Imaging soft sphere packings in a novel triaxial shear setup

Joshua A. Dijksman, Hu Zheng, and Robert P. Behringer

Citation: AIP Conference Proceedings 1542, 457 (2013);

View online: https://doi.org/10.1063/1.4811966
View Table of Contents: http://aip.scitation.org/toc/apc/1542/1
Published by the American Institute of Physics

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 Imaging Soft Sphere Packings in a Novel Triaxial Shear
Setup
Joshua A. Dijksman∗ , Hu Zheng†,∗ and Robert P. Behringer∗
∗
Department of Physics, Duke University, Science Drive, Durham NC 27708-0305, USA
†
Department of Geotechnical Engineering, Tongji University, Shanghai 20092, P.R. China

Abstract. We describe here how to design a triaxial shear setup suitable for both stress and structure measurements on
granular packings. Our novel setup makes use of refractive index matched scanning techniques. It can thus be used to study
any kind of material compatible with that method. We describe in particular how to use hydrogel spheres, which we have found
to have properties which make them particularly well suited for stress and structure measurements of granular packings. We
discuss here some mechanical properties of hydrogel spheres and methods to use them in refractive index matched scanning
devices such as the triaxial shear setup discussed.
Keywords: granular mechanics, granular packings, hydrogel
PACS: 81.05.Rm, 83.50.-v

INTRODUCTION (a)
piston
(b)
index matching fluid piston
Granular materials such as sand, rice, powders and
coffee beans have surprising mechanical behavior. Even piston
piston
force sensor
though they are defined as collections of particles whose
20 x 20 x 25 cm tank
thermal energy is negligible, they can behave as liquids,
solids and gases [1, 2]. Both packing fraction and shear camera laser motion
stress have emerged as crucial variables necessary to de- laser
scribe the state of the granulate. One can cross the phase (hydrogel) particles
boundary between solid and liquid granular materials
thus jamming the granulate, either by shear [3] or com-
slice imaging
paction [4]. Most of these effects have been observed (c) (d) (e)
in numerical simulations or quasi two dimensional
experiments. However, experimental studies that explore
the relation between microstructure and mechanical
response of granular materials in three dimensional
systems are rare [5]. Here we describe a rectangular FIGURE 1. (a) Schematic overview of the triaxial shear
triaxial shear setup in which a model granular packing setup. The force sensor that measures the wall pressure is
can be deformed by shear or compression. The setup mounted as indicated in panel (b). (c) Imaging of the pack-
allows us to probe the boundary pressures and internal ing by illuminating a single slice. The sample appears regular
in the sketch; in experiments packings are disordered as indi-
packing structure simultaneously. Boundary pressures cated by (d) which shows a packing of hydrogel spheres index
are measured with pressure transducers; to image pack- matched in water. The assembly is mounted on an optical table
ing structure and evolution we use refractive index (not shown). (e) Flasks with demineralized water and hydrogel
matched (RIM) imaging [7]. We explore in particular the spheres, and three different dyes, exposed to UV light. From
potential of hydrogel particles in the study of granular left to right: Rhodamine 110, Rhodamine B, Rhodamine 6G.
materials [8, 9], whose properties make it possible to Only Rhodamine 6G displays strong hydrogel affinity.
study the role friction and packing mechanics and allow
for the extraction of contact and force networks [5, 10].
TRIAXIAL SHEAR SETUP
Traditional triaxial tests frequently consist of applying
from one surface a compressive/shear stress or uniax-
ial deformation on a sample confined in a cylindrical
rubber membrane, while keeping pressure on the mem-

Powders and Grains 2013

AIP Conf. Proc. 1542, 457-460 (2013); doi: 10.1063/1.4811966
© 2013 AIP Publishing LLC 978-0-7354-1166-1/$30.00

457
brane constant with a fluid. As such, they study the rela- (a)
tion between vertical stresses σzz at constant horizontal 11
stress components σxx,yy . We perform triaxial shear dif-

Diameter [millimeter]
ferently. We confine a granular material in the corner of a
9
container with three independently movable pistons, and
carry out compression and shear by moving the pistons 1 cm
— see Fig. 1a. This method has several advantages: we 7
have flexibility in imposing particular deformations, and
we measure all normal stresses σii independently. The
sides of the container have flat faces, which gives visual 5
access to the sample, making RIM studies of the packing Time [minutes]
structure possible (Fig. 1d). In this section we describe 3
the experimental setup. Mechanics — The container with 0 100 200 300 400
pistons is an acrylic box of size 20 x 20 x 25 cm. Two 60
(b) 2
sides of the box have a hole for the pistons. Force sen-

log force
sors (Loadstar RSB4-005M-A) are mounted on the pis- 1

tons, in line with the axis as indicated in Fig. 1b. This 40 0 1.5
assembly allows us to measure pressure and independent
movement of the piston plates, with the limitations de- −1
log strain
scribed below. Force sensor and piston rods are isolated

from the liquid in the tank with a flexible latex membrane
(Durex) whose stiffness is low enough not to interfere
with wall pressure measurements. This membrane also
makes the whole tank leak tight. Piston plates are acrylic
and perforated with 5 mm holes in a 2.54 cm grid spac-
ing to reduce fluid flow during piston movement. Hole
edges are machined with a rounded chamfer that removes
sharp edges, to prevent potential damage to particles in
the packing.
The piston walls are W x H = 15 x 15 cm and con-
nected via an aluminum rod to three linear stages (New-
port MTM250) controlled by a closed loop controller
(Newport XS4). Their step resolution is 1 micro meter,
and their speed is set to 0.1mm per second during exper-
iments to reduce the fluid induced shear stresses on the
particles. However, when a fluid of low enough viscosity
is used, faster piston movement can be used, creating tur-
bulent flow in the box, which can mix particles or change
the packing structure before an experiment. The piston
plate spacing is such that the edge between piston walls
is never large enough for a particle to escape from the
confines of the three pistons. This limits strain amplitude
to γ ∼ d/W ∼ 10% with d the particle diameter. Imaging
— A camera (Basler ava1000-120) equipped with 12mm
F/2.0 lens, and laser sheet (Lasiris SNF 635nm, 25mW,
30o fan angle) are mounted on the same stage, a design
similar to Ref [6]. To allow for fast imaging, the stage is
a screw driven DC stage (Intellidrives) with closed loop
controller (Accelnet). Imaging is done through a long
pass filter (Edmund Optics) with a cutoff wavelength of
650 nm. Camera triggering, camera and piston move-
ment and force measurements are coordinated through
LabVIEW based software.
Force [mN]
−2 −1 0 1
20
100 sec cycle
0
1000 sec cycle
Strain [%]
-1 0 1 2 3
FIGURE 2. (a) Typical growth dynamics of a single hydro-
gel sphere in demineralized water. The inset shows a dry and
fully grown sphere. (b) Compression force as a function of
strain for a single fully grown hydrogel sphere. Total cycle time
is 100 seconds (blue) and 1000 seconds (dashed red). The inset
shows the same data on double 10-logarithmic scale, with a
power law of exponent 1.5 indicated.
USING HYDROGEL SPHERES
RIM studies are mostly carried out using particles made
from either plastic or glass [7, 11, 12], index matched
with viscous and/or expensive liquids. However, recently
spherical particles made out of hydrogel (or polyacry-
lamide gel) have become commercially available [13].
Hydrogel offers considerable benefits over other materi-
als, the most important being that it is cheap, safe and
easily index matched with water. In addition, hydrogel
is soft, with a Young’s modulus in the 10 kPa range, so
it allows for the detection of contacts through its macro-
scopic deformation under modest forcing. Here, we de-
scribe hydrogel sphere properties such as their swelling
dynamics, compression resistance and frictional prop-
erties. We also discuss dying and density/index match-
ing techniques that make imaging of hydrogel parti-
cles practically possible. Swelling Dynamics — Poly-
acrylamide hydrogel spheres (proprietary formula from

458

JRM Chemicals) grow as indicated in Fig. 2a when sub-
mersed in demineralized water. They are purchased as
millimeter sized hard spheres; their final size depends
on the properties of their chemical environment such
as salinity, pH and temperature [14, 15]. The swelling
is reversible; upon drying, the particles revert to their
dry spherical shape. We describe the properties of these
spheres throughout the paper unless otherwise noted.
Note that hydrogel particles can be custom made with a
droplet pinch-off technique [16, 17] or by injection mold-
ing [18]. Mechanical Behavior — To measure the re-
sponse of a single sphere, we perform compression tests
in a TA Instruments Micro Strain Analyzer III. We com-
press a single hydrogel sphere vertically and uniaxially
between two steel plates and measure the resultant force
F as a function of strain γ . We use a fully swollen hy-
drogel sphere with no liquids on its surface to minimize
liquid bridge induced capillary forces. We perform ex-
periments in an open container and hence evaporation is
present. Linear elasticity theory would predict an expo-
nent of 1.5. Typical experimental results are shown in
Fig. 2. The force response F(γ ) is consistent with an ex-
ponent of 1.5. The prefactor Y in F = Y γ α is related to
the Young’s modulus of the hydrogel. Experimental re-
sults shown in Fig. 2a suggest that the Young’s modulus
for the hydrogel spheres grown in demineralized water is
∼10 kPa. This is in line with literature values [14], and
also depends on the chemical environment of the spheres
as they are grown [14, 15]; we always used demineral-
ized water as growing environment.
The hydrogel spheres are made out of cross-linked poly-
mers which form an elastic network. At any finite tem-
perature however, the elastic network bonds can discon-
nect and reattach randomly, allowing it to lower its in-
ternal stresses. The hydrogel network will therefore ad-
just to applied stresses [19, 20, 21]. This is also visi-
ble in Fig. 2 from the finite surface area of the force
loop; during the compression cycle of the sphere, the
polymer network evolves, leading to a different force re-
sponse. The pressure adjustment is more noticeable when
the compression loop is slowed. To characterize this re-
laxation more quantitatively, we compress a packing of
∼1000 spheres in a fixed volume and probe the pres-
sure response over time. The packing is fully submersed
to prevent evaporation of water in the hydrogel parti-
cles. Fig. 3a shows the typical pressure response. At late
times, an exponential relaxation can be observed, with a
decay timescale of about 5.1 hours. Subtracting the late
time behavior reveals an exponential early time relax-
ation process with a considerably faster decay timescale
of about 0.5 hours. This double relaxation process is ro-
bust: it is also present as a background process when the
packing is sheared quasi-statically. Although the com-
pression tests of a single sphere clearly shows a relax-
ation process, it is not known whether a single sphere
459
0
(a) 10
(b)
Pressure [Pa]
10
0
−2
10
−1
10
Time [sec] x 104 −4 Time [sec] x 103
10
0 1 2 3 0 5 10
FIGURE 3. (a) Pressure evolution of a packing of hydrogel
spheres kept at constant volume (blue solid line). An expo-
nential decay to zero at late times can be observed; the green
dashed line is a best fit with time constant of 5.1 hours. (b)
Subtracting the late time exponential decay, an early time ex-
ponential relaxation process with a different time constant is
observed (blue solid line). The red dashed line is a fit with
decay time of 0.5 hour. Note the different time scales in panel
(a) and (b).
also exhibits the same dynamical behavior as a packing
of spheres. Due to the thermal nature of the relaxation
process, a reduction in temperature may be sufficient in
order to reduce stress relaxation effects in hydrogels.
Hydrogel Friction — Hydrogels are readily ob-
served to be very slippery and have been shown to
have very low friction coefficient with glass or plastic
substrates [22, 23, 24]. We mesure the friction coeffi-
cient of a hydrogel-hydrogel (HH) contact by stacking
two dyed polyacrylamide hydrogel cubes (Educational
Innovations) on top of each other in a demineralized
water bath. The inclination angle at which the cubes
start to slide gives us an upper bound for HH friction
coefficient of < 0.03. The low friction of HH contacts
offers the possibility of probing the role of contact
friction on the stability of granular packings [4, 25].
Moreover, since low friction contacts cannot support
shear stresses, a deformation of the contact in a hydrogel
sphere is only due to normal forces. Linear elasticity
theory then provides a relationship between the con-
tact deformation and the applied normal force. Thus,
imaging the deformation of hydrogel spheres allows
for the extraction of contact forces in granular packings
in three dimensions. Density & Index Matching —
Hydrogel spheres contain 80-99.5% water by volume,
depending on their chemical environment. Thus, the
index of refraction of hydrogel spheres is higher, but
close to that of water. To image a dense packing of
particles, index matching of the fluid phase needs to be
fine tuned to that of the spheres to image as many layers
as possible [7]. Ordinarily, index matching is achieved
by dissolving a second component in the fluid phase. In
the case of hydrogel spheres, this approach can fail due
to the porosity of the hydrogel. Any small water-soluble
molecule, such as glycerol, will diffuse into the hydrogel
polymer network, raising both the index of the fluid and
the particle. There are two approaches to resolve this.
Macromolecules above a particular size are physically
too large to diffuse into the polymer network and stay
in the fluid phase. We found that polyethyleneglycol
(PEG) with a molecular weight of 40,000 diffused
into the hydrogel spheres on a timescale of hours, but
polyvinylpyrrolidone (PVP) 360,000 did not diffuse into
the hydrogel over a timescale of weeks. We measured the
diffusion speed by dissolving macromolecules in water
in which also hydrogel spheres were present. Since the
macromolecules also make the fluid denser, sufficient
solvent makes hydrogel particles float in the solution.
Diffusion of the molecules into the hydrogel network
can then be observed from the sinking of the particles.
A concentration gradient of PVP creates an osmotic
pressure on the hydrogel spheres, but this is not large
enough to result in any visible size change. The other
approach is by using water soluble components that do
not affect the swelling of the hydrogel too much, while
having a limited solubility inside the liquid environment
of the hydrogel matrix itself. For the spheres we used,
sodium thiosulfate (Na2 S2 O3 ) seemed to have desirable
properties [26]. Note that PVP can also be used to
density match the hydrogels to their fluid environment,
thereby creating a microgravity environment. It is not
known whether the concentration necessary to density
match the hydrogel spheres is identical to the PVP con-
centration necessary to index-match hydrogels. A third
water-soluble component can be used to both density
and index match a hydrogel sphere to that of its fluid
environment; acids are a possible candidate since they
do not affect the index or density of the fluid phase, but
selectively raise the index of the hydrogel, by making it
swell less. Note that PVP has been found to modify the
rheology and tribology of HH contacts [26].
In order to image the packing structure, an imaging
contrast agent is required. In standard RIM applications,
this is a fluorescent dye that is dissolved in the fluid
phase of the system. As mentioned above, the hydrogel
spheres are permeable to small molecules, including all
fluorescent dyes. A dye dissolved in the fluid phase will
therefore also be able to penetrate the hydrogel. Yet,
there are some fluorescent dyes that prefer to stay in the
hydrogel network rather than in the fluid phase. Upon
dissolving them in the fluid phase, they diffuse out of
the fluid, and into the hydrogel network, thus creating
a contrast. We have found several fluorescent dyes that
have this property, such as Nile Blue 690 (Exciton)
and Rhodamine 6G. For the image in Fig. 1b, we have
used Nile Blue 690. We do not have an explanation for
this behavior as very similar dyes have very different
hydrogel affinity – see Fig. 1e: out of the three different
rhodamine dyes used, only Rhodamine 6G has a sub-
stantial hydrogel affinity.
460
CONCLUSIONS
We have described how both the microstructure and
force response of a granular packing can be studied with
a triaxial shear setup in which shear and compression is
achieved through the movement of independent pistons.
We have discussed the use of hydrogel spheres as a
model granular system, by mapping out various essential
mechanical properties of such spheres, and by indicating
how they can be used in the triaxial shear setup.
We thank Jie Ren, Emily Lim and Ryan Pasca for
assisting with experiments, and Richard Nappi for
help in the machine shop. Discussions with Stefan
Zauscher, Walter Simmons and Daniel Morales are
gratefully acknowledged. This project was funded by
NSF-DMR0906908 and ARO-W911NF-11-1-0110;
Ryan Pasca acknowledges funding from the Durham
Public Schools Scientifica Program.
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