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EFFECTS OF CONSOLIDATION PROCESS ON THE TENSILE STRENGTH OF

UHMWPE FILAMENTS EXTRACTED FROM COMPOSITE PANELS

Conference Paper · September 2023

DOI: 10.12783/asc38/36615

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Session Topic Number and Topic Title: Verification and Validation – 7. Materials Characterization

Effects of Consolidation Process on the Tensile Strength of UHMWPE Filaments

Extracted from Composite Panels

Ahmad Abu Obaid 1 , Sagar M. Doshi1 , Michael Yeager2 ,

Travis A. Bogetti2 , Joseph M. Deitzel1 , John W. Gillespie, Jr.1
1 - Center for Composites Materials, University of Delaware, Newark, DE, 19716, USA
2-Army Research Laboratory, Aberdeen, MD, 21005, USA

ABSTRACT

This research focuses on the investigation of damage mechanisms induced through

the processing and consolidation of UHMWPE composites (HB210). The HB210
composites consist of Dyneema® fibers and thermoplastic polyurethane resin. The
composite panel consisting of 72 sheets was processed following the manufacturer’s
recommended temperature and pressure profile of 100°C and 2 MPa (290 psi) for 10
minutes, followed by 125°C and 20.7MPa (3ksi) for 30 minutes. Each sheet consists of
0/90/0/90 ply orientation with an average sheet thickness of 200 µm.
To quantify the effects of consolidation pressure on fiber deformation and tensile
strength distribution, a technique for extracting fibers from the processed panels was
developed. Specimens (11 x 19 x 152 mm) were cut from the panel and immersed in
tetrahydrafuran (THF) fluid for 7-20 days (dependent on the specimen thickness). The
THF effectively dissolved the matrix enabling UHMWPE fibers to be extracted at
different locations through the thickness. The baseline tensile strength distribution was
based on testing virgin fibers from the spool and fibers extracted using the THF method
from a single as-received layer of HB210. The two baselines exhibited statistically
equivalent tensile strength distributions proving the THF extraction method did not
affect the fiber properties and that degradation of tensile strength is a result of the
consolidation process. From tensile test data, strength distributions for extracted fibers
from consolidated panel were generated, and strength at 50% failure probability was
evaluated. Compared to the baseline, the fibers extracted from the processed panel
showed a 15% reduction in the average tensile strength.
SEM microscopy of the extracted fibers from the consolidated panel exhibits
different damage modes. Surface cracking and flattening damage modes were induced
by the consolidation pressure (20.7 MPa) applied in the thickness direction of the panel.
Additionally, axial kinking was observed along the length of the fibers. The possible
mechanisms for the formation of these kinks are – viscous forces from the resin during
the consolidation process, where fibers loaded in compression are observed to kink into
large voids between fibers, or due to the CTE mismatch between the fibers and the resin
within a layer or between the 0 and 90 layers within a sheet during the cooling stage.
DSC experiments carried out on extracted fibers from different regions (top, middle,
and bottom) of the panel show no change in the onset and melt temperature (~147°C)

Ahmad AbuObaid, Sagar M. Doshi, Joseph M. Deitzel and John W. Gillespie, Jr., Center
for Composites Materials, University of Delaware, Newark, DE, 19716, USA
Michael Yeager and Travis A. Bogetti, DEVCOM Army Research Laboratory, Aberdeen,
MD, 21005, USA
when compared to results from virgin fibers. This indicates that the fibers did not
undergo any thermally induced change in the crystalline phase of the fiber.

INTRODUCTION

Ultrahigh molecular weight polyethylene (UHMWPE) fibers possess excellent

specific strength, wear-resistance, toughness, and chemical inertness. UHMWPE fibers
are used in wear, biomedical, structural, and protection applications [1-8]. The impact
performance of UHMWPE composites is highly dependent on the axial tensile
properties of the fiber. Studies characterizing these composites have shown the presence
of voids within the fibers and the matrix regions [6,7]. Upon consolidation, the porosity
is reduced and can increase the fiber volume fraction and tensile properties. However,
excessive consolidation pressures or processing temperatures can induce fiber damage
by flattening, kinking, or fibrillating. Previous studies have shown residual tensile
strength after transverse compression of single fibers is reduced by ~10%, and
molecular level models have shown a reduction in tensile strengths after kinking [9,10].
Therefore, the consolidation process, temperature, pressure, and heating/cooling ramps
are critical for the optimum performance of the UHMWPE composites [8].
It is expected that the fiber properties can be significantly affected during the
consolidation of UHMWPE fibers which is due to the nature of the fiber microstructure
created during gel-spinning followed by the drawing process. It has been shown in the
literature [11,12] that the gel-spun UHMWPE fiber consists of extended chain fibrils
(shish), interlocking, epitaxial crystals, and voids between the fibrils. McDaniel et al.
[11] observed thickening of the epitaxial structure of UHMWPE fiber after annealing
above 120°C. The effect of transverse compression on the properties of UHMWPE
fibers was investigated in literature [9,13]. It was found that the cross-sectional area of
Dyneema® SK76 fibers subjected to transverse compression was found to increase up
to a maximum of 1.83 times the original area at 46% nominal strain [9], where this effect
was attributed to the fibrillation mechanism that generates non-uniform fibril nesting
and nucleation of voids between the fibrils. For the same type of fiber, Sockalingam et.
al [13] found that the transverse compression induces an inelastic behavior of the fiber,
which was attributed to microstructural damage. Chowdhury et al. [10] used molecular
dynamics (MD) simulations to explain the experimental observation of tensile strength
reduction of UHMWPE crystals after exposure to transverse compression is due to a
disruption of the crystal structure at the atomistic scale.
Since inelastic responses, as well as structural properties of UHMWPE composites,
are highly dependent on the tensile strength of the fiber, this work focuses on damage
modes that adversely affect the property of the UHMWPE fibers. Therefore, the main
goal of this effort is to isolate the effects of the consolidation process on the tensile
strength and microstructure of fibers at filament scale using a standard mechanical test
and high-resolution microscopy methods.
EXPERIMENTAL METHODS
MATERIALS

Dyneema®SK99/resin sheet (HB210) consists of four unidirectional layers

impregnated with high elongation thermoplastic resin (i.e., thermoplastic polyurethane)
with a stacking sequence of 0/90/0/90. HB210 sheet has a nominal thickness of 200
µm, a nominal areal density of 136 g/m2, and a nominal resin content of 20%. More
details, particularly for HB210 sheets, are kept proprietary by the supplier.
Dyneema®SK99 fibers are described to have nominal properties, such as a strength 4.1
GPa, a failure strain of 3.5%, and an elastic modulus of 155 GPa [14].

CONSOLIDATION OF THE HB210-PANELS

HB210 laminates were processed applying the manufacturer’s recommended

Temperature and pressure profile (see Figure 1) of 100C and 2MPa (290 psi) for 10
minutes, followed by 125°C and 20.7 MPa (3 ksi) for 30 minutes. Each processed panel
consists of 75 HB210 sheets and has dimensions of 381 mm x 381 mm x 11.4 mm.
Based on the nominal thickness of each HB210 layer, the consolidation process reduced
the thickness after the process by 24%.

Figure 1. Recommended consolidation profile for Dyneema HB composite materials (Left) and
Dyneema HB210 composite panel (Right)

EXTRACTION OF FILAMENTS FROM CONSOLIDATED HB210-PANEL

To investigate the effect of processing of HB210 composites on fiber properties
(morphology/deformation, local damage, and strength), filaments were extracted from
consolidated panels for mechanical testing and microscopy. Because UHMWPE fibers
are chemically resistant to most organic solvents at room temperature, the most
straightforward approach to extract these fibers was to dissolve the thermoplastic matrix
using Tetrahydrofuran (THF), which is an effective solvent for the matrix used in this
composite. This conclusion was obtained from conducting several trials, such as
changing the type of solvent (such as Toluene) and varying the soaking time. The fiber
extraction procedure was carried out after immersion of the samples (as-received and
consolidated HB210 sheets) in THF liquid at room temperature for 7-20 days,
depending on the sample thickness. As received HB210 sheets (200µm thick) were
immersed in THF for 7 days allowing the extraction of the fibers from the sheet
sublayers, without inducing damage. Thick consolidated HB210 samples with
dimensions of 11 x 19 x 152 mm were cut from the center of the consolidated panel and
fully immersed in THF for 20 days, where the THF partially dissolved the matrix,
enabling us to separate the sublayers. Then, the filaments were extracted from these
sublayers after 7 days of soaking in THF (see Figure 2).

Soaking the sublayers Extracted fibers from the sublayers.

for 7 days

Figure 2. Extraction procedure of the fibers from sublayers after soaking in THF for 7 days.

SEM images (Figure 3) for both virgin fibers and fibers from the as-received HB210
sheets are free of damage and show negligible differences in terms of diameter (~11.5
µm) and morphology. These results confirm that the extraction procedure has no
significant effect on the surface morphology of fibers extracted from the HB210 sheets.
The effect of extraction procedure on the strength of the fiber will be discussed in the
results and discussion section of this paper.

1.

Virgin Fibers Unprocessed HB210 Fibers

Figure 3. SEM micrographs of virgin fibers from the spool and fibers extracted from unprocessed
HB210 sheets.

TENSILE MECHANICAL TESTING ON FILAMENTS

To investigate the effect of the consolidation parameters (Temperature, pressure,

and dwell time) on the strength of the filaments, single filament tensile testing was
performed. Single filament tensile testing, particularly of UHMWPE fiber, is
challenging because the surface of PE fiber has an inherently low friction coefficient,
making the gripping of filament ends extraordinarily difficult. Several tension
methods from the literature [15-16] were examined and tried with limited success.
The main issue of these methods is that filament ends would pull out from the grips
before tensile failure was achieved. Alternatively, increasing grip pressure on the
filaments to reduce fiber slippage leads to premature failure at the grips rather than
in the gauge length, yielding skewed strength results.
To overcome this challenge, a novel procedure was developed (Figure 4). The
approach employs two capstan-type grips, where the circumference of each gripping
surface was wrapped with heavy duty double sided adhesive tape. In this method, the
double-sided tape strongly holds the wound fiber in place to reduce slippage during
tensile loading and promote acceptable tensile failure within the gauge length.
In this effort, the capstan grips were mounted in a mechanical test frame (Instron
Micro tester 5848 test frame) equipped with a 5 N load cell. Using the developed
winding method discussed above, tensile testing was conducted at 25 mm gauge length
and 5 mm/min cross head speed (see Figure 4). Tensile testing was conducted on three
sets of single fibers, virgin fibers from the spool, fibers extracted from as received
HB210 prepreg (without consolidation in the hot press), and fibers extracted from the
consolidated HB210 panel subjected to the recommended process cycle.
It is noteworthy that, prior to tensile testing, the fiber diameter on 7-10 different
locations within the gauge length range for each single filament specimen using a high-
resolution microscope (VHX) at 1000x. This diameter was used to calculate the filament
cross section for determination of the ultimate tensile strength. For each type of fiber
condition, at least 80 specimens were tested and evaluated.

A) B)

Filament

Capstan grip covered

with double sided
tape.

Figure 4. A) Modified capstan grips for UHMWPE single filament tensile testing and B) Mounting
the sample in the capstan grips installed in the micro-mechanical test frame.

DIFFERENTIAL SCANNING CALORIMETRY (DSC) TESTS

Differential Scanning Calorimetry (DSC) tests were conducted on virgin fibers and
extracted fibers from three regions of the processed composite panel. The primary aim
of the DSC test is to investigate the effects of the consolidation process on thermal
properties and validate that the fibers weren’t subjected to higher temperatures where
they could have melted or undergone phase change that would affect tensile strength. It
is noteworthy that the specimen preparation can significantly affect the thermal results.
Therefore, DSC samples were prepared following the methodology established in the
literature by Wunderlich et al. [17-18]. For DSC tests, a group of filament fibers was
cut into 4 mm lengths and placed flat in the DSC pan. A ~0.4 mg weight of the sample
was used to minimize the artifacts that arise from thermal lag in the sample and
confinement of the fiber during heating. DCS tests were performed at a heating rate of
10°C/min, where the analysis was carried out for the first heating ramp of the DSC.

RESULTS and DISCUSSION

DSC TEST RESULTS

The effect of processing on the thermal properties of UHMWPE fibers (virgin and
extracted fibers from three regions (top, middle, and bottom) of the consolidated panel
have been investigated using DSC). From these tests, melting temperature at the peak
and onset temperature were measured and listed in Table I. Clearly, virgin and extracted
fibers from different regions exhibit insignificant differences in the average values of
melting and onset temperature. This indicates that the consolidation process did not
change or distort the crystalline structure of the fibers through the thickness of the
consolidated panel.
Table I. DSC melting parameters obtained for virgin fibers (Dyneema SK99) and fibers extracted from
the three regions of the consolidated panel.
Fiber Melting temperature (°C ) Onset Temperature
(°C)
Top region 147.1±0.3 144.2±0.1
Middle region 147.8±0.3 144.3±0.1
Bottom region 147.2±0.9 144.1±0.1
Average Values 147.4±0.4 144.2±0.1
Virgin Fiber 146.7±0.1 144.2±0.2

DAMAGE MODES OF EXTRACTED FIBERS

To identify the damage modes caused by the processing of HB210 composites,

scanning electron microscopy (SEM) was carried out on virgin fibers, baseline fibers
(extracted fibers from as received HB210 sheet), and extracted fibers from the processed
HB210 composite panel. Figure 5 shows SEM micrographs of extracted fibers from the
consolidated panel. The fibers exhibit different deformation and damage modes, such
as kinks/buckling, fiber surface splitting/cracking, fibrillation, plastic deformation in the
form of scalloped depressions, and in extreme cases, fiber flattening. Using SEM
images, the spacings between the axial kink bands were measured in the order 50µm.
For UHMWPE fibers, microdamage deformations induced by transverse compression
and their effects on crystalline structure and structural properties of the fiber were
addressed in the literature [10,19]. Golovin et al. [19] observed that the transverse
compression on UHMWPE fibers induces a reduction in crystallite size, causing the
strength of the fiber to be reduced. Generally, polymer fibers experience
kinking/buckling when a filament undergoes either bending [20] or axial compression
[21]. Chowdhury et al. [10] conducted MD studies on the effects of transverse and axial
loading on the residual tensile strength of Kevlar (KM2) and UHMWPE crystals. Their
results showed that these loads distort the crystal structure inducing bond breakage in
KM2 and fibrillation in UHMWPE. Axial loading induced chain buckling/kinking in
UHMWPE. Residual tensile modulus and strength were reduced in both materials.
UHMWPE was predicted to have a 12% reduction in residual tensile strength.

Figure 5: SEM micrographs of fibers extracted from consolidated HB210 sheets.

Some of the possible mechanisms for the formation of kinks/buckling during

processing are: (i) As the plies are compacted under pressure, the resin redistributes and
flows into large void regions present in the sheets. The movement of resin along the
length of the fibers (that aren’t supported by resin due to voids) induces shear stress on
the fiber surface and compressive load on the fibers, potentially leading to the observed
kinks; (ii) the mismatch in the CTE between the fibers and matrix within a layer,
between the 0 and 90 layers in the sheet and the metallic tooling. During the cooling
cycle, because of the CTE differences, there could be relative motion due to the
shrinkage of the matrix (αm =100 x 10-6 /°C [22]), which could lead to compression
forces on the fiber. As the temperature reduces (cooling), the resin modulus increases,
leading to higher levels of axial compression stress/strain in the fiber. At some point
during cooling, the critical stress for fiber kinking may be exceeded. Another possible
mechanism for fiber kinking can be related to the significant draw ratio used during
fiber processing (draw ratios greater than 50 are typical). In this case, the molecular
structure may be highly strained, and during heating, the fiber may relax, leading to
shrinkage in the axial direction, which may also contribute to the kinking observed. Our
future work will attempt to identify when the onset of kinking occurs through
experiments on the single fiber level. (iii) negative CTE (-12 x 10-6 /°C) [23] of the
UHMWPE fibers.
These microdamage mechanisms can be reduced by controlling the most important
processing parameters (pressure and temperature) that are being applied during panel
consolidation. To investigate the effect of these processing parameters, two types of
tests were performed on as-received HB210 sheets (samples). The first test was
conducted on a sample (as-received HB210 sheet) using a calibrated hot stage (by
Mettler Toledo, Inc). In this test, the sample was exposed to ramp heating with a rate of
10°C/min to heating to 125°C and held at this temperature for 30 minutes, followed by
cooling down to RT, where no axial pre-strain or through-thickness pressure was
applied. The fibers from this sample were extracted using the THF based methodology
described previously and subjected to SEM microscopy (see Figure 6). Clearly,
filaments exhibit kink bands and buckling associated with intensive surface cracks and
fibrillation (especially in the kinked regions). Note in Figure 6 that entire arrays of fibers
are kinking into adjacent voids. Since this specimen was not subjected to pressure, the
compressive loading required to kink the fibers is likely due to the various sources of
CTE mismatch discussed above.

Figure 6: SEM micrographs of fibers from unprocessed HB210 after exposure to heating /cooling cycles
according to first type of thermal test featuring kinks associated with surface cracks.

To isolate the effect of the consolidation pressure on the filaments, a compaction

test was conducted on an unprocessed HB210 sheet at 20.7 MPa (3 ksi) at RT, followed
by soaking the compressed HB210 sheet in THF for fiber extraction, as described above.
Then, SEM microscopy was used to study surface morphology fibers from the dissolved
laminate. Figure 7 shows that the fibers undergo several types of damage modes, such
as surface splitting into microfibrils, plastic deformation, and flattening. These damage
modes were observed by fibers extracted from the 20.7 MPa (3 ksi) consolidated panel
(see Figure 7). The pressure applied during the consolidation process affects the
evolution of the damage modes experienced by filaments (such as surface splitting/
cracking, fibrillation, and flattening). It is noteworthy that the sheets compacted at RT
do not exhibit fiber kinking, while the consolidated panels that followed the
recommended process cycle (heated to 125°C dwell temperature) do exhibit fiber
kinking. The consolidated panels in hot press at temperature and pressure have both
kinking of fibers and damage from transverse compression. This comparison indicates
that kinking is triggered by temperature, but consolidation pressure/void reduction
mechanisms are a contributing factor.

Figure 7: SEM micrographs of fibers from unprocessed HB210 after compaction test at RT and 3ksi,
showing fiber surface flattening and splitting.

TENSILE STRENGTH OF EXTRACTED FIBERS

Tensile strength experiments were performed on single fibers following the
procedure that was described previously. The evaluated fibers were baseline fibers
(virgin fibers and extracted from as-received HB210 prepreg) and extracted fibers from
the consolidated HB210 panel. Strength was calculated from the failure load and the
cross-sectional area of the fiber, where the average fiber diameter for each specimen
was measured via optical microscopy at a resolution of 0.214 um /pixel. Strength
distributions (cumulative density function (CDF)) for baseline fibers and extracted
fibers from the consolidated panel were generated using Minitab software and plotted
in Figure 8. From this plot, the CDF curves of both virgin fibers and fibers from as
received HB210 sheet exhibit insignificant differences. These results confirm that the
extraction procedure has no significant effect on the strength of fibers extracted from
the HB210 sheets.
From these CDF curves, the strength values at 50% probability were quantified and
listed in Table II. Clearly, CDF curves of extracted fibers exhibit shifts to lower strength
levels with respect to baseline fibers. The reduction strength was quantified as 15% for
extracted fibers. These results indicate that the processing parameters (temperature and
pressure) applied in the consolidation of the panel caused the strength of fibers to be
reduced. This strength reduction is consistent with the level of the damage modes
observed in the SEM micrographs, where the kinking/buckling damage modes are
mostly controlled by the heating/cooling cycle and other damage modes (such as surface
cracks along the fiber and surface flattening) are mostly induced by the consolidation
pressure (see Figure 7). Golovin et al. [19] reported that the transverse deformation
could cause the strength of UHMWPE fibers to be reduced by 26%, and Sockalingam
et al. [13] observed a plastic deformation and surface flattening of the fiber and
quantified a 20% strength reduction after exposure of the fiber to transverse compressive
strain of 60%. Chowdhury et al. [10] explained the reduction in strength (~12%) of
UHMWPE fiber after exposure to transverse compression by the distortion of
crystalline structure and the breakage of molecular bonds.
Table II: Strength values at 50% failure probability quantified from CDF curves for baseline fibers and
extracted fibers from the three regions of the consolidated panel.
Fiber Strength (GPa) at 50%
probability
Virgin Fiber 4.81

As received HB210 Fibers 4.81

Consolidated Panel- Fibers 4.15

Figure 8: Strength distributions (CDF curves) generated for baseline fibers and extracted fibers from the
consolidated panel.

SUMMARY AND CONCLUSIONS

The influence of processing conditions (temperature and pressure) on the

UHMWPE fibers used in HB210 panels was investigated in this study. A process to
extract single fibers from a consolidated panel was developed by dissolving the matrix
in THF. The process doesn’t degrade the strength of the fibers. UHMWPE single fibers,
extracted from a consolidated HB210 panel, were evaluated under low and high
magnification microscopy (SEM) and mechanically tested in tension. From SEM
microscopy, it was found that extracted fibers from processed panel exhibit
buckling/kinking, surface cracking/splitting, plastic deformation, and surface flattening.
The potential causes of these damage modes observed in the extracted fibers were
discussed. Based on the surface morphology analysis of the fibers from HB210 after
compaction at RT and 3ksi, the pressure being applied to HB210 laminates during the
consolidation process influences the damage modes experienced by filaments (such as
surface splitting/cracking, fibrillation, and flattening). The possible mechanisms for the
formation of axial kinks are the forces applied on the fibers due to resin redistribution
upon consolidation, the CTE mismatches causing resin shrinkage during cooling (which
could apply axial forces on the fiber through shear mechanism), and the inherent
shrinkage of the UHMWPE fibers. Future work will be focused on understanding and
evaluating these mechanisms by conducting experiments at different length scales.
From the tension test results of fibers extracted from the processed panel, relative to the
strength values of baseline fibers, the strength reduction at 50% probability of failure
was quantified as 15%, which could be attributed to the damage modes discussed earlier.

ACKNOWLEDGEMENTS
"Research was sponsored by the Army Research Laboratory and was accomplished
under Cooperative Agreement Number W911NF-21-2-0208. The views and
conclusions contained in this document are those of the authors and should not be
interpreted as representing the official policies, either expressed or implied, of the Army
Research Office or the U.S. Government. The U.S. Government is authorized to
reproduce and distribute reprints for Government purposes notwithstanding any
copyright notation herein."
Comments from Jerry LaSalvia from Army Research Laboratory are appreciated.

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