Kulkarni 2012
Kulkarni 2012
Kulkarni 2012
Copyright
C Taylor & Francis Group, LLC
109
110 M. C. KULKARNI AND O. O. OCHOA
FIG. 1. Schematic of an uncoated walnut shell flake. (Color figure available online.)
3.7 GPa. The stress-strain response of plant tissues is observed tives. The two microscopes are employed for microstructure and
to be biphasic and it is related to changes in the cellulose fibril image studies.
orientations [16]. Various models have been proposed to under-
stand the viscoelastic and plastic yield limits in plant tissues [17].
E3-ESEM Images of Walnut Shell
Herein, we report a study on ground walnut shell particles,
Three different walnut shell particle sizes are used in the
exploring their microstructure and mechanical response com-
microscopy studies; large uncoated (4 × 6 sieve mesh), coated
putationally and experimentally to enable the development of
particles, and uncoated particles 20 × 30 sieve. Specimens are
virtual parametric test bed capability.
prepared by fracturing with a sharp blade. ESEM images are
acquired on the fracture surface of the flakes (large uncoated
MICROSTRUCTURE AND IMAGE ANALYSIS particles; Figures 1a, 1b) scanning from the external to the in-
The study of the walnut shell microstructure is carried out to ternal edge along the shell thickness reflecting the variation in
(a) estimate the material properties based on its cellular struc- cellular structure. The ground particles can aid in addressing
ture and (b) to detect the polymer coating layer on the coated the presence of isotropy since the grinding procedure may have
particles as well as the state of further infiltration. Electroscan resulted in random orientation of the cell walls.
E3–ESEM can operate up to pressures of 50 torr with a resolu- The ESEM images in Figures 2a and 2b are captured along
tion of 5 nm. Its magnification ranges from 100 × to 100,000 ×. the thickness of the shell on the fracture surface from the ex-
Additionally, it has a Peltier cooling stage and a heating stage ternal edge towards the internal edge to display any variation
with a range up to 1000◦ C. Zeiss Axiophot light microscope in cell structure. The walnut shell has a porous soft layer near
is equipped for bright field and phase contrast, transmitted and its inner edge. A layer of suberin with little porosity constitutes
reflected polarization, and Nomarski differential interference the outer surface. This layer provides a barrier for moisture and
contrast microscopy. Its optics range from 2.5 × to 40 × dry other chemical attacks and protects the nut. A high magnifica-
objectives and 63 ×/1.40 and 100 ×/1.3 oil immersion objec- tion image of the fracture surface near the external edge, which
FIG. 2. ESEM image on fracture surface of 4 × 6 mesh flakes: (a) near external surface and (b) near internal surface. (c) A high magnification ESEM image of
the region in Figure 2a.
LIGHT WEIGHT COMPOSITE PROPPANTS STUDY 111
FIG. 5. Traces of polymer infiltration into the particle ∼25 µm deep. (Color
FIG. 3. Image of a fracture surface of coated particle. figure available online.)
112 M. C. KULKARNI AND O. O. OCHOA
FIG. 7. Segregation of particles in groups (coated particles). (Color figure available online.)
LIGHT WEIGHT COMPOSITE PROPPANTS STUDY 113
175 175
Load (N)
flat top 5
Load (N)
Cone top 5
75 75
50 50
25 25
0 0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
Displacement (mm) Displacement (mm)
(a) (b)
175
rounded top 1
150
rounded top 2
rounded top 5
100
Load (N)
rounded top 4
75
50
25
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Displacement (mm)
(c)
FIG. 8. (a) Force vs. displacement for flat top particle group. (b) Force vs. displacement for cone top particle group. (c) Force vs. displacement for rounded top
particle group. (Color figure available online.)
conducted in displacement controlled mode at a rate of 0.01 banding is observed in the coated particles compared to uncoated
mm/sec. The tests are terminated at a peak load of 150 N with particles.
a 10 N initial preload.
The particles are classified into three geometric groups to
reduce statistical scatter. Herein, they will be referred to as flat- Nonlinear Material Response in Compression
top, round-top, and cone-top particles as displayed in Figure 7. Uniformly shaped cuboids with dimensions of ∼2 mm ×
Note that the round-top particles have a fairly curved profile, the 2 mm × 1 mm are cut from the 4 × 6 mesh size flakes with a
cone-top has a seemingly sharp profile angle, and the flat-top jeweler’s saw. An image of one typical cuboid is presented in
particles resemble cuboids. Figure 10. The loading direction is along the 1 mm direction. In
The results from force versus displacement responses are total, 6 particles were tested. The loading rate was maintained
summarized in Figures 8a–8c. The stiffest response with the at 0.025 mm/sec as per the specifications in ASTM standard
least scatter is obtained with the flat top particles in the data. The D695–02a [20]. The load versus displacement response for the
significant variation in the response of the particles subjected test is presented in Figure 11a.
to compression can be attributed to the shape effect since the The particles, on average, were crushed at 550–600 N at an
material property is assumed to be isotropic due to isodiametric axial cross-head displacement of about 0.8 mm. The inelastic
sclereid cells. constitutive relationship for the finite element analysis (FEA)
The force versus displacement response of the coated models was based on cuboid-3 particle. The load versus dis-
and the uncoated flat top particles are presented in Figure placement data was transformed to true stress versus strain data
9 revealing minor differences. It also appears that a closer for the FEMA models (Figure 11b).
114 M. C. KULKARNI AND O. O. OCHOA
180
160
140
120 rawflat1
rawflat2
Load (N)
100 rawflat3
rawflat4
80 rawflat5
coalat1
60
coalat2
coalat3
40
coalat4
20 coalat5
flatcoat6
0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35
Displacement (mm)
FIG. 9. Comparison between coated and uncoated flat top particles. (Color figure available online.)
COMPUTATIONAL MODELS the density ratio and the effective properties of the cell wall
[10], the axial elastic modulus is defined as Eaxial = Ewall ∗
Effective Elastic Modulus Estimate
(ρmaterial /ρwall ); similarly, the transverse modulus is defined as
The elastic modulus of walnut shells depends on the ratio Etransverse = 0.54 ∗ Ewall ∗ (ρmaterial /ρwall )3 [7] for wood. The two
of walnut shell density and the density of its cell wall. The relationships are derived based on considering a honeycomb
density of the cell wall for different wood species is specified structure for wood with thin walls. The normal loading on this
as 1500 kg/m3 [7]. From the experimental data [21], the density structure (i.e., along the wall depth) gives the equation for Eaxial
of raw (uncoated) walnut shell particle is 1290 kg/m3 leading to from a simple rule of mixtures. The transverse loading on this
a density ratio of about 0.86. This value is also corroborated by structure results in the bending of walls and gives the expression
our ESEM and LM study of the microstructure and cell type of for Etransverse . For the current study, the cell structure for walnut
walnut shells as sclereids, which indicate a very low porosity in shells is assumed to be similar to that of wood and the relations
the structure. are applied to obtain a rough estimate of the range for elastic
The cell walls of the ground walnut shells are treated as a modulus of walnut shells. The cell wall elastic modulus will vary
composite where cellulose is considered to be the reinforcing with cellulose fibril angle, which accounts for the range. The
fiber and hemicelluloses and lignin form the matrix. Based on highest values are for fibril angles 0◦ and lowest for fibril angles
FIG. 10. Two different views of uniformly cut cuboid particle. (Color figure available online.)
LIGHT WEIGHT COMPOSITE PROPPANTS STUDY 115
1400 160
140
1200
Cuboid test 1
Stress (MPa)
800
Load (N)
Cuboid test 5
80
Cuboid test 6 Nominal stress strain
600
60 True stress strain curve
400
Complete crush of 40
the particles
200
20
0 0
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80
Displacement (mm) Strain (mm/mm)
(a) (b)
FIG. 11. (a) Load vs. displacement response for uniformly cut walnut shell flakes. (b) Nominal and true stress strain curve for Cuboid test 3 data. (Color figure
available online.)
50◦ [10]. These values for the axial modulus are estimated to model under compression. The elastic modulus for the uncoated
be in the range of 8.6–30.1 GPa, while the transverse modulus walnut particle was assigned as 3700 MPa. This selection was
is expected to be within 3.5–10 GPa. It is further assumed that, based on the range of elastic moduli values for nut shells [13–15]
due to random grinding to produce small mesh size particles, and the material isotropy in the case of ground walnut shells.
the particle is isotropic. The platens are modeled as rigid surfaces. Contact interaction is
defined between the platens and the particle models to transmit
FEA Models of Uncoated Particles the incremental compressive load to the particle [22].
Since the OM and ESEM images confirmed that the par- The three-dimensional FEM meshes for the three shape
ticles are far from any idealized regular shape, realistic shapes classes are displayed in Figure 12. FT1 represents the flat top
guided by the images are created for the ABAQUS© FE models. particle class with 21,521 elements whereas CT1 represents the
Three-dimension tetrahedral C3D4 elements with three dis- cone top particle class with 23,723 elements, while model RT1 is
placement degrees of freedom at each node are employed. Static based on the round top particle class and has 32,591 elements.
analysis with nonlinear geometry and nonlinear material are se- The dimensions of the models based on the test particles are
lected for computing displacement, strain, and stresses in the ∼1.5 mm × 1.2 mm × 1 mm. A fine mesh is maintained in the
region of initial contact with the platens and graded outwards to
economize computational resources.
120
100
Cone top
Flat top Round top
80
Uncoated 1
Load (N)
Uncoated 2
60 Uncoated 3
Uncoated 4
Uncoated 5
40 3D-FT1
3D-RT1
3D-CT1
20 FT1-NONLINEAR
RT1-NONLINEAR
CT1-NONLINEAR
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Displacement (mm)
120
Figure 13 in comparison to the elastic, which gives a highly
stiff response depicted in the curves on the left hand side of the
100
figure. The significance of shape on the particle response is also
highlighted through the implementation of nonlinear material
80
definition.
Load (N)
60
3D - FT1
40
3D - CFT1 FEA Models of Coated Particles
3D - RT1
3D - CRT1
Coated particles are modeled by introducing a layer of phe-
20 3D - CT1 nolic polymer coat on the irregular shaped 3D particles (FT1,
3D - CCT1 RT1, and CT1) with inelastic material properties. The polymer
0 coat thickness is 10 µm. The elastic modulus and the tensile
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Displacement (mm) strength of the polymer are obtained from the literature [24].
The polymer coat is also assumed to possess nonlinear (plastic
FIG. 14. Comparison of load vs. displacement response of walnut particle
isotropic hardening) behavior. The hardening slope of polymer
when coated and uncoated. (Color figure available online.)
is assumed to be equivalent to the walnut shell cuboid test-3 re-
sponse. It is not based on any experimental or literary evidence;
The nonlinear material response is assumed to be also, the tensile strength mentioned in the literature is assumed
elastic–plastic with isotropic hardening. The stress strain data to be the yield strength of the polymer. The true stress versus
from the true stress versus true strain curve generated from the true strain response is used to model the nonlinear behavior.
cuboid walnut particle tests are used as input into ABAQUS© To study the effectiveness of the resin coat in improving the
to simulate the elastic–plastic isotropic hardening response of stiffness of the particles, displacements in the walnut core of the
the uncoated particles. It is assumed that the particles undergo coated particles are reported at the node just underneath the first
non-recoverable deformation at a very low stress and the linear contact point on the coating and on the coated walnut interface.
behavior observed is a hardening response. Similar conclusions The comparison of the response of walnut shell particles with
have been drawn for the plastic stress versus strain response of and without coating is presented in Figure 14. The difference is
some plant tissues by Niklas [23]. In the FEM models, the onset marginal.
of plasticity is triggered at a very early stage at a low stress of ∼5 The contour plots depicting the Von Mises stress and LE22
MPa to reflect test data. The analysis is defined as geometrically (logarithmic strain in 2-2 direction) for the walnut core of the
nonlinear to account for large displacements. coated flat top particle and the uncoated flat top particle (CFT1
The vertical displacements of the platens are 0.329, 0.477, and FT1) are presented in Figures 15 and 16. Even though
and 0.6823 mm, respectively, for FT1, RT1, and CT1 models at the coated walnut shell particle experiences the same value of
100 N load. The flat top particle provides the stiffest response maximum Von Mises stress, its distribution is over a smaller area
followed by round top and cone top. This is in accordance with at the same load level when compared to the uncoated particle.
the observations from the single particle tests on geometrically In both cases, the particle is plastically deformed but the extent
classified particles. The inelastic material definition is better of plastic deformation is less in the coated particle. The same
suited to simulate the compression response as shown in observations hold for the strain in the 2-2 direction.
FIG. 15. Comparison of Von Mises stress distribution in walnut region of coated and uncoated flat top particle at 100 N load. (Color figure available online.)
LIGHT WEIGHT COMPOSITE PROPPANTS STUDY 117
FIG. 16. Comparison of true strain in (2-2) direction contour on the walnut region of coated and uncoated flat top particle at 100 N load. (Color figure available
online.)
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linear-elastic range, Planta, vol. 215, pp. 33–40, 2002. Providence, RI, USA, 2005.
18. H.D. Brannon, C.J. Stephenson, and R. Maharidge, Personal Communica- 23. K.J. Niklas, Plant Biomechanics: An Engineering Approach to Plant Form
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