CERMES

MINERALOGIE, CONSTITUTION ET
CARACTERISATION DES SOLS FINS - 2

Pierre DELAGE
ENPC – Navier/CERMES
 Observation de microstructure
• Méthodes les plus utilisées:
– Microscopie électronique à balayage (MEB),
échantillons déshydratés
– MEB Environnemental, échantillons humides
– Porosimétrie par injection de mercure,
échantillons déshydratés
• Plus récemment
– Microtomographie aux rayons X
– FIB: Focused Ion Beam
 Déshydratation des sols fins
• Séchage: forte rétraction de la
microstructure par l’action des ménisques
air-eau
• Déshydratation par lyophilisation
– Congélation ultra-rapide dans l’azote liquide
sous vide (-210°C, pas d’ébullition)
– Sublimation de la glace sous vide: pas d’effet
des ménisques capillaires
• Fracturation à l’état congelé: observation
MEB d’un plan intact
Déshydratation des sols fins

Congélation (-210°C) évaporation

Sous vide
Sublimation

http://fr.wikipedia.org/wiki/Diagramme_de_phase
Observations au MEB
Argile sensible, Grande Baleine (Québec)

St > 1000, Ip = 8

10µm
10 µm
Delage (2012)
Argile sensible de St Marcel, Canada

St = 30, Ip = 20
Argile du Golfe de Guinée
 Limon compacté
Optimum Proctor
Loess
Loess
Loess
Argilite du Callovo-Oxfordien
 Argilite du Callovo-Oxfordien
P. Delage and D. Tessier / Geomechanics for Energy and the Environment xxx (xxxx) xxx

Grains arrachés par fracturation congelée (25% calcite, 20% quartz)

Fissures d’hydratation
Pyrite

Matrice argileuse
(50%)

Fig. 16. SEM observation of a freeze-fractured plane of the Callovo–Oxfordian claystone.45

 Argile raide: Romainville
a b

5 µm 8 µm

a) état naturel (w = 29,8%) b) après un gonflement libre de 10,4% (w = 37,5%).

Porosimétrie des sols
 Porosimétrie
Détermination de la courbe de distribution de la taille des pores
(« granulométrie » des pores): POURQUOI ?
Les pores sont un reflet de l’organisation des éléments constitutifs
des sols structurés: microstructure
Leur taille et distribution conditionne :
- les transferts d’eau en saturé et non saturé : loi d’écoulement de
Poiseuille dans un tube cylindrique – effet de viscosité
- la rétention d’eau (w = f(Sr) lors de la désaturation (et
resaturation)
- la réponse mécanique:
- matrice poreuse plus fragile et compressible avec des
gros pores
- analyse de la compression et du gonflement
- résistance au cisaillement
Effet de structure en compression

Argile de Grande Baleine

 Porosimétrie au mercure
Un liquide non mouillant doit être mis sous pression pour
pénétrer un milieu poreux
Une pression plus forte est nécessaire pour pénétrer des pores
plus petits
Rayon r1 Rayon r2
Augmentation de pression

pi = f(ri ) ?
 Capillarité
æ1 1ö
• Loi de Laplace : p = s cosq çç + ÷÷
è r1 r2 ø

• Hypothèse de pores cylindriques: r1 = r2

æ1ö
p = 2s cosq çç ÷÷
è r1 ø

• Contact mercure-argile: s = 0,484 N / m

q = 141°
• Une pression de plus en plus forte permet de
pénétrer des pores de plus en plus petits
 Porosimétrie au mercure
Suivi électronique
Un échantillon est mis sous vide dans undilatomètre du niveau
Le dilatomètre est empli de mercure Bain d’huile sous
pression
Il est placé dans un cellule emplie d’huile mise croissante
(max. 200 MPa)
incrémentalement sous pression jusqu’à 200 MPa
On suit l’évolution du niveau du dilatomètre à
chaque incrément de pression
Les pressions sont reliées à des dimensions de pore
selon les lois de la capillarité
Porosimétrie au mercure

Leca (1990)
 Porosimétrie au mercure
• A quelle diamètre de pore correspondent
– la pression atmosphérique?
– Une hauteur de 20cm de mercure dans le
dilatomètre?
– Une pression maximale de 200 MPa

æ1ö s = 0,484 N / m
p = 2s cosq çç ÷÷
è r1 ø q = 141°
Courbe
porosimétrique
cumulée
Courbe
porosimétrique
cumulée
Courbe
porosimétrique
cumulée
Courbe
porosimétrique
cumulée
Courbe de retrait

Diminution de pression
Porosité piégée

Porosité piégée
Courbe de pénétration cumulée
increasing Hg pressure

200 MPa

Hg penetrating Pore size distribution curve

in smaller and smaller pores

 Porosimétrie au mercure
• Calculer les rayons et pressions correspondantes:
argile de St Marcel

æ1ö s = 0,484 N / m
p = 2s cosq çç ÷÷
è r1 ø q = 141°
 Porosimétrie au mercure
• Calculer les rayons et pressions correspondantes:
argile de grande baleine

æ1ö s = 0,484 N / m
p = 2s cosq çç ÷÷
è r1 ø q = 141°
 Porosimétrie au mercure
• Calculer les rayons et pressions correspondantes:
limon de Bapaume

æ1ö s = 0,484 N / m
p = 2s cosq çç ÷÷
è r1 ø q = 141°
 Porosimétrie au mercure
• Calculer les rayons et pressions correspondantes:
P. Delage and D. Tessier / Geomechanics for Energy and the Environment xxx (xxxx) xxx 9

argilite du Callovo-Oxfordien

Fig. 16. SEM observation of a freeze-fractured plane of the Callovo–Oxfordian claystone.45

æ1ö s = 0,484 N / m
p = 2s cosq çç ÷÷
è r1 ø q = 141°
Courbe cumulée, St Marcel
Courbe cumulée, Grande Baleine
 Limon compacté
Distribution

côté sec

Courbe cumulée
 Limon compacté
Distribution

agrégat

côté sec

Courbe cumulée

Pore inter-agrégat
 Limon compacté humide

Même densité,
côté humide

Les grains de limon sont contenus

dans la matrice argileuse
 Limon compacté humide

Même densité,
côté humide

Les grains de limon sont contenus

dans la matrice argileuse
Limon à l’optimum Proctor

Optimum
Limon à l’optimum Proctor

Optimum
Bouchons de
« bentonite »
compactée:
smectites
Compacted Kunigel clay (Japan)

5 µm

r = 2 Mg/m3, w = 8%
2 µm s = 57 MPa
 Bentonites properties
• Clay FoCa7 clay (F) Kunigel (Japan) MX 80 (USA)
• Mineralogy Kaolinite 64% 85%
smectite Na smectite Na-Ca smectite
• wL (%) 112 474 520
• wP (%) 50 27 62
• IP 62 447 458
• S (m2/g) 300 687 700
• CEC 54 73,2 68
(mEq/100 g)
• Suction 115 MPa 57 MPa

• Highly compacted (60 MPa for FoCa at w = 10%, rd = 1.85 Mg/m3)

Bentonite compactée
5 µm

Calcigel clay
rd = 2 Mg/m3, w = 9%, s = 22.7 MPa
2 µm

intra-aggregate : ≤ 0.1 µm

inter-aggregate :
between 5 and 30 µm

Agus & Schanz 2005

Changements de teneur en eau

Calcigel clay
rd = 2 Mg/m3, w = 9%,
s = 22.7 MPa
 OVEN DRYING

OVEN-DRYING (s from 22 MPa to 1GPa) HAS LITTLE EFFECT ON

MICROSTRUCTURE
Calcigel clay
rd = 2 Mg/m3, w = 0%
s = 1GPa
Hydratation à succion nulle
SWELLING CONCERNS BOTH VERY SMALL PORES (< 3.5 nm)
AND LARGE PORES (around 1 µm)
Calcigel clay
rd = 2 Mg/m3, w = 19%
s = 0 MPa
EFFECT OF INITIAL WATER CONTENT
1.1
e = 1.008
1.0

0.9 w = 12.5%, s = 30 MPa

Intruded mercury void ratio, em
0.8 0.812
MX 80 clay
w = 28.5% r = 2 Mg/m3
0.7 w = 12.5 %
s = 2 MPa
0.6 0.597

SAMPLE
0.5 AT HIGHER WATER CONTENT HAS MORE WATER
LOCATED IN VERY SMALL PORES (< 3.5 nm)
0.4
w = 28.5 % 0.293
0.3

0.2 0.230

0.1

0.0
0.001 0.01 0.1 1 10
Porous radius (µm)
Marcial et al.
 !"# !$#

0 days of the looser and wetter sample, e 0.998 and w 28.5% (picture width is 40 !m) at

The nW hydration of compacted MX80 (Na+)

<=
Fig. 12 Hydration mechanisms
678+9 B+/"2*)' Tetrahedral sheet
9.6 Å

%>*)"?*+&5'-"1@*A+9
in MX80 (after Saiyouri et al. 30 Octahedral sheet
2004) investigated through
:= <+/"2*)' 18.6 Å Tetrahedral sheet
X-Ray diffractometry
:+/"2*)'15.6 Å
4 layers
3 layers

distance (Å)
20
;+/"2*)
2 layers
18.6 Å
:! ;= 11 couche
layers ETAT SEC
15.6 Å
12.6 Å
12.6 Å
Distance inter-
Interlayer

10 basale = 9.6 Å
:;+9
= 0.96 nm
=
=7==; =7=; =7; ; ;= ;== ;===
0
7 MPa
CD@-5(1A+EF" v
50 MPa

0.001 0.01 0.1

!"#
1 10 100 1000
Suction (MPa)
B==
GD0$*)+(4+'3**-'+H*)+H")-5@/*

een two layers of montmorillo- 350 sheets per platelet

1W
adsorbed at suctions larger than 50 MPa, two layers also depended on the nature of the cation considered. They
between 50 and 7 MPa, and three <== layers below 7 MPa, showed that different numbers of water layers (0, 1 or 2 W)
with a fourth layer adsorbed at low suctions smaller than could coexist at a given suctions above 30 MPa (relative
0.1 MPa. This mechanism is illustrated in Fig. 12. humidity—RH—smaller than 80 %). However, the aver-
Ferrage et al. (2005) worked :== on purified homoionic age trend that they observed was compatible with the data
yers above a 50SWy-1
kPa montmorillonites
suction, saturated with cations of different of Saiyouri et al. (2004). On a Na montmorillonite, mainly
ressively decreasing down to ? ?
valences (including Na , K and;== ??
Ca ). They observed one layer (1 W) was adsorbed at relative humidity smaller
layers at 3 MPa. Hence mechanisms
that hydration the were in fact more complex and than 60 % (suction of 70 MPa) with the transition between
heterogeneous,
om high suction is the result and confirmed that hydration mechanisms one and two layers occurring between 60 and 80 % RH
=
=7==; =7=; =7; ; ;= ;== ;===
CD@-5(1A+EF" 123
of successive layers of water
!$# Sayiouri, Tessier and Hicher (2004)
spaces inside the particles
s into thinner ones that are Fig. 13. Effect of a suction decrease (hydration) on MX80
mber of stacked layers. particles: (a) increase in the number of adsorbed water layers;
(b) decrease in the number of stacked layers per particle
morphology inside aggregates
(Saiyouri et al., 1998)
 !"# !$#

0 days of the looser and wetter sample, e 0.998 and w 28.5% (picture width is 40 !m) at

The nW hydration of compacted MX80 (Na+)

<=
Fig. 12 Hydration mechanisms
678+9 B+/"2*)' Tetrahedral sheet
9.6 Å

%>*)"?*+&5'-"1@*A+9
in MX80 (after Saiyouri et al. 30 Octahedral sheet
2004) investigated through
:= <+/"2*)' 18.6 Å Tetrahedral sheet
X-Ray diffractometry
:+/"2*)'15.6 Å
4 layers
3 layers

distance (Å)
20
;+/"2*)
2 layers
18.6 Å
:! ;= 11 couche
layers
15.6 Å
12.6 Å
12.6 Å
Interlayer

10
:;+9
=
=7==; =7=; =7; ; ;= ;== ;===
7 MPa 50 MPa
0 CD@-5(1A+EF"
0.001 0.01 0.1
!"#
1 10 100 1000
Suction (MPa)
B==
GD0$*)+(4+'3**-'+H*)+H")-5@/*

een two layers of montmorillo- 1W

adsorbed at suctions larger than 50 MPa, two layers also depended on the nature of the cation considered. They
between 50 and 7 MPa, and three <== layers below 7 MPa, showed that different 2W
numbers of water layers (0, 1 or 2 W)
with a fourth layer adsorbed at low suctions smaller than could coexist at a given suctions above 30 MPa (relative
0.1 MPa. This mechanism is illustrated in Fig. 12. humidity—RH—smaller than 80 %). However, the aver-
Ferrage et al. (2005) worked :== on purified homoionic age trend that they observed was compatible with the data
150 sheets per platelet
yers above a 50SWy-1
kPa montmorillonites
suction, saturated with cations of different of Saiyouri et al. (2004). On a Na montmorillonite, mainly
ressively decreasing down to ? ?
valences (including Na , K and;== ??
Ca ). They observed one layer (1 W) was adsorbed at relative humidity smaller
layers at 3 MPa. Hence mechanisms
that hydration the were in fact more complex and than 60 % (suction of 70 MPa) with the transition between
heterogeneous,
om high suction is the result and confirmed that hydration mechanisms one and two layers occurring between 60 and 80 % RH
=
=7==; =7=; =7; ; ;= ;== ;===
CD@-5(1A+EF" 123
of successive layers of water
!$# Sayiouri, Tessier and Hicher (2004)
spaces inside the particles
s into thinner ones that are Fig. 13. Effect of a suction decrease (hydration) on MX80
mber of stacked layers. particles: (a) increase in the number of adsorbed water layers;
(b) decrease in the number of stacked layers per particle
morphology inside aggregates
(Saiyouri et al., 1998)
 !"# !$#

0 days of the looser and wetter sample, e 0.998 and w 28.5% (picture width is 40 !m) at

The nW hydration of compacted MX80 (Na+)

<=
Fig. 12 Hydration mechanisms
678+9 B+/"2*)' Tetrahedral sheet
9.6 Å

%>*)"?*+&5'-"1@*A+9
in MX80 (after Saiyouri et al. 30 Octahedral sheet
2004) investigated through
:= <+/"2*)' 18.6 Å Tetrahedral sheet
X-Ray diffractometry
:+/"2*)'15.6 Å
4 layers
3 layers

distance (Å)
20
;+/"2*)
2 layers
18.6 Å
:! ;= 11 couche
layers
15.6 Å
12.6 Å
12.6 Å
Interlayer

10
:;+9
=
=7==; =7=; =7; ; ;= ;== ;===
73MPa
MPa 50 MPa
0 CD@-5(1A+EF"
0.001 0.01 0.1
!"#
1 10 100 1000
Suction (MPa)
B==
GD0$*)+(4+'3**-'+H*)+H")-5@/*

een two layers of montmorillo- 1W

adsorbed at suctions larger than 50 MPa, two layers also depended on the nature of the cation considered. They
between 50 and 7 MPa, and three <==layers below 7 MPa, showed that different 2W
numbers of water layers (0, 1 or 2 W)
with a fourth layer adsorbed at low suctions smaller than could coexist at a given suctions above 30 MPa (relative
0.1 MPa. This mechanism is illustrated in Fig. 12. humidity—RH—smaller than 80 %). However, the aver-
Ferrage et al. (2005) worked :==on purified homoionic age trend that they observed was compatible with the data
yers above a 50SWy-1
kPa montmorillonites
suction, saturated with cations of different of Saiyouri et al. (2004). On a Na montmorillonite, mainly
ressively decreasing down to ? ?
valences (including Na , K and;== ??
Ca ). They observed one layer (1 W) was adsorbed at relative humidity smaller
3W
layers at 3 MPa. Hence mechanisms
that hydration the were in fact more complex and than 60 % (suction of 70 MPa) with the transition between
10 sheets per platelet
om high suctionheterogeneous,
is the resultand confirmed that hydration mechanisms one and two layers occurring between 60 and 80 % RH
=
=7==; =7=; =7; ; ;= ;== ;===
CD@-5(1A+EF" 123
of successive layers of water
!$# Sayiouri, Tessier and Hicher (2004)
spaces inside the particles
s into thinner ones that are Fig. 13. Effect of a suction decrease (hydration) on MX80
mber of stacked layers. particles: (a) increase in the number of adsorbed water layers;
(b) decrease in the number of stacked layers per particle
morphology inside aggregates
(Saiyouri et al., 1998)
 !"# !$#

0 days of the looser and wetter sample, e 0.998 and w 28.5% (picture width is 40 !m) at

The nW hydration of compacted MX80 (Na+)

<=
Fig. 12 Hydration mechanisms
678+9 B+/"2*)' Tetrahedral sheet
9.6 Å

%>*)"?*+&5'-"1@*A+9
in MX80 (after Saiyouri et al. 30 Octahedral sheet
2004) investigated through
:= <+/"2*)' 18.6 Å Tetrahedral sheet
X-Ray diffractometry
:+/"2*)'15.6 Å
4 layers
3 layers

distance (Å)
20
;+/"2*)
2 layers
18.6 Å
:! ;= 11 couche
layers
15.6 Å
12.6 Å
12.6 Å
Interlayer

10
:;+9
=
=7==; =7=; =7; ; ;= ;== ;===
73MPa
MPa 50 MPa
0 CD@-5(1A+EF"
0.001 0.01 0.1
!"#
1 10 100 1000
Suction (MPa)
B==
GD0$*)+(4+'3**-'+H*)+H")-5@/*

een two layers of montmorillo- 1W

adsorbed at suctions larger than 50 MPa, two layers also depended on the nature of the cation considered. They
between 50 and 7 MPa, and three <==layers below 7 MPa, showed that different 2W
numbers of water layers (0, 1 or 2 W)
with a fourth layer adsorbed at low suctions smaller than could coexist at a given suctions above 30 MPa (relative
0.1 MPa. This mechanism is illustrated in Fig. 12. humidity—RH—smaller than 80 %). However, the aver-
Ferrage et al. (2005) worked :==on purified homoionic age trend that they observed was compatible with the data
yers above a 50SWy-1
kPa montmorillonites
suction,
ressively decreasing down to ?
saturated with cations of different
?
valences (including Na , K and;== ??
Ca ). They observed
of Saiyouri et al. (2004). On a Na montmorillonite, mainly
one layer (1 W) was adsorbed at relative humidity smaller
similar data
3W
layers at 3 MPa. Hence mechanisms
that hydration the were in fact more 4W
EXFOLIATION complex and than 60 % (suction of 70 MPa) with the transition between
om high suctionheterogeneous,
is the result 10 sheets
and confirmed that hydration per platelet
mechanisms one and two layers occurring between 60 and 80 % RH on other compacted bentonites
=
=7==; =7=; =7; ; ;= ;== ;===
CD@-5(1A+EF" 123
of successive layers of water
!$# Sayiouri, Tessier and Hicher (2004)
spaces inside the particles
s into thinner ones that are Fig. 13. Effect of a suction decrease (hydration) on MX80
mber of stacked layers. particles: (a) increase in the number of adsorbed water layers;
(b) decrease in the number of stacked layers per particle
morphology inside aggregates
(Saiyouri et al., 1998)