \up0 \expndtw-2\charscalex10
0 \ul0\nosupersub\cf1\f2\fs20 41 \par\pard\sect\sectd\fs24\paperw11900\paperh168
40\pard\sb0\sl-240{\bkmkstart Pg10}{\bkmkend Pg10}\par\pard\ql \li1418\sb0\sl-23
0\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230
\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y
mtodos \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb216\sl-276\s
lmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\f4\fs24 3.3.4.1. CALORI
METRA DIFERENCIAL DE BARRIDO (DSC) \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\p
ard\qj\li1418\ri1220\sb20\sl-412\slmult0 \up0 \expndtw-2\charscalex100 En los ma

teriales polimricos, las transiciones trmicas ms importantes en DSC son la temperat


ura de \line \up0 \expndtw0\charscalex108 transicin vtrea (T\ul0\sub\cf5\f6\fs24 g
\ul0\nosupersub\cf3\f4\fs24 ) y la temperatura de fusin (T\ul0\sub\cf5\f6\fs24 f\
ul0\nosupersub\cf3\f4\fs24 ). En los polmeros amorfos la T\ul0\sub\cf5\f6\fs24 g\
ul0\nosupersub\cf3\f4\fs24 es la nica \line \up0 \expndtw0\charscalex103 transic
in que se registra y aparece como un cambio abrupto de la lnea base. Por otra part
e en los \line \up0 \expndtw0\charscalex100 muy cristalinos la T\ul0\sub\cf5\f6\
fs24 g\ul0\nosupersub\cf3\f4\fs24 es difcil de observar debido a la baja proporc
in de parte amorfa en el polmero. \line \up0 \expndtw-2\charscalex100 Los procesos
de fusin/cristalizacin dan informacin cualitativa sobre la temperatura del pico de
fusin \line \up0 \expndtw0\charscalex104 y cuantitativa sobre la cristalinidad d
el polmero (rea del pico). La fusin se manifiesta en un pico \line \up0 \expndtw0\c
harscalex103 endotrmico con subida ms o menos gradual y regular segn la naturaleza
e histria trmica de la \line \up0 \expndtw-1\charscalex100 muestra, y bajada brusc
a hasta recobrar la lnea base, que si se mantiene tras la fusin, puede decirse \li
ne \up0 \expndtw0\charscalex100 que el material es estable para ser procesado po
r fusin. Lo contrario es indicio de descomposicin y \line \up0 \expndtw-2\charscal
ex100 debe estudiarse con ms detalle por anlisis termogravimtrico. La cristalinidad
se evala usando como \line \up0 \expndtw0\charscalex108 referencia el calor de f
usin de un material 100% cristalino que puede estimarse a partir de las \line \up
0 \expndtw0\charscalex104 contribuciones de grupo.\ul0\super\cf5\f6\fs23 83\ul0\
nosupersub\cf3\f4\fs24 Los valores utilizados fueron -2.5 kJ/mol para el grupo s
ter, 2.0 kJ/mol \line \up0 \expndtw-2\charscalex100 para el grupo amida, 4.7 kJ/
mol para el grupo CH(CH\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 ), 4.0
kJ/mol para el grupo metilnico y 5.0 kJ/mol \line \up0 \expndtw-3\charscalex100 p
ara el grupo p-fenilnico. \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li
1418\ri1220\sb15\sl-413\slmult0 \up0 \expndtw0\charscalex105 Normalmente en una
calorimetra rutinaria se registran 4 barridos. En el primer barrido se obtiene \l
ine \up0 \expndtw0\charscalex113 informacin acerca de la fusin de una muestra cris
talizada directamente en el proceso de \line \up0 \expndtw0\charscalex102 polime
rizacin. Inmediatamente despus de la fusin se procede el enfriamiento lento de la m
uestra \line \up0 \expndtw0\charscalex102 para observar la cristalizacin del fund
ido \up0 \expndtw0\charscalex102 (2 barrido). Posteriormente se realiza un segund
o \par\pard\qj \li1418\ri1220\sb0\sl-413\slmult0 \up0 \expndtw0\charscalex104 ca
lentamiento (3 barrido) para verificar la fusin de la muestra cristalizada a parti
r del fundido y la \up0 \expndtw0\charscalex100 reproducibilidad de las fusiones
observadas. Por ltimo, despus de haber sometido la muestra a un \up0 \expndtw-2\c
harscalex100 enfriamiento rpido, se hace un tercer calentamiento (4 barrido) que p
ermite determinar la temperatura \up0 \expndtw-3\charscalex100 de transicin vtrea
del material. \par\pard\qj \li1418\ri1221\sb409\sl-420\slmult0 \up0 \expndtw-1\c
harscalex100 Los anlisis trmicos se han efectuado en un calormetro diferencial de b
arrido Perkin-Elmer DSC-30 \line \up0 \expndtw-2\charscalex100 equipado con un t
ermoanalizador TA400 y en un calormetro Perkin-Elmer DSC-PYRIS 1. El calibrado \l
ine \up0 \expndtw0\charscalex102 se realiz con ndio (T\ul0\sub\cf5\f6\fs24 f\ul0\n
osupersub\cf3\f4\fs24 = 429.75 K, \ul0\nosupersub\cf6\f7\fs24 \u8710?\ul0\nosup
ersub\cf3\f4\fs24 H\ul0\sub\cf5\f6\fs24 f\ul0\nosupersub\cf3\f4\fs24 = 3.267 kJ
/mol). Las calorimetras se han registrado a una \line \up0 \expndtw0\charscalex10
2 velocidad de calentamiento de \up0 \expndtw0\charscalex102 20\ul0\super\cf5\f6
\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min y de \up0 \expndtw0\charscalex102 10\ul0\
super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min para el enfriamiento, determi
nando las \par\pard\qj \li1418\ri1221\sb17\sl-400\slmult0 \up0 \expndtw-2\charsc
alex100 variaciones de entalpia con la temperatura. Se utilizaron muestras en po
lvo (5-10 mg) depositadas en \up0 \expndtw-3\charscalex100 cpsulas de aluminio. \
par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \p
ar\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par
\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb211\sl-230\slmult0 \up0
\expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 42
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{\sp{\sn fFillOK}{\sv 1}}{\sp{\sn fFilled}{\sv 1}}{\sp{\sn fillColor}{\sv 0}}{\s
p{\sn fLine}{\sv 0}}{\sp{\sn lineType}{\sv 0}}{\sp{\sn fArrowheadsOK}{\sv 1}}{\s
p{\sn fBehindDocument}{\sv 1}}{\sp{\sn lineColor}{\sv 0}}
}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g11}{\bkmkend Pg11}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\s
b0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charsc
alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\ql \li1418\sb0\
sl-276\slmult0 \par\pard\ql\li1418\sb216\sl-276\slmult0 \up0 \expndtw-3\charscal
ex100 \ul0\nosupersub\cf3\f4\fs24 3.3.4.2. ANLISIS TERMOGRAVIMTRICO (TGA) \par\par
d\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri1217\sb20\sl-412\slmult0 \
up0 \expndtw0\charscalex105 En esta tcnica se detectan los cambios de peso que ti
enen lugar en una muestra sometida a un \up0 \expndtw0\charscalex100 determinado
tratamiento trmico. Los experimentos pueden realizarse midiendo el cambio de pes
o de \up0 \expndtw-2\charscalex100 la muestra al variar la temperatura a una vel
ocidad constante, o bien, variando el tiempo y manteniendo \up0 \expndtw0\charsc
alex100 constante la temperatura. El anlisis resultante se denomina, respectivame
nte, dinmico e isotrmico. \up0 \expndtw0\charscalex108 Tambin es posible medir el g
radiente de la variacin del peso con la temperatura o el tiempo, \up0 \expndtw-3\
charscalex100 constituyendo el anlisis trmico diferencial (DTA). \par\pard\qj \li1
418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb20\sl-410\slmult0 \up0 \expn
dtw0\charscalex105 El anlisis de TGA representa una forma fcil y rpida de anlisis de
la estabilidad trmica de los \up0 \expndtw0\charscalex100 polmeros y puede ser ut
ilizada como medida de las posibilidades de transformacin por encima de la \up0 \
expndtw-3\charscalex100 temperatura de fusin del polmero. \par\pard\qj \li1418\ri1
220\sb408\sl-413\slmult0 \up0 \expndtw0\charscalex106 Las termogravimetras se reg
istraron con una termobalanza Perkin-Elmer TGA 6, acoplada a un \up0 \expndtw0\c
harscalex106 sistema de control por microprocesador y una estacin de procesamient
o de datos. Se oper en \up0 \expndtw0\charscalex100 rgimen dinmico a 10\ul0\super\c
f5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min, con muestras en polvo (10-20 mg) ba
jo atmsfera de nitrgeno y en el \up0 \expndtw-3\charscalex100 rango de 50-600\ul0\
super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C. \par\pard\ql \li1418\sb0\sl-276\
slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw-3\charscalex100 3
.3.4.3. ENSAYOS TERMODINAMOMECNICOS (DMTA) \par\pard\qj \li1418\sb0\sl-420\slmult
0 \par\pard\qj\li1418\ri1220\sb26\sl-420\slmult0 \up0 \expndtw-4\charscalex100 E
l anlisis trmico dinamomecnico suministra informacin cuantitativa de la variacin que
experimenta \line \up0 \expndtw-2\charscalex100 el mdulo durante las transiciones
termodinmicas o relajaciones del material, pudindose detectar la \line \up0 \expn
dtw-2\charscalex100 transicin \ul0\nosupersub\cf6\f7\fs24 \u945?\ul0\nosupersub\c
f3\f4\fs24 , asociada a segmentos de la cadena principal, y otras transiciones \
up0 \expndtw-3\charscalex100 (\ul0\nosupersub\cf6\f7\fs24 \u946?\ul0\nosupersub\
cf3\f4\fs24 , \ul0\nosupersub\cf6\f7\fs24 \u947?\ul0\nosupersub\cf3\f4\fs24 , et
c.), \par\pard\qj \li1418\ri1221\sb9\sl-410\slmult0 \up0 \expndtw0\charscalex100
correspondientes a movimientos moleculares locales. La tcnica es particularmente
adecuada para \up0 \expndtw0\charscalex105 estudiar la transicin vtrea pues suele
ser ms sensible que la calorimetra, especialmente con \up0 \expndtw-3\charscalex1
00 polmeros cristalinos. \par\pard\qj \li1418\sb0\sl-416\slmult0 \par\pard\qj\li1
418\ri1220\sb10\sl-416\slmult0 \up0 \expndtw-1\charscalex100 La aplicacin de una
tensin a un material viscoelstico se traduce en el almacenamiento de energa \up0 \e
xpndtw0\charscalex100 elstica y en una disipacin de energa en forma de calor. El co
mportamiento mecnico-dinmico se \up0 \expndtw0\charscalex108 evala en funcin de la t
emperatura. Para ello se aplica una tensin de forma cclica con una \up0 \expndtw0\
charscalex100 frecuencia angular (\ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosuper
sub\cf3\f4\fs24 ), la deformacin causada por dicha tensin tambin vara de forma sinus
oidal \up0 \expndtw0\charscalex103 pero con un cierto retardo en la respuesta. E
l fenmeno se interpreta descomponiendo la tensin \up0 \expndtw-1\charscalex100 apl

icada en dos componentes, uno en fase con la deformacin y otro en desfase con res
pecto a ella. \up0 \expndtw-2\charscalex100 La expresin que corresponde a la defo
rmacin sinusoidal de la muestra es: \par\pard\ql \li10287\sb0\sl-230\slmult0 \par
\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb38\sl-230\slmult0 \up
0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1\f2\fs20 43
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bxpage\shpbypage\shpwr3\shpwrk0\shpfblwtxt1\shpz29\shplid0
{\sp{\sn shapeType}{\sv 0}}{\sp{\sn fFlipH}{\sv 0}}{\sp{\sn fFlipV}{\sv 0}}{\sp{
\sn geoRight}{\sv 3168}}{\sp{\sn geoBottom}{\sv 20}}
{\sp{\sn pVerticies}{\sv 8;4;(0,20);(3168,20);(3168,0);(0,0)}}
{\sp{\sn pSegmentInfo}{\sv 2;10;16384;45824;1;45824;1;45824;1;45824;24577;32768}
}
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p{\sn fLine}{\sv 0}}{\sp{\sn lineType}{\sv 0}}{\sp{\sn fArrowheadsOK}{\sv 1}}{\s
p{\sn fBehindDocument}{\sv 1}}{\sp{\sn lineColor}{\sv 0}}
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{\shp {\*\shpinst\shpleft2131\shptop9103\shpright5822\shpbottom9123\shpfhdr0\shp
bxpage\shpbypage\shpwr3\shpwrk0\shpfblwtxt1\shpz188\shplid1
{\sp{\sn shapeType}{\sv 0}}{\sp{\sn fFlipH}{\sv 0}}{\sp{\sn fFlipV}{\sv 0}}{\sp{
\sn geoRight}{\sv 3691}}{\sp{\sn geoBottom}{\sv 20}}
{\sp{\sn pVerticies}{\sv 8;4;(0,20);(3691,20);(3691,0);(0,0)}}
{\sp{\sn pSegmentInfo}{\sv 2;10;16384;45824;1;45824;1;45824;1;45824;24577;32768}
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{\sp{\sn fFillOK}{\sv 1}}{\sp{\sn fFilled}{\sv 1}}{\sp{\sn fillColor}{\sv 0}}{\s
p{\sn fLine}{\sv 0}}{\sp{\sn lineType}{\sv 0}}{\sp{\sn fArrowheadsOK}{\sv 1}}{\s
p{\sn fBehindDocument}{\sv 1}}{\sp{\sn lineColor}{\sv 0}}
}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g12}{\bkmkend Pg12}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\s
b0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charsc
alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\ql \li5245\sb0\
sl-276\slmult0 \par\pard\ql\li5245\sb216\sl-276\slmult0 \up0 \expndtw-4\charscal
ex100 \ul0\nosupersub\cf6\f7\fs24 \u949?\ul0\nosupersub\cf3\f4\fs24 (t) = \ul0\n
osupersub\cf6\f7\fs24 \u949?\ul0\sub\cf5\f6\fs24 o\ul0\nosupersub\cf3\f4\fs24 s
en(\ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\cf3\f4\fs24 t) \par\pard\qj
\li1418\ri1221\sb29\sl-440\slmult0 \up0 \expndtw-2\charscalex100 donde \ul0\nos
upersub\cf6\f7\fs24 \u949?\ul0\sub\cf5\f6\fs24 o\ul0\nosupersub\cf3\f4\fs24 es
la deformacin mxima aplicada, \ul0\nosupersub\cf6\f7\fs24 \u969?\ul0\nosupersub\cf
3\f4\fs24 es la frecuencia angular y t es el tiempo. La ecuacin \up0 \expndtw-5\
charscalex100 correspondiente a la tensin (\ul0\nosupersub\cf6\f7\fs24 \u963?\ul0
\nosupersub\cf3\f4\fs24 ) producida por el material es: \par\pard\ql \li5033\sb1
56\sl-276\slmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf6\f7\fs24 \u96
3?\ul0\nosupersub\cf3\f4\fs24 (t) = \ul0\nosupersub\cf6\f7\fs24 \u963?\ul0\sub\c
f5\f6\fs24 o\ul0\nosupersub\cf3\f4\fs24 sen(\ul0\nosupersub\cf6\f7\fs24 \u969?\
ul0\nosupersub\cf3\f4\fs24 t + \ul0\nosupersub\cf6\f7\fs24 \u948?\ul0\nosupersub
\cf3\f4\fs24 ) \par\pard\ql \li1418\ri1177\sb29\sl-440\slmult0\tx5112 \up0 \expn
dtw0\charscalex100 donde \ul0\nosupersub\cf6\f7\fs24 \u963?\ul0\sub\cf5\f6\fs24
o\ul0\nosupersub\cf3\f4\fs24 es la tensin mxima y \ul0\nosupersub\cf6\f7\fs24 \u9
48?\ul0\nosupersub\cf3\f4\fs24 es la diferencia de fase entre la deformacin apli
cada y la tensin \up0 \expndtw-3\charscalex100 producida. Las propiedades dinamom
ecnicas se describen mediante el mdulo complejo (E\ul0\super\cf10\f11\fs23 \u8727?
\ul0\nosupersub\cf3\f4\fs24 ): \line \tab \up0 \expndtw-4\charscalex100 E\ul0\no
supersub\cf10\f11\fs16 \u8727?\ul0\nosupersub\cf3\f4\fs24 = \ul0\nosupersub\cf6
\f7\fs24 \u963?\ul0\nosupersub\cf3\f4\fs24 /\ul0\nosupersub\cf6\f7\fs24 \u949?\u
l0\nosupersub\cf3\f4\fs24 = E\u8217? + i E\u8217?\u8217? \par\pard\qj \li1418\r
i1221\sb0\sl-420\slmult0 \up0 \expndtw-1\charscalex100 donde E\u8217? es el deno
minado mdulo de almacenamiento, que es una medida de la energa que puede \up0 \exp
ndtw-3\charscalex100 recuperarse de la deformacin producida en el material y E\u8
217?\u8217? es el mdulo de prdidas que se relaciona \up0 \expndtw-3\charscalex100

con la energa disipada por el material viscoelstico y que no puede recuperarse. La


diferencia de fase \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf6\f7\fs24 \u9
48?\ul0\nosupersub\cf3\f4\fs24 , que es la que determina la evolucin de calor en
un material viscoelstico sometido a una tensin \up0 \expndtw-3\charscalex100 cclica
, queda determinada por la relacin entre estos dos componentes, mediante la llama
da tangente \up0 \expndtw-4\charscalex100 de prdidas o factor de disipacin (tan \u
l0\nosupersub\cf6\f7\fs24 \u948?\ul0\nosupersub\cf3\f4\fs24 ). \par\pard\ql \li5
392\sb136\sl-276\slmult0 \up0 \expndtw-3\charscalex100 tan \ul0\nosupersub\cf6\f
7\fs24 \u948?\ul0\nosupersub\cf3\f4\fs24 = E\u8217?\u8217?/E\u8217? \par\pard\q
j \li1418\ri1222\sb54\sl-410\slmult0 \up0 \expndtw0\charscalex100 El anlisis DMTA
se llev a cabo en un analizador Rheometrics PL-DMT MK3 con una frecuencia de \up
0 \expndtw-1\charscalex100 1 Hz. Las probetas utilizadas fueron de 25 x 10 mm\ul
0\super\cf5\f6\fs23 2\ul0\nosupersub\cf3\f4\fs24 de tamao y 0.4 mm de espesor. E
l calentamiento \up0 \expndtw-1\charscalex100 se efectu en atmsfera de nitrgeno a 2
\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C/min en un intervalo de -150
a 150\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 C. \par\pard\ql \li1418\s
b0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw0\charsc
alex104 3.3.5. Solubilidad \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\
li1418\ri1220\sb38\sl-413\slmult0 \up0 \expndtw0\charscalex108 La disolucin de un
polmero es un proceso lento que ocurre en dos etapas. En la primera, las \line \
up0 \expndtw0\charscalex100 molculas de disolvente se difunden lentamente dentro
del polmero produciendo el hinchamiento del \line \up0 \expndtw0\charscalex108 mi
smo. El proceso de disolucin puede detenerse en esta fase, si las fuerzas intermo
leculares \line \up0 \expndtw-3\charscalex100 polmero-polmero \up0 \expndtw0\chars
calex108 (reticulacin, cristalinidad o enlaces por puentes de hidrgeno) so
n lo \par\pard\qj \li1418\ri1221\sb0\sl-415\slmult0 \up0 \expndtw0\charscalex10
0 suficientemente grandes como para impedirlo. En caso de que estas fuerzas pued
an superarse por la \line \up0 \expndtw0\charscalex110 formacin de interacciones
intensas polmero-disolvente, tendr lugar la segunda etapa de la \line \up0 \expndt
w-1\charscalex100 disolucin. En sta, el polmero hinchado se desintegra gradualmente
convirtindose en una verdadera \line \up0 \expndtw-2\charscalex100 disolucin. El
proceso de disolucin puede ser bastante lento (das o semanas) para materiales de m
uy \line \up0 \expndtw-3\charscalex100 alto peso molecular. \par\pard\qj \li1418
\ri1221\sb387\sl-420\slmult0 \up0 \expndtw0\charscalex112 La temperatura es un f
actor importante que debe ser controlado durante el experimento. La \line \up0 \
expndtw-1\charscalex100 polidispersidad es una caracterstica de los polmeros que d
ificulta sus pruebas de solubilidad debido a \line \up0 \expndtw-1\charscalex100
la coexistencia de molculas de bajo peso molecular; ms fcilmente solubles, y de al
to peso \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
lmult0 \par\pard\ql\li1418\sb217\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \u
l0\nosupersub\cf1\f2\fs20 44 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\p
ard\sb0\sl-240{\bkmkstart Pg13}{\bkmkend Pg13}\par\pard\ql \li8764\sb0\sl-230\sl
mult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slm
ult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodo
s \par\pard\qj \li1418\ri1220\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex100
\ul0\nosupersub\cf3\f4\fs24 molecular; que se disuelven con mayor dificultad. Po
r esta razn, en un polmero pueden darse varios \up0 \expndtw-3\charscalex100 casos
de solubilidad: \par\pard\ql \li2126\sb123\sl-276\slmult0 \up0 \expndtw-3\chars
calex100 Insolubilidad total en el disolvente. \par\pard\qj \li2127\ri1220\sb34\
sl-410\slmult0 \up0 \expndtw0\charscalex105 Insolubilidad parcial: cuando tiene
lugar la solubilizacin de las molculas de menor peso \up0 \expndtw0\charscalex102
molecular o cuando se produce un hinchamiento del polmero al penetrar el disolven
te en el \up0 \expndtw-3\charscalex100 material sin llegar a disolverlo. \par\pa
rd\qj \li2127\ri1221\sb10\sl-410\slmult0 \up0 \expndtw-1\charscalex100 Solubilid
ad parcial: en este caso las molculas de menor peso molecular pueden disolverse e
n \up0 \expndtw0\charscalex102 fro y las de mayor peso molecular al calentar la p
reparacin. Estas, sin embargo, vuelven a \up0 \expndtw-3\charscalex100 precipitar
al enfriar. \par\pard\ql \li2126\sb121\sl-276\slmult0 \up0 \expndtw-3\charscale
x100 Solubilidad total en el disolvente. \par\pard\qj \li1418\sb0\sl-413\slmult0
\par\pard\qj\li1418\ri1221\sb18\sl-413\slmult0 \up0 \expndtw0\charscalex102 Los

ensayos de solubilidad consisten en depositar una pequea cantidad del polmero (1


mg) en un \up0 \expndtw-1\charscalex100 tubo de ensayo al que se aade alrededor d
e 0.5 mL de disolvente. Tras la agitacin de la preparacin \up0 \expndtw0\charscale
x100 se observa si se produce algn cambio en el ndice de refraccin del lquido, indic
ativo del proceso de \up0 \expndtw0\charscalex111 disolucin. Por el contrario, si
no se detecta ningn cambio, se dice que no hay disolucin a \up0 \expndtw0\charsca
lex100 temperatura ambiente. Cuando se observa una variacin en el aspecto del polm
ero se considera que \up0 \expndtw-1\charscalex100 se ha disuelto parcialmente.
En aquellos tubos donde no se ha apreciado disolucin se calientan como \up0 \expn
dtw-2\charscalex100 mximo a la temperatura del disolvente y se observan los cambi
os en la solucin. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0
\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb113
\sl-276\slmult0 \up0 \expndtw-2\charscalex100 3.4. CARACTERIZACIN ESTRUCTURAL \pa
r\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb268\sl-276\slmult0 \u
p0 \expndtw-2\charscalex100 3.4.1. MICROSCOPA ELECTRNICA \par\pard\qj \li1418\sb0\
sl-413\slmult0 \par\pard\qj\li1418\ri1220\sb18\sl-413\slmult0 \up0 \expndtw0\cha
rscalex100 En la ciencia de los polmeros generalmente el trmino morfologa se refier
e a la organizacin y forma \line \up0 \expndtw-1\charscalex100 superior al orden
atomstico y el trmino estructura se refiere a los detalles de la disposicin atomstic
a \line \up0 \expndtw0\charscalex105 y molecular. La microscopa electrnica de tran
smisin (TEM) es capaz de resolver estructuras a \line \up0 \expndtw-1\charscalex1
00 nivel atomstico y molecular y presenta un importante papel con respecto al anli
sis morfolgico de los \line \up0 \expndtw-2\charscalex100 polmeros. Su principal l
imitacin es el efecto destructivo que ejercen los electrones sobre los polmeros \l
ine \up0 \expndtw0\charscalex105 y las muestras orgnicas en general. Aunque morfo
lgicamente la muestra parezca inalterada, el \line \up0 \expndtw-2\charscalex100
deterioro de la estructura cristalina se manifiesta con la extincin progresiva de
l diagrama de difraccin. \line \up0 \expndtw0\charscalex106 No slo se destruyen la
s interacciones moleculares de tipo secundario, sino tambin los propios \line \up
0 \expndtw0\charscalex107 enlaces covalentes. El control riguroso de la dosis de
radiacin y el uso de sistemas de registro \line \up0 \expndtw-2\charscalex100 ex
traordinariamente sensibles hace posible obtener los mejores diagramas de difrac
cin de electrones. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\
sb0\sl-230\slmult0 \par\pard\ql\li10287\sb99\sl-230\slmult0 \up0 \expndtw-2\char
scalex100 \ul0\nosupersub\cf1\f2\fs20 45 \par\pard\sect\sectd\fs24\paperw11900\p
aperh16840\pard\sb0\sl-240{\bkmkstart Pg14}{\bkmkend Pg14}\par\pard\ql \li1418\s
b0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb1
0\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Mater
iales y mtodos \par\pard\qj \li1418\sb0\sl-420\slmult0 \par\pard\qj\li1418\ri1221
\sb354\sl-420\slmult0 \up0 \expndtw0\charscalex105 \ul0\nosupersub\cf3\f4\fs24 E
l fundamento de la microscopa electrnica es esencialmente el mismo que el de la mi
croscopa \line \up0 \expndtw0\charscalex102 ptica, siendo la naturaleza de la radi
acin empleada en cada caso la principal diferencia entre ellas \line \up0 \expndt
w-3\charscalex100 (Tabla 3). \par\pard\ql \li3075\sb0\sl-276\slmult0 \par\pard\q
l\li3075\sb243\sl-276\slmult0 \up0 \expndtw-2\charscalex100 TABLA 3. Diferencias
entre la microscopa ptica y la electrnica. \par\pard\li2693\sb176\sl-276\slmult0\f
i0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 Caracterstica\tab \up0 \expndtw-1\
charscalex100 Microscopa\tab \up0 \expndtw-1\charscalex100 Microscopa\par\pard\li2
693\sb0\sl-274\slmult0\fi2449\tx7034 \up0 \expndtw-1\charscalex100 ptica\tab \up0
\expndtw-1\charscalex100 electrnica\par\pard\li2693\sb16\sl-276\slmult0\fi0\tx51
43\tx7034 \up0 \expndtw-1\charscalex100 Tipo de radiacin\tab \up0 \expndtw-1\char
scalex100 UV o visible\tab \up0 \expndtw-1\charscalex100 Haz electrnico\par\pard\
li2693\sb137\sl-276\slmult0\fi0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 Reso
lucin\tab \up0 \expndtw-1\charscalex100 300 nm\tab \up0 \expndtw-1\charscalex100
0.2 nm\par\pard\li2693\sb136\sl-276\slmult0\fi0\tx5143\tx7034 \up0 \expndtw-1\ch
arscalex100 Rango de aumentos\tab \up0 \expndtw-1\charscalex100 2 - 2000\tab \up
0 \expndtw-1\charscalex100 200 - 2 x 10\ul0\super\cf5\f6\fs23 6\par\pard\li2693\
sb138\sl-276\slmult0\fi0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 \ul0\nosupe
rsub\cf3\f4\fs24 Entorno\tab \up0 \expndtw-1\charscalex100 Ambiente\tab \up0 \ex
pndtw-1\charscalex100 Alto vaco\par\pard\li2693\sb137\sl-276\slmult0\fi0\tx5143\t

x7034 \up0 \expndtw-1\charscalex100 Destructiva\tab \up0 \expndtw-1\charscalex10


0 No\tab \up0 \expndtw-1\charscalex100 Si\par\pard\li2693\sb137\sl-276\slmult0\f
i0\tx7034 \up0 \expndtw-1\charscalex100 Preparacin de muestras Fcil\tab \up0 \exp
ndtw-1\charscalex100 Difcil\par\pard\li2693\sb137\sl-276\slmult0\fi0\tx5143\tx703
4 \up0 \expndtw-1\charscalex100 Observacin\tab \up0 \expndtw-1\charscalex100 Supe
rfcies\tab \up0 \expndtw-1\charscalex100 Pelculas\par\pard\li2693\sb136\sl-276\slm
ult0\fi0\tx5143\tx7034 \up0 \expndtw-1\charscalex100 Detecta orientacin\tab \up0
\expndtw-1\charscalex100 Si\tab \up0 \expndtw-1\charscalex100 Si\par\pard\qj \li
1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1221\sb57\sl-410\slmult0 \up0 \exp
ndtw0\charscalex100 La TEM se ocupa de la informacin suministrada por los electro
nes que traspasan una muestra slida \up0 \expndtw0\charscalex100 sobre la que se
ha hecho incidir un haz electrnico coherente y a gran velocidad. La interaccin de
los \up0 \expndtw-3\charscalex100 electrones con la materia es un fenmeno complej
o. \par\pard\qj \li1418\ri1221\sb407\sl-414\slmult0 \up0 \expndtw0\charscalex100
Cuando hacemos incidir un haz electrnico sobre una muestra los electrones pueden
no desviarse de \line \up0 \expndtw0\charscalex100 la trayectoria inicial, o se
r desviados elstica o inelsticamente dependiendo, respectivamente, de que \line \u
p0 \expndtw0\charscalex103 la interaccin sea con el ncleo o con algn orbital electrn
ico de alguno de los tomos que forman \line \up0 \expndtw0\charscalex107 parte de
l material. Los electrones desviados de forma inelstica experimentan un cambio en
su \line \up0 \expndtw0\charscalex103 velocidad como consecuencia de la energa p
erdida en la colisin con la muestra, mientras que los \line \up0 \expndtw0\charsc
alex105 desviados de forma elstica mantienen su velocidad y son los responsables
de los fenmenos de \line \up0 \expndtw0\charscalex100 difraccin. Los electrones no
desviados y los desviados elsticamente son los nicos que contribuyen \line \up0 \
expndtw0\charscalex100 de forma constructiva a la formacin de la imagen, mientras
que los desviados de forma inelstica son \line \up0 \expndtw-2\charscalex100 los
responsables del ruido de fondo presente en toda imagen de microscopa electrnica.
La proporcin \line \up0 \expndtw0\charscalex100 de electrones dispersados de for
ma elstica es directamente proporcional al grosor de la muestra. Por \line \up0 \
expndtw0\charscalex100 esta razn, los experimentos de difraccin se realizan a un v
oltaje mayor (100 kV) que los de anlisis \line \up0 \expndtw-3\charscalex100 morf
olgico (80 kV). \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\s
l-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb8\sl-23
0\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 46
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bxpage\shpbypage\shpwr3\shpwrk0\shpfblwtxt1\shpz93\shplid0
{\sp{\sn shapeType}{\sv 0}}{\sp{\sn fFlipH}{\sv 0}}{\sp{\sn fFlipV}{\sv 0}}{\sp{
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{\sp{\sn pVerticies}{\sv 8;4;(0,30);(6658,30);(6658,0);(0,0)}}
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{\sp{\sn shapeType}{\sv 0}}{\sp{\sn fFlipH}{\sv 0}}{\sp{\sn fFlipV}{\sv 0}}{\sp{
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{\shp {\*\shpinst\shpleft2624\shptop7796\shpright9282\shpbottom7826\shpfhdr0\shp
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{\sp{\sn shapeType}{\sv 0}}{\sp{\sn fFlipH}{\sv 0}}{\sp{\sn fFlipV}{\sv 0}}{\sp{
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{\sp{\sn fFillOK}{\sv 1}}{\sp{\sn fFilled}{\sv 1}}{\sp{\sn fillColor}{\sv 32768}
}{\sp{\sn fLine}{\sv 0}}{\sp{\sn lineType}{\sv 0}}{\sp{\sn fArrowheadsOK}{\sv 1}
}{\sp{\sn fBehindDocument}{\sv 1}}{\sp{\sn lineColor}{\sv 0}}
}}\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart P
g15}{\bkmkend Pg15}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\s
b0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charsc
alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri12
20\sb380\sl-412\slmult0 \up0 \expndtw0\charscalex108 \ul0\nosupersub\cf3\f4\fs24
El microscpio electrnico de transmisin consta de un sistema de iluminacin formado p
or un \line \up0 \expndtw0\charscalex108 filamento de tungsteno o wolframio que
emite electrones, que sern acelerados por la elevada \line \up0 \expndtw0\charsca
lex102 diferencia de potencial a que son sometidos (80-100 kV). El haz de electr
ones es enfocado hacia la \line \up0 \expndtw0\charscalex100 muestra mediante do
s lentes condensadoras, la primera recoge la imagen del filamento y la segunda \
line \up0 \expndtw0\charscalex109 controla el rea de iluminacin. El vaco existente
en la columna permite la transmisin de los \line \up0 \expndtw-1\charscalex100 el
ectrones, a travs de ella, hacia la muestra. A continuacin, se encuentra la lente
objetivo que amplia \line \up0 \expndtw0\charscalex103 la imagen y finalmente la
lente proyectora que la dirige hacia la pantalla fluorescente que recoge la \li
ne \up0 \expndtw0\charscalex103 imagen final. Todas las lentes son de naturaleza
electromagntica y su potencia se puede controlar \line \up0 \expndtw-3\charscale
x100 variando el voltaje. \par\pard\qj \li1418\ri1221\sb402\sl-420\slmult0 \up0
\expndtw-1\charscalex100 La resolucin es una ventaja importante de sta tcnica frent
e a la de difraccin de rayos X y depende \up0 \expndtw-3\charscalex100 de la long
itud de onda del haz de electrones segn la ecuacin: \par\pard\ql \li5307\sb0\sl-27
6\slmult0 \par\pard\ql\li5307\sb263\sl-276\slmult0 \up0 \expndtw-3\charscalex100
d = \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 / n sen \ul0
\nosupersub\cf6\f7\fs24 \u952? \par\pard\qj \li1418\sb0\sl-420\slmult0 \par\pard
\qj\li1418\ri1220\sb46\sl-420\slmult0 \up0 \expndtw0\charscalex104 \ul0\nosupers
ub\cf3\f4\fs24 siendo d la resolucin, \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosu
persub\cf3\f4\fs24 la longitud de onda, n el ndice de refraccin del medio y \ul0\
nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs24 el ngulo de \up0 \expnd
tw-3\charscalex100 apertura de las lentes de microscopio. \par\pard\qj \li1418\r
i1222\sb384\sl-440\slmult0 \up0 \expndtw0\charscalex103 Las modificaciones en el
voltaje (V) modifican la longitud de onda del haz de electrones segn la \line \u
p0 \expndtw0\charscalex100 frmula \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupers
ub\cf3\f4\fs24 = (1.5/V)\ul0\super\cf5\f6\fs23 1/2\ul0\nosupersub\cf3\f4\fs24 .
As, para voltajes de 80 y 100 kV las longitudes de onda de los electrones son \p
ar\pard\qj \li1418\ri1222\sb4\sl-412\slmult0 \up0 \expndtw-1\charscalex100 0.041
756 y 0.037013 , respectivamente.\ul0\super\cf5\f6\fs23 84\ul0\nosupersub\cf3\f4\
fs24 La mxima resolucin se obtiene con longitudes de onda \up0 \expndtw0\charscal
ex100 ms cortas, es decir, diferencias de potencial ms elevadas y lentes de gran a
pertura. Generalmente, \up0 \expndtw0\charscalex100 para una substancia estable
en un microscopio operando correctamente, la resolucin prctica viene \up0 \expndtw
0\charscalex100 determinada por la aberracin cromtica debida a la presencia de ele
ctrones inelsticos. Dado que su \up0 \expndtw0\charscalex100 proporcin aumenta de
forma exponencial con la cantidad de materia con la que colisiona, el espesor \u
p0 \expndtw-3\charscalex100 de la muestra es decisivo para obtener buenas imgenes
. \par\pard\qj \li1418\ri1222\sb408\sl-413\slmult0 \up0 \expndtw0\charscalex108
La preparacin de las muestras para microscopa electrnica de transmisin se efectu con
un \line \up0 \expndtw-2\charscalex100 evaporador de alto vaco Balzers BAE 080T.
Los cristales se observaron con Microscpios Electrnicos \line \up0 \expndtw0\chars

calex103 Philips EM301 y Philips Tecnai 10/12. El calibrado de los diagramas de


difraccin de electrones se \line \up0 \expndtw-2\charscalex100 realiz con oro (d\u
l0\sub\cf5\f6\fs24 111\ul0\nosupersub\cf3\f4\fs24 = 2.35 \ul0\nosupersub\cf4\f5
\fs24 \ul0\nosupersub\cf3\f4\fs24 ) y la rotacin de la imagen se determin mediante
cristales de MoO\ul0\sub\cf5\f6\fs24 3\ul0\nosupersub\cf3\f4\fs24 . \par\pard\qj
\li1418\sb0\sl-400\slmult0 \par\pard\qj\li1418\ri1222\sb38\sl-400\slmult0 \up0
\expndtw0\charscalex109 La caracterizacin por microscopa electrnica de barrido (SEM
) de los materiales polimricos \line \up0 \expndtw-1\charscalex100 comprende una
serie de aplicaciones que difieren en su estructura y micromorfologa. En cada cas
o la \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\sl
mult0 \par\pard\ql\li10287\sb21\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul
0\nosupersub\cf1\f2\fs20 47 \par\pard\sect\sectd\fs24\paperw11900\paperh16840\pa
rd\sb0\sl-240{\bkmkstart Pg16}{\bkmkend Pg16}\par\pard\ql \li1418\sb0\sl-230\slm
ult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmu
lt0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos
\par\pard\qj \li1418\ri1221\sb390\sl-400\slmult0 \up0 \expndtw0\charscalex108 \
ul0\nosupersub\cf3\f4\fs24 estrategia de la exploracin es distinta dependiendo de
la naturaleza de cada material y de las \up0 \expndtw-3\charscalex100 posibilid
ades que se tienen para la preparacin de las muestras. \par\pard\qj \li1418\sb0\s
l-410\slmult0 \par\pard\qj\li1418\ri1221\sb22\sl-410\slmult0 \up0 \expndtw0\char
scalex100 El microscopio electrnico de barrido forma la imagen con los electrones
secundarios que se generan \up0 \expndtw0\charscalex100 en la interaccin de la r
adiacin electrnica con una capa superficial y fina de la muestra mediante un \up0
\expndtw-3\charscalex100 proceso de rastreo. \par\pard\qj \li1418\ri1221\sb409\s
l-412\slmult0 \up0 \expndtw0\charscalex109 Una analoga simple que describe perfec
tamente el mecanismo de operacin del microscopio \line \up0 \expndtw0\charscalex1
02 electrnico de barrido es una habitacin completamente oscura en donde se sita un
exposmetro y \line \up0 \expndtw-1\charscalex100 una luz flash que va iluminando
las paredes de manera continuada y sistemtica. El exposmetro mide \line \up0 \expn
dtw0\charscalex106 la luz reflejada sealando mximos para las zonas blancas y lisas
, y mnimos para las oscuras y \line \up0 \expndtw0\charscalex103 rugosas. El regi
stro del exposmetro para toda la habitacin proporciona el mapa de la pared. En el
\line \up0 \expndtw0\charscalex108 caso de una muestra observada con SEM las reas
oscuras corresponden a las zonas de baja \line \up0 \expndtw0\charscalex104 ref
lectividad y las rugosas a los relieves superficiales. Podemos tener un contrast
e composicional, \line \up0 \expndtw0\charscalex100 dependiendo de la composicin
qumica de la muestra, o un contraste topogrfico, dependiendo de la \line \up0 \exp
ndtw-3\charscalex100 morfologa superficial de la muestra. \par\pard\qj \li1418\sb
0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\sb15\sl-413\slmult0 \up0 \expndtw-1\
charscalex100 La resolucin espacial de una observacin por SEM viene dada por el rea
de la muestra reflectante, y \line \up0 \expndtw0\charscalex102 depende del gra
do de interaccin de la radiacin con la muestra. Esta interaccin genera electrones \
line \up0 \expndtw-3\charscalex100 reflejados \up0 \expndtw0\charscalex112 (secu
ndarios o elsticos) que son atrados por un detector para dar las imgenes \line \up0
\expndtw-3\charscalex100 topogrficas. \par\pard\qj \li1418\ri1220\sb408\sl-412\s
lmult0 \up0 \expndtw0\charscalex100 La simplicidad en la preparacin de muestras p
ara SEM es quizs la principal ventaja que ofrece esta \line \up0 \expndtw0\charsc
alex100 tcnica. El hecho de que la observacin de la muestra se haga punto a punto,
permite la utilizacin de \line \up0 \expndtw0\charscalex104 muestras de cualquie
r tamao y forma, y da lugar a una gran profundidad de campo. De hecho, la \line \
up0 \expndtw-1\charscalex100 preparacin de muestras finas para microscopa ptica (0.
1-0.3 mm) o hiperfinas para TEM (5-100 nm) \line \up0 \expndtw0\charscalex106 co
nstituye la mayor limitacin prctica en el anlisis microscpico de muestras de polmeros
por \line \up0 \expndtw-3\charscalex100 transmisin. \par\pard\qj \li1418\sb0\sl413\slmult0 \par\pard\qj\li1418\ri1220\sb15\sl-413\slmult0 \up0 \expndtw0\charsc
alex100 En la SEM el metalizado de las muestras polimricas es indispensable y su
funcin, adems de hacer \up0 \expndtw-1\charscalex100 conductiva la superficie, es
eliminar la electricidad esttica, minimizar el dao por radiacin y aumentar \up0 \ex
pndtw0\charscalex106 la reflectividad electrnica. Normalmente, el metal utilizado
suele ser el oro en presencia de una \up0 \expndtw-3\charscalex100 atmsfera ioni

zante de argon. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\


sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl
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00 \ul0\nosupersub\cf1\f2\fs20 48 \par\pard\sect\sectd\fs24\paperw11900\paperh16
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40051451400514514005145140051451401fffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg17}{\
bkmkend Pg17}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex10
0 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\ri1221\sb3
82\sl-410\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 La mo
rfologa de la superficie de las pelculas de polmero sometidas a un proceso de degra
dacin se \up0 \expndtw0\charscalex100 observ con un Microscopio Electrnico de Barri
do JEOL JSM-6400. Los films fueron metalizados con \up0 \expndtw-3\charscalex100
oro usando un evaporador Balzers SCD-004 Sputter Coater. \par\pard\ql \li1418\s
b0\sl-276\slmult0 \par\pard\ql\li1418\sb245\sl-276\slmult0 \up0 \expndtw0\charsc
alex104 3.4.1.1. Morfologa cristalina \par\pard\qj \li1418\sb0\sl-413\slmult0 \pa
r\pard\qj\li1418\ri1219\sb38\sl-413\slmult0 \up0 \expndtw0\charscalex102 Los niv
eles de organizacin supramolecular de un polmero cristalino se identifican con dos
tipos de \up0 \expndtw0\charscalex111 morfologias: las lamelas y las esferulita
s. As pues, un fenmeno peculiar en la organizacin \up0 \expndtw0\charscalex100 mole
cular de los polmeros cristalinos es el plegamiento molecular con la consiguiente
formacin de la \up0 \expndtw0\charscalex102 estructura lamelar (Figura 24). Las
lamelas son microcristales de espesor muy pequeo (< 25 nm) y \up0 \expndtw-2\char
scalex100 dimensiones basales que pueden llegar a ser de decenas de micrmetros. E
n estos cristales, la cadena \up0 \expndtw-2\charscalex100 molecular se dispone
mas o menos perpendicularmente a las bases y se pliega sobre si misma con una \u
p0 \expndtw-3\charscalex100 cierta periodicidad que determina el grosor de los m
ismos. \par\pard\qj \li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\sl
mult0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmu
lt0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmult
0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmult0
\par\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\sb0\sl-240\slmult0 \p

ar\pard\qj\li3743\sb0\sl-240\slmult0 \par\pard\qj\li3743\ri3524\sb90\sl-240\slmu
lt0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figura 24. Modelo
de la formacin de lamelas cristalinas en \line \up0 \expndtw-3\charscalex100 polme
ros con una nica direccin de puentes de hidrgeno. \par\pard\qj \li1418\sb0\sl-420\s
lmult0 \par\pard\qj\li1418\ri1221\sb112\sl-420\slmult0 \up0 \expndtw-2\charscale
x100 \ul0\nosupersub\cf3\f4\fs24 Mediante cristalizacin en disoluciones diluidas
es posible obtener estos microcristales con hbitos bien \up0 \expndtw-2\charscale
x100 definidos que suelen revelar la geometra de la celdilla cristalina (Figura 2
5). \par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\p
ard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167
\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-23
0\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\
par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\l
i3167\sb0\sl-230\slmult0\par\pard\li3167\sb169\sl-230\slmult0\fi0 \up0 \expndtw1\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figura 25. Cristales lamelares de p
olietileno cristalizados en xileno a 83\ul0\super\cf11\f12\fs19 o\ul0\nosupersub
\cf9\f10\fs20 C.\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\s
lmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par
\pard\li3167\sb0\sl-230\slmult0\par\pard\li3167\sb0\sl-230\slmult0\par\pard\li31
67\sb101\sl-230\slmult0\fi7119 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1
\f2\fs20 49\par\pard\sect\sectd\fs24\paperw11900\paperh16840{\shp
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28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
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28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
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28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a
28a00fffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg18}{\bkmkend Pg18}\par\pard\ql \li1
418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li141
8\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20
Materiales y mtodos \par\pard\qj \li1418\ri1219\sb377\sl-416\slmult0 \up0 \expndt
w0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Los monocristales de polmero suelen
tener un grosor adecuado (< 100 \ul0\nosupersub\cf4\f5\fs24 \ul0\nosupersub\cf3\f
4\fs24 ) para su estudio por sta \line \up0 \expndtw0\charscalex110 tcnica, pero p
resentan una imagen de bajo contraste, porque ste suele ser inversamente \line \u
p0 \expndtw-2\charscalex100 proporcional al peso atmico de la muestra. Este incon
veniente se soluciona sombreando los cristales \line \up0 \expndtw0\charscalex10
8 con una fina capa de un metal pesado (Cr, Pt, Pd, U, etc). El metal es evapora
do a alto vaco \line \up0 \expndtw0\charscalex102 (10\ul0\super\cf5\f6\fs23 -4\ul
0\nosupersub\cf3\f4\fs24 - 10\ul0\super\cf5\f6\fs23 -5\ul0\nosupersub\cf3\f4\fs
24 torr) sobre las rejillas a un cierto ngulo y se deposita sobre los cristales
resaltando las \line \up0 \expndtw-2\charscalex100 caractersticas topogrficas de l
a muestra. Conociendo el ngulo de sombreado y midiendo la longitud \line \up0 \ex
pndtw-2\charscalex100 de las sombras resultantes se puede conocer el grosor apro
ximado de las lamelas del cristal. En este \line \up0 \expndtw-2\charscalex100 t
rabajo, el sombreado se realiz con Pt-C con un ngulo de aproximadamente 15. En la F
igura 26 se \line \up0 \expndtw0\charscalex102 muestra esquemticamente el ngulo de
sombreado (\ul0\nosupersub\cf6\f7\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 ) y su
relacin con el grosor lamelar (a). La \line \up0 \expndtw-3\charscalex100 morfol
oga de los monocristales es un buen indicador, aunque no infalible, de la simetra
presente en la \line \up0 \expndtw-4\charscalex100 estructura cristalina. \par\p
ard\qj \li1418\ri1221\sb401\sl-420\slmult0 \up0 \expndtw0\charscalex103 En gener
al, las celdillas tetragonales proporcionan cristales de base cuadrada, las hexa
gonales y \line \up0 \expndtw-2\charscalex100 trigonales proporcionan cristales
de forma hexagonal y las rmbicas cristales con forma de rombo. \par\pard\ql \li33
12\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312
\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\s
b0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0
\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\s
l-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl230\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-23
0\slmult0 \par\pard\ql\li3312\sb0\sl-230\slmult0 \par\pard\ql\li3312\sb0\sl-230\
slmult0 \par\pard\ql\li3312\sb7\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul
0\nosupersub\cf9\f10\fs20 Figura 26. Esquema del sombreado para determinar el gr
osor lamelar. \par\pard\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri1221
\sb28\sl-412\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 La
esferulita consiste en un agregado esfrico con un tamao que puede oscilar entre dc
imas de \up0 \expndtw0\charscalex100 micrmetros y varios milmetros, y pueden ser o
bservadas claramente en el microscopio ptico. Una \up0 \expndtw-1\charscalex100 m
orfologa esferultica se obtiene por la cristalizacin del polmero a partir del estado
fundido o por la \up0 \expndtw0\charscalex108 cristalizacin del polmero a partir
de soluciones muy concentradas por evaporacin lenta del \up0 \expndtw0\charscalex
104 disolvente. En el microscopio ptico de luz polarizada son fcilmente reconocibl
es como crculos \up0 \expndtw-4\charscalex100 fuertemente birrefringentes que exh
iben una cruz de malta caracterstica (Figura 27). \par\pard\ql \li1418\sb0\sl-230
\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
lmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slm
ult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmul
t0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0
\par\pard\ql\li1418\sb109\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nos

upersub\cf1\f2\fs20 50 \par\pard\sect\sectd\fs24\paperw11900\paperh16840{\shp
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028a28a0028a28a0028a28a0028a28a0028a28a00fffd9}}}}}\pard\sb0\sl-240{\bkmkstart P
g19}{\bkmkend Pg19}\par\pard\ql \li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\s
b0\sl-230\slmult0 \par\pard\ql\li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charsc
alex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li3456\sb0\
sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl
-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-2
20\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220
\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\s
lmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slm
ult0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmul
t0 \par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\sb0\sl-220\slmult0
\par\pard\qj\li3456\sb0\sl-220\slmult0 \par\pard\qj\li3456\ri3233\sb99\sl-220\s
lmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figura 27. Esfe
rulita simple presentando extincin en forma de cruz \line \up0 \expndtw-3\charsca
lex100 de malta observada en el microscopio ptico de luz polarizada. \par\pard\qj
\li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\sb108\sl-413\slmult0 \up0
\expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Las esferulitas estn consti
tuidas internamente por lamelas que irradian del centro. En muchos casos la \up0
\expndtw0\charscalex103 lamela se retuerce sobre si misma, de forma que la orie
ntacin del eje molecular gira alrededor del \up0 \expndtw0\charscalex104 radio es
ferultico. Este fenmeno se refleja en la esferulita como una serie de bandas de ex
tincin \up0 \expndtw-1\charscalex100 concntricas que muestran una periodicidad dep
endiente de las condiciones en que ha cristalizado. La \up0 \expndtw0\charscalex
100 medida de la birrefringencia permite diferenciar dos tipos de esferulitas: l
as positivas y las negativas. \up0 \expndtw-2\charscalex100 De esta manera, si e
l ndice de refraccin en la direccin radial es mayor que en la direccin tangencial, \
up0 \expndtw-3\charscalex100 la esferulita es positiva, en caso contrario es neg
ativa. \par\pard\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb265\sl-276\
slmult0 \up0 \expndtw0\charscalex103 3.4.1.2. Difraccin de electrones \par\pard\q
j \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb24\sl-410\slmult0 \up0
\expndtw0\charscalex104 Los diagramas de difraccin de monocristales consisten en
retculos puntuales que representan la \up0 \expndtw0\charscalex105 proyeccin de l
a red cristalina sobre el plano perpendicular al haz electrnico. Suponiendo que l
a \up0 \expndtw-2\charscalex100 radiacin electrnica es paralela al eje cristalogrfi
co c las manchas de difraccin se indexan como hk0, \up0 \expndtw0\charscalex103 a
unque en ocasiones pueden observarse reflexiones hkl con l distinto de 0 debido
a una inclinacin \up0 \expndtw-2\charscalex100 parcial de los cristales o a una d
isposicin no ortogonal de la celdilla unitaria. \par\pard\qj \li1418\sb0\sl-410\s
lmult0 \par\pard\qj\li1418\ri1221\sb20\sl-410\slmult0 \up0 \expndtw0\charscalex1
09 El diagrama de difraccin de una muestra refleja su organizacin estructural a ni
vel atmico y \line \up0 \expndtw0\charscalex104 molecular. Para las muestras amor
fas consiste en un halo difuso que rodea a una mancha central \line \up0 \expndt

w0\charscalex100 correspondiente a la radiacin no desviada, mientras que para las


cristalinas se observan diagramas \line \up0 \expndtw0\charscalex103 con mximos
y mnimos, cuya disposicin en el espacio viene determinada por el tipo de estructur
a \line \up0 \expndtw-3\charscalex100 presente. \par\pard\ql \li10287\sb0\sl-230
\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230
\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230
\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230
\slmult0 \par\pard\ql\li10287\sb109\sl-230\slmult0 \up0 \expndtw-2\charscalex100
\ul0\nosupersub\cf1\f2\fs20 51 \par\pard\sect\sectd\fs24\paperw11900\paperh1684
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a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800
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a28a2800a28a2800a28a2800a28a2800a28a2800a28a2803ffd9}}}}}\pard\sb0\sl-240{\bkmks
tart Pg20}{\bkmkend Pg20}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li
1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\
charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li141
8\ri1219\sb369\sl-426\slmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\
f4\fs24 Las posiciones de las reflexiones definen los espaciados de los planos c
ristalogrficos, realizndose su \up0 \expndtw-1\charscalex100 determinacin segn la le
y de Bragg. Dado que los ngulos \ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub
\cf3\f4\fs24 con que son difractados los electrones \up0 \expndtw-2\charscalex1
00 son muy pequeos (1-2\ul0\super\cf5\f6\fs23 \ul0\nosupersub\cf3\f4\fs24 ) se pue
de admitir la aproximacin tan 2\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\
cf3\f4\fs24 = 2 sen\ul0\nosupersub\cf6\f7\fs24 \u952?\ul0\nosupersub\cf3\f4\fs2
4 y puede utilizarse la ley de \up0 \expndtw-3\charscalex100 Bragg simplificada
: \par\pard\ql \li5455\sb138\sl-276\slmult0 \up0 \expndtw-3\charscalex100 R d\ul
0\sub\cf5\f6\fs24 hkl\ul0\nosupersub\cf3\f4\fs24 = \ul0\nosupersub\cf6\f7\fs24
\u955?\ul0\nosupersub\cf3\f4\fs24 L \par\pard\qj \li1418\sb0\sl-420\slmult0 \pa
r\pard\qj\li1418\ri1221\sb26\sl-420\slmult0 \up0 \expndtw0\charscalex108 donde R
es la distancia de la mancha de difraccin al centro del diagrama, d\ul0\sub\cf5\
f6\fs24 hkl \ul0\nosupersub\cf3\f4\fs24 el espaciado \line \up0 \expndtw-3\cha
rscalex100 interplanar, L la longitud de cmara entre la muestra y la placa de reg
istro y \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 L la const
ante de cmara \line \up0 \expndtw-4\charscalex100 (Figura 28). \par\pard\ql \li30
23\sb0\sl-230\slmult0 \par\pard\ql\li3023\sb0\sl-230\slmult0 \par\pard\ql\li3023
\sb0\sl-230\slmult0 \par\pard\ql\li3023\sb0\sl-230\slmult0 \par\pard\ql\li3023\s
b0\sl-230\slmult0 \par\pard\ql\li3023\sb0\sl-230\slmult0 \par\pard\ql\li3023\sb0
\sl-230\slmult0 \par\pard\ql\li3023\sb0\sl-230\slmult0 \par\pard\ql\li3023\sb0\s
l-230\slmult0 \par\pard\ql\li3023\sb0\sl-230\slmult0 \par\pard\ql\li3023\sb0\sl230\slmult0 \par\pard\ql\li3023\sb0\sl-230\slmult0 \par\pard\ql\li3023\sb0\sl-23
0\slmult0 \par\pard\ql\li3023\sb0\sl-230\slmult0 \par\pard\ql\li3023\sb0\sl-230\
slmult0 \par\pard\ql\li3023\sb147\sl-230\slmult0 \up0 \expndtw-3\charscalex100 \
ul0\nosupersub\cf9\f10\fs20 Figura 28. El microscopio electrnico considerado como
una cmara de difraccin. \par\pard\qj \li1418\ri1220\sb414\sl-420\slmult0 \up0 \ex
pndtw0\charscalex109 \ul0\nosupersub\cf3\f4\fs24 El anlisis de la difraccin de ele
ctrones requiere un calibrado previo del aparato para poder \up0 \expndtw0\chars
calex100 correlacionar las manchas de difraccin obtenidas en el diagrama con las
distancias reales de la red \up0 \expndtw-2\charscalex100 cristalina. Los valore
s de \ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\fs24 y L pueden v
ariar de un registro a otro debido a inestabilidades del circuito \up0 \expndtw0

\charscalex104 elctrico, pequeos desajustes del alto voltaje utilizado o de la cor


riente en las lentes objetivas y \up0 \expndtw-1\charscalex100 proyectoras. Por
esta razn, se debe determinar de forma precisa la constante de cmara para cada \up
0 \expndtw-3\charscalex100 conjunto de lentes utilizadas. \par\pard\qj \li1418\r
i1220\sb406\sl-413\slmult0 \up0 \expndtw0\charscalex110 El calibrado de la const
ante de cmara se realiza evaporando una fina capa de un material \line \up0 \expn
dtw0\charscalex107 policristalino sobre las rejillas con la muestra problema. Su
bstancias cristalinas que presenten \line \up0 \expndtw-3\charscalex100 espaciad
os prximos a los del problema como (Au, Al, TlCl, etc.) son adecuadas como patron
es. En el \line \up0 \expndtw-3\charscalex100 campo de los polmeros se utiliza no
rmalmente oro (reflexiones caractersticas a 4.08, 2.35, 2.04, 1.44, \par\pard\qj
\li1418\ri1221\sb0\sl-420\slmult0 \up0 \expndtw0\charscalex100 1.23, 1.18 y 1.02
\ul0\nosupersub\cf4\f5\fs24 \ul0\nosupersub\cf3\f4\fs24 ) como substancia patrn p
ara calibrar la constante de cmara. Su evaporacin \up0 \expndtw-1\charscalex100 so
bre las rejillas se realiza a partir de 1 cm de un filamento de 0.25 mm de dimetr
o cuidadosamente \up0 \expndtw-4\charscalex100 enrollado alrededor de otro filam
ento (en este caso de tungsteno) en forma de V. \par\pard\ql \li1418\sb0\sl-230\
slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\sl
mult0 \par\pard\ql\li1418\sb9\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\
nosupersub\cf1\f2\fs20 52 \par\pard\sect\sectd\fs24\paperw11900\paperh16840{\shp
{\*\shpinst\shpleft0\shptop0\shpright11900\shpbottom16840\shpwr3\shpfblwtxt0\shp
z-10000\shplid20
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fc3c0bfe0b33ff004afdf8c3ff001675fb117ff26d1ff0f02ff82ccffd2bf7e30ffc59d7ec45ff00
c9b5fb9d45007e18ff00c3c0bfe0b33ff4afdf8c3ff1675fb117ff0026d1ff000f02ff0082ccff00
d2bf7e30ff00c59d7ec45ffc9b5fb9d45007cb1fb217c5efda4fe357c30d53c57fb537ec87aafec5
7f11acfc69aae83a7fc28d5fe387c2cf8ff36b1e13b4d2340bed33c77078dbe115cdcf86ed2db57d
4f53d6b431e1dbef235cb19fc37717d7309d3f53d3279bea7a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002

8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002

8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a002
8a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a00f
ffd9}}}}}\pard\sb0\sl-240{\bkmkstart Pg21}{\bkmkend Pg21}\par\pard\ql \li8764\sb
0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb10
\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materi
ales y mtodos \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\
sb366\sl-413\slmult0 \up0 \expndtw0\charscalex105 \ul0\nosupersub\cf3\f4\fs24 Po
r ltimo, debe tenerse en cuenta que no es posible relacionar directamente una dir
eccin en el \up0 \expndtw0\charscalex103 diagrama de difraccin y la misma en la im
agen morfolgica porque existe una cierta rotacin entre \up0 \expndtw0\charscalex10
9 ambas imgenes (Figura 29). La rotacin del diagrama de difraccin con respecto al c
ristal se \up0 \expndtw0\charscalex109 determina experimentalmente, superponiend
o la imagen morfolgica de un cristal de xido de \up0 \expndtw0\charscalex100 molib
deno y su diagrama de difraccin de electrones en una misma placa de registro, de
forma que la \up0 \expndtw0\charscalex102 direccin de mayor crecimiento coincida
con el eje de la red recproca cuyo parmetro es menor. La \up0 \expndtw-3\charscale
x100 rotacin del diagrama debe calibrarse para cada constante de cmara. \par\pard\
li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0
\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\sl
mult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\
pard\li3871\sb0\sl-276\slmult0\par\pard\li3871\sb0\sl-276\slmult0\par\pard\li387
1\sb0\sl-276\slmult0\par\pard\li3871\sb1\sl-276\slmult0\fi0\tx7630 \up0 \expndtw
0\charscalex100 a)\tab \up0 \expndtw0\charscalex100 b)\par\pard\ql \li2511\sb202
\sl-230\slmult0 \up0 \expndtw-1\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figur
a 29. Correlacin entre la imagen de difraccin y la morfolgica: a) incorrecta, b) co
rrecta. \par\pard\qj \li1418\ri1220\sb354\sl-420\slmult0 \up0 \expndtw0\charscal
ex106 \ul0\nosupersub\cf3\f4\fs24 Las tcnicas ms habituales para la preparacin de l
as muestras para su observacin mediante \up0 \expndtw-3\charscalex100 microscopa e
lectrnica de transmisin son: \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\
li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb97\sl-230\slmult0 \up0 \expndtw3\charscalex100 a) \ul0\nosupersub\cf9\f10\fs20 CRISTALIZACIN EN DISOLUCIN \par\pa
rd\qj \li1418\sb0\sl-412\slmult0 \par\pard\qj\li1418\ri1219\sb48\sl-412\slmult0
\up0 \expndtw0\charscalex102 \ul0\nosupersub\cf3\f4\fs24 Los monocristales se pr
eparan a partir de soluciones diluidas y estn generalmente constituidos por \line
\up0 \expndtw-2\charscalex100 pequeas lamelas de 50-100 de grosor. Su obtencin es
la fase de mayor dificultad en la preparacin \line \up0 \expndtw-2\charscalex100
de muestras para microscopa. La cristalizacin del polmero siempre se realiza a par
tir de disoluciones \line \up0 \expndtw0\charscalex106 muy diluidas (0.05-0.20 %
) en un disolvente a temperatura ambiente o elevada y bajo un estricto \line \up
0 \expndtw0\charscalex100 control de concentracin y temperatura. Los mtodos utiliz
ados habitualmente para obtener cristales \line \up0 \expndtw-2\charscalex100 co
n el grosor adecuado y estudiarlos por TEM son los que se describen a continuacin
. \par\pard\qj \li1418\ri1221\sb402\sl-420\slmult0 \up0 \expndtw0\charscalex107
Cristalizacin isotrmica: consiste en solubilizar el polmero en un mal disolvente a
temperatura \line \up0 \expndtw-2\charscalex100 elevada y dejarlo cristalizar a
una temperatura menor en un bao de cristalizacin. Los disolventes ms \line \up0 \ex
pndtw-2\charscalex100 utilizados para la cristalizacin de los polmeros de este tra
bajo fueron: \up0 \expndtw-3\charscalex100 2-metil-2,4-pentanodiol, \par\pard\ql
\li1418\sb99\sl-276\slmult0 \up0 \expndtw-3\charscalex100 1,4-butanodiol, hexan
ol y glicerina. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb
0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb
192\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 53
\par\pard\sect\sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg2

2}{\bkmkend Pg22}\par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0


\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0 \up0 \expndtw-2\charscal
ex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \par\pard\qj \li1418\sb0\sl
-415\slmult0 \par\pard\qj\li1418\ri1220\sb363\sl-415\slmult0 \up0 \expndtw0\char
scalex106 \ul0\nosupersub\cf3\f4\fs24 Cristalizacin por precipitacin: en este caso
se disuelve el polmero en un buen disolvente y se \up0 \expndtw0\charscalex112 c
ristaliza con la ayuda de un agente precipitante. Como disolventes se utilizan ci
dos como \up0 \expndtw0\charscalex103 dicloroactico o frmico y como precipitantes
agua o alcoholes como etanol, metanol o butanol. La \up0 \expndtw0\charscalex110
degradacin de estos cristales en los disolventes empleados se evita al mximo trab
ajando a \up0 \expndtw-3\charscalex100 temperatura ambiente o prxima a ella. \par
\pard\qj \li1418\ri1218\sb405\sl-416\slmult0 \up0 \expndtw0\charscalex103 Los cr
istales obtenidos se separan por centrifugacin, se lavan con un no-solvente sufic
ientemente \up0 \expndtw-3\charscalex100 voltil \up0 \expndtw0\charscalex106 (n-b
utanol) hasta eliminar totalmente el disolvente utilizado para su crist
alizacin, y \up0 \expndtw0\charscalex102 posteriormente se suspenden en el mismo
no-solvente. Una gota de esta suspensin es depositada \up0 \expndtw0\charscalex1
03 sobre una rejilla de cobre de 3 mm de dimetro, cubierta por un film de carbono
delgado (< 200 ), \up0 \expndtw0\charscalex100 obtenido por evaporacin de grafito
a alto vaco (10\ul0\super\cf5\f6\fs23 -4\ul0\nosupersub\cf3\f4\fs24 - 10\ul0\su
per\cf5\f6\fs23 -5\ul0\nosupersub\cf3\f4\fs24 torr) sobre una lmina exfoliada de
mica y \up0 \expndtw-3\charscalex100 flotado posteriormente sobre las rejillas.
\par\pard\qj \li1418\ri1221\sb409\sl-410\slmult0 \up0 \expndtw0\charscalex106 E
l film de carbono es el sustrato ms idneo para trabajar con monocristales porque e
s bastante \up0 \expndtw0\charscalex104 resistente, amorfo y relativamente trans
parente a los electrones. Despus de dejar evaporar el no\up0 \expndtw0\charscalex
100 solvente sobre la rejilla quedan los cristales adheridos sobre el film de ca
rbono y puede obtenerse el \up0 \expndtw0\charscalex107 diagrama de difraccin. La
visualizacin de los detalles de superfcie de los cristales requiere el \up0 \expn
dtw-3\charscalex100 sombreado posterior de la muestra. \par\pard\ql \li1418\sb0\
sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb119\
sl-230\slmult0 \up0 \expndtw-3\charscalex100 b) \ul0\nosupersub\cf9\f10\fs20 CRI
STALIZACIN EPITAXIAL \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\
ri1220\sb26\sl-413\slmult0 \up0 \expndtw0\charscalex106 \ul0\nosupersub\cf3\f4\f
s24 Esta cristalizacin consiste en el crecimiento inducido de un cristal sobre la
superfcie de otro en \up0 \expndtw0\charscalex106 contacto con l. En el campo de
los polmeros se utilizan como substratos sustancias fcilmente \up0 \expndtw0\chars
calex105 solubles y de bajo peso molecular como el cido benzico o la hidroquinona.
\ul0\super\cf5\f6\fs23 85\ul0\nosupersub\cf3\f4\fs24 Estas substancias \up0 \ex
pndtw0\charscalex100 tienen un parmetro cristalogrfico prximo a 5 \ul0\nosupersub\c
f4\f5\fs24 \ul0\nosupersub\cf3\f4\fs24 , valor cercano a la distancia reticular e
ntre cadenas \up0 \expndtw0\charscalex102 de diferentes polmeros como polietileno
, polisteres alifticos y poliamidas (en stas la distancia es \up0 \expndtw0\charsca
lex107 ligeramente menor por la presencia de puentes de hidrgeno). Los planos sep
arados por estas \up0 \expndtw-2\charscalex100 distancias se disponen perpendicu
larmente a la superficie del sustrato. \par\pard\qj \li1418\ri1220\sb407\sl-413\
slmult0 \up0 \expndtw0\charscalex103 Esta tcnica puede resultar complementaria a
la difraccin de electrones de cristales obtenidos por \line \up0 \expndtw0\charsc
alex106 cristalizacin isotrmica o por precipitacin, porque puede proporcionar orien
taciones cristalinas \line \up0 \expndtw0\charscalex105 diferentes. As, en la cri
stalizacin epitaxial puede conseguirse que el eje molecular se encuentre \line \u
p0 \expndtw-2\charscalex100 orientado perpendicularmente al haz de electrones y
no de forma paralela como normalmente ocurre en \par\pard\ql \li1418\sb0\sl-230\
slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb99\sl-230\s
lmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 54
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celda unitaria aumenta la \up0 \expndtw0\charscalex104 informacin cristalogrfica,
aunque las reflexiones suelen ser ms arqueadas debido a una mayor \up0 \expndtw-3
\charscalex100 desorientacin de los cristales.\ul0\super\cf5\f6\fs23 86 \par\pard
\qj \li1418\ri1219\sb406\sl-415\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupe
rsub\cf3\f4\fs24 La cristalizacin epitaxial empieza con la evaporacin de una soluc
in diluida de polmero en un buen \up0 \expndtw-1\charscalex100 disolvente como el c
ido frmico. As, se obtiene un film delgado de polmero sobre el que se aade el \up0 \
expndtw-1\charscalex100 inductor de la cristalizacin. Ambos, se funden conjuntame
nte sobre un portaobjetos hasta obtener una \up0 \expndtw-2\charscalex100 disolu
cin homognea que posteriormente se enfra lentamente bajo un gradiente de temperatur
as. Los \up0 \expndtw0\charscalex108 cristales orientados del inductor favorecern
la cristalizacin del polmero. Mediante un lavado \up0 \expndtw0\charscalex102 exh
austivo con metanol se elimina el inductor del crecimiento. A continuacin, se eva
pora sobre los \up0 \expndtw0\charscalex106 cristales un film de carbono y por m
icroscopa ptica de luz polarizada se seleccionan las zonas \up0 \expndtw0\charscal
ex106 orientadas epitaxialmente. stas se separan del portaobjetos con la ayuda de
una gota de cido \up0 \expndtw-3\charscalex100 poliacrlico que puede eliminarse p
osteriormente en un bao de agua. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\par
d\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb98\sl-230\slmult0 \up0 \exp
ndtw-3\charscalex100 c) \ul0\nosupersub\cf9\f10\fs20 PELCULAS ORIENTADAS UNIAXIAL
MENTE \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\li1418\ri1220\sb26\sl
-413\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 La orient
acin uniaxial de un polmero requiere el estiramiento del material, procedente del
fundido o de \up0 \expndtw0\charscalex105 una disolucin muy concentrada, en
una nica direccin del espacio. El procedimiento es \up0 \expndtw0\charscale
x100 esencialmente idntico a la obtencin de fibras o pelculas orientadas para difra
ccin de rayos X, pero \up0 \expndtw-2\charscalex100 en este caso el grosor de la
muestra es crtico para obtener buenas difracciones. \par\pard\qj \li1418\ri1217\s
b407\sl-413\slmult0 \up0 \expndtw-1\charscalex100 La tensin aplicada sobre el mat
erial se realiza con la ayuda de un material inerte como el tefln capaz \up0 \exp
ndtw0\charscalex109 de producir una fuerte cizalla durante el proceso simultneo d
e orientacin-cristalizacin.\ul0\super\cf5\f6\fs23 87\ul0\nosupersub\cf3\f4\fs24 S
e \up0 \expndtw-1\charscalex100 seleccionan las zonas birrefringentes y despus de
evaporar sobre ellas un film de carbono se separan \up0 \expndtw-2\charscalex10
0 de forma anloga a la cristalizacin epitaxial. \par\pard\ql \li1418\sb0\sl-230\sl
mult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb119\sl-230\sl
mult0 \up0 \expndtw-3\charscalex100 d) \ul0\nosupersub\cf9\f10\fs20 DECORACIN DE
CRISTALES CON POLIETILENO \par\pard\qj \li1418\sb0\sl-413\slmult0 \par\pard\qj\l
i1418\ri1220\sb26\sl-413\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf
3\f4\fs24 Esta tcnica fue desarrollada por Wittmann y Lotz en 1985.\ul0\super\cf5
\f6\fs23 88\ul0\nosupersub\cf3\f4\fs24 El fundamento es el mismo que el de la \
up0 \expndtw0\charscalex103 cristalizacin epitaxial, slo que en este caso el polmer
o es el substrato y sobre l se deposita una \up0 \expndtw0\charscalex103 substanc
ia, de estructura cristalina conocida, que cristaliza sobre los monocristales de
l mismo. Nos \up0 \expndtw-3\charscalex100 permite determinar las caractersticas
superficiales de las lamelas. \par\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard
\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard
\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard

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28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a

28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a
28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2800a28a2803fffd9}}}}}\pard\s
b0\sl-240{\bkmkstart Pg24}{\bkmkend Pg24}\par\pard\ql \li1418\sb0\sl-230\slmult0
\par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-230\slmult0
\up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y mtodos \pa
r\pard\qj \li1418\ri1220\sb380\sl-412\slmult0 \up0 \expndtw-1\charscalex100 \ul0
\nosupersub\cf3\f4\fs24 La observacin detallada de los cristales polimricos sugier
e que debe existir un cierto plegamiento de \line \up0 \expndtw0\charscalex100 l
as cadenas debido a que en general, el espesor de las lamelas resulta mucho meno

r que la longitud \line \up0 \expndtw0\charscalex100 promedio de las cadenas. Ad


ems, se acepta generalmente que ste debe ser paralelo a la direccin \line \up0 \exp
ndtw0\charscalex106 de crecimiento del cristal.\ul0\super\cf5\f6\fs23 89\ul0\nos
upersub\cf3\f4\fs24 As, esta tcnica permite conocer la sectorizacin de los cristal
es del \line \up0 \expndtw0\charscalex107 polmero asociada a una direccin privileg
iada de plegamiento molecular durante el crecimiento \line \up0 \expndtw-3\chars
calex100 cristalino (Figura 30a). \par\pard\qj \li1418\ri1219\sb406\sl-415\slmul
t0 \up0 \expndtw0\charscalex100 En la prctica se evapora lentamente bajo vaco (10\
ul0\super\cf5\f6\fs23 -4\ul0\nosupersub\cf3\f4\fs24 - 10\ul0\super\cf5\f6\fs23
-5\ul0\nosupersub\cf3\f4\fs24 torr) una pequea muestra de polietileno \up0 \expn
dtw-1\charscalex100 (~ 2 mg, M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24
= 20.000 y M\ul0\sub\cf5\f6\fs24 w\ul0\nosupersub\cf3\f4\fs24 /M\ul0\sub\cf5\f6
\fs24 n\ul0\nosupersub\cf3\f4\fs24 = 1.1) en un filamento de tungsteno. Durante
este proceso se produce la \up0 \expndtw0\charscalex100 escisin parcial de las c
adenas moleculares de polietileno que cristalizan epitaxialmente en forma de \up
0 \expndtw-2\charscalex100 pequeas barritas alargadas sobre las lamelas del polmer
o a decorar (Figura 30b). Todas las muestras \up0 \expndtw-2\charscalex100 son s
ombreadas con Pt/C despus de la decoracin para su observacin microscpica. \par\pard\
li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0
\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\sl
mult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\
pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li376
1\sb0\sl-276\slmult0\par\pard\li3761\sb0\sl-276\slmult0\par\pard\li3761\sb235\sl
-276\slmult0\fi0\tx8174 \up0 \expndtw0\charscalex100 a)\tab \up0 \expndtw0\chars
calex100 b)\par\pard\ql \li1583\sb0\sl-230\slmult0 \par\pard\ql\li1583\sb101\sl230\slmult0 \up0 \expndtw0\charscalex105 \ul0\nosupersub\cf9\f10\fs20 Figura 30.
a) Cristal simple de polietileno cristalizado en p-xileno a 70\ul0\super\cf11\f
12\fs19 \ul0\nosupersub\cf9\f10\fs20 C y decorado con vapores de polietileno. \pa
r\pard\qj \li1583\ri1503\sb10\sl-230\slmult0 \up0 \expndtw0\charscalex106 b) Rep
resentacin esquemtica de la decoracin de cristales con polietileno. Disposicin de la
s lamelas sobre \up0 \expndtw0\charscalex104 parafina exenta de plegamiento que
da lugar a una disposicin del polietileno decorador completamente al azar \up0 \e
xpndtw-2\charscalex100 (izquierda), y polietileno con planos de plegamiento 110
que origina una decoracin sectorizada (derecha). \par\pard\ql \li1418\sb0\sl-276\
slmult0 \par\pard\ql\li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb0\sl-276\sl
mult0 \par\pard\ql\li1418\sb44\sl-276\slmult0 \up0 \expndtw-2\charscalex100 \ul0
\nosupersub\cf3\f4\fs24 3.4.2. DIFRACCIN DE RAYOS X \par\pard\qj \li1418\sb0\sl-4
20\slmult0 \par\pard\qj\li1418\ri1221\sb26\sl-420\slmult0 \up0 \expndtw0\charsca
lex104 Los rayos X son una radiacin electromagntica cuya longitud de onda se encue
ntra comprendida \line \up0 \expndtw0\charscalex108 entre la radiacin UV y los ra
yos \ul0\nosupersub\cf6\f7\fs24 \u947?\ul0\nosupersub\cf3\f4\fs24 . Las propieda
des ms importantes de sta radiacin fueron \line \up0 \expndtw0\charscalex102 descri
tas por Rntgen en 1896, pero no fue hasta principios del siglo pasado que von Lau
e (1912) y \line \up0 \expndtw0\charscalex106 Bragg (1913) demostraron que los c
ristales, debido a su ordenacin regular, podan difractar los \line \up0 \expndtw0\
charscalex105 rayos X dispersados por todos los elementos que los const
ituyen, segn unas direcciones \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\par
d\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\
ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb217\sl-230\slmult0 \up0 \expn
dtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 56 \par\pard\sect\sectd\fs24\pap
erw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg25}{\bkmkend Pg25}\par\pard\ql
\li8764\sb0\sl-230\slmult0 \par\pard\ql\li8764\sb0\sl-230\slmult0 \par\pard\ql\
li8764\sb10\sl-230\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\
fs20 Materiales y mtodos \par\pard\qj \li1418\ri1222\sb390\sl-400\slmult0 \up0 \e
xpndtw0\charscalex103 \ul0\nosupersub\cf3\f4\fs24 determinadas. Este descubrimie
nto fue til para la determinacin de la estructura tridimensional de \up0 \expndtw2\charscalex100 numerosas molculas biolgicas,\ul0\super\cf5\f6\fs23 90 \ul0\nosupe
rsub\cf3\f4\fs24 pero tambin en el caso de los polmeros sintticos.\ul0\super\cf5\f6
\fs23 91 \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1220\sb22
\sl-410\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf3\f4\fs24 Esta tc

nica permite obtener el diagrama de difraccin del material y la ordenacin de sus to


mos en el \up0 \expndtw-1\charscalex100 espacio mediante anlisis de Fourier. Aunq
ue es aplicable a muestras slidas, lquidas o gaseosas, en \up0 \expndtw0\charscale
x108 el campo de los polmeros su uso est restringido casi completamente a la deter
minacin de la \up0 \expndtw-1\charscalex100 ordenacin atmica en la parte slida crist
alina, es decir, regularmente ordenada como mnimo en una \up0 \expndtw-3\charscal
ex100 de las tres direcciones del espacio. \par\pard\qj \li1418\ri1221\sb420\sl423\slmult0 \up0 \expndtw0\charscalex102 Cuando los electrones emitidos por un f
ilamento calentado a temperatura elevada se hacen incidir \line \up0 \expndtw0\c
harscalex104 sobre un nodo metlico, de forma que las capas ms internas de los tomos
que lo constituyen \line \up0 \expndtw-1\charscalex100 puedan producir transicio
nes, se generan rayos X cuya longitud de onda se sita entre 10\ul0\super\cf5\f6\f
s23 -7\ul0\nosupersub\cf3\f4\fs24 y 10\ul0\super\cf5\f6\fs23 -11\ul0\nosupersub
\cf3\f4\fs24 m. \line \up0 \expndtw-3\charscalex100 Normalmente se utiliza un no
do de cobre y se obtiene un espectro de rayos X formado por una banda \line \up0
\expndtw-2\charscalex100 ancha responsable de la radiacin blanca y unas lneas car
actersticas (CuK\ul0\sub\cf10\f11\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 y CuK\u
l0\sub\cf10\f11\fs24 \u946?\ul0\nosupersub\cf3\f4\fs24 ) que se pueden \line \up
0 \expndtw0\charscalex103 separarse mediante filtros adecuados. Para el estudio
de los polmeros se utiliza la lnea CuK\ul0\sub\cf10\f11\fs24 \u945?\ul0\nosupersub
\cf3\f4\fs24 de \line \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf6\f7\fs24
\u955?\ul0\nosupersub\cf3\f4\fs24 = 0.154 nm y un filtro de nquel para eliminar
al mximo la radiacin CuK\ul0\sub\cf10\f11\fs24 \u946?\ul0\nosupersub\cf3\f4\fs24
y la continua. \par\pard\qj \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri12
21\sb18\sl-410\slmult0 \up0 \expndtw-4\charscalex100 La difraccin de rayos X sigu
e el principio de Huyggens, donde cada rendija presente en el cristal acta \line
\up0 \expndtw-1\charscalex100 como un nuevo foco emisor de ondas que interfieren
constructiva o destructivamente para producir la \line \up0 \expndtw-1\charscal
ex100 difraccin. nicamente se produce interferencia constructiva cuando se cumple
la ley de Bragg: \par\pard\ql \li5195\sb0\sl-276\slmult0 \par\pard\ql\li5195\sb2
65\sl-276\slmult0 \up0 \expndtw-3\charscalex100 n \ul0\nosupersub\cf6\f7\fs24 \u
955?\ul0\nosupersub\cf3\f4\fs24 = 2 d\ul0\sub\cf5\f6\fs24 hkl\ul0\nosupersub\cf
3\f4\fs24 sen \ul0\nosupersub\cf6\f7\fs24 \u952? \par\pard\qj \li1418\sb0\sl-44
0\slmult0 \par\pard\qj\li1418\ri1221\sb9\sl-440\slmult0 \up0 \expndtw-3\charscal
ex100 \ul0\nosupersub\cf3\f4\fs24 donde d\ul0\sub\cf5\f6\fs24 hkl\ul0\nosupersub
\cf3\f4\fs24 es el espaciado de los planos de Miller, \ul0\nosupersub\cf6\f7\fs
24 \u952?\ul0\nosupersub\cf3\f4\fs24 el ngulo de incidencia o reflexin, n el nmero
de \line \up0 \expndtw-4\charscalex100 orden y \ul0\nosupersub\cf6\f7\fs24 \u95
5?\ul0\nosupersub\cf3\f4\fs24 la longitud de onda de la radiacin utilizada \up0
\expndtw-4\charscalex100 (Figura \up0 \expndtw-4\charscalex100 31). El conjunto
de espaciados \par\pard\qj \li1418\ri1220\sb0\sl-430\slmult0 \up0 \expndtw0\char
scalex103 cristalogrficos permite determinar la celdilla unitaria determinada por
los parmetros a, b, c y los \up0 \expndtw-1\charscalex100 ngulos existentes entre
ellos \ul0\nosupersub\cf6\f7\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 , \ul0\nosu
persub\cf6\f7\fs24 \u946?\ul0\nosupersub\cf3\f4\fs24 , y \ul0\nosupersub\cf6\f7\
fs24 \u947?\ul0\nosupersub\cf3\f4\fs24 . Esta celdilla representa la unidad ms pe
quea que refleja la \up0 \expndtw-5\charscalex100 simetra del cristal. \par\pard\q
l \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\
ql\li10287\sb65\sl-230\slmult0 \up0 \expndtw-4\charscalex100 \ul0\nosupersub\cf1
\f2\fs20 57 \par\pard\sect\sectd\fs24\paperw11900\paperh16840{\shp
{\*\shpinst\shpleft0\shptop0\shpright11900\shpbottom16840\shpwr3\shpfblwtxt0\shp
z-10000\shplid25
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0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a
0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a
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0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a
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}}}\pard\sb0\sl-240{\bkmkstart Pg26}{\bkmkend Pg26}\par\pard\ql \li1418\sb0\sl-2
30\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb10\sl-23
0\slmult0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 Materiales y
mtodos \par\pard\li1871\sb0\sl-276\slmult0\par\pard\li1871\sb0\sl-276\slmult0\pa
r\pard\li1871\sb0\sl-276\slmult0\par\pard\li1871\sb187\sl-276\slmult0\fi0\tx7344
\up0 \expndtw0\charscalex100 \ul0\nosupersub\cf3\f4\fs24 a)\tab \up0 \expndtw0\
charscalex100 b)\par\pard\ql \li7954\sb0\sl-276\slmult0 \par\pard\ql\li7954\sb0\
sl-276\slmult0 \par\pard\ql\li7954\sb0\sl-276\slmult0 \par\pard\ql\li7954\sb0\sl
-276\slmult0 \par\pard\ql\li7954\sb0\sl-276\slmult0 \par\pard\ql\li7954\sb0\sl-2
76\slmult0 \par\pard\ql\li7954\sb0\sl-276\slmult0 \par\pard\ql\li7954\sb0\sl-276
\slmult0 \par\pard\ql\li7954\sb0\sl-276\slmult0 \par\pard\ql\li7954\sb137\sl-276
\slmult0 \up0 \expndtw0\charscalex100 \ul0\nosupersub\cf6\f7\fs24 tan 2\u952? =
D/2L \par\pard\qj \li1871\sb0\sl-240\slmult0 \par\pard\qj\li1871\ri1713\sb34\sl240\slmult0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf9\f10\fs20 Figura 31
. a) Geometra de la difraccin de rayos X, b) relacin entre el dimetro de la difraccin
(D) y el ngulo \up0 \expndtw-4\charscalex100 de dispersin (2\ul0\nosupersub\cf1\f
2\fs20 \u952?\ul0\nosupersub\cf9\f10\fs20 ). \par\pard\qj \li1418\sb0\sl-430\slm
ult0 \par\pard\qj\li1418\ri1220\sb34\sl-430\slmult0 \up0 \expndtw0\charscalex100
\ul0\nosupersub\cf3\f4\fs24 La difraccin de rayos X se realiz utilizando cmaras Wa
rhus (W.H. Warhus, Wilmington, Delaware, \line \up0 \expndtw0\charscalex104 USA)
tipo Statton con monocromador de grafito incorporado que selecciona la radiacin
K\ul0\sub\cf10\f11\fs24 \u945?\ul0\nosupersub\cf3\f4\fs24 del Cu \line \up0 \ex
pndtw0\charscalex106 (\ul0\nosupersub\cf6\f7\fs24 \u955?\ul0\nosupersub\cf3\f4\f
s24 = 0.154 \ul0\nosupersub\cf4\f5\fs24 nm\ul0\nosupersub\cf3\f4\fs24 ) y un ge
nerador Phillips modelo P-W 1130/90 provisto de un tubo Phillips sellado \line \
up0 \expndtw0\charscalex111 (PW 2113 de 1200 W) de foco plano y con filtro de ni
quel. El calibrado se realiz con calcita \line \up0 \expndtw-2\charscalex100 d\ul
0\nosupersub\cf5\f6\fs16 B\ul0\nosupersub\cf3\f4\fs24 = 0.3035 \ul0\nosupersub\
cf4\f5\fs24 nm\ul0\nosupersub\cf3\f4\fs24 o sulfuro de molibdeno d\ul0\nosupers
ub\cf5\f6\fs16 002\ul0\nosupersub\cf3\f4\fs24 = 0.6147 \ul0\nosupersub\cf4\f5\f
s24 nm\ul0\nosupersub\cf3\f4\fs24 dependiendo de la longitud de cmara. \par\pard
\ql \li1418\sb0\sl-276\slmult0 \par\pard\ql\li1418\sb242\sl-276\slmult0 \up0 \ex
pndtw-3\charscalex100 Las muestras analizadas por difraccin de rayos X correspond

en a: \par\pard\ql \li1418\sb0\sl-241\slmult0 \par\pard\ql\li1418\sb0\sl-241\slm


ult0 \par\pard\ql\li1418\sb91\sl-241\slmult0 \up0 \expndtw-3\charscalex100 a) \u
l0\nosupersub\cf9\f10\fs20 DIAGRAMAS DE POLVO \par\pard\qj \li1418\sb0\sl-413\sl
mult0 \par\pard\qj\li1418\ri1219\sb24\sl-413\slmult0 \up0 \expndtw0\charscalex10
7 \ul0\nosupersub\cf3\f4\fs24 Son los diagramas de difraccin de muestras totalmen
te desorientadas y se caracterizan por la \line \up0 \expndtw0\charscalex100 pre
sencia de una serie de anillos concntricos cuya intensidad y dimetro son caracterst
icos de cada \line \up0 \expndtw0\charscalex105 polmero. Estos anillos estn ligado
s a la reflexin producida por los planos cristalogrficos de los \line \up0 \expndt
w0\charscalex110 cristales del polmero. Se obtienen colocando una muestra del polm
ero finamente triturado y \line \up0 \expndtw0\charscalex102 fuertemente compact
ado en un capilar de vidrio sin plomo con dimetro variable entre 0.5 y 1.5 mm. \l
ine \up0 \expndtw-1\charscalex100 Dado que cada uno de los cristales est dispuest
o al azar con respecto al resto, la difraccin final tiene \line \up0 \expndtw0\ch
arscalex106 forma de anillo que ser tanto ms definido cuanto ms cristalino sea el p
olmero. El nmero de \line \up0 \expndtw-1\charscalex100 reflexiones presentes en e
stos diagramas es muy reducido, por lo que en muchas ocasiones la celdilla \line
\up0 \expndtw0\charscalex103 unitaria no queda inequvocamente designada. As pues,
para tener una buena aproximacin de la \line \up0 \expndtw-2\charscalex100 estru
ctura es de vital importancia disponer de diagramas de difraccin de muestras orie
ntadas. \par\pard\ql \li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\s
lmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slm
ult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb89\sl-230\slmu
lt0 \up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 58 \par\pard\sect\
sectd\fs24\paperw11900\paperh16840\pard\sb0\sl-240{\bkmkstart Pg27}{\bkmkend Pg2
7}\par\pard\li1418\sb0\sl-230\slmult0\par\pard\li1418\sb0\sl-230\slmult0\par\par
d\li1418\sb21\sl-230\slmult0\fi7346 \up0 \expndtw-3\charscalex100 \ul0\nosupersu
b\cf1\f2\fs20 Materiales y mtodos\par\pard\li1418\sb0\sl-276\slmult0\par\pard\li1
418\sb207\sl-276\slmult0\fi0 \up0 \expndtw-3\charscalex100 \ul0\nosupersub\cf3\f
4\fs24 b) \ul0\nosupersub\cf9\f10\fs20 DIAGRAMAS DE FIBRA\par\pard\qj \li1418\sb
0\sl-413\slmult0 \par\pard\qj\li1418\ri1221\sb16\sl-413\slmult0 \up0 \expndtw0\c
harscalex103 \ul0\nosupersub\cf3\f4\fs24 Un diagrama de fibra muy orientado prop
orciona una informacin ms precisa que un diagrama de \line \up0 \expndtw0\charscal
ex102 difraccin de polvo, en cuanto a la asignacin de los ndices de Miller correspo
ndientes a los planos \line \up0 \expndtw-1\charscalex100 difractados y a la det
erminacin de la simetra cristalina. Las propiedades trmicas y el peso molecular \li
ne \up0 \expndtw0\charscalex106 del polmero son condicionantes para la aplicacin d
e este mtodo. Debido a que el polmero es \line \up0 \expndtw0\charscalex100 estira
do segn el propio eje molecular, estos diagramas se caracterizan por la aparicin d
e manchas \line \up0 \expndtw0\charscalex100 relacionadas con la repetitividad d
e cadena con orientacin meridional (M) o fuera del meridiano (oM) \line \up0 \exp
ndtw-1\charscalex100 segn el sistema cristalino, y manchas ecuatoriales \up0 \exp
ndtw-1\charscalex100 (E), relacionadas con el empaquetamiento \par\pard\qj \li14
18\ri1220\sb10\sl-410\slmult0 \up0 \expndtw-1\charscalex100 cristalino. La orien
tacin de la muestra se consigue a partir del estirado de la masa polimrica fundida
. \up0 \expndtw0\charscalex105 sta puede mejorarse al someter la muestra a un pro
ceso posterior de templado que consiste en \up0 \expndtw-1\charscalex100 \u8220?
reestirarla\u8221? bajo tensin constante en estufa o en atmsfera de vapor de agua.
El grado de orientacin \up0 \expndtw0\charscalex106 de la fibra resultante se es
tima cualitativamente mediante la birrefrigencia de la muestra bajo un \up0 \exp
ndtw-3\charscalex100 microscopio de luz polarizada. \par\pard\ql \li1418\sb0\sl230\slmult0 \par\pard\ql\li1418\sb0\sl-230\slmult0 \par\pard\ql\li1418\sb99\sl-2
30\slmult0 \up0 \expndtw-3\charscalex100 c) \ul0\nosupersub\cf9\f10\fs20 DIAGRAM
AS DE SEDIMENTO CRISTALINO \par\pard\qj \li1418\sb0\sl-411\slmult0 \par\pard\qj\
li1418\ri1219\sb50\sl-411\slmult0 \up0 \expndtw0\charscalex102 \ul0\nosupersub\c
f3\f4\fs24 Estos diagramas estn orientados parcialmente segn el eje de apilamiento
de las lamelas. Aportan \line \up0 \expndtw0\charscalex108 informacin adicional
sobre la naturaleza lamelar de los cristales, ya que aparecen reflexiones \line
\up0 \expndtw-2\charscalex100 meridionales relacionadas con el espesor de la lam
ela debido a que la muestra se irradia paralelamente \line \up0 \expndtw0\charsc

alex100 a la superficie de deposicin. Tambin proporcionan informacin acerca de la i


nclinacin de la cadena \line \up0 \expndtw-1\charscalex100 respecto a la lamela y
del nmero de unidades repetitivas que pueden existir en el interior de la misma.
\line \up0 \expndtw0\charscalex103 Cuando ste es reducido, se producen unas refl
exiones dbiles adicionales denominadas mximos \line \up0 \expndtw-1\charscalex100
subsidiarios. El nmero de los mismos observado entre las reflexiones correspondie
ntes a dos rdenes \line \up0 \expndtw-1\charscalex100 consecutivos de la repetiti
vidad de residuo es igual al nmero de unidades repetitivas menos dos. \par\pard\q
j \li1418\sb0\sl-410\slmult0 \par\pard\qj\li1418\ri1222\sb20\sl-410\slmult0 \up0
\expndtw0\charscalex111 La preparacin de estos sedimentos requiere una optimizac
in previa de las condiciones de \line \up0 \expndtw0\charscalex100 cristalizacin d
el polmero. Entre 20-25 mg de polmero perfectamente cristalizados son centrifugado
s \line \up0 \expndtw0\charscalex104 para obtener el sedimento de cristales que
se separa por decantacin. Despus de lavarlos varias \line \up0 \expndtw0\charscale
x106 veces con n-butanol, son suspendidos en l y filtrados lentamente en un dispo
sitivo como el que \line \up0 \expndtw-3\charscalex100 muestra la Figura 32. \pa
r\pard\ql \li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \p
ar\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \p
ar\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb0\sl-230\slmult0 \p
ar\pard\ql\li10287\sb0\sl-230\slmult0 \par\pard\ql\li10287\sb189\sl-230\slmult0
\up0 \expndtw-2\charscalex100 \ul0\nosupersub\cf1\f2\fs20 59
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