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Mechanical Characterization of Natural Nano-Structured Zeolite Polyurethane Filled 3D Woven Glass Fiber Composite Sandwich Panels
Mechanical Characterization of Natural Nano-Structured Zeolite Polyurethane Filled 3D Woven Glass Fiber Composite Sandwich Panels
Polymer Testing
journal homepage: www.elsevier.com/locate/polytest
A R T I C LE I N FO A B S T R A C T
Keywords: 3D woven glass fibers sandwich panels have become the focus of interest due to their inherent light weight and,
3D woven glass fiber fabric thus, their remarkable stiffness. However, a question is that whether their hollow galleries could be filled with
Composite sandwich panels still light materials which even at the same time contribute to their mechanical performance. This work ex-
Nano-structured zeolite amines the effect of porous polymer nanocomposites filling galleries of such panels on mechanical response of
Polyurethane
newly formed hybrid composites. To achieve this, the nanocomposites of natural nano-structured zeolite/
Mechanical properties
Energy absorption
polyurethane foams were fabricated and injected within 3D woven glass fibers sandwich panels. Mechanical
characterization techniques including the flatwise compression, edgewise compression, three-point bending and
drop weight impact were carried out to understand the effect of addition of the reinforced foam on the me-
chanical response of the specimens. It is shown that the polyurethane foam reinforced with natural nano-
structured zeolite particles significantly improves the flexural strength, ultimate load and energy absorption of
the filled composite sandwich panels. It is also demonstrated that the damage and local wrinkling failure
compared with other typical sandwich panels do not occur due to the presence of the glass fiber yarns vertically
located between panel sheets. These type of composites provide high specific strength results from high-per-
formance and low-density structure.
1. Introduction multilayer structure with ordered fibers along the plane. The main
feature of the two-dimensional multilayer is lack of fibers in the vertical
Fiber reinforced polymer (FRP) composites due to their lower direction [8]. Nevertheless, the absence of fibers in the thickness di-
weight, higher specific strength and stiffness [1] and excellent corro- rection may not be favorable in terms of mechanical performance in-
sion-fatigue resistance [2] have recently drawn a great deal of atten- cluding the impact damage resistance in that multilayers composites
tion. In view of their stiffness, this class of material is comparable to exposed to projectile impact are subjected to delamination as frequently
conventional metallic alloys such as steel and aluminum alloys. Their reported [9]. In the case of two-dimensional multilayer composites, the
low thermal expansion and high dimensional stability are other ad- absence of bonding agents along the direction perpendicular to layers
vantages of these composites as frequently reported elsewhere [3–7]. A means that the layers must be ordered separately and collected.
combination of significant physical, thermal and mechanical properties Therefore, the production time increases significantly. Moreover, high
of composites, especially if required in light weight structures has made cost, poor transverse mechanical properties occurring due mainly to the
such composites a suitable replacement for metals in many applica- lack of fibers in the vertical direction are other disadvantage of two-
tions. dimensional multilayer composite structures [10].
FRP composites can be described as multi-component materials in- The development of three-dimensional (3D) composites has been
cluding fibers embedded in a polymer matrix. Although a veracity of recently addressed due to the need for the reduction of the production
composites in engineering applications are made from glass fibers due cost [11], and the enhancement of the mechanical behavior across the
to their mechanical properties, excellent chemical resistance and very thickness, impact damage resistance [12], maximum bending moment
low cost. capacity and maximum strength-to-weight ratio. One of the fabrication
Polymer matrix of FRP composites is classified to thermosets such as methods in textile industries is the 3D woven fabric wrap-weft knitting
epoxy and polyester as well as thermoplastic polymers. Continuous process. In this process, two layers of wrap-weft woven yarns at a
fiber-reinforced composites are described as a two-dimensional certain distance from each other are connected utilizing vertical woven
∗
Corresponding author.
E-mail addresses: hamid.safari@me.iut.ac.ir (H. Safari), mkarevan@cc.iut.ac.ir (M. Karevan), hnahvi@cc.iut.ac.ir (H. Nahvi).
https://doi.org/10.1016/j.polymertesting.2018.03.018
Received 18 January 2018; Received in revised form 4 March 2018; Accepted 10 March 2018
Available online 12 March 2018
0142-9418/ © 2018 Elsevier Ltd. All rights reserved.
H. Safari et al. Polymer Testing 67 (2018) 284–294
fibers. As a result, a tight connection between the two layers is expected sandwich structures, however, is their processability since the skins
to be developed, which in turn promotes the resistance to delamination must be separately prepared and glued to the composite core. In ad-
of the sandwich structure. Such characteristics lead to epoxy based 3D dition, skin delamination observed in sandwich composites under
woven glass fiber fabric sandwich structures exhibiting a low density flexural loadings, torsion or impact forces may lead to their separation
and remarkable strength. from the core. A key hypothesis is that whether a reinforced core of
To date, only a few experimental studies in respect of 3D woven sandwich composites made of 3D fabric could overcome the issued
fabric composite sandwich panels have been reported. In view of the mentioned due to the presence of secondary mechanisms contributed
elastic response of this class of structures, the Young's modulus of 3D by fibers perpendicularly connecting surface skins together.
woven composite materials, may be lower [13,14] or [15,16] greater Zeolites are very stable aluminosilicate solids with honeycomb
than that exhibited by the 2D multi-layers using the same fiber content. framework of micropores that resist the kinds of environmental con-
Brandt et al. [17] addressed the mechanical performance of a type of ditions that challenge many other materials [34]. Zeolites have dif-
woven composites including monolithic and sandwich by the compar- ferent dimensions of pores, high surface areas and channels responsible
ison of in-plane properties such as stiffness and strength, damage tol- for their physical and chemical properties. Also, they have relatively
erance, energy absorption capability. Judawisastra et al. [18] in- high melting points (over 1000 °C), resist high pressures, don't dissolve
vestigated the bending fatigue behavior and damage development in water or other inorganic solvents, don't oxidize in the air and don't
during fatigue of polyurethane (PUR)-epoxy sandwich composites. cause health issues due to unreactive and based on naturally occurring
Bannister et al. [19] examined a type of composite sandwich structures. mineral and eco-friendly nature [35].
Flatwise compression, edgewise compression, climbing drum peel and Zeolites have found multifarious applications as adsorbents, ion
flexure tests were conducted. Van Vuure et al. [20] studied the me- exchangers and catalysts in industry [36], medicine [35,37–41], food
chanical properties of sandwich panels core and their potential for cost- science [42], sanitation and environmental protection [43,44].
effective sandwich construction. They evaluated the basic mechanical This study aims at evaluating the effect of natural nano-structured
performance of the sandwich core under compressive and shear zeolite/polyurethane on the mechanical properties of 3D woven glass
loading. Moreover, Van Vuure et al. [21] reviewed the sandwich panels fiber fabric composite sandwich panels. Addressing the effect of nano-
to be utilized as an alternative spacer material in a constrained layer structured zeolite addition into polyurethane filled sandwich composite
damping configuration. Wu et al. [22] developed a composite sandwich on mechanical properties has not been carried out previously. To un-
structure with foam core reinforced with composite columns and tested derstand mechanical response of fabricated samples, flatwise com-
all types of the samples with different consisting structural parameters pression, edgewise compression, three-point bending and drop weight
under compressive load. Kus et al. [23] investigated the flexural be- impact tests were carried out according to respective standards. Load-
havior of the integrated woven spacer composites incorporating carbon displacement profile diagrams were used to determine the mechanical
fiber reinforced polymer face sheets accompanying epoxy and polyester properties and failure mechanism of the sandwich panels.
matrix. Significant changes in the flexural properties of the composites,
first related to the temperature and then to the resin type were ob- 2. Experimental
served. Tekalur et al. [24] examined the impact resistance of sandwich
composite structures. They analyzed the photographs of the ballistic 2.1. Materials
events of penetration and damage. The results showed that reinforced
panels with 3D woven backing had a higher ballistic efficiency than the 3D woven E-glass fiber fabric (Hardener HE 1515 and epoxy resin
2D stacking layers panels. Xia and Wu [25] explored impact perfor- LR-2025) was used to fabricate the specimens. The resin and hardener
mance of foam core sandwich composites consisting of various facings mixing ratio of ten-to-one was used to fabricate 3D woven E-glass fiber
composed of glass, carbon woven, carbon/Kevlar hybrid, and Kevlar composite sandwich panel. Careful measuring of epoxy resin and
fabrics. Fan et al. [26] conducted three-point bending tests to reveal the hardener and thorough mixing are essential for proper curing according
failure mechanisms of the textile composite. Fan et al. [27] performed to the manufacturer. Polyurethane foams consisting of polyol and iso-
low-velocity dynamic compression tests to reveal the failure mechanism cyanate with mixing ratio of one-to-one were prepared.
and the energy absorption capacity of a specific woven sandwich
composite. The results were correlated to the dynamic effects of the 2.2. 3D woven glass fiber composite specimens
strength and the energy absorption by the dynamic buckling of the
woven struts in the core. Hu et al. [28] studied the deformation, To fabricate the 3D woven glass fiber fabric composite specimens,
strength, and failure modes of sandwich composites by experiments and the fabric was cut for flatwise and edgewise compression specimens
extracted failure modes of composites. Jin et al. [29] fabricated a new with the dimensions of 54 × 54 mm2 according to the ASTM C365 [45]
integrated sandwich composite and examined the mechanical proper- and ASTM C364 [46], respectively. Moreover, to perform the flexural
ties and the failure mechanism. The experiments verified the high characterization, the 3D woven fabric was sliced into specimens of
skin–core debonding resistance. Luo et al. [30] determined the trans- 154 × 54 mm2 according to the ASTM C363 [47] and 210 × 100 mm2
verse impact behaviors of orthogonal hybrid woven fabric composites in the case of the drop weight impact according to the ASTM D7136
to analyze the strain rate sensitivity of energy absorption. Fan et al. [48]. The upper and lower surfaces of the fabric were coated with the
[31] conducted mechanical tests to reveal the failure mechanisms and mixture of epoxy resin and hardener giving proper soaking time to wet
the energy absorption capacity of the sandwich materials. In another the surfaces across the thickness. Finally, the upper and lower fabric
work conducted by them [32] multi-layered panels were prepared by skins were separated to form the 3D structure. Specimens were fully
stacking thin monolayer panels to improve the energy absorption per- cured at the ambient temperature for 24 h.
formance of the sandwich followed by the quasi-static compression
experiments for the evaluation of the energy absorption mechanism. 2.3. Natural nano-structured zeolite/polyurethane filled composite
Sedighi et al. [33] studied a finite element simulation followed by ex- specimens
perimental characterization of fabricated samples in order to in-
vestigate the mechanical behavior of glass-fiber sandwich composites. To fabricate the foam composite specimens, the polyol-isocianate
The literature review furthermore emphasizes that the sandwich mixture was injected into the sandwich core allowing a few minutes for
structures made of a new type of 3D woven fabric can be used to the foam formation. The polyurethane foam was cured at room tem-
overcome many common downsides observed in thin layers or honey- perature for 2 days. To fabricate the zeolite/polyurethane filled speci-
comb core sandwich composites. One key shortcoming of regular mens, 5–30 wt% of zeolite was added into the polyol-isocianate mixture
285
H. Safari et al. Polymer Testing 67 (2018) 284–294
Fig. 1. (a) Composite sandwich panel made of 3D woven glass fiber fabric and; (b) zeolite/polyurethane filled 3D woven glass fiber composite specimens; with dimensions of
54 × 54 × 24 mm3 and their cross-section parts.
and homogenized following the above procedure. Fig. 1(a) and (b)
show a 3D woven glass fiber fabric sandwich panel composite specimen
and a zeolite/polyurethane filled 3D woven glass fiber composite, re-
spectively.
286
H. Safari et al. Polymer Testing 67 (2018) 284–294
Table 1
Ultimate loads for flatwise compression test against zeolite wt%.
Table 2
Compressive properties of flatwise compression test specimens.
Fig. 3. Comparative average force-displacement curves for flatwise compression tests of Table 3
plain 3D fiber composites versus neat polyurethane. Compressive properties of flatwise compression test specimens reinforced with containing
zeolite powder.
fibers were started to crush at around 1.17 kN force value in the plain Zeolite wt% σ (MPa) E (MPa)
composites.
5 1.2±0.02 18.5± 0.8
The comparative force-displacement curves for flatwise compres- 10 1.15± 0.02 18.4± 0.8
sion tests of zeolite/polyurethane filled composite sandwich panels are 20 1 ± 0.03 18.4± 0.7
represented in Fig. 4. It is clearly observed that the composites re- 30 1± 0.02 18.3± 0.8
inforced with 30 wt% zeolite obtained maximum value of energy ab-
sorption until the specimens become fully compressed.
The ultimate loads values obtained are summarized in Table 1. P fibers to reshape into a single yarn twisting in parallel state relative to
represents the maximum load obtained in the flatwise compression test each other. The fibers continue to rotate under increasing load until the
for three specimens of each composite system. Average compressive vertical yarn becomes unstable and then breaks along a well-defined
strengthσ , and average compressive modulus, E, are given in Tables 2 plane known as a kink band. The kink bands in first initiate in the most
and 3. severely distorted yarn, which are usually at the skin surface where
According to the results, 5wt% zeolite/polyurethane composite has they are tangled by the vertical fibers. As a result, composites fail
the best performance. 3D woven glass fiber fabric composite sandwich gradually at discrete locations throughout the structure, leading to ul-
panels were crushed by twisting (kinking) of vertical yarns because of timate failure as illustrated in Fig. 5.
axial compression. Kinking failure was started in areas with lower re-
sistance to shear deformations (the defective area such as the cracked
3.2. Edgewise compression test
areas) or in areas where the fibers were deviated from the force di-
rection. Kinking was begun when the axial yarn applied compressive
This test method covers the compressive properties of structural
stress in the resin matrix was reached a plastic shear value. The plastic
sandwich construction in a direction parallel to the sandwich facing
yielding of resin–fibers in the vertical fiber-skin connection zone allows
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H. Safari et al. Polymer Testing 67 (2018) 284–294
Table 5
Compressive properties of edgewise compression test specimens.
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H. Safari et al. Polymer Testing 67 (2018) 284–294
Table 7
Bending and shear strength of three point bending test.
Table 8
Bending and shear strength of three point bending test specimens loaded with zeolite
powder.
Table 9
Fig. 10. Three point bending curves of plain, neat polyurethane and wt% zeolite/poly-
Flexural properties of three point bending test specimens.
urethane filled composites.
Three point bending Δ (mm) D (N.mm−1) U (N) G (MPa)
Table 6
Plain 3D fiber 5 49.4 ± 9.8 1522.7 ± 304.5 1.2 ± 0.2
Ultimate tensile loading of three point bending test as a function of zeolite wt%.
composites
Neat polyurethane 5 206.6 ± 8.2 5801.6 ± 232 4.5 ± 0.1
Three point bending P1 (kN) P2 (kN) P3 (kN) P (kN)
filled composites
Plain 3D fiber 0.55 0.42 0.4 0.45 ± 0.06
composites
Neat polyurethane 1.35 1.28 1.2 1.28 ± 0.06 Table 10
filled composites P5%Z (kN) P10%Z (kN) P20%Z (kN) P30%Z (kN) Flexural properties of three point bending test specimens loaded with zeolite powder.
Zeolite/ 1.21± 0.0.3 1.01 ± 0.07 1.1 ± 0.0.9 0.96 ± 0.05
polyurethane Zeolite wt% Δ (mm) D (N.mm−1) U (N) G (MPa)
filled fiber
composites 5 5 229.7 ± 36.7 6856.2 ± 596.9 5.2 ± 0.6
10 5 187.5 ± 18.7 4918.3 ± 491.8 3.8 ± 0.3
20 5 175.1 ± 22.7 4365.2 ± 395.2 3.3 ± 0.4
30 5 182.3 ± 27.3 4073.1 ± 610.9 3.1 ± 0.4
core material. Table 6 elucidates the Ultimate tensile loading of three
point bending test as a function of zeolite wt%.
The occurrence of failures such as the misalignment of fibers in the The deflection Δ was experimentally determined by the three-point
vertical direction could be thought to weaken the ultimate loads of 3D bending test whilst the only unknown variable is the shear modulus G
woven composites. The core shear stress was calculated using equation that can be easily obtained through solving equations (3) and (4). The
(1) according to the ASTM C393 standard [47]: flexural properties of composite sandwich panels are given in Tables
P 7–10.
τ=
(d + c ) b (1) According to the results of Tables 7–10, material properties has
increased by adding neat polyurethane and 5wt% zeolite/polyurethane
where τ is core shear stress, P is load, d is sandwich thickness, c is core to maximum values and continually decreased by adding more zeolite
thickness, and b is sandwich width. The ultimate shear strength was up to 30wt%. The force-deflection curves shown in Fig. 10 clearly show
obtained using equation (1) where P is the maximum load. Facing that, in the case of the plain sandwich panels, lower forces was required
bending stress was calculated by equation (2) [47]: to initiate cracks and damage in the skin while in the case of the foam
PL core sandwich panel specimens greater loadings was required for the
σ= damage initiation. The results indicated that the average core shear
2t (d + c ) b (2)
modulus of polyurethane foam filled sandwich panel specimens was
where σ is the facing bending stress, t is facing thickness and L is the around 4.5 MPa that was 270% greater compared to that exhibited by
span length. The beam deflection could be ascribed to both flexural and the plain sandwich panel specimens. Moreover, the sandwich panels
shear deformations. The shear deformation is dominant in the core and, filled with polyurethane loaded with 5wt% of zeolite yield the greatest
hence, the approximate expression for the elastic deflection of sandwich shear modulus being around 5.2 MPa among of all other fabricated
beam can be given by equation (3) [47]: composite systems. In addition, it was clearly understood that the core
PL shear modulus and panel shear rigidity of composites sandwich panels
Δ= filled with zeolite/polyurethane foam at 5wt% of the filler content
4U (3)
were greater than those observed in the case of other composite sand-
where Δ is total beam midspan deflection. Also, the panel bending wich panels.
stiffness, D, is the slope of force-deflection curve in the three point The findings, moreover, confirmed that the skin crushing and shear
bending testing. The panel shear rigidity was calculated by equation (4) failure dominate the load capacity of the composite sandwich panels
[47]: based on the three-point bending observations. Moreover, the failure of
G (d + c )2b fibers in the vertical direction, crimp and kinking leaded to the domi-
U= nant failure mechanism of the sandwich panels as seen in Fig. 11. The
4c (4)
results indicated that the crack propagation initiated from the resin-rich
where G is the core shear modulus.
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H. Safari et al. Polymer Testing 67 (2018) 284–294
region around vertical yarns and propagates along the vertical yarns E = mgH (6)
with skin delamination in composites.
where E is the impactor potential energy, m is the impactor mass, g is
gravity acceleration and H is the height of the impactor.
3.4. Specific strength
The results indicated that impact resistance of the specimens in-
creased with the increase in the impact velocity. At the initial stage of
The specific strength is the ratio of strength and density. Under the
premise of equal weight, they are indices of measuring bearing capacity the impact loading, the energy absorption slightly was increased fol-
lowed by the fibers failure and absorbance of a larger amount of impact
and stiffness properties of the material. Such properties are very im-
portant for lightweight structural materials to work in the air or the energy by the matrix. As the impact velocity increases, the damage of
composite specimens were became more severe that could be correlated
space. The density of composite sandwich panel was approximated
according to the ASTM C271 [49] using equation (5): to the high energy absorption provided by composite panels. The fiber
tension failure, debonding, fibers pulled out, and the matrix spallation
w
d= were the main damage mechanisms observed in the skin surface.
v (5)
Consequently, it could be concluded that this type of 3D woven com-
where d is the density of specimen, w is the final mass after curing, and posites had high delamination resistance since a lower degree of dela-
v is the final volume after curing. The density of plain composite mination was observed compared to that occurred in the case of the
sandwich panel and polyurethane filled composite sandwich panel were stacking thin 2D monolayers composite in other investigations.
calculated to obtain the strength-to-weight ratio value of composites. It was also observed that the drop test in the case of 1.8 m height did
The specific strength values of sandwich structures (strength to density not lead to any damage throughout the specimens. In the case of the
ratio) are given in Table 11. It could be understood that the increased impact energy of 59 J and the impactor height of 2 m, the impact on the
weight of composites by injecting the polyurethane foam resulted in composites resulted in the perforation of the sandwich panel and the
150% and 30% increase in the specific strength of flatwise compression projectile therefore rebounded after the incidence. The failure of the
and edgewise compression specimens, respectively. vertical fibers under the impact is clearly shown in Fig. 13.
By using CES EduPack 2013 material selector software, it is possible The observations further indicated that, in the case of the poly-
to draw comparisons between of a wide range of material by their urethane foam filled specimens, the impact damage area when the
properties. Here, graphs of Fig. 12 were used to observe that choosing energy value of 59 J and the impactor height 2 m were used was nar-
3D woven composites can be the most optimal material. rower than that occurring in the case of plain specimens. The findings
were ascribed to the presence of polyurethane foam core as an energy
3.5. Drop weight impact test absorber medium within the specimens. Local denting, cracking and
fiber fracture on the uppermost surface were observed in the plain
The drop weight impact test was carried out on the composites. To better explore the failure mechanisms occurring
24 × 100 × 210 mm3 neat polyurethane filled composites and plain 3D through the impact test, a sandwich panel was subjected to the incident
fiber specimens according to the ASTM D7136 standard [48]. Three energy of 59 J was sectioned. Fig. 14 depicts the impact damage in-
specimens were used for characterization and the average values were curred to a specimen showing resin cracking and delamination. The
reported. The specimens were secured in place using four clamps to damage occurred onto the upper skin is clear, taking the form of
prevent the specimen from rebounding during the impact event. To denting by debonding, a small delamination adjacent to the impact
perform the experiment, a 3 kg conical impactor released from the location. The natural zeolites have a unique three-dimensional honey-
height of 1.8 and 2 m ensuring the impact energy of 52 J and 59 J, comb structure, which creates an absorbing framework [43,44,51]. This
respectively. The impact energy was calculated according to the energy structure can be effective under impact loading. Deformations caused
balance equation as expressed by equation (6): by impact loading crushes these structures while absorbing impact
Table 11
Specific strength values of studied 3D woven composites considering of two types of Al-sandwich panel composites.
Sandwich structure Specific flatwise compression strength (Pa.m3/kg) Specific edgewise compression strength (Pa.m3/kg) Density (kg/m3)
290
H. Safari et al. Polymer Testing 67 (2018) 284–294
Fig. 12. . Graphs of comparative mechanical properties for woven epoxy/fiber composite, stainless steel-aluminum honeycombs and aluminum foams (a) tensile strength versus com-
pressive strength; (b) specific tensile strength versus price and (c) yield strength versus poisson's ratio.
energy. The external load is transferred to cell walls at the cell level and composites.
deflections is reflected at macro-level. The schematic diagram of this Fig. 18 represents the SEM of polyurethane foam/nano-structured
process is shown in the following Fig. 15. zeolites composites. It was observed that the zeolite presented in an
irregular and heterogeneous granulometry. It is worth noting that to
improve the foam quality, granulometry aside, the ideal is to utilize a
3.6. Scanning electron microscopy chemically pure material that does not contain substances reacting with
the polyurethane. The SEM images also indicated the presence of zeo-
The scanning electron microscope (SEM) technique was employed lite particles of spherical shapes with the dimension of 100–1000 nm.
in morphological characterization of nano-structured zeolite/poly- Figs. 19 and 20 are used to detect the various elements of zeolite
urethane composites. The porous structure of neat polyurethane is elemental constitution. Zeolites are generally a group of alumina sili-
clearly shown in Fig. 16. Fig. 17 exhibits the SEM image of poly- cate minerals with porous structures. The EDX data analysis was
urethane network and glass fibers interaction in transversal section of
Fig. 13. Failure of vertical fibers occurring under the local impact region.
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H. Safari et al. Polymer Testing 67 (2018) 284–294
Fig. 14. The damage area of composite sandwich panel by drop weight impact test.
4. Conclusion
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H. Safari et al. Polymer Testing 67 (2018) 284–294
Fig. 18. SEM of polyurethane foam filled with nano-structured zeolite particles with magnification of (a) 200× and (b) 400×.
293
H. Safari et al. Polymer Testing 67 (2018) 284–294
Table 12 integrated woven spacer composites at room and subzero temperatures, J. Sandw.
Characterized chemical elements of natural nano-structured zeolite by EDX analysis. Struct. Mater. (2016) 1–14.
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