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Project C Tensile Test

Author: Austin Dowell, Joshua Phonpadith


WSU ME406, Pullman, WA
5/24/2019
Summary
We were tasked with re-creating, designing, and operating a tensile test for a polymer
based gel in order to characterize the performance of the material. To do so, we needed to
create a clamping system to fix the material and then observe the crack propagation using a
camera to record the velocity. In order to replicate the original paper titled “Fracture of a
biopolymer gel as a viscoplastic disentanglement process”, we tested one sample that had no
initial cut in the gel and two samples with a 20 mm cut in the middle where the fracture should
propagate. We decided to deviate slightly from the original gel design by tapering the ends of
the sample in a concave manner, which would allow the crack to propagate down the middle
and give us correct data that we can analyze.

Introduction
In our experiment, we performed a tensile test on a biopolymer hydrogel, which can
essentially replicate liver tissue. A hydrogel is a three-dimensional polymeric network filled with
mostly water. Biopolymer hydrogels have been attracting increased attention from researchers
due to their extensive use in the biomedical and food industries, specifically for their use in cell
therapeutics, wound healing, and cartilage regeneration research. Studying the fracture
mechanics of these hydrogels is important because the fracture process is responsible for the
rate dependence of their strength. Additional research into this relationship is necessary for
improvements in current industrial uses.
The procedure for creating our biopolymer was thoroughly described by Ding [2]. By
mixing mineral oil and Poly (styrene-b-ethylene-co-butylene-b-styrene) triblock copolymer
(SEBS) produced by Kraton Polymers LLC (G1650, Houston, TX, USA), we are able to create
the hydrogel simulant of a biological tissue. The densities of SEBS and mineral oil are 0.91 g/ml
and 0.85 /ml, respectively. To process the simulant, SEBS powder and white mineral oil are
mixed by weight. The fraction of the polymer used in this study is 15%. The mixture was heated
in the oven at 120℃ for 2 to 8 hours (the more SEBS the mixture contains, the more time will be
needed for melting) and was stirred occasionally to produce a homogeneous solution without
any visible undissolved powder. The solution is degassed to eliminate any air bubbles trapped
in the solution and then poured into the mold. The molded mixture is left in the room
temperature for it to cool down before being removed from the mold. Fig. 1 below shows the 3
biopolymer samples that we used in our experiments.

Fig. 1 A picture of the three biopolymer gels used in our experiments.


Objectives
Our objective is to characterize the fracture toughness of the biopolymer simulant. A
sufficient amount of data to characterize the material was collected by observing the fracture
process during a tensile test under a high speed camera and using a load cell to measure the
force on the specimen during the experiment. Our goal was to perform a successful experiment
on the three specimens created and successful is defined as a clean tear in the middle of the
specimen with minimal deviation.

Approach
Starting from the beginning, we first had to create the molds that were used to actually
create the hydrogels we would be testing. Daniel Portillo and Juan Reyes, members of Group B
performing a similar type of tensile test, assisted in 3d printing a top and bottom cover of the
mold, shown in Fig. 2 below. 3d printed covers were necessary to create because rather than a
purely rectangular gel, we wanted to indent triangles in the sides of the gel in order to ensure
the crack would propagate directly through the middle of the gel for the entire length of the body.
The triangle housing on the top of the 3d printed part what gives the gel in the indent that we
desired. There is a staircase like structure because the gels that we were testing 30 mm wide
whereas the gels that Group B were sampling were only 15 mm wide. The staircase structure
was a solution that allowed both us and Group B to use the same top and bottom 3d printed
pieces to create our gel molds. We then laser cut and glued together acrylic in order to create
the sides of the mold housing that encase the specific dimensions of the gel we wanted to mold,
shown in Fig. 3. Our gel was 30 mm wide, 10 mm wide (5 mm at the shortest point) and 300
mm long, which was later cut to 250 mm to get more accurate data while testing. The entire
housing put together can be seen in Fig. 4, where a 3d printed top and bottom are locked within
the acrylic housing sides.

Fig. 2 A picture of the 3d printed cover used to create our gel mold.
Fig. 3 A picture of the acrylic sides of the mold housing.

Fig. 4 A picture of the gel housing pieced together, with a gel mold inside.

We then had to manufacture two aluminum plates and one aluminum block for our
tensile test. The aluminum plates were used to clamp the gel together and the block was held in
a clamp and screwed to the bottom plate. A Solidworks drawing of the block is shown in Fig. 5
below and a Solidworks drawing of the aluminum plate is in Figure 6. The block is 1 inch x 1
inch x .5 inch block with a ¼” Nf thread size in the top middle. The plates are 320 mm x 20 mm
x 6.25mm with a ¼” Nf thread size in the middle of the plates.
Fig. 5 The Solidworks drawing of the block for our experimental system.

Fig. 6 The Solidworks drawing of the aluminum plates for our experimental system.

A diagram of the experimental setup can be seen in Fig. 7 below with each item labeled
for clarity. Our final setup was extremely similar, albeit rotated 90 degrees to the left and seen in
Fig. 8. The gel was glued between both of the aluminum plates and thoroughly dried before
being tested. The bottom plate was screwed into an aluminum block and clamped to the instron
tensile load machine while a 5 kg load cell was screwed into the top of the plate in order to
measure the force exerted on the gel during the test. Before beginning the test, a speed was
selected for how fast the top plate would extend upwards (we used both .05 and .10 mm/s) and
how fast data should be collected (every 50 ms). When started, the machine pulled the top
clamp upwards while leaving the bottom clamp fixed, thus adding a tensile force to the top of the
specimen and stretching it out. The experiments were run until the material crack propagated
through the entire length of the body. We tested a total of three gel specimens, one with a 20
mm cut in the middle of the specimen at .05 mm/s, one with a 20 mm cut in the middle of the
specimen at .10 mm/s, and one with a no initial cut in the middle of the specimen at .10 mm/s.
Fig. 7 A schematic diagram of our experimental setup based on the original experiment we are
recreating.

Fig. 8 A picture of our experimental setup moments before running the tensile test.

Analysis
During each trial, a computer connected to the tensile testing machine and load cell
would measure the time (s), machine extension (mm), and the load (N) on the load cell every 50
ms. This data was recorded from the start of every trial to the very end when the crack
propagated fully through and the material and was split into two pieces. After taking data for
three trials, with different conditions described in Table 1 below, we exported the data to an
Excel file to analyze. For each load data point, 1.78 N was added in order to take into account
the amount of force coming from the bottom half of the gel, the bottom aluminum plate, and the
rod and aluminum block on the load cell. The crack propagation velocity was measured by
taking a video of each trial and including an inch scale measuring tape in the background and
then stop the video at two distinct times and measuring the difference in crack length. The
length difference divided by the time difference gave us the velocity of the crack propagation,
which was fairly steady during the trials due to the machine loading rate being constant.
For the test without the initial 20 mm cut in the middle, a stress-strain relationship was
analyzed using the data gathered during the experiment and presented in Fig. 10. The stress
was calculated by multiplying the force on the load cell by the sample area and dividing by 1000
to get units in kPa. Strain was calculated by dividing the extension of the machine by the original
height of the specimen (30 mm). For the tests with an initial 20 mm cut, crack area was
determined by multiplying the width of the crack (5 mm) by the extension of the machine. Work
was calculated by dividing the load cell force by 1000 and then multiplying by the machine
extension to get units of J. Finally, fracture toughness was calculated by dividing the work by the
crack area for units of J/m^2 and then averaging those values to get an overall usable value that
can be graphed against the crack propagation velocity.

Table 1. A table of all three trials and the variables changed during each one
Test Machine Loading Rate Initial Cut?

1 .05 mm/s Yes

2 .10 mm/s Yes

3 .10 mm/s No

Results and Discussion

Fig. 9 Fracture Energy vs Crack Velocities with 20 mm cut at different loading speeds.
Test 1 and Test 2 were graphed in this plot to illustrate the relationship between fracture
energy, crack velocity, and machine loading speed. Test 1 represents the sample data at a
loading speed of 0.05 mm/s and Test 2 represents data at a loading speed of 0.1 mm/s
(doubled that of test 1). The biggest detail to take note on is the slope between the two points.
We can clearly see an upward trend of the fracture energy as velocity of the crack increases.
We can also determine that fracture energy increases as loading speed increases, thus
increasing propagation speed as well. If we compare our analysis to the data plot from our
reference paper [1], they are relatively the same, which goes to show our experiments worked
successfully. We only have two points on the graph because we were only able to test two gel
specimens with an initial crack in them due to time constraints, whereas the reference paper [1]
has hundreds of plotted points because they tested hundreds of specimens.

Fig. 10 Stress/Strain curve for specimen 3 (no initial 20 mm cut).

In Fig. 10, we see a stress/strain curve for the one specimen without the initial 20 mm
cut down the middle. The orange curve represents the ideal curve from the modulus of
elasticity. From this curve we can identify that the specimen had more resistance to fracture as
the stress increased. Then, as the cut starts to propagate from around 8 kPa, the curve’s slope
starts to decrease until around 0.31 (mm/mm). At this point the sample is completely torn apart
and the point of complete fracture is made. One thing to consider when looking at this graph is
that the test sample starts to come apart at the top glue between the sample and aluminum
plate, which could have skewed some of the data (possibly between 0.36 mm/mm to 0.5
mm/mm). However, the graph above closely resembles the one in the reference paper [1], so
we can conclude the data is accurate enough.

Conclusion
We encountered a variety of issues throughout the entire process, and from those issues
have come up with useful solutions if further tests will be performed. We first encountered
issues with our aluminum plates. When set up in the testing machine, they were not exactly
parallel, most likely due to the ¼” NF holes being tapped at an angle, which would affect the
forces measured during the experiment. In order to solve this problem, we would recommend
having a machining expert make new aluminum plates that are parallel and have perpendicular
tapped holes that don’t only go halfway through and use ½” thick aluminum rather than ¼” thick.
Every time we glued the gel to our aluminum plates, glue would get stuck inside the tapped
holes and we’d have to clean them out before every test. Making the plate thicker and not
tapping the holes all the way through will guarantee that no glue will get stuck inside when
gluing the gel to the plates. We also recommend finding a better way to guarantee that no air
pockets exist within the gel during the gel forming process. We had reduce our samples from
300 mm in length to 250 mm due to an air pocket that made it so we couldn’t adequately glue
the top of the gel to the aluminum plate. Finally, we’d recommend possibly switching to an
epoxy glue. The glue we used (M-Bond 200 Adhesive) doesn’t fill in voids or bubbles when
applied unlike an epoxy that would. Our glue would also take at least 10 minutes per side to fully
dry and the glue gave out before the tear in the gel did on 3 separate occasions, drastically
increasing the amount of time it took to test 3 samples. Lastly, we would recommend testing
different material percentages, 10% and 20% being the next most common.

References
[1] T. Baumbergera , C. Caroli, and D. Martina, 2006, “Fracture of a biopolymer gel as a
viscoplastic disentanglement process,” The European Physical Journal, pp. 81-89.
[2] J. Ding, 2019, “Project C - supplemental information,” pp. 1.
[3] A. Hoffman, 2012, “Hydrogels for biomedical applications,” ScienceDirect, pp. 18-23.

Appendices

Equipment List
Instron tensile testing machine
5 kg load cell
2 aluminum plates (320 x 20 x 6.35 mm) with ¼” NF
1 aluminum block (1 x 1 x 0.5 in) with ¼” NF
Gel specimens (30 x 10 x 250 mm)
Gel mold (Acrylic housing sides with 3d printed top and bottom)

Sample Data
Fig. 11 A screenshot of sample data collected and analyzed from Test 1.

Fig. 12 A screenshot of sample data collected and analyzed from Test 2.


Fig. 13 A screenshot of sample data collected and analyzed from Test 3.

Sample Calculations

Sample Calculations from Test 2 @ 0.05 sec:

Real Load Cell (including the added weight of bottom fixture) = Load Cell Force (N) + Added
Weight (N)
Load Cell Force = -0.05801 N, Added Weight = 1.78 N
Real Load Cell = -0.05801 N+1.78 N = 1.72199 N

Crack Area = Extension (m)*Crack Width (m)


Extension = 0.00000029 m
Crack Width = 0.005 m
Crack Area = 0.00000029 m*0.005 m = 1.45 E-9 m^2

Work = Extension (m) * Real Load Cell (N)


Extension = 0.00000029 m
Real Load Cell = 1.72199 N
Work = 0.00000029 m*1.72199 N = 4.99377E-7 J

Fracture Energy = Work (J)/Crack Area (m^2)


Work = 4.99377E-7 J
Crack Area = 1.45E-9 m^2
Fracture Energy = 4.99377E-7 J/1.45E-9 m^2 = 344.398 J

Sample Calculations from Test 3 @ 0.15 sec:

Stress (kPa) = (Force (N)/Sample Area (m^2))/1000 = (Force (N)/Sample Width (m) * Sample
Length (m))/1000
Force = 0.86963 N
Sample Width = 0.005 m
Sample Length = 0.25 m
Stress = 0.86963 N/(0.005 m*0.25 m)/1000 = 0.695704 kPa

Strain (mm/mm) = Extension Height (mm)/Original Height (mm)


Extension Height = 0.00006 mm
Original Height = 30 mm
Strain = 0.00006 mm/30 mm = 0.000002 (mm/mm)

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