Literature review on the study of

changes in pore size distribution

of clay upon loading
Jun Kang Chow
Supervisor: Prof. YH Wang
Outline
1. Current stage of research on the
change in pore size distribution of
clay
2. Methods available to quantify the
pore size distribution of clay
3. Future work
Interpret the changes in pore
size distribution of clay
during the loading processes.
Preconsolidation
SEM MIP
Loading
Freeze drying
Washing
Adjust properties
Direct observation
(from SEM)
Measurement
(from MIP)
+
Current stage of research
(Wang, Y.H. & Xu, D., 2007; Wang, Y.H. & Yu, C.Y.,
(unpublished))
Sample: Speswhite
kaolin
Mechanical responses of kaolinite clay
depend on cluster-to-cluster interactions
rather than particle-to-particle interactions
Samples obtained before and
after loading for MIP test are
not identical.
Freeze-drying process may
alter the pore size
distribution of clay
specimens.


Preconsolidation
SEM MIP
Loading
Freeze drying
Washing
Adjust properties
Results of MIP test show that
larger pores reduce in size after
loading.
This does not guarantee the
pores involved are inter-
aggregated pores.


PROBLEMS ?
Current stage of research
(Wang, Y.H. & Xu, D., 2007)
~ 0.42 m (pore C of pH 4 spec.)
~ 0.18 m (pore B of spec. with
salt)
~ 1.22 m (pore D of spec. with
salt)
~ 0.42 m (pore B of pH 7.8
spec.)


Existence of smaller/larger Types B, C and D pores than the
sizes indicated.
SEM image shows that particles that form aggregated
associations can be unevenly arranged, creating larger intra-
aggregates pores.
Result of MIP test
(Wang, Y.H. & Xu, D., 2007)
Figure is taken from Wang, Y.H. and Xu, D.
(2007)
We are unable to observe
the loading process.
We are unable to visualize
how the arrangement of clay
fabric is altered due to
loading.
To search the suitable method that
allows the visualization of changes
in clay fabric arrangement upon
loading
HOW
?
Methods to study pore size
distribution of clay
Direct
observation
Measurement
technique
Scanning Electron
Microscope (SEM)
Environmental
Scanning Electron
Microscope (ESEM)
X-ray computed
topography (CT
scanning)
Mercury Intrusion
Porosimetry (MIP)
Nitrogen sorption
method
Non-polar liquid
desorption
Water-desorption
Systematic errors due to:
Inappropriate pore model (assuming cylindrical pore model)
Variation in surface tension and contact angle
Measurement of pore size distribution
of clay (Lawrence, G.P., 1977; Westermack, S., 2000)
Mercury intrusion
porosimetry
Nitrogen sorption Non-polar liquid
desorption
Water desorption
Measure pore
size of ~ 3 nm
200 m
Measure the
pressure required
to force mercury
into pores
Errors due to:
distribution of
pore volume and
pore collapse
Carried out at
low temperature
(~ -196C)
Able to
determine range
of pore size ~ 0.3
- 300 nm
Interactions
between non-
polar liquids
and clay
surfaces are
weak
Equilibrium
times are long

Most fine-
textured soils
shrink and
particle
rearrangement
takes place
Stresses on
pore walls
during an
increase in
suction cause a
reduction in
pore size
A pore system cannot be adequately
characterised by the use of only one
method.
Combine both methods to measure the
pore size distribution of clay. (Sills, I.D. et
al. 1973a, 1974)
Technology available
At this T, only a modest gas pressure is
required to stabilize water (achieve saturation)
Method
Focus

Type of samples


Sample Size

Preparation


Resolution


Working
temperature
Method SEM ESEM CT Scan
Focus Morphology (characteristics of surface) of
materials
Images of the
inside of opaque
objects
Type of samples Dry samples
(Absence of water)
Hydrated samples
(Presence of
water/solutions)
Hydrated samples
Sample Size ~ few mm in
diameter
10 x 10 mm
2
~ few mm in
diameter
Preparation Freeze-drying &
coating of samples
are required
Samples can be
kept at fresh &
live condition
No
Resolution ~ <1 20 nm ~ 5 nm (depend on
operating voltage &
degrade due to
noise)
~ 1m
Working
temperature
Room temperature ~ 2 4 C Room temperature
SEM
Morphology of
materials
Dry samples
(Absence of water)

~ few mm in
diameter
Freeze-drying &
coating of samples
are required
~ <1 20 nm


Room temperature

CT Scan
Images of the
inside of opaque
objects
Hydrated samples


~ few mm in
diameter
No


~ 1m


Room temperature

ESEM
Morphology of
materials
Hydrated samples
(Presence of
water/solutions)
10 x 10 mm
2
(depend)
Samples can be
kept at fresh &
live condition
~ 5 nm (depend on
operating voltage &
degrade due to
noise)
~ 2 4 C

An electron beam is emitted
towards a conductive sample in
high vacuum conditions.
Secondary electrons are released
from the sample, collected by
detector and amplified to produce
an image.
The conductive coating of sample
(gold) improves the image quality.
The vacuum ensures the effective
operation of the electron gun.
Working principle of SEM
(Absence of
water)
Working principle of ESEM
1 torr = 133 Pa
A high vacuum condition is
ensured only in a limited zone
surrounding the electron gun.
The relative humidity around the
sample stays relatively high.
Working principle of ESEM
When electrons are emitted, they
have to travel through the gas.
Secondary electrons (with low
energies) have a high collision
cross-section with the gas
molecules.
Ionizing collisions lead to the
generation of addition daughter
electrons a cascade
amplification.

At the same time, positive ions are
also produced.
These ions drift down towards the
sample compensate the charge
build-up at the surface of insulators.

ESEM Quanta 250 FEI
NanoCharacterization
Metals & alloys,
magnetic &
superconducting
materials
Ceramics, composites,
plastics
Films/coatings
Geological materials
minerals
Soft materials
polymers, gels,
tissues, plant
Particle, porous
materials, fibers
Application of ESEM
Journal Description
Montes-H, G. et al.
(2005)
To study the swelling-shrinkage behavior of compacted
bentonite submitted to hydration/dehydration conditions
Vaunat, J. et al. (2007) To study the residual shear strength of a plastic clay
(Boom clay) under high suction
Zhang, G. et al. (2004) To study how Fe oxides alter the soil structure of a
highly weathered oil alluvium
Selvam, A. &
Barkdoll, B. (2005)
To observe changes in clay fabric using ESEM &
correlate it to the permeability changes occurring in clay
One Sample
Preparation Stage:
Washing
Adjusting
Properties
Preconsolidation
Loading
ESEM
Vary
loading
Many Samples
Preconsolidation
SEM MIP
Loading
Freeze drying
Washing
Adjust properties



Future work/
Challenge:
Design of cell
Digital image
analysis