Beruflich Dokumente
Kultur Dokumente
Dian-Sen Li,1,2 Chuang-Qi Zhao,1 Lei Jiang,1 Na Lu,1 Li-Ming Chen,3 Nan Jiang4
1
Key Laboratory of Bio-inspired Smart Interfacial Science and Technology of the Ministry of Education,
School of Chemistry and Environment, Beijing University of Aeronautics and Astronautics, Beijing 100191,
People’s Republic of China
2
State Key Laboratory of Structural Analysis for Industrial Equipment, Dalian University of Technology,
Dalian 116023, People’s Republic of China
3
Chongqing Key Laboratory of Heterogeneous Material Mechanics, College of Resource and Environment
Science, Chongqing University, Chongqing 400030, People’s Republic of China
4
China Academy of Machinery of Science & Technology, Beijing 100044, People’s Republic of China
POLYMER COMPOSITES—2014
architectures at room and liquid nitrogen temperatures.
The damage and fracture morphology of the composites
after failure are observed from the macroscopic and
microscopic views and the failure mechanism is demon-
strated. Finally, the influences of fiber architecture on the
tensile properties and failure mechanism of composites at
room and liquid nitrogen temperature are also analyzed.
The aim of our study is to establish the database for the
potential applications of 3D MWK composites. It is
FIG. 1. Multi-axial warp knit system. [Color figure can be viewed in
expected that the study will provide an experimental basis
the online issue, which is available at wileyonlinelibrary.com.]
for the structural design of the 3D MWK composites at
room and liquid nitrogen temperatures.
knitted stitches. Edgren et al. [12, 13] developed an analyt-
ical constitutive model for MWK composites and focused MATERIALS AND SAMPLES
on the formation and development of the damage. They
The 3D MWK preforms are made from layers of non-
found longitudinal and transverse cracks are developed
crimp fabric (made with unidirectional tows) stacked in
under tensile loading and revealed stress concentrations are
the required orientations and then bound together with
caused by 0 fiber bundle waviness. In addition, Zhou
binder yarns inserted in the through-thickness direction by
et al. [14] studied the low-velocity impact energy absorp-
warp knitting needles. Figure 1 shows the schematic dia-
tion characteristics of MWK composites with double loop
gram of MWK preform manufacturing. In this study, E-
pillar stitch and common tricot stitch. Saito et al. [15]
glass fiber bundles are used for unidirectional reinforcing
evaluated the impact damage and growth behavior of T700
in 0 , 90 , 45 , or 245 directions while polyester fibers
MWK composites based on nondestructive and destructive
are used for knitted linking, four types of structure with
observation methods. Their results showed that transverse
different fiber orientations A[0 /0 /0 /0 ], B[0 /90 /0 /
cracks near the impact point were found to be joined with
90 ], C[0 /90 /145 /245 ], and D[145 /245 /145 /
propagation of cracks. Sun et al. [16] tested the high-
245 ] are manufactured. Twelve fiber layers with non-
strain-rate compressive properties of E-glass/epoxy MWK
crimp are used in the 3D MWK composites and the fiber
composites and their results indicated that the stress–strain
volume fraction is 60%. Figure 2 shows the photographs
curves, compressive stiffness, maximum stress, and corre-
of the face and the back of four types of orientation pre-
sponding strain are strain-rate sensitive. Recently, Vallons
forms (0 , 90 , 145 , and 245 ). The epoxy resins are
et al. [17] studied the tensile–tensile fatigue properties of
injected into 3D MWK preforms by the Vacuum Assisted
0 /90 multi-ply carbon fiber fabric reinforced epoxy com-
Resin Transfer Molding (VARTM) process and then con-
posites and their results showed that specimens in machine
solidated to produce 3D MWK composites. The compo-
and cross direction did not fail up to 106 cycles while
sites are then cut into dog-bone shape for tensile tests at
specimens in bias direction had an average fatigue life of
room and liquid nitrogen temperatures. Here, the samples
3 3 105 cycles. Mattsson et al. [18] discussed the influ-
notations for four types of composites at room tempera-
ence of the layer stacking sequence on the tensile behavior
ture are AR, BR, CR, and DR, and at liquid nitrogen tem-
and the damage development. Their results showed that
perature are AC, BC, CC, and DC. Figure 3 shows the
layer stacking sequence has little influence on the initial
geometry of tensile sample and the specifications of the
stiffness of the material, but a large influence was found
tested samples are summarized in Table 1.
on the stiffness evolution during the test.
However, the cryogenic respond of 3D MWK compo-
EXPERIMENTAL PROCEDURE
sites for modern cryogenic applications have been paid
little attention, especially at liquid nitrogen temperature. The test procedure is in accordance with the ASTM
It is valuable to study the mechanical properties and fail- standard D3916-02 and Chinese standard GB1447-83
ure mechanism of the 3D MWK composites at liquid about fiber reinforced composites. The uniaxial tensile
nitrogen temperature because of the wide potential appli- test at room and liquid nitrogen temperature (low as
cations in engineering. For example, the composite struc- 2196 C) is carried out on a MTS CMT5000 test
ture of a satellite in flight or a liquid nitrogen cryogenic machine. At low temperature, a sweating guarded hot ten-
tank may be exposed to the temperatures as low as sile fixture has been developed by modifying the one
2196 C. Recently, some scholars [19–21] aimed at specified at room temperature so that the new device can
braided, woven, and nonwoven-fabric-reinforced compo- be used under frozen conditions. A cryogenic cylinder
sites; and they found that changes in the interior structure filled with liquid nitrogen is used for dipping the tensile
and mechanical response of composite materials may fixture and then measuring the low-temperature mechani-
occur under such cryogenic conditions. cal properties of the composites. Before the experiment,
This article presents an experimental study of tensile the samples and the tensile fixture are dipped into the liq-
properties for 3D MWK composites with different fiber uid nitrogen for at least 2 h, respectively. Then they are
Sample no. Fiber architecture Width (mm) Thickness (mm) Weight (g) Density (g/cm3) Test temperature
FIG. 5. A comparison of stress versus strain curves for four types of composites. (a) At room temperature.
(b) At liquid nitrogen temperature. [Color figure can be viewed in the online issue, which is available at
wileyonlinelibrary.com.]
temperature are improved significantly than that of at force is augmented and higher interface bond strength is
room temperature. The tensile strength for materials A, B, attained, which has improved the mechanical properties
C, and D are increased by 67.89%, 37.54%, 49.37%, and of composites significantly [22].
103.92%, respectively; and the tensile modulus are
increased by 9.97%, 18.62%, 35.15%, and 83.41%,
Failure Mechanism at Room Temperature
respectively. This is due to the fact that the mobility of
the polymer chains within the resin matrix will be As the damage phenomena in textile composites are
reduced and the molecules of polymer matrix are more much more complicated than that of in unidirectional
closely compacted at liquid nitrogen temperature. At the laminates, which involves processes and parameters on
same time, the transverse shrinkage of glass fibers is different scale levels. The morphology of fractures is
smaller than that of resin matrix, the interface friction observed with photos and a JSM 7500F scanning electron
microscopy (SEM) from the macroscopic and microscopic same time, fiber/matrix interface debonding can be
views to investigate the type of damage and failure mech- observed and a large number of fibers are pulled out from
anisms. Figure 7 shows the fracture photographs of tensile the matrix (Fig. 8a and b). So, for material A, the 0
samples at room temperature. Figures 8–11 show the fibers act as the main load-bearing object and the main
SEM photographs of tested composites at room failure mode is the fibers fracture along 0 direction
temperature. under tensile normal stress.
From Fig. 7a, for material A, it can be seen that the For the material B, due to the introduction of 90
fracture is flush, the 0 fibers become loose, and there is fibers layer, the interlayer between the 0 and 90 fibers
obvious pull out. By SEM observation, it can be found layer are bearing the coupling of tensile and shear stress
that the matrix is cracked and peeled off from the fiber which lead to the delaminating. From Fig. 7b, the delami-
bundles due to the interfacial shear stress (Fig. 8a), at the nation phenomenon along the material thickness can be
FIG. 8. The SEM photographs of AR sample. (a) Matrix peel off; (b) interfacial debonding; and (c) fibers
pull out.
observed. For the 90 fiber layer, the fibers hardly bear fiber–matrix interface. While for fibers in 145 /245
loading and are broken, firstly the interface is damaged layers, the main failure mode is that the fibers are torn
under the tensile stress, then the fibers tear from the along 145 /245 fiber–matrix interface. From Fig. 10b
cracked matrix. By SEM observation, it can be observed and c, SEM observation shows that 245 layer, serious
that serious interface debonding occurs between the 90 fiber–matrix interface debonding appeared due to the ten-
fibers and matrix, and the 90 fibers are torn obviously sile and shear stress. At the same time, shear deformation
(Fig. 9a and b). While for the 0 fibers layer, SEM obser- occur in the matrix and the fibers distorted breakage can
vation show that the 0 fibers are pulled out and broken also be clearly observed. So, the main damage for mate-
at different levels (Fig. 9b), and the fracture for fibers are rial C is in the form of interlayer delaminating, matrix
all flush due to the tensile normal stress (Fig. 9c), which cracking and yielding, interface debonding, and breakage
proved that the 0 fibers still act as the main load-bearing of the fibers.
object, which is similar to the material A. From Fig. 7d, the material D is delaminated from the
From Fig. 7c, for material C, the fibers appear cluster- surface toward inward and the fracture are along 145 or
ing and zigzag delaminating fracture can be observed. 245 direction. The main failure mode is the fibers torn
The SEM observations also show that serious delaminat- along 145 /245 direction, as well as the fiber shear
ing occurred for the fiber layers in 0 , 90 , 145 , and breakage. From Fig. 11, SEM observations indicate that
245 directions (Fig. 10a). It is due to the discontinuity the matrix is peeled off and occurred shear deformation
of stress state for different fiber layers and the fibers due to the tear of 145 and 245 fibers along the inter-
breakage is not simultaneous. On the other hand, the face. And the fibers which are not parallel to the interface
fibers in different layers have different failure mechanism. are cut in shear form. So, due to the absence of 0 fiber,
Similarly, the fibers in 0 layers are broken under tensile the 645 fiber–matrix interface dominate the failure of
normal stress. The fibers in 90 layers are torn along the material, and it is more easier to cause interface
FIG. 10. The SEM photographs of CR sample. (a) Delaminating fracture; (b) interfacial damage; and (c)
matrix deformation.
debonding under the coupling of tensile and shear stress, damage and failure morphology are different depending
which leads to low-mechanical properties of composites. on the test temperatures. At liquid nitrogen temperature,
Moreover, it is the degradation of the interface properties for material A, Fig. 12a shows that the materials are burst
and the damage accumulation for the matrix plastic defor- open and are clearly scattered into the 0 fiber bundles.
mation, which cause the elastic/plastic transition and long This is due to the fact that the breakage of the 0 fibers
plastic platform in the stress–strain curves. at different layers must overcome the interlaminar
stresses. However, the interlayer adhesion strength has
improved significantly at liquid nitrogen temperature,
Failure Mechanism at Liquid Nitrogen Temperature
then microcracks inside the material increase and extend
Figure 12 shows the fracture photographs of compo- constantly, resulting in the materials are burst open in
sites at liquid nitrogen temperature. It can be seen that brittle eventually. This also proves that the material have
FIG. 12. The fracture photographs of tensile samples at liquid nitrogen temperature. (a) AC sample; (b) BC
sample; (c) CC sample; and (d) DC sample. [Color figure can be viewed in the online issue, which is avail-
able at wileyonlinelibrary.com.]
FIG. 14. The SEM photographs of BC sample. (a) Delamination; (b) interfacial bond; and (c) 0 fibers
fracture.
larger strain than that of at room temperature. From Fig. fibers and matrix is enhanced significantly, which
13a, SEM observations found that the scattered fibers at improve the load-bearing capacity of composites.
fracture surface are damaged and broken, further the From Fig. 12b, for material B, it can be seen for 0
fibers pull-out phenomenon is also obvious. From Fig. direction, the fibers bundles are pulled out, while for 90
13b and c, the matrix material is solidified at liquid nitro- direction, the fracture is flush, which is similar to that of
gen temperature and the interfacial adhesion between at room temperature. However, the whitening damage
FIG. 15. The SEM photographs of CC sample. (a) Delamination; (b) matrix shear breakage; and (c) fibers breakage.
area expands significantly at liquid nitrogen temperature. from Fig. 16c, the damage and the degradation in proper-
This is because that more local microcracks occur and ties of the matrix are more stiffen due to the low temper-
accumulate. By SEM observations, it can be found that ature solidification which proves the bilinear tendency in
the material is suffered with obvious delaminating (Fig. the stress versus strain curves.
14a) due to the tensile and shear stress. From Fig. 14b,
the 90 fibers are bonded more closely and the interfacial
CONCLUSIONS
bond ability has been enhanced significantly. Moreover,
the 0 fibers fracture is flush due to the tensile normal The tensile properties of 3D MWK composites with
stress and the damaged fibers are not scattered (Fig. 14c). four types of fiber architecture are studied at room and liq-
So, the main damage for material B at liquid nitrogen uid nitrogen low temperature. The results indicate that the
temperature is in the form of matrix cracking, interlayer stress versus strain curves for materials A, B, and C have
delaminating, the 0 fibers breakage, and the 90 fiber– obvious linear elastic feature up to failure at room and liq-
matrix interface debonding. uid nitrogen temperature. However, for material D, the
From Fig. 12c, the material C also shows zigzag material shows significant nonlinear transition at room
delaminating fracture at liquid nitrogen temperature and temperature and bilinear process at liquid nitrogen temper-
the fibers are broken in cluster. As shown in Fig. 15, ature. Moreover, the tensile properties at liquid nitrogen
SEM observations show that the matrix peels off between temperature are improved significantly than those of at
the fiber layers and shear deformation is occurred due to room temperature. In addition, the tensile properties can be
the shear stress. And there is obvious breakage of the 0 affected greatly by the fiber architecture and these decrease
fibers. So, the main failure mechanism is still the fiber significantly with the increase of the fiber orientation angle
delaminating due to the discontinuity of the interlayer at room and liquid nitrogen temperature.
stress, matrix shear yielding, the 90 /145 /245 fiber– The macro- and microfracture morphology examinations
matrix interface debonding as well as breakage of the 0 indicate that the damage and failure patterns of composites
fibers. On the other hand, from Fig. 15, more of matrix vary with the fiber architecture and test temperature. For
remain around the fibers and the interfacial adhesion material A, the failure behaves as the fibers bundles frac-
between fibers and matrix is improved significantly. ture along 0 direction under normal tensile stress. For
From Fig. 12d, for material D, similar to that at room material B, the main failure is that the 0 fibers are pulled
temperature, the fracture for different layers at liquid out and broken while the 90 fibers are torn along the
nitrogen temperature is along 145 and 245 direction. interface. For material C, the main damage is in the form
By SEM observations, obvious interlayer delaminating, of interlayer delaminating, matrix cracking, and yielding,
the fibers tearing on the 645 fiber–matrix interface as 90 /145 /245 fiber–matrix interface debonding and
well as fibers breakage in shear can be clearly observed breakage of the 0 fibers. For material D, the failure pat-
(Fig. 16a and b). So, the 645 fiber–matrix interface also tern is the tearing of fibers along 145 /245 fiber–matrix
dominate the failure of the material. And due to the interface as well as the fiber shear breakage. At liquid
absence of the 0 fibers, material D show lowest mechan- nitrogen temperature, more microcarcks occur and damage
ical properties in the four types of material. On the other accumulation within the material is alarming, however, the
hand, the matrix solidification and interfacial bonding is matrix is solidified and the interfacial adhesion between
increased significantly (Fig. 16c) which improves the fibers and matrix is enhanced significantly which show
mechanical properties at room temperature. Moreover, higher mechanical properties of composites. In addition,