16 17

INllo.'OtlU<
11\ IN 1111'1\\11 MUALttJlo.'t.Y
II I.:
POWDER METALLURGY SCIENCE  ~.
I arc combined with other phases such as ceramics or lymcrs. An important charactcris
lie of a powde.r i~ its relatively high surface area to volume ratio. The particles exhibit
behavior t~at IS intermediate between that of a 011 and a liq I • Powders will flow
under gravity to fil~ con~ainers or die cavities. so in t IS sense they behave like liquids.
They ar~ com~resslble like. a gas. But the compression of a metal powder is csxcntiilly
Irreversible. like the plastic deformation of a metal. Thus. a metal powder is casilv
I
shaped. with the desirable behavior of a solid after processing. .
. P?wder metall~rgy. is the study of the processing of metal powders. including the lab
neutron. charactenzat.,on. and conversion of metal powders rnto useful engineering com '.
ponents. The .processmg sequence involves the application of basic laws of heat. work.
powders chemistry
and defonnallon to the powder. It is the processing which changes the shape. properties
and structure of a powder into a final product. An extended list of definitions relating to
powder metallurgy is given in Appendix A.
The three main steps in the scheme of powder metallurgy are illustrated in Figure 1.1.
1'1
18
POWDER METAlLlJRC,y \('n.NC I I.
Brief History The initial interest in powder metallurgy grew from an expanding materials base,
forming the common elements like copper and,iron by a new. lower cost t~hnology.
The very early uses of metal powders have been traced to several parts of the world.
Sir.ce the 1940·s. several less common materials have been processed fro!" powders.
: \ .: For example. gold powder was fired 0010 jewelry by the Incas. and Egyptian uses of iron
incluJing the refractory metals and their alloys (Nb, W. Mo. Zr. TI. and Re).
powder date back to 3000 Be. Another early example is the Delhi column in India which
Additionally. the structural metals have come through a _major growth during the. ~e
dates from about 300 AD. This column is made from approximately 6.5 tons of reduced
iron powder. During the 1800's the use of powder metallurgy techniques began in time period. The majority of the structural powderproduced parts ~re .ba5ed on I~~':\.:.....
Hcwevcr, several compositions tailored for nuclear, aerospace, eicctn.clli. and magnetl~ .. ' .
earnest: The need for platinum laboratory apparatus led to the development of chemically
precipitated powder and new consolidation routes which avoided high tempe:atures. applications arc processed by P/M techniques, ., .. . . '. .'
": Such activities occurred in both Russia and England where precipitated powders were
Equally exciting has been the evolution in applications. The spint 10 DpplylO~ PIM.
'. has undergone a recent change. Initially. powderbased components were selected Simply
hotworked to overcome the inability to obtain the high temperatures needed for casting
for .heir low costs. More recently, the basis for selecting D powder metallurgy route has
platinum. About this same time. coins were fabricated from pressed and sintcrcd copper.
been associated with improved quality, homogeneity. or properties. coupled with, an : .
silver. and lead powders. The modern era of powder metallurgy is traced to Coolidge
attractive cost and productivity. The high temperature nickelballed lIu~ralloys: high
who used' tungsten powder to develop a durable lamp filament for Edison. Subsequently.
specific stiffness aluminum aircraft alloys. and. cOOlroll~d thermal expansron alumlO~m,.
cemented carbides, porous bronze bearings, and coppergrnpbue electrical Contacts were
matrix composites offer gnod examples of this evolution. Not only, can they be mad.e, i .
developed in the 1930·s. By the 1940·s. P/M was involved in the fabrication of new
with h:ller material economy hy powder approaches. but new and Improved cornpon
tungsten alloys, ferrous structural alloys, and refractory metals.
rions arc being developed to take advaruagc of the chemistry an~ microst~cture con~rol.
The expansion or P/M prll\:e~sillg into areas requiring high quality materiuls and uruque
properties will creat~ even more opportunities in the future.
70
11
I'OWOLU METAlLU/~(jY ~LlINU
IN II/UUL}( II! ,,~ II I I', IWUlIl MlIl\J I UIIGY
Economic
..,
cost
precision iron and steel
productivity
(example: automobile gears) aluminum
copper
Unique
alloys nickel
microstructures
CapUve composites
refractory (example: stainless steel tungsten
reactive filters)
(example:
stainless steel
tin
Ideal Applications
(example: porous tantalum capacitors)
relative production
Agure 1.3. The three main reasons for using powder metallurgy are shown in the form of
a VeM diagram. The Intersection of the circles represents an ideal area for applying pow
der metallurgy In the future. Figure 1.4. A comparison of the relative production for some common metal powders.
Note the logarithmic scaling and dominant role of iron and steel.
lurgy techniques are attractive since all of the processing can be performed in the solid fonn microstructures, 4) Economical consolid.uion of specialty alloys. typically compos
state. .
ites containing mixed phases; these will often be fabricated by enhanced dCllsificat.ioll
Usually elements from all three categories exist in most P/M applications. Indeed. the processes. 5) Synthesis of nonequilibrium materials such as a~lOrphous. microcrystalline.
major growth and expansion will most likely come from further combinations of eco or metastable alloys. 6) Processing of complex paris with unique ingredients or UIlCOIll,
nomic, captive, and unique aspects in. forming unique.lowcost. high quality products. man shapes.
22
POWDER METAllURGY SCIENCE
Powder metallurgy is in a prolonged, if not steady. growth phase. The use of metal wing structures. Contrast the expected powder requirements (or these two nelda.
"
'.
'
powders continues to expand and the field is growing faster than other metalworking
technologies. Moreover, the need for trained personnel is growing even more rapidly 1.2. ?owder metallurgy contributes to a range of automcdveeompceeau, Identify one
because of the diverse and difficult applications being developed for PIM processing. . such component and give the chief performance requlrements (check Table 1.1 and
The feedback from design engineers indicates that as knowledge about PIM expands Chapter Eleven for ideas).
there will be 'many more applications. The majority of the current uses relies on econom 1.3. Consider the alternatives to powder metallurgy for the tabricalion of lamp filaments :"
ical netshape processing. The future promises more challenges with the combination of from tungsten. Why are fusion techniques not applied to Ihis product? :' "
cost savings and factors such as reliability, quality. strength, dimensional control. and
unique shaping capabilities. Widespread appreciation of these advantages will provide IA. Powder metallurgy was once known as "metal ceramics." What similarities with ' '
both economic and technological growth opportunities. Research using metal powders ceramic processing does this name suggest?
offers hope for even more diverse applications, including rapidly solidified magnetic 1.5. What are some of the key differences between ceramic and metal powders and how
, alloys. new aircraft alloys. improved metal matrix composites, and ultrahigh strength might these differences influence processing?
structures involving very small scale microstructures.
1.6. One of the challenges of PIM processing is to minimize tooling costs, especially din ,
Suggested References ing product development efforts. The need is to reduce errors in the construction of pro
duction tooling to ensure final dimensions and properties meet specifications. What steps
K. J. Anderson, "Materials for Incandescent Lighting: 110 Years for the Light Bulb." might help to minimize preproduction tool costs?
MRS Bulletin, 1990, vol. IS, no. I, pp. 5253.
1.7. In spite of a low melting temperature (232·C). tin is widely used as a powder.
1 ,F. Clark, Advanced Experimental Techniques in Powder Metallurgy, Rowrnan and Identify some possible applications for tin powders. '
Littlefield. New York, NY. 1963, pp.I60163.
1.8. Give <I short definition of powder metallurgy in lay terms and embellish this defini
C. G. Goetzel, Tre~iise On Powder M~fall~i'~~~"f~ur '~~'I~;"es. Interscience Publishers. tion in engineering terms.
I powders, New York, NY. 1949.
1.9. Metal powders exhibit fluidlike behavior. Identify a common object or product that •
H.H. Hausner and M. K. Mal, Handbook of Powder Mmllurgy, second edition. relies on this attribute.
Chemical Publishing Co., New York, NY, 1982.
I)' C~111POS'
L Jenkins and J. Y. Wood (eds.), Powder Metallurgy: An Overview. The Institute of
1.10. Metal matrix composites. such as aluminum reinforced with silicon carbide
whiskers. are a new application area for PIM. Identify and explain some of the concerns •.
msli rcat lOll
Metals. London, UK. 1991.
crystalline.
or 1IIlCOIl1· W. D. Jones, fundamental Principles of Powder Metallurgy, Edward Amold Publishers.
associated with' the fabrication of such materials.
.
,.:
24
25
POWf)F.R MFTt'J ItJR(,y mrN(J 1\ l'NIll Il nWW:llNIIAJION'
, ,
I
I,
i
,
... ,, Chapter !".!~
_,._
Powder Characterization
Concepts
All powder processing starts with a powder; therefor~; one must understand the nature
of powder to understand the process. A particle is defined as the smallest unit of a pow
der that can not be subdivided. Generally. powder metallurgy deals with particles that arc
larger than smoke (0.0 I to 1 urn), but smaller than sand (0.1 to 3 mm). Many metal pow
ders are similar in size 10 the diameter of a human hair (25 to 200 urn). The scanning
electron microscope (SEM) is one of the best tools available for observing the discrete
characteristics of metal powders. An array of SEM micrographs for several different
powders is shown in Figure 2.1. In this series of micrographs. variations in shape from
flake to spherical and in particle size from the submicron to I mm illustrate the wide
range of possible characteristics.
Concerns beyond particle appearance require quantitative data. including the following:
I) particle size and distribution.
2) particle shape and its variation with particle size.'
3) surface area.
4) interparticle friction.
s) now and packing.
6) the internal particle structure. and
7) composition. homogeneity. and 'Contamination .
. T~ fully specify the ,nature of a powder it is also necessary .to qualitatively describe
I "
h?w It was. fabricated. When dealing with powders. not only the properties of both indi
Thee, partl~les but also the collective (bulk) properties of a powder lot must be studied.
", ; ~ropertles of a single particle include size. shape. chemistry. microstructure. density.
an ~ness. For a bulk lot of powder, characterization implies measurement of those
dPro~nl~s, and packing, now, and surface attributes. Both quantitative and qualitative
escnpllons are av '1 bl C' .... .
d'bed al a e. onsider the particle Image 111Figure 2.2. The Image can be
escn as a rou d db' I
value I ~ e ut irregu ar shape. However, such information is of limited FIgure 2.1: S<;~e examples of the diverse 6~ a~ Iizes of metal powde'* u seen In
of th~ n c~~~.t, dimensioning the particle is quite difficult because of the shape. Some the scanning eiectron microscope. These exMIpiea Illustrate. variety of materials, fabrl·
min t·poSSI e size. measurements are shown with the image. Widely differing size deter cation methods, and particle shapes: a) tellurium, milled, acicular, b) Iron alloy, argon
a Ions are POSSIble d dl , atomized. spherical with aggtomerated fines, c) tungsten, gas reduced, polygonal aggre
difficult epen mg on the Size parameter used and the shape. Shape is a
: t,,· sary tor~~:;:; t~ m~asure. Usually a simplifying assumption for the shape is neces
e Size II1formation to a single parameter.
ga!es, d) tin. air atomized. rounded and IIgamental, e) Iron alloy, centrifugally atomized.
'. ,
(COfIt1nuftd)
28
POWDER MI: IN..LURGY SCllNCl 1'( 'WI '1 I . 11·\1,··\, 111.'11/\111 IN
Figure 2.2. The projected image of a rounded but irregular particle. Six possible mea
sures of the particle size are shown. three of which are based on projected dimensions
and three of which are based on equivalenl spherical diameters. .
This chapter introduces a hroad spectrum IIr tests as an armamentarium for asscssing a
powder. Such characterization of a powder is an important aspect of powder production.
research. product. development. process control. and property optimization. As a rule.
tests should be applied selectively to measure the critical powder features.
17 2.4. 10 17
Irregular, h) palladium, eIecttoIytIc, sponge, I) nickel. carbonyl decomposition, porous and 0.01 7.0.10 9.9·10Ih
cubic, D 'Ironbued metallic glass, CN5hed ribbon, angular plates. k) titanium. sodium 1.0 7.0.1011 2~~. 10" 9.9·10'fl
reduced and milled, lrreguIar,and I) niobium hydride, milled, angular (photograptu cour 2.4· 10~
1000 7.0· 10~ 9.9· 101
tesy of P. Hugo, D. KubIah. T. S. WeI, R. iaeecea, and J. Murray).
30
POWDER METALlURGY SCIENCE
~..
taken from a moving stream, not from stagnant lots. A major problem arises if the sam powders, especially those below lOO..,n, will ~ibit suffICient capillary rorc:cs to.lpan.
pleis taken after shipping or after experiencing other forms of vibration. In such cases, it raneously agglomerate with water contenu of t~ by. volume (as liule as O.l~ by':
is important to blend the lot before sampling so that settling effects are ·minimized. The weight). The capillary forcf actually increases as the meinure content decreases.
sample should be taken from maay points. Lowest sampling errors occur through the use Consequently, polar molecules are used u dis~rsant(with smaller powders.. These polar.
of a rotary riffler, which divides a flowing powder into rotating containers. If a static mo'ecules typically <Irecarbon chains with charged anwn'icor cationic terminal gtoups.·
. sampling procedure is necessary, then many small samples taken from random locations scch as hydroxyl (OH·). sulfonate (SO)'). sulfate (O~O):). andl1:Jllmonia (NH/). Shear: '
eters: avoids bias. No matter what approach is taken, it is necessary to critique the possible forces are effective in conjunction with the disPersant indeagglomenuing fine powders. ..
sampling errors and their effect on skewing the measurement of powder characteristics. The shear can be delivered using ultrasonic agitation ~ intensive mixina.
Dividers or thieves that take multiple random samples aid that task. Sample quality is
highest when it is a blend of several small specimens taken from a moving powder
The internal energy of a material is temperature' dependent, but ~tially ilis
stream, such asa conveyor belt.
Most metal particles are cohesive because of their small sizes. Thus, they are not easi
independent of the surface area. However, ,!,he interfacial coeri)' ~CI with the .. ~:
size of a particle. Consider the size scale where ihc i~terflClal enctJ)' eqUJ:ls.thC
ly dispersed. Although van der Waals forces are small, adsorbed moisture causes particle
,'.
'.internal energy for a particle. For gold, the interfacial enc:raY is ~ product or the·
agglomeration. (Adsorbed surface films are loosely bound to a surface, in contrast with
specific surface area times the surface energy .r. At room temperature, the internal r
,
Ie mea
ensicns absorbed films that are chemically attached and are difficult to remove  water forms an
energy of gold is approximately 600 MJ/m and the surface energy is approxi~
adsorbed film on stainless steel, but chromium oxide is an absorbed film.) An agglorner '
mately 1.4 11m2. Equation 2.2 can be solved for the' particle size where the internal'
ate is defined as a cluster of particles held together by weak forces that can be overcome
ssing <J and surface energies are equal. giving
by a stress much below the intrinsic material strength. An example of an agglomerate is
uction,
dried mud, which can be crumbled by low stresses. In contrast, an aggregate can not be
a rule.
dispersed easily since it is a cluster of crystals or particles held together by strong bonds.
~ = 6 r! D.
such as cementing agents. The concern here is with dispersion of agglomerated particles.
The solution gives a particle size of 14 nrn, which corresponds to approximately'
A particle represents both internal energy (that scales with the particle volume) and
150,000 gold atoms. At this size. approximately O.3%.of the atoms I1tC on the par
surface energy (that scales with the particle surface area). Let Er represent the total ener
ticle surface, but the disrupted bonds as~atcd withlhose atoms contribute SO%
msider gy, V represent the particle volume, and A represent the particle surface area. Then the
cf the particle energy. In a nanoscale powder, it is ~t1mated that the first five Jay,
;ample total energy is a linear sum,
ers of atoms exhibit disrupted bonding. which corresponds to about '2~ of the
mxtru.
article
e; = YA + ~V (2.1 1 atoms for the 14 nm gold particle.
nsily). . : l.:· r
where is the surface energy (J/m2) and ~ is the internal energy (JIm"). Assuming a
rl..:s of sphere, the area will scale with the square of the particle diameter D and the volume will
t gr<J1ll scale with the cube of the diameter. Thus, the energy per unit volume is effectively a
measure of the cohesive potential per. particle, expressed as, Particle Size
. ,
EIV = ~ + 6 rID [2.21 Particle size is a determination of the dimensions of a particle. The size of a particle.
depends on the measurement technique. specific parameter being measured, and particle: "•.
~ecause the energy per particle scales inversely with. the size of the particle, the driving shape. Particle size analysis can be achieved by ~y or several instruments which USUAlly. .
~~ for agglomeration becomes larger as the particle size decreases. That creates a sig do nOI gl~e eq~ivalenl determinations due t~di(ferences in the measured ~fllSlef5;; .
: ~cant problem in powder characterization because an agglomerated small powder will Most particle Size analyzers use one geometncpararneter and make the assumpllo~ of a,
s' Improperly assigned a larger particle size than is representative of the actual powder. spherical particle shape. The basis for analysis ca{l be any of the obvious geometric: val~: .
ince ~any processing attributes depend on particle size, improper characterization can ues, such as surface area, projected area, maximum dimension, minimum crosssectional
create,dlffiCulties. To characterize a powder for size or other attributes requires that it be area, or volume; Particle size is probably Orlc.p! the n:lost important characteristics to the :
prot.perly dispe~, which becomes more difficult as the particle size decreases. Surface er metallurgist. Size data are most use(ul when presented within the context of the
. ac
to rve agents can great I'y in f1uence power
d co hesi
esion or diispersion.
. Th us, th e nrst
 .
step IS irernent basis and the assumed particle shape.
pa~~ove adsorbed moisture or other agents that cause particle agglomeration. For large e example size parameters are diagrammed in Figure 2.3. For a spherical particle,
. ICes that may be sufficient for dispersion and accurate characterization. Smaller ~the s is a single parameter. the diameter. However. as the particle shape becomes more
32 33.
1'()wt)~ll MEIN.LUI~u'( ~LI~Nll I't 1\v11I1,',11!\1.:J\llllilLl\lIUN
complex, the difficulty in defininga single size parameter is obvious, Consider a plate Table 2.2. Comparison of Particle Size Determinations for the Particle Shown in
or flakeshaped panicle (Figure 2.3b):. at least two parameters are needed to fully figure 2.2
describe the size: Diameter and width. As the shape becomes less regular. the number of
possible size parameters increases. For the rounded shape in Figure 2.3c. the size can be Measurement Value
described in terms or the projected height (random). maximum Icngth. horizontal width. linear measures
equivalent spherical volume, diameter of a sphere with an equivalent surface area. and so projected height 1.00
•
on. For the irregular shaped particle shown in Figure 2.3d. there is great difficulty in
defining a single panicle size. Since the size depends on the attribute measured. it is
projected width
maximum cord length
"
IV
I'vI
0.72
1.03
common to find disagreement between the particle size distributions obtained by many
equivalent spherical diameters
different instruments. Usually a spherical particle shape is assumed and the size is given
projected area 0.76
in terms or a single parameter, the diameter. The use 'of scanning electron microscopy
surface arca ' 1.45
provides a mechanism for demonstrating how well this assumed shape relates to the actu
volume 0.95
al particle character.
It is important to use a particle dimension characteristic of the powder. The particle in
Figure 2.2 illustrates the approach. The size may be given in several ways. Equivalent thus.
spherical diameters are generated from values such cis the projected crosssectional area DA = (4 At tu'" 11.41
or particle volume. Table 2.2 lists the results of various measurement tech1iques for
comparison. The maximum horizontal width W is termed Ferer's diameter.'~ similar Alternatively .. for ;1 measured volume \ ', the equivalent spherical volume diameter D, is
parameter is Mvtin's diameter. which is the particle width me~sured on the ~orizontal given as, '
bisector. The muimum cord length M and height H are. equally viable measurements of D" = (6 V I iu'" 11.51
particle size. For nonspherical powders, these measurements aredependent on the pani
cle orientation. ' " If the external surface area S is measured. Ihcl1, the equivalent spherical surface diameter
The equivalent spherical 'diameter can be determined from surface area. volume. pro D, is simply.
jected area or settling rate _measurements. For example. the panicle in Figure 2.2 has a D~ = (5/n)ll.' 12.61
, projected area A. The equivalent spherical projected diameter DAis calculated by setting
the projected area equal to the equivalent area of a circle, It is possible to combine such mcasurcmcurs 10 form ratios as new coefficients for shape
and size., "
, A = rtD/14
'
(2.31
I
1
\
w
~I For a cubic panicle with a size of I um as measured on each edge the projected
(0
area A. surface area S. and volume V give the equivalent spherical diameters,
A = I 11m x I 11m = I (urn)? .
,
,
H 5 = 6 r\ = 6 (um)?
V = 1 urn x I prn x I urn = I (urn)!
34
POWDER METALlURGY SCIENCE
... ~  : .
12.41 A wetting liquid causes agglomeration of small panicles because of the strong
capillary force at the panicle contact. For example. the capillary force between a guish the actual particle size and shape. One technique (or dhpersing II microscopic sam,
iamctcr D, is
panicle and a flat substrate depends on the wetting angle and quantity of liquid. pie is to mix the powderwith a 40% naphthalene and 69% camphor eutectic composi
but approximately equals. . tion. This mixture melts at 32"C and can be easily mixed with powder (or dispersion on II
12.51 mounting slide. Subsequently. the eutectic is removed by vacuum sublimation. leaving
F" = 5 Dy the panicles dispersed for observation. .
'ace diameter
where F" is the capillary force.' D is the panicle diameter (assumed spherical). and Intelligent discrimination between single and multiple panicles is a common problem
y is the surface energy of the liquid. Consider the panicle size where that force in particle size analysis. Counting two or more small panicles as II large panicle will,
12.61 will equal the gravitational force on the particle. The panicle would adhere to the skew the distribution toward the coarse sizes. This. is significan: since processing
top of a container. The gravitational force on a panicle is given as the mass times response and final properties arc sensitive to panicle size. Improper size measurements
mx for shape
acceleration: will give false indicuticns. There are problems with measurements dependent on pOlnfde
orientation. Generally it is preferable to rely on parameters which lire orientation inde
F = re DJ ~ P 16
.1:. • III
pendent. The equivalent spherical projected diameter D~.OlSshown in Figure 2.2. is par
where g is the gravitational acceleration. D is the particle diameter. and P", is the ticularly useful for such measurement.
projected particle density. Combining the above two equations and solving for the particle
ers, size gives the critical condition where the capillary force equals the gravitational Screening
force. Screening is a common technique for rapidly anulyiing panicle si,le. A square grid of
evenly spaced wirescreates a mesh. The mesh size is deterrnined by' the number of wires
D = [30 yl (re g Pm)JII1
per unit length, The opening ~ii'.e varies inversely :~ith the mesh size: large mesh sizes"
If the fluid is water and the solid has a density of 10 g/cm\' then the surface imply ~Illall ~pening sil.e~ and vice v~rsa. Th~ most common convention (o~ spe.ci(~ipg
energy is 0.07 11m2 and the critical panicle diameter is 1850 prn, indicating a large mesh size relies .a." .{he number of Wires per inch. For example, 200 mesh implies ~OO
panicle. The calculation demonstrates the difficulty in dispersing metal powders wires per inch. or '1'27 urn between wire centers. For thllt mesh. the wires are 52 11min
when they have adsorbed moisture films. diameter. thus. the remaining opening size is 75 prn, Mesh sizes cannot go to v~ry small
opening sizes. Consequently. the screening t~~£lique is usually applied on.ly to panicles
rtiele can larger than 38 urn. There arc electroformed meshes available down to 5 urn, but agglom
the para. eration and particle adhesion to the mesh generally make the smaller electroformed
Obtaini~g a dispersed sample for image analysis is a major problem. Frequently. screens of lillie practical use. The opening sizes for the standard series of screens appears
agglomeration or coincidence OCcurs as shown in Figure 2.4. making it difficult to distin in Table 2.3. That screen series has openings nominally spaced at a ratio of the fourth
~ 36 ]7
" .
Tllble 2.3. Standard Sieve Sizes interval pcrccnt calcul.ucd I'm each \1/,' 11;1,·lillll.1\ fully automatic cycle is possible. The
mesh size powder passing through a mesh is designated by a  sign and that retained on a mesh is
mesh size opening. 11m opening. 11m
i • c
designated by a + sign. For example. 100/+200 mesh powder would have passed
'1 18 1000 100 150 through a toO mesh screen but nOI a 2nn mesh screen and would be between I SO and 75
20 850 120 125 pill in size. By convention. powder h<.:lllw.JS um (325 mesh) is termed subxicve powder.
25 710 140 106 Although screening is the most widely used size analysis technique. il is not without
30 600 170 90 its problems. Screens will have from .Vir, 10 7'/()'pcnni$sible variation in average opening
II 35
40
500
425
200
.230
75
.03
size as a manufacturing tolerance. Further. individual openings can be up to 50% larger
than the prescribed mesh size. That creates a softcut point rather than a sharp division. A
45 .. 355 270 53 common problem is overloading. especially with the smaller screen openings.
50 .300 325 45 Overloading blocks the mesh openings. thereby inhibiting powder from reaching the lim
60 Z50 400 38 iting screen size. Hence, the size dal;1 arc skewed toward the cOflrser panicle sizes. The'
70 ... .,211 450 3? problem increases with the arnouru of powder per unit screen. area, content of fine parti
80 180 500 25 cles." and SID'Il\cr screen openings. Another difficulty results. from the differences in
600 20 screens and techniques. In general. with any powder an R% error can be expected in a
screen analysis if the screens and techniques are not fully specified. The difference
root of two (in the ratio 1.19). between results can be. reduced 10 approximately 4%. if the.screens are the same.
Screen analysis begins with 11 !>IaCIcof screens with decreasing mesh openings. As Differencesas.small as 1.% can be achieved if full control is e.xercised over the analysis.
illustrated in Figure 2.5. the smallest opening size is at the bottom. The powder is loaded Thus. it is pointless to ascribe better than I % accuracy to a sieve analysis. Defects in
onto the top screen arid thescreen staclc is agitated for a period of 15 minutes. For pani screens will allow oversized panicles In pass. Also. too long a screening dural ion may
cle size analysis •• sample size of 100 g is usually sufficient when using 20 em diameter result in the panicles breaking into finer pieces. Too short.a screening duration will give
screens. After vibration. the amount of powder in each size interval is weighed and the insufficient time for fines to pass all the way through the screen stack. Because of those
difficulties. it is important to use standardized lest methodologies.
InItial
The following test results were obtained using sieve analysis with two sieve
. (1009) .'.
sets and 100 g samples from the x.unc powder 101.
f'.:~ ..
. ......lI~_
•
set I
....
mesh size ill1
. Increasing
mesh,
+20
20/+30
30/+40
0.5.
2.\.2
17,6
0.4
16.1
·24.7
".
,,:;
final
.... pan«
decreasing
particle
size
40/+50
50/+70
70/+100
100
26.5
·1X.4' ..
.•. t, ••., ·•.
7.5
6.3
26.2
18.5·
7.7
6.4
Note that the samples may not be totally random. However. here the cumulative
* motion
particle size distributions (obtained by adding the retained weightsjare very simi
lar except at the 20/+30 and 30/+40 mesh points. That indicates the possibility
that the 30 mesh screens were significantly differerU!~An appropriate next step
would be to inspect both 30 mesh screens for damage (rips or oversize openings)
Figure 2.5. Sieve an8.tysis relies on use of a stack of mesh screens of progressively
and to repeat the analysis with a calibrated 30 mesh screen,
smaller opening sizes (~r mesh numbers) for capture of particles based on the pro
jected cross sectional siz.e •. "
38
l?
POWDER METAllURGY SCIENCE
f,,,,,,,,, The Screening is also useful in obtaining sized powders. This procedure is termed classili
cation and is used to tailor size distributions. In several applications the ability to process buoyancy
on a mesh is force
a powder is dependent on controlling the particle size. Consequently. screening provides
ave passed
a means for removing specific size, fractions.
I 150 and 75
CV\! powder.
Sedimentation
t ~ FV
" '.'
40 ~I
PO\.VDER METAlliJRGY SCIENCE 1'( )WI '11.' f "'\",''' III,VAIIC IN
,
A~ with all panicle sizing techniques, size analysis by sedimentation is nut without it~
error sources, First, the basic approach is limited to a narrow size range with some flexi
.
To demonstrate the limiting sizcIor sedimentation analysis in air for tungsten \
bility possible through adjustment of the acceleration and fluid viscosity. However. for
powder is 17 urn. combine Stokes law with the assumed maximum allowed \
particles below I pm slow settling and turbulence (thermal gradients) can make it unrcli
Reynolds number or 0.2. Solving I1clIl1Stokc, law and the Reynolds number equa \
able. The upplicuiion of centrifugal forces in thcrmalty ivol.ucd cluunbcr, ha" been uvcd
tions for velocity and then cqu.uinj; the IWI! velocities gives.
with success in some laboratories. That has allowed extension or sedimentation tech
niques to panicles a.~ small as 0.01 ~111. Certain particle characteristics can be qui.c trou f) 11141\ =118RNll'I(~p • J to r))/"
I
III
blesome. Intemal porosity in the powder decreases the mass. thereby causing slowc.: par
where D •• " is the maximum particle size, N,\, is the Reynolds number (assume the
ticle settling. For irregular panicles. the size parameter is somewhat difficult to visualize
lower limit of 0.1). 1) is the fluid viscosity (I,R· \O'~ kg/m/s).!: is the gravitational
slnce settling depends on the hydraulic diameter. Furthermore, an irregular shaped pani
constant (9.8m/s1). p, is the fluid density (1.2 kg/m'), and POll is the metal density
cle may not take a ,tmight trajectory: hence its nonconstant velocity and uncertain path
(19.3· I O~ kg/m'). Solving the above equation with these values gives D of' 17 ,I
length hinder accurate sizing. Foreknowledge is necessary (appr?x,irrate particle size and
prn. If water is selected instead (viscosity or 10'" kg/m/s and density of I03'kg/m").
panicle density) before setting up such a test. In those cases of an unknown powder.
then the upper particle size increases to approximately 27 prn.
mixed powders of 4iffering densities (for example copper and tungsten), or newly syn
thesized powders, those parameters may not be known.
There are mathematical limits to Stokes law. The derivation assumes that viscosity
controls settling. but this breaks down when thc Reynolds number RN increases over
approximately 0.2. In term~ of the settling parameters. the Reynolds number is given as.
powder
feed
{2.12\
rotating
disk
Also. the panicles are assumed to reach terminal velocity rapidly. These factors usual
Iy limit the technique to particle sizes below approximately 60 prn. For exarnpic, the
maximum"'panicle size for aluminum (density 2.7 g/cm.l) settling in air is about _'\5urn,
while for tungsten (19.3 g!cm·'). settling in air it is about 17 prn, The container walls
should not interact with the particles during settling. The particlepanicle in.eruction air __ 1 , f
must be zero: consequently; concentrations should be kept below one volume percent . flow t
with no agglomeration. Finally. the fluid and powder can not react chemically. so combi
nations such as iron powder in water are not advised. In spite of these several ditficulties,
sedimentation techniques are in use for several powder systems. such as th~ refractory
metals. '
Elutriation applies to sedimentation techniques where the fluid flow is in the opposite II I :::: air
direction to gravity. This variation of the sedimentation technique provides a means of
generating panicle size distribution information. as well as separating a powder lot into ~ ~
.,,.. .• ~~ •.•  •.•.•. e..J
[[[[1' ••....• _ .•..•.• ;1t ..
~ ~ flow
sized fractions. The greater the fluid flow rate. the larger the particle size carried away by
I I ~"'"
A\
• .> ~ disk "" •••
the flow.
Another variation of the sedimentation technique is air classification. Air classifica
tion achieves a separation of powders into selected size fractions using a cyclone or a
ifj t ::::
II..
:::: fine't
. coarse
"It
r>.
spiMing disle. (up to 12.000 RPM) and a crosscurrent air now as shown in Figure 2.7.
Tfle centrifugal forte provides a constant panicle velocity, while the .air flow achieves dll/fder
size separation by Stokes law effects. Figure 2.8 sketches how the particle trajectory is
aligned intermediate between the fluid flow and drag force vectors. Differences in the Figure 2.7. Particle size separation based on air classification of a powder using a rotat
deceleration of panicles exiting from the disk are based on the particle diameter and ing disk and constant air flow. The smaller particle sizes are separated from the larger
sizes based on the centrifugal terce and air velocity.
42
powrXR ME1Al LlJJ.:tiY \ClLNC I
ungsten
t~put!rp
". "0'
J:
~ ~I~W ~ .~','
J/owed powder . ..
. ..
Q
. \ ~'
:
er cqua feed
particle ce~~;~~gal "
~. .
" .. '
. ,',
rrne the
~ trajectory . : .....~ .
drag
tationa! force ,':. '
enxity
• of' 17 . I
Figure 2.8. The particle trajectory in air classification depends o~ h~w the particle
Will'). responds to the combination of centrif~Qal an~ viscous drag forces. which In turn depends
on t~e particle size and mass. . . ." ~·1··· '." . '.
mass. Consequently. lighter or smaller particles are deflected by th\! air flow and separat . ,',.
ed from the larger particles. Control of the disk rotational speed ana air flow velocity. sample
provides the means of altering the particle size separation. Air classifiers are generally cell
applicable to the size range from I to 150 prn, although the actual behavior varies with
the inverse squareroot of the material density.
',:i
Light Scattering Figure 2.9. The principte of particle siie analysis using. forward laser light scattering~'Th~:~: /.,
",' In streaming techniques for size analysis. particles are dispersed in a moving fluid. powder is dispersed and fed into the sample cell wherescatte,ring takes place, The defec.:; <,.'
Size determination ..is based on a discontinuity in the fluid strearridue to the presence of tor system measures the angular'intensity tor subsequent computer calculation 01 !hElper.· .
the particles. With careful instrument calibration, the discontinuity size can be related to ticle size distribution. . . . . '.:. . .'
.~.'
particle size. Most devices are highly automated. so particle size analysis by streaming is ')'
popular, but expensive. Streaming methods provide a large dynamic ratio; the ratio of the
largest to smallest particles that can be measured simultaneously. In modem instruments 'detector
"Iens array
.
relying on multiple detectors. the dynamic ratio can be as large as8000. There is. howev
er, a minimum particle size that can be detected. _ .
A versatile streaming technique available for analysis of particle size is based on light incident
scattering. Low angle Fraunhofer light scattering using monochromatic (laser) light and
laser beam
••• ; .' .,.
 ..
..".,:. 
dispersed particles is widely used for automatic size analysis. Particle size affects both
the intensity and ungular extent of scattering. A fluid stream with dispersed particles is
.
~:
small"
. 
large .........
passed in front of a detector system, such as diagrammed in Figure 2.9. The data rclati.tg particle particle
t~ panicle size are collected using a photodiode detector array. With coherent (laser)
h~ht the angle of scattering varies inversely with the particle diameter. as illustrated in
Figure 2.10. The intensity of the scattered signal varies with t~e square of the particle Figure 2.1 oj Small particles provide a wider scattering angle than large particles, giving a
basis for particle size analysis based on laser light scattering.
diamete, Computer analysis of the intensity versus angle data will determine the particle
SI2.edistribution. Depending on instrument design, the dynamic ratio can range from 30 *(. '. .
~o 5~. far in excess of most other automatic instruments. Fraunhofer forward scattering tion is difficult, but can be: mi~imi2.ed by proper dispersion and ultrasonic deagglomera
a rotat_ IS typically applied to the I to 200 urn size range. The smallest particles should be at tion. The technique is in widespread use because data 'collection is easy:
e larger leas~ twi~e the wavelength of the laser light for detection. As with other approaches to Mie scattering is applicable to particles generally below 3 11m and overlaps with
particle Size analysis, the particle shape is assumed to be spherical. Detecting agglornera Fraunhofer techniques. Here. the detector is located at 90" with respect to an incident
 ,.:..__._.
44 4~ .
POWDER ME1N.LURGY SClENCl ,'( )WI)II·:,It"I:", II I;I/A/I(IN
light beam. Consequently, both detectors can be incorporated into one instrument to
expand the dynamic ratio during. an analysis. Modern laser light scancring inxtnuncrus combine 'various light sources and
Another light scattering technique uses the Doppler frequency shift. associated with detection techniques to give dynamic ratios of 7000 (0.1 to 700 urn) or more.
moving particles. For huge particles. the sample is dispersed in air' and accelerated Consider this range in terms of the number or particles, The mass of one spherical
through u nozzle into a partial vacuum, initially propelling the panicles at nearly sonic panicle at 700 um equals the m;I~' or 3.4 . 10s particles at 0,1 !lm.'ln terms or
velocities. As the particles slow. twolaser Doppler shift readings are made to extract the familiar size scales. a ratio or 7()()() Icngth, to I is the same as i4 ntm out of I km
time of flight and estimate the particle size. The approach can size panicles between 0,5 or <} inches out or r mile. The nonual ruler has an accurate dynamic ratio of 300 .
.and 200 JIm at count rates of I()~per second. that is I nun increments in a total length or JOO nun.
For smaller particles, the thermally induced random motion. known as Brownian
motion, provides sufficient velocity for sizing the particles. The StokesEinstein equation
gives the relation between the particle diameter D and, the translational diffusivity DT as
Electrical Zone Sensing
follows: '
The electrical conductivity or ;1 fluid p;I""1g through ;1 small aperture in all iusul.uor
provides a method of measuring the number alld size or part ides suspended in the fluid.
12,13\
Conductivity mcasurcmcut is achieved I", 111;lkillgthe fluid conductive and applying ;1
small voltage across the opening. A COIlIIIlOIltechnique for measuring blood cells. it call
where k is Boltzmann's constant, T is the absolute temperature. and 1] is the fluid viscosi
he applied to sizing powders, The main katllrl'~ or the d~vicc arc shown in Figure ~,12,
,ty. In a size lUUIly~istechnique termed photocorrclationspcctroscopy. laser light is used
to detect the Doppler frequency shift of particles in a fluid. The approach uses an internal
beam splitter for calibration as sketched in Figure 2,1'1. Over the panicle size range from
I approximatety 0.00510 ~ .prn, the reflections from the particles 'give frequency ,hif:s
(rom 1000 to I Hz, depending on the inverse of the panicle 'size. TIle,' intensity versus ire
.quency information is collected over a period of minutes. The output is analyzed to
deconvolute the particle slze distribution from the signals. To use that approach one must
: know the optical properties of the fluid and panicles, fluid viscosity, and temperature. to pump
... The advantage is it's applicability to very small panicles with few assumptions about the
tttt '
.
inherent particle size distribution.
• . '; '""e.
•
~ . ::::0f" ~
scatterIng • !.. • aperture
r+sampl~ cell ~./
partIcle
fluid
electrode
•
•
particle
•
•
., .: electrode
~
~
partial
..............,
'"" electrolyte
•
photo reflection '"' ,
detector
FIgure 2.11. Very ~ particles undergo Brownian motion in a fluId, the velocity c'! the Figure 2.12. The principle of partictesize analysis using electrical conductivily changes in
motion provides Infonnatlon on particle size as measured by the Doppler shift of .:I laser a small aperture zone due to the streaming 01 particles dispersed in an electrolyte flowing
OO~. . through the insulating aperture.
46 47
POWL>ER MEiAlLURGY SCIENCE
higher dcusity materials xuch ~IS iron and tungsten. For tungsten powder. the technique is
)un:es and limited to particles below 6 urn. Another difficulty is maintaining 11 low powder coneen
, or more. tr••tion to avoid coincidence (multiple particles) in the aperture. Experience has shown
sphcri<.:al lIuld the instruments are susceptible' to electrical noise and aperiure 'plugging by agglomerates ~.
1 terms or flow or large particles. Generally. better results are obtained.fer low density materials (such u.~
III of I kill ceramics and polymers).·
io or 300.
Light Blocking .; ..
Particle size analysis based on light blocking iOimilJir to electrical conductivity and'.
is another variation of streaming analysis, A light beam is' interrupted by a now or dis
current
persed particles a~ shown in Figure 2.14. As a particle passes in front or the window. it ..
partially blocks the light reaching the photocell. Assuming a spherical particle shape. the
an insulator amount oflight blockage is equated to an equivalent circular crosssectional area. The
time (expanded scale)
in the fluid. dynamic ratio for the technique is 45. The lower particle size is determined by the optical
cI "pplying a resolution. with I urn being typical. Particle dlspersion in the fluid is important to avoid .
~ cells. it can inf coincidence. Measurements are similar to those obtained using electrical zone sens
Figure ~.I~. current ing techniques in terms of both problems and ·Iimitations.
X·Ray Techniques .. .
time Two xray techniques call be applied 10 size analysis of very small particles. .'
Diffraction line broadening for crystalline materials. has several causes, including. strain .
Figure 2.13. An expanded view of the aperture from Figure 2.12. The streaming fluid car
and small crystal size. The destructive interference from the crystal is not complete at ,
ries a particle through the aperture. During passage, the particle reduces Ihe current in
proportion to its volume and provides a basis for counting and sizing. angles slightly off the Bragg condition. .·1
of the distribution. Particle settling in the outer chamber during analysis causes the data
to be .skewed to the finer particle sizes. As an empirical rule, the electrical zone sensing wlndows . ~
techOlque is only valid when, . . .. .~••(j
,·r· .'.

if changes in
D (p~ . P,Y'} < 500 . 12.141 time . J.,
olyte flowing ~~:~ D is ih.e particl~ diam~ter in }l~, P., is the theo~etical d~nsity of the. powder in FigL're 2.14. Particle size analysis based on. light blocking, where the Interrupted light
.: .and P,IS the fluid density, also In g/cnr'. The particle settling problem IS acute for beam is used to size and count particles based on their proJected area,
'i>OVmr·r.
~
....•..~.,....
¥ll ~ lUI~t', Y \( IL Nt I
.. 
1"'\\,1111., 'I I"l 1111."\111" J
xray traced directly 10 Ihal assumption. Because (If the differing physical attributes tested hy
Intensity each technique and the assumption of a~phl'ril'al particle.shape. the various size analysis
techniques will yield very different rculr, Oil '<line powders. Table 2.4 and Figure 2.10
provide comparisons of the several technique available for panicle size analysis and
give the approximate size range of upplicabilitv. dynamic ratio. approximate sample size,
B = broadening approximate analysis lime. and basis for the distribution (population or weight). The fig
1
Imax
ure and table generally reflect the best posxihle measurement range obtainable
powders. Often . larger panicle size ranges or dynamic ratios are claimed. bUI nOI demon
for metal
strutcd with the denser metallic panicles and the courser panicle sizes. With respect 10
relative cost, automated instruments arc expensive. In the simplest sense, an accurate
panicle size analysis is possible uxing simple instrumentation and basic physical princi
ples (for example with a watch and water filled graduated cylinder). The selection of a
technique depends on several factors including availability and approximate particle size
range.
" .. so '>1
"I .,:
. .' ;..
POINDER MF.TAlLURGY SOENCr
rn i~ rnixvd
r I )1111) lilL' ..
by dividing each increment by "ilie: .toti.I.~ple
.;
Table 2.4. Comparison or Particle Size Analysis Approaches ~ntages weight. The histogram (or
I measured
these data is generated b.y plotting the incremental percenta~ venus the screen opening
,ing the dif size dynamic sample relative
technique size. Sucha plot ;s given in Figure 2.17 for the data frdm 'Table 2.5. Notice (or chis plot'
range. jim ratio size. g speed· basis"
e., the particle size is converted to a log scale. thereby. miXing the increment widths equal.
microscopy
12.'171 optical In most instances. metal powders are found to ~xhibit a bell shaped curve (Gausshln or ' ..
0.1l and up 30 <I 'S P
electron 0.001400 30 <I S P
icd 10 pari i· sieving (wet and dry) Table 2.5. Example Particle ~ile Dlstrlbutlon Data
uk broaden wire mesh 38 and up 20 100 I w mesh opening weight' '. interval cumulative
niquc givcs electroform 5' 120 20 >5 S w size ~m retained. g percent percent
sedimentation
IlC the size gravity 0.2· 100 50 5 I w 70 212 0,0' . 0.0 0.0
by a small
centrifugal 0.0210 50 I s w 80 180 1.1 0.9 '. 0.9 ..
light scattering
.. . 2.5, '
••••• Il:=j
electrical zone lensing
Brownian light scattering
15 ' ,.. 
ical princi • velocity ilgh! scattering
eCliol1
,mick size
of a
•
•••• II1Mle light scattering
Fraunhofer light scattering
10 ' . screen 
__ I centrifugal sedimentation analysl1
I
r_Igravlty sedlmantatlon
electrofcrm sieves
5 '  ,,
iSlribUlion.
wire mesH sieves
electron. microscopy o
10 100
rh 1000
0.001 ' optical microscopy
rhe amounl 0.01 0.11 1 :i'fO ""'''100 ····1000
nlclc size.
particle size, um
.,..
particle 8Ize,~m
led on each
neremellIul Figure 2.16 A co . Figure 2.17. A histogram plot of the screening data from.TabIe 2.5 with the particleSIze
ful size ranges
. formpara!' I of particle
'. size.anatysls techniques and the nominal use .
52
axis en a logarithmic basis. The most populous size Is termed the mode, her& It Is
between 75 and 90 urn,
t
53
_____ ...:. .__ '_'1 _JW_'_" r,.• II,W,\, _'_"_"_/A_'_'I_IN _
PowoER METmURGY SCIENCE
size intervals), Finally, the standard deviation a is calculated from thc arithmetic mean as
cumulative percent finer. follows:
100r.~wt~~~ 12.201'
a= II /IN)!: n,: \.,. l) .....: I"!
75 Basis lur Plots
An analysis determined by micr\l~(lIp) techniques giws the pupulution of p.miclc,
versus their size. However. an analysis taken by sieving techniques provides a weight
50
distribution. It is important to state the hasis for plotting particle size information.
Consider the difficulties ill comparing tW(I ~ets of data on differing bases. The weight
2S distrihution is skewed to the coarser particle sizes in comparison to the population based
. distribution. The particle size data from Figure 2.1 X have been replotted in Figure 2.19
.0.L_......c::J1:::...L...l ....J t ••. ,
along with i1i~'population bused distribution for the same powder. The obvious differ
cncc in placement of the two distr!I)\I~~o'.l~c;.~,.lhe seen in comparison of the median sizes
10 1000
(72 IIIll VcTSUS' 12 um). For any partil'ic Sill'. ';I~suming a spherical shape allows calcula,
tion of the number (If particles 1/ kunwin;; till' weight \I' and thcuretic,tlllletallit:llsity I~",:'
Figure 2.18. The cumulative particle size distribution plot lor the data in Table 2.5. The 1/ = (I \II I (P .., IT IJ') 12.211
arrows Indicate the standard deviations lor the distr;ibution.
where D is tll'e diameter. Direct comparison llf weight ,II1dpopulation based particle size
distributions is invalid.
normal distribution) when plotted on a log size scale. termed lognormal. A cumulaiivc
. particle size distribution is generated by adding the interval percentages and plotting the
result versus the lower incremental panicle size. An analogous distribution could te gen
. crated by plotting the cumulative percent larger than a given size. The raw data trcrtrncnt
cumulative % finer
. is outlined in Table 2.5 while the resulting plot is shown in Figure 2.1 X. The information
100 1
. given in a screening analysis is with respect to the weight of powder larger than the spe I
/
I
cific screen sizes. In Figure 2.18. a smooth curve h~s been used to connect the known I
points. population,'
75 I
On the smooth cumulative. particle size distribution. the median size corresponds to I
I
the 50% value, The mode. particle size corresponds to the most frequent particle size. I
I
I
which ill the highest peak on the histogram distribution. The standard deviation and mean 50 I
I
size can both be calculated by usual procedures. The standard deviation sizes (+ or· one I
I
standard deviation) correspond to the particle sizes at roughly 84% and 16% (more pre I
I
cisely 84.13% and 15.87%). , 25 I
I
For histogram data; the ari.lhmet'ic mean size D ",., and the geometric mean size. D x'" arc I
I
I
calculated as follows: . . ,. I
0 '"
10 100 1000
I~.IX}
particle size, IlITI
S4 55
POWDER METALLURGY SCIENCE " IW! JI,.;IIINW II J.V J\IIOl'f
. ;.
ithmctic mean as
. Common Distributions (rilonn<iispcrse). The t"ypi\'al pnxluc: is polydispcrsc, ~iih II wide rall~~:uf:Jlartich: lIii'.cs. .
It is useful 10 review some of the shapes of panicle size distributions encountered in Vr;ry special efforts a(\' lll'l'Ik'd tll achieve amonesizcd powder. rllh~.lluently. II median
P/M. TIle typical bell curve' which occurs when 'the interval panicle si·,.e data are ploucd or mean size and the dispersion in particle srze.arene<i:e$S~:tyinform;lIio!l. The disPeisioq,
on a log basis is shown in Figu'ie 2.17. In contrast, the plots in Figure 2.20 show varia is effectively the standard deviation. A common pr3c~ice'in P/Mh io·distillthepart;icle ..
tions including broad and narrow distributions as well as a bimodal distribution (two si:·.e distribution information into three points c!esi~~'icci /)vii D.I!;: and DIU' corres .
iion or p:trltck,
peaks). Normal powder fabrication practices can not form a single sized powder pOmling III the pari ides sizes at the 90. SO. ~and' 10 petceru, paints on the cumulative
'ovides a weight
distribution. . ' ".' , , : / , .',' . , ... . ', ::..
zc information. .:
scs. The weight
Dopulation based cumulative LogNormal SizeDistributions ',' ., ;. z . ..' '~'. ':.
frequency frequency Most powders follow the lognormal form in th~ir .nril.ur.&I.unscreened state. A log! ' '
d in Figure 2.19
obvious differ GaussIan 100 normal size distribution gives a bell curve when die fr~quen~y is plotted on a linear scale, .
he median sizes (lognormal) against the log of the panicle size. This distribution !=ant>edeseribedmathematically .by,·· .',•
: allows culculn, a modified form of the Gaussian probability function,;Let P(x) be the probabilit~ of
% observing a part iclc size described by .r=!I/(si:r ),~iving " , ' .. ':.' "'.
ctal dcnsirv •. /),'/1 :'
% 12.231 .
Figure 2.21 gives a xchcm.u ic comparison of a panicle size distribution ploued on S/:ver: ,
o •....•~.....,..;... al lJa:c:s. The linear scaling shows a skewed particle size distribution while the log seal.:, '
log size log size ing gives the expected bell curve. The cumulative particle size distribution Fix) c!n be
monodlsperse expressed in tenus of the iutcgr.rl or P(.I'} over the. interval (rom 0 to r,
: Ft.r)= t: Ptxtdx
ill
\2.241
 I the frequency and cumulative plots. plot. giving a straight line for the distribution.
/., '1'.'/./ f'. ""f"\' "/.'1/'1/1, f1l
I'OWDl~ M.lllII.tUh'l,n( II NIt
.
I
. ,
standard.
devlatl~~..
d)/""
' plot
log
lognormal ;i,. ,
particle size, ~ m
Figure 2.22.'The Ioqnorrnal particle size orstnbution plot of the data from Table 2.5 using
the standard deviation points from Figure 2.18. . .
that such comparisons (or data transfurm.uionx) are relatively simple. If tl~e slope and
~~~Iog intercept ofa distribution are known. then the other distribution can be estimated by a
translation. In 'transfonnarions. the slope remains constant on a lognormal basis.
FJgure 2.21. The particle size distribution shown on four different bases; a) the frequency Transformation ~f the data requires culcul.u iun of the displacement parameter 8 shown in
versus particle size .on a linear scale. 'b) the frequency versus particle size on a log scale, Figure 2.23. To convert from a weight distribution to a population distribution. the dis .
c) the cul'!'lulative frequency versus log particle size. and d) the lognormal distribution
showing the standard deviations as a function· of the log particle size..
J',' : standard deviations
Table 2.6. The Percentage Points and Stan~ard Deviations on a Cumulative Particle
Siu Distribution POPUlatiOn//!
, ,
deviations percentage
,,,
,
2.0 2.28 median /'
1.5 6.68 a ······················>l················
1.9. 15.87 ,
0.5 31.85
,,
0.0 50.00 /\ s =6.908/m
,/slope=m
0.5 .. 69.15
, ,,
1.0 84.13 ,,
1.5 93.32
.2.0 97.72 x=log,o (particle size) "
Reali the problem of comparing analyses taken from screening and microscopic Figure 2.23. The use of the lognormal particle size distribution to transform from a
'measurements. Screening gives size data on a weight basis while microscopy gi les it on weight to a population basis. The vertical translation distance 0 depends on the slope of
the distributi~n. .
• population buis. One of the fundamental attractions of the lognormal distribution is
;
I placement is upward and the magnitude is dependent on the slope m where D,. is the largest particle size. A similar distribution is the DingerFunk distribb.
1. tion which uses both th~ smallest size Ds and largest size DL•
1) = 6,908'1 m 12,251
j F(D) = (0"  D")
~ 1(;) ··0, \
") 12.lll
whcn the panicle size is expressed on a basel 0 logarithmic scale. I ore, 6.90R equals :I ...
times the loge I O. where e is the basis for the natural logarithm and :I represents the size 'Problems in Particle Size A'"a'Y~is
exponent in Equation 2.21. To convert from a population to a weight distribution. the
There arc several problems with particle siz~ ao~ly~is.lt is quit~. difficult to resolve a:
displacement is negative (downward) with equal magnitude. Once the transformation is
'~id.e ran~c of particle sizes simultaneously during an analysis. Almost all devices·hav~·;i
completed. determination of the median size is straightforward (zero standard deviations
. lir.iitcd size range they can accurately resolve and .l.anatyze at one time. Often thnt Hmiia.,
on the new distribution). On the other hand. mathematical detcrmination of the median
tion results in a realistic dynamic ratio less thap th:e advertised runge. If the particle. size:
size is possible. For a weight distribution the median size D., •. is given as.
distribution is broader than that, the methods are noi.accuraie. Additionally. each tech •. '
nique has a range of optimal uirability, For sieves .. it i~ generally above 38 jJm.,Optical.'
12.261
microscopy is restricted l\l purticlcs aboveupproxlmutely lum. Techniques such a:~scdi.'
mentation arc only applicable l\l a narrow size r.ll}ge :~cause of limltations imPosed'by 
and then the median population size 0 is g~'~:~'as
/1111 •
the fundamental physic».  . .
The particle shape problem was emphasized earlier in this chapter; more on shaPe >
D = /O'lh+oYm 12.271
"'I' . analysis follows in the next section. The more irregular the particle shape.rhe more parol"
meters necessary to size a particle. Most rncasurement techniques assume a srhcri~oll
Ie 2,5using where" is the intercept (the standard de'viation corresponding to the I prn panicle size)
sl.apc, Accurate description of shape and its variation with size is tedious. It is notewor '.'
and 11/ is the slope, The steeper the particle size distribution. the smal!er 1) will be or.
tll:' rh,u shape. like size. is a distributed property or" pOwder.· . ..: ,," ,
alternatively. the closer the median sizes by the two techniques.
e slope and ; In general. the finer particle sizes arc poorlycharacterized .by sieving techniques. Tli~·.
atcd by a limited ;m;t1ysi~ range coupled with a bias toward weight based dimibutions results'ii\:,
Other Size Distributions
rmal basis, disregard for the filler particle sizes. In many instances; the disregard is not \\Iarr~ied.
Generally. the lognormal distribution is the most useful when dealing with metal
1) shown in powders. Others arc sometimes applied to panicle size data. One is the RosiuRammler
sin~e t~e fil~er particle, Il(l'~':'~ the greater su'rface .~rea and kinetic activity. Ai. a ~i~e::
on. the dis~ ' rauo '11 25. It takes 15625 Ill' the smallest particles 10 equal the malls of just one' ontlc':'
distribution. given as follows:
largest pan icles. . .
There arc common problems with automatic size analyzers. The finn is COincidence;"
F(D) = I  exp!D"ID/)
: When more than one particle i~ in the detection zone of IU1 analyzer. they are si~(fas one
large particle. Conscqucurly. the particle size distribution becomes artificially skewet1' .
where F(D) is the cumulative particle size distrib~tion and 0 is a characteristic size cor
toward the coarse particle sizes. To minimize the problem. lower the ccncerurationof
respo~ding to D,l~' the 'panicle size a(::n%' ~;;"ihe di'stributio~.' The exponent 1/ indicates
powders inthe detector wile. For the streaming devices. that requires dilute conceritrl!~:
the W.ldth of thc distribution. A plotting basis takes the double logarithm to give a lincir
equation. . tions of the powder in the carrier tluid. Secondly. agglomeration causes firie particles to'
appear as coarser particles. Dcagglornenuion requires agitation. milling. and chemica)
treatments to maintain particle dispersion. Another problem results from the relativCiy .
log,ofll/!I  F(D))) ;" 1/ log (D)  1/ 10" (0 ) 12.291 <'
'U "'II II h IJn SpeCI'fiIC gravity
. 01. most metal powders. Streaming techniques assume a uniform ~
where 1/ is the s'1ope 0 f t h e p If'ot 0 the left hand Side versus 10gio(D).
, random dispersion of particles in the feedstock for the detector. The measurementscan'
The Andreasen . I . di 'b' . . become qi~~d because of preferential settling of the coarse particles. To aS5u~e mini
. . panic e size istn unon has been linked to optimized packing proper
ties mum error from sell ling. it is good practice to pass the entire sample through the detec
. and IS sorn e t'imes . use fl'u m working. with .. high packing
, density. metul powders. It is
tor. ;t~ .
given as follows: '
Many examinations of particle size analyzers have been performed. Under critical
F(D)=AD"ID" assessment. it appears that the particle size distribution can be reproduced with.a 2 per
L 12.301
cent to 3 percent variation. Figure 2.24 illustrates the cumulative particle size distribution ..
m from a of a coarse spherical iron powder. Between instruments it is common to see at least a
e Slope of
.'
(,1)
.__ .. _ /01
1\)\V()1 II MllAllUI;C,y \(11 Nll . 1'( 1\v1 II ,.', '1'\1"\' II 1I11A III IN'
.\1
~. •.
Q.
.1
..'
;':
\
80 Iron spheres
c!) tear drop'
60 urn
. ~CUblc ~/'
:.\t· sponge or
porous
/'CiCUI,ar
~yllndrical
" ;.''''
'e'
:Jjf~egular
fI.ake
...
··'·~am,ental
~rous
20 . . . :",;
'();iPOlygOnal . .:':
. :":
O~'~~~~~~~~~~
" .
'. rffI:? ~ggregate
10 100
particle slze,llm
V dendritic .: . .~':
.r..;
. "
;",
FIgure 2.24. A demonstration of scatter for particle sizes analysis results using Ihe same Figure 2.25. A cotlccuon of possible particle shapes and the suggested qualitative
powder and seven measurements of the size distribution with four laser scattering descriptors. .
devices. The powder was nominally a 60 101m spherical iron. Note the variation at thp. 0'0
and 010 particle sizes. '
I,
,
:
descriptor is th~ aspect ratio. defined as the maximum particle dimensio~ divided by the
s,
10% difference in the median particle size. and many instruments will disagree by 30 minimum particle dimension. For a sphere. the aspect ratio is unity, while for a ligament I.
percent to SO percent. It is inappropriate to assign high accuracy to panicle size distribu a value near 3 to 5 is more likely. A flake particle can have an aspect ratio in excess of
10. and in some instances can be as high as 2()(). Generally, microscopy techniques are , .
. tions. "'" "
most appropriate for quantifying shape.
Consider the irregular shaped particle diagrammed in Figure 2.26. Various shape l..
~·
: :Partlcle Shape parameters result from the projected image. Particle shape can also be expressed by the
I •• '''~'.: ;
Particle shape inf1uence~ packing. flow. and compressibility, provides information on ratio DjD A' where Do is the diameter or the .outer embracing circle and DAis the equiva
the powder fabrication route, and help~ explain many processing characteristics. Because lent spherical diameter based on the projected area. By far. the microscopy based shape
,iUs difficult to quantify panicle shape, qualitative descriptors are frequently used to con descriptors are the. easiest to understand and arc relatively easy to obtain from projected
. vey a sense of the shape. Figure,t.2S gives a collection of particle shapes and shows the images. , ,
.appropriate qualitative descriptors. A more complex shape parameter can be generated from a profile analysis of a parti
Particle shape varies with size and manufacturing technique, A panicle size analysis cle. If a radial coordinate system were centered inside a panicle. such as in Figure 2.27,
which assumes I constant shape Could potentially have a large error. For many analyses, then a plot of the surface profile could be constructed. The plot might look as shown on ..'0
~ . .a'simple quantitative shape desc~iptor proves adequate. The most straightforward the right in Figure 2.27. The tracing of the surface position becomes a contour in terms
62
POWDER MET.A.l.LURGY SCtENCE
.r
:..... •. ,
....
" ,
,. ,
" particles. Useful because, it often correiates' with ,various ~;and ~etric chara~te'r~
istics. surface area provides. insight into the. powderbc:ha ••• ior·durinl chemical activity.
""~"""
,I , .J', ' catalysis. friction. adsorption. contamination', P.l'eSS~1 i9d Iintuina. However, the sui
, ," t;Dol' , \
;,
,
I'
"....
~ ,
\
Do = diameterof "c;wl~r
face i.ru of a powder lot tells nothing about the dlsttlbut10n In propcrtiea. pqwdcr texture
or :n~ernal structure. So, it is combined with. C)thti'·paramerers as part or an overall
'/
I' , \
embracing circle
description' of the powder. Two main analysis techniquei ror measuring lurface area an:
I
DA = diameter of ctrcle with gas adsorption and s= permeability. ',' '. ' j,
__ ..• uum or inert gas~Jkeout. The clean powder surface Is cxpolCd CO VlI)'inl partial pres
'
'•...... ',' sures of known a!sl)roing vapors. A measurement Is made or the amounl or IU adsorbed
on tho powder surface versus the panial pressure. The mcuUrcmcnl Is often referred to .
Figure 2.26. The projected Image of an Irregular particle and two forms of measuring the as the BET specific surface area, after Brunauer, Emmett ancs Teller who developed the'
size 11'1 terms of the clrcular diameters. concept in 1938. 
,. Under equilibrium. the rate of adsorption equals the rate or evaporation. As illustrated
in Figure 2.28. the BET technique measures the qUJl\llty of iU needed CO saturate the
R powder surface. By assuming each gas molecule occupies a pRelsc area. the surface area
of the powder can be calculated from the adsorptlon behavior. Leuinl P equal tbe panial
nlilalive ~'.
.'
,.;.'
I,
',.
~'.:
;
e
Figure 2.27. A two dimensional particle profile showing one appioach to particle shape .'
tJ by the
ana/yala. The outer particle contour Is used to create a tunctlonal ralation between the
igaillcilt
radial length R and the angle e.
~ce~s of
ues are or the lWOcoordinates. Such an approach to conveying particle shape is a specialized
. /.
pressure of adsqrbale, f" equal the saturation pressure of adsorbate (which depends Oil
\.
signal
the gu and temperature), X equal the amount ofgas adsorbed at a pressure P. X •• equal OUIpUI
the monolayer capacity of the powder (the amount of gas necessary to form a saturated
surface coating one atomic layer thick), and C equal a constant relating 10 the adsorption
enthalpy. give~
time \
Note the linear relation between the term on the left of the equal sign and the par.ial pres·
sure ratio PIP". The BET equatlon is generally valid for powders in the: pressure range
PIP" from O.OS to 0.30. Equation 2.32 can be rewritten in a general form as. flowmeter
thermal
stabilizer \ I
P IIX (PH' P)/. 8 + A PIP" ID:\I ' ...J powder I
bath
where .
Figure 2.29. A schematic drawing 01 a nitrogen BET specific surface area analyzer. A
X:''' (A + 8}'1 ID41 clean powder sample is chilled to a tempera lure where adsorption will occur (liquid nitro
gen temperature in this case). The helium and nitrogen flows are adjusted for a specific
partial pressure .ratio. The gas sample is exposed to the gas mixture. resulting in a
with A as the slope and 8 as the intercept of the linear Equation 2.:\:\. Finally. the specific change in gas thermal conductivity as nitrogen is selectively adsorbed. The area 01 the
surface area is calculated as adsorption peak provides a means of measuring the surface area.
(.7
66
POWDER" Mr TAl It JI~(iY \( II NCI
the partial pressure and adsorption data, a least squarl's analysis gives the slope ;IIHIinter drop is IIII'aslln.'1I III d,'t\'rlllill,' Ilk' pcnlll.'ahility. llsin~ powder pIIRlllily an,llhcuMi~'al
cept. which .gives• X .11'.. densily. Ihl' specific xurt.u'c area is calculated using Equation 2•.l1(. vCllcrnlly. the tech
I~ niquc is restricted 10 p,'.rtic.:1l:sill the 0,5 to 50 um range. Often the measured surface otrea
Gas Permeability Surface Area Analysis is converted into an equivalent spherical surface diameler and expressed in' Ihis mlUlllCr
Ison The pcnncability of a gas:'passing through a porous structure is dependent on (he sur rather than as a surface area. This is commonly reported as lhe subsieve size. Either wuy.
face area. assuming viscous flow of the gas, The Darcy equation for flow in a porous. it i~ \1111)'an approximate measurement 1601 since it docs nol IL~SCSS the dead ended sur,
material gives the tlow rate Q in m,l/s based on the pressur~l~rop M = Pu . PL and the f;ll'~ connected 'poruxity which contributes to the 'BET surface area, However. because
gas viscosity T) as follows: u.e permeability measurement is relatively simple ~n(hhe devices are widely available. ~
:] the subsievc si~es arc used frequently to detail the properties of fine powders, " ;,';
ectors
Q=MK"A/(LT)) 12,361
.....
l Surface Area as a Shape Index , '
where the sample length Land crosssectional area A are as shown in Figure 2.3 I, The The specific surface area is expressed in terms of the area per unit mau (ml/g), Fo;.,.
parameter K" is known as the perrneability.cocfflcienr. The gas velocity exiting from the monoxizcd spheres, the area per sphere A and the volume per sphere \I arc:,given as. :
low pressure side is given as.
12.371
\I = n 1)'/,6 12.401
! area analyzer, A with V equal to the flow rate per unit area (Q/A). Based on an analysis b), Kozeny and
Cannan. the surface area ofthe compact is related to the permeability through the porosi Note the area per unit solid volume is 6/D, The weight W of a solid particle is calculated
occur (liquid nitro
Isted lor a specific from the particle volume and theoretical metallic density P",
ty e as.
ura, resulting in a
d. The area of the IV = P., V 12.411
s= _[I ' E,I
]1/2 12J!l1
P"' 5K( "E)2
Consequently. the area per unit weight (S = A/W) is given as
with PHI equal tothe theoretical density of the material. In Equation 2.38 the porosity E is
.J=o/(DP.,J " 12.421, ..
the fractional void' space out of the total volume:
Surface area measurements based on the permeability of the powder use a subsieve
sizer.·A preweighed amount of powder is exposed to a known ,f1?W rate and the pressure where S i~ the specific surface area, For a polydisperse powder (a powder with a wide'
..' . . . size range). the mean particle size on a population basis provides a first estimate for the'
di ••meter in Equations 2.39 through 2.42, Convenient units for size. surface area. and
density are 11m. m2/g, and g/cnr'. respectively, When these units arc used. the conversion
factors cancel in Equation 2.42.
If a different particle shape is assumed'in Equation 2.42. then the relation between
particle size and surface area would be different, A general fonn would be as follows:",:
 PI,.!)o PL
toP = Pu PL S = k.' (D p ••J
,,
\2,431
,
 , .' .. .':." ",
.
.
of,
A powder tube basis) and specific surface area through theplculated proportionality constantk'. Use"
simple shape models to determine the shape 1:onstant for a monosized powder, ' ',
Figure 2.31. The deterrnt r
measuring the flow rat I~a Ion 01 powder surface area by gas permeability is possible by
regular tantalurTl ferential. e a a gas through a packed powder bed at a known pressure dit : .:
68 69
POVJDER METN.LU~GY ~CI(NLI
"OW""." : 1"1'". " III/Allr)N
A shape factor Ie, tllat Iinkri panicle size and specific surface area can be calcu
\,
lated for most geometric shapes. It is influenced by the parameter selected to mea
,
sure the particle size. Consider a cylinder shaped particle with a length twice the I,
diameter D. Using the diameter as the size parameter measured by screening. thc
~urface area A is given as: ' a = angle of
repose
A = 2 1t [)1 + Tt D112 = 512 1t D!
and the volume is tan(a) = hlr
V. (1t [)114)(2 D) = 1[/2 [)1
and the weight is the density times the volume P. V. Thui the specific surface
area S. is
S , A I (V P.) = (512) 1t D11/(//2) P,. D' Tt/ = 51 (D P••i
"Figure 2.32, Theang:e of repose is a measure of the interparticle friction, It can be deter.
For screening, the particle will orient to pass through a mesh that is equal to or mined from the height and radius of a powder pile passed thr?ugh a funnel.
larger:than the particle diameter. Thus, the average particle size will be measured ••• ~ ••••
" II,
Half Scott
Interparticle Friction
I
I
\ #
Under the general heading or interparticle friction come two main concerns: powder
flow and packing. The friction between particles is dominated by the surface area, sur
Figure 2.33. The basic components of the Hall flowmeter and seen volumeter for mea.
suring the flow and packing of powders.
face roughness, and surface chemistry. As the surface area increases. the amount of fric
book density for a powder: the density when there is no porosity present. The angle of
tion in a powder mass increases. Consequently, the particles exhibit less efficient flow
repose is another friction index, It is the angle a formed by pouring a powder into a pile"
and packing. Those concerns are important to automatic die filling during powde! com
as shown in Figure 2.32, where the tangent of a equals the height divided by the radius
paction, as well as packaging, transportation, blending. and mixing, '
of the loose powder pile. The angle of repose is also observed by tilting or rotating pow
Resistance to now il a main feature of friction. The density or packing properties
der to the angle 'where it naturally flows. Finally, the [low. rate is a measure of the rate a
decrease because of poor now past neighboring particles, Consequently, attention is
powder will feed under gravity through a small opening. Mos!.small, subsieve powders
given to measures of the interparticle friction. Apparent density. or bulk density. of a will not flow due to high interparticle friction. Such powderxarc termed nonfree flow
powder is the density (mus/volume) when the powder is in the loose state without agita ing and arc difficult to fonn,
tion. Tap density il the highest density that can be achieved by vibration or a pcwdcr
Various devices can measure apparent density, Examples of both the Hall flowmeter
without the application of extemiJ pressure. 'Theoretical density corresponds to the hand
and the Scott volurnercr are given in Figure 2,:n, The Hall flowmeter is used for the
, ,.
70 ", .
/I
POWDER METAllURGY SCIENCE
coarser particles measuring both the flow rate and the apparent density. The Scott device Thus. as the only unknown. the powder volume can'be calculated.
is applied to smaller powders which do not freely flow because of a high interparticle
friction, The Arnold meter minimizes powder flow by using a ring containing powder to VI' = VJ'"+ V (I  PIP :
)./ (2.45)
directly fill a 20 ern? cylindrical volume. That technique best correlates with the filling. of
die cavities in powder compaction operations., ' , The powder mass divided hy the volume gives the pycnometer density. Since sealed
The flow rate is usually expressed as the time for 50 g of powder to flow through the pores in the particles can not be accessed by the test gas, the pycnometer density can be
, Hall flowmeter. Short flow times indicate free flowing powders while long times indicate lower than the theoretical density. The typical accuracy is 1%.
high interparticle friction. The apparent density and flow times are easily obtained with , In most all applications involving powders, high packing densities are desired.
the Hall flowmeter by combining a precision volume cup with the funnel. The apparent Improved packing densities arc possible by adjustment of the particle size.. shape, and
density is the weight of powder divided by the cup volume. The precision falls between I size distribution. The higher the packing coordination, the higher the observed powder
percent and 5 per~ent and .the, typical apparent density is between 30 percent to 60 per oensity. The f.o;ordination number is the number of touching neighbors that any p~icle
cent of the theoretical density. ' has in a po~tr ensemble. and is synonymous, with the number of nearest neighbors.
Another simple test for interparticle friction is the tap density. Powder is vibrated in a Small particles will have more interparticle friction, giving a lower number of nearest
cylinder for IOOOto 3000 cycles at 284 cycles per minute using '1 3.2 m~ throw from ~n neighbors. Everything else being equal, the smaller the mean panicle size, the lower the
eccentric cam. Usually the initial powder volume is 25 rnl. The occupied volume Will apparent density. For a coarse spherical powder, the packing fraction for loose p~cking'
decrease rapidly with initial vibration and eventually reach a plateau value. giving the tap (corresponding to the apparent density) is usually near 60% of theoretical and the tap
r can be deter density as the weight divided by the final volume, It is higher than the apparent density, density is near 64* of theoretical. The cocrdinatlonnumber exhibits a distribution
Both the tap and apparent densities can be expressed as fractions of theoretical density. around a mean value. For louse packed, monosized spheres, the mean coordination is..'
The pycnometer density is sometimes given to assess the theoretical density of an between six and seven. Generally. in random packing, spheres pack more efficiently than
unknown powder or the amount of closedoff (internal) porosity. A pressurized gas (usu any other shape. .
ally helium) is used to measure the volume of pores in a powder of known mass. in a It is possible to assess particle shape and friction characterization through the apparent
sample chamber of known volume V, but unknown powder volume VI" Initially. the and tap densities. The ratio of the tap to apparent densities gives a signature characteris
chamber is at a pressure PI" As shown in Figure 2.34. there is a calibration chamber with tic of the interparticle friction. and is called the Hausner ratio. useful in categorizing rela
volume V" connected to the sample volume. It is initially evacuated. After the connecting rive interparticle friction. For a spherical powder. the tap to apparent ratio will be slightly
valve is opened. the pressure decreases to Pr Applying the ideal gas law gives. above unity. More irregular particle shapes undergo a larger density increase with vibra
'ion. resulting in a higher Hausner ratio. .
P, (V  V ) = P, (V  V + V) \2.441
J t • J " "
C;ompressibility
"," ,,' ' .••·1··· One of the main uses for metal powders is for fabricating complex shapes by com
paction. Accordingly. the compaction behavior is an important characteristic.
, pre!jsure
sensor calibration Compressibility. or compactability, measures the ability to densify a powder under an
~ chamber applied load. The typical test geometry is a sjmple cylinder or rectangle. The die is
ter for mea /'" (volume = V e) loaded with powder and the density is measured after compaction at a predetermined
~~~vacuum pressure. often near 414 MPa (corresponding to 30 ton/in1 or 60,000 psi). That is termed
valve the green density and is the basis for expressing the compressibility. For a com~tion
h~ allg'le of sample grade of iron or steel powders the green density might be 85 to 90% of theoretical. A
Illto a pile, powder chamber parameter used in tool design is the compression ratio C/I'
the radius (volume = V p) (volume = V 5)
tating pow ,·r· 12.46}
f the rurc a Figure 2.34. A schemSitic d' '
using a p cno t lag ram of the true volume measurement for a loose powder
e POwders pressure ~ea:~eer. The powder of known weight is placed into the sample chamber. and where \lL is the volume of the! loose powder, Vc' is the' volume of the compacted powder,
free now ed calibration VOluments are made before and after equilibration with an initially evacuat p. is the green density. and P" is the apparent density. A high interparticle friction will
me. give a low initial density. but other factors such 3S panicle size, chemistry, lubrication.
flownJcter
ed for the 72 73
POWDER METAlLURGY SCIENCE 11;,i,,\lrERIZI\TI()N
 1'0 vt)1 I; (
B
and metallurgical properties will determine the pressed density. ofth
cncc
on
pcrut
. A'typic;!1 atomized iron powder has ,10 apparent density of 2.9 glcm \ and com
pacts to a density of 6.71( gjcm" at 414 MPa pressure. The compaction ratio is redu
then.
Figure 2.36. The scanning electron microscope is a polent tool in characterizing metal
.
powders. In example a) three layers are evident in the fractured particle. The picture also
Powder Structure shows satellite formation and agglomeration In this gas atomized alloy powder, In exam beo
ple b) the fractured centrifugally atomized particle shows clear evidence of the solidifica diffr'
A magnified crosssection through 'a powder reveals artifucts that indicate 1';lbriCltion tion events (photo courtesy of.J. Hawers). . :.
and
1
conditions and possible processing problem's. Cro,ss~ectional analysis provides inlonna
• appr
tion orliftlternol pores, segregation and can he Lsefu{ in detecting inclusions and oxidcv, production. III Ih;11c.rc. rhc pll\\li.:r i, cuu.uucd ill ;1 nickel ekt:troplatill!! d.:pn,il where Adv
. Figure 2,:l~ shows Ihe internal structure of two powders. TIle first powder i~ a ~pheric;d il is ~uhst:qu.:nlly 'l'Clil1l1.:d .IIHI illil nul lvd rill' electron truuxparcncy. However. uch Mici
_ ..!!!l.oy pow.der,_1]le, ~Ich~d ~_r:os.s~~,C!!ol1
show~ a large gasfjlle.(LW.fe and radial crack, efforts arc uvuallyrcu'ictcd to the 'l'c'CI;dl\ powder», such as supcralloys .. sitio
. ' ~ The second powder i••irregular in shape with con ••ider ••ble porosity in the panicles which In xumc ill~talln·'. uuportanr microuucuu c iuform.uion can he gained hy SEM analy· sine,
inhibit!! packing. compaction. nnd attainment of high final properties. Such' microxtruc ~is. Fieurc 2..~6 illll'lr;IIl', one ilhlal1c·,· 1\ here the particle fractured to reveal I\VO vhclls usin
lures indicate subsequent processing problems since internal pores arc difficult to climi around a ~mall p;Ir\lck core. '\ddllilll1;dl~, uuclc.uion ~il':~. cout.uuination. t:lllllill~ rail'. near
nate. To observe the internal powder structure, mix loose powder wit~l a metallurgical !!r••ill size. ;1I1d,..:!!rl·!!;lIi'"1call he' a",'",11 Irom SEM examinations. Further information pre.
mounting epoxy resin. The particles seule during curing of the resin. Subsequent polish on the powder C;l;l I~' ~;Iin,d hy ,urran' ;l1l;dy,i~ tonlx. These arc appropriate 111the char
ing and etching of the mount brings out the panicle microstructure. Tranxmiscion clcc al'leri/alilln 111'1'"I\(kr, cnxitivv 111,'lIlll;lIl1il1;l!io1\,Thermal analysi •• providc, another
Iron mi~mscopy ha.•• also been u~d to observe the solidification events during powder A
imponan: mcan, 111'a"c'"ing Iii..: I'",,,kr, Included in these techniques arc ditfcrcnriul
thermal analvsi, for detection or phac u'auIoruuuiou» and melting events. dirrt;r':lltial
scanning c;Ii;lriml'lry ror quantific.uion of endothermic and exothermic events. and thcr teri
mogravimctric analy,i, for determination I\l'ight loss due to desorption and evaporation
:1 pro
during hearing. mir
res
ane
Chemica. Characterization pol
When di~cussillg their chemistries. powders must be subdivided into three groups, pol
The elemental powders arc rel.uivc ly high·purity materials where chemical analysis
focuses on the impurity concentration. Premixed powders arc combinations or two or to
more distinct powders that will diffusionally alloy in sintering. An example would be the bu:
use of mixed 'copper and tin powders 10 Iorrn a bronze a1l9)1.Impurity levels and proper we
'. Ty
compounding of the mixture arc chcmicul conccrns with tile premixed powders, The pre
pal
Agure 2.35. Two example micrographs of crosssectioned metal powders showirg how alloyed powders constitute microcastingx with multiple elements in a predetermined
Internal mlc:roauctutal details can help In characterization of,the powders; a) cp.ntrifugally ratio. For the preulloycd powders. uucntion is given to the alloy composition as well as
atomized steel alloy powder. and b) water atomized Iron poWd8[1(photos courtesy of J. the impurity concentrations. Normal analYlical chemistry techniques are appropriate for
O\napandJ ..~), . ,f',,,
all powders.
,.
~'I' "'"'''i'~'
Beyond the bulk chemical information, the surface condition is an important property Tablr 2.7, Puwdt'r Cha"'oIrh'ri1~lliclIIfur Ihr TunJ:.<ilen Powder Shown In "i~ur~2.'7
of the powder. Hence, there is concern with oxides, adsorbed organic films, and the prcs,
encc of surface coatings like silica to determine appropriate cleaning treatments. A loss Material = Tungsten
on reduction is reported to show the weight loss when heated in hydrogen at a low tern Designation = 325 mesh
perature. This measures the surface oxidation as well as volatile organic content and Metallic Chemistry =
99.99% W •
reducible compounds and is less sophisticated as compared to thermogravimetric analy Impurities (ppm) = C (10), Cu (I I. Fe '(2), K (15), Mg (4), Mo (10). N (100), Nu (6), .•
sis. Likewise, the inclusion concentration is measured by acid dissolution. For some 0(740), Si (2)
materials, the powder hardness provides a gross gauge of the impurity level and assures Apparent Density = 4.37 g/cnr' (23%)
that the powder has been annealed. Often the elemental iron powders are derived either Tap Density =8.05 g/cm' (42%)
from ores or metal scrap. The ore based elemental powders will usually have less lotto Flow Time for 50 g = not free flowing
lot chemistry variations than the scrap based powders. On the other hand, the ore based =
BET Specific Surface Area 0.12 m!/g
powders tend to have higher inert or oxide inclusion contents. Powders fabricated by =
Gas Permeability Surface Area O.02X m!/g
melting techniques provide greater opportunity for chemical refining. and can be expect Particle Size by Sedimentation
·terizing metal ed to have higher purity. .
Depending on the desired sensitivity. bulk chemical characterization 01 a powder (an
DII.= 3.0 prn
e picture also D". = 6.4 ~1l1
der. In exam
the soiiditlca .'
be obtained from wet analysis. emission or name spectroscopy. atomic absorption. xray
diffraction, xray fluorescence, or neutron activation analysis. Emission spectroscopy
DVI.= 12~m
.. and xray fluorescence are typically used for routine analysis. with lower sensitivities of Particle Size by Electrical Zone Scnving
approximately 10 ppm (pprn is the standard abbreviation for parts per million or l O'"), D." = 3.5 pm
ep("il where Advanced techniques arc capable of extending analytical accuracy to the 0.0 I ppm level. 0.".= 6.2 ~1l1'
1Wl·\,er. such Microanalysis by electron or ion beams is useful for characterizing the chemical compo D",. = X.9 ~1l1
sition in small volumes. The microanalysis techniques are not useful for routine analysis
• SEM analy· since they are typically semiquantitative and slow. Finally. surface analysis is possible
I
al 1\\'1I ,Ilells using Auger or other research techniques. Here low energy electrons arc stimulated from
(llolin~ rate. nearsurface regions. These electrons convey infonnation related to the chemical species
informalion present on the powder surface. •
! 10 Illl' char
ide, annllll'!'
, dil'kreillial A Minimum Characterization Battery
. dil'i't;rl:llIi'al
.It is rare that a full battery of measurements is either needed or warranted to charuc
IS. and thcr
: ('d tenze a metal powd er, Th' e typical goal 111 . powder metallurgy is to control the process to
eVaporalion provi e a standardiz d ad
. . e pr uct. Powder characterization is geared toward performing the
m1l11mum amount of t . .
research dd estll1g necessary to ensure consistent feedstock to the process. In
and und an evelopment
di
a I" h ... ..
pp icanons, c aractenzauon IS necessary for future repetition
powder to
ersran 1I1gof the I F
resu ts. or that purpose. a few tests should be performed on a ,
(I
2.3. For a cubic panicle of sides 3 urn. a) what is the equivalent spherical surface diame gJ
W. I. Huppmann and K. Dalal, Meta!J0CC30hic Atlas of Powder Metallurgy. Verlag
Schmid. Frieburg. Gennany. 1986. ter. and b) the equivalent spherical volume diameter? ;.. , 2
B. H. Kaye, "Review' of New Methods for Characterizing the Shape and Texture of Fine 2.4. Iron powder is screened into 'I &)/~2(i() m'~sh and 325 m~sh fractions. The apparent P
Particles." I. Powder Bylk Solids Tech., 1982. vol, 6. no. 2. pp. 14. density of the coarse fraction is 2.6 g!cm \ and the line fraction has an apparent dc~slty of
2.3 g/cm'. When a blend is prepared using. 20% fine panicles in the coarse Iruction, the
Eo K1ar (editor). Powder MetaJltu:EY, vol. 7, ninth edition of Metals Handbook. ASM , .
I
18
POWOFR MrTAltt JR(,Y \(JFN( I
1\ "VIII /( U ~nRllATION
nt density is measured as 2.8 g/crn'. Explain the effect. prn. However. the other properties are quite different as noted below:
appare
5 Air is penneated through a tube of I cm2 cross sectional area by I em lone contain I. [l9wder A powder B
specific surface area. m~/g 0.26 0.12
Dara." Testin~ ~.. Iybdenum powder with an apparent density of 4.5 g/crn'. At one atmosphere pres
apparent densuy, g/cm' :U 4.5
. Meloy (cds.), . rno
mg differential (2 atmospheres to I atmosphere) the measure d fl ow ve I"ocuy IS 0 " I 'i tap density. g/cm
sur/c. What is the equivalent spherical diameter'! (air viscosity = 1.8· 10'· gicm/s. Mo ~,6 8.1
em s. . , .
1 Porosity. John theoretical density = 10.2 g/cm ) a) Explain why there might he a difference in surface areas.
2 .,6 Exp lain why the flow time (in the Hall flowmeter) is observed to increase with the b) What equivalent sp~erical dial.Heler woul~ give the same surface area.~ for each powder'!
ratio of the tap density to apparent density? c) What differences might explain the packing propenies?
d) What addiuonat information would be useful?
2.7. The' oxide on the surface of aluminum powder can be used to form a dispersion :or
strengthening the consolida~ed powder. For. a 10 11mparticle di.amet~r and ~ ;5 nm thick 2.17. ~alculate th: upward gas Ilo~"'.velocit~ for air so that a 10 urn panicle of le'l2 will
oxide surface layer. what will be the consolidated percent of OXIde dispersoid? be levlt~ted (held III a constant posinon) against gravjty, (air viscosity =
1.8.101 giS/em.
arr density = 1(;··1g/cm', Pb theoretical density = 11.4 g/cm')
2.8. What powder characteristics might cause the surface areas to differ when measured
by permeability and by gas adsorption? 2.1 It Data arc collected by sedimentation for an aluminum powder (theoretical density =
2.7 g/crn:') as follows:
I. Powde'r Rulk 2.9. The Reynolds number must be below approximately 1.0 for Stokes law to be valid in
siz: r;J.nge. pm weit:hl,:,:
performing a sedimentation analysis for particle size. For aluminum spheres settling in o to I (1.O
lnd Sons. New water, what is the maximum particle diameter for which sedimentation is valid? (density I to 2 0.4
of AI = 2.7 g/cm', density of water = 1.0 g/crrr'. viscosity of water = I0 ~ gis/cm)
.. 2 to 4 5.5
2.10. Set up a quality control flow chart for testing incoming powders at a P/M parts 4 tu X ., 2.l4
8. vol. 67. pp.
plant. The flow chart should include the minimum. but necessary. steps needed to ensure 8 to 12 IlJ.O
, an acceptable and repeatable powder. Nominally. the powder is I ()() mesh iron. 12 to 20 17.6
Arbor Science 20 to 32 5.lJ
2.11. The ratio of the tap to apparent densities has been proposed as a particle shape
32 to 44 1.1
index. Discuss such a ratio and the possible combined influence of particle shape and
size. 44 to XX 0 ..1
UK.19X7.
over XX 0.0
!luers." Powder 2 '.12. A polydisperse powder sample is analyzed for particle size using optical a) Give a particle size distribution plot showing the cumulative weight percent versus the
te of Materials. microscopy, giving a mean size of 13 urn. A second analysis is performed using scdi 10glOof the particle size. .
mentat~on. giving a mean size of 28 11m.Give some possible reasons for the difference in b) What is the mean panicle size 1111 a weight basis?
mean sizes.
c) Estimate the mean panicle size on a population basis.
2..13 ·Calc~late the shape index k in Equation 2.43 for a regular parallelepiped panicle d) What techniques could be applied tll the size analysls of this powder?
wit han axial ratio of 1:2:8.
('I powder. The
. '2.14. Two laborator' d
J •
.
=
2.19 ':A spheri~al .20 11m part ide lIf ~itallium (theoretical density 4.5 glcm·1) has a ~ urn
Ii density is X.lJ laborat res con uct sieve analyses of an irregular shaped powder. The first
spherical VOId 111 ItS center. What will be the terminal settling velocity for this particle in < I
a few ;~i~I~;s the mean size as 54 11m,while the second claims it to be 75 urn. Offer water? .How d.oes that com.pare to the terminal velocity for a porefree particle of the '
)0 urn) is sized ypotheses Why the values differ. same diameter? (water density = I g/cm:', viscosity = 10.2 glcm/s)
» 2.15. Approximatel h . 2.20. How might mixed P'~~;ides of copper and tin be separated from one another?
mesh iron powd y ow ma~y panIcles are contained in a 10 g sample of +325/270
surface diarne g/cml)
er and what IS th
.
. ..
e estimated surface area? (theoretical density = 7.86 , (.
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