The temperature effect on the inter-laminar shear properties and failure mechanism of 3D orthogonal woven composites

Abstract

Recent increases in the use of carbon fiber reinforced plastics, especially for high-temperature applications, has induced new challenges in evaluating their mechanical properties. The effects of temperature on the shear performance of 3-dimensional orthogonal and 2-dimensional plain woven composites were compared in this study through double-notch shear tests. A scanning electron microscope was employed to investigate the fiber/matrix interface properties to reveal the failure characteristics. The results showed that temperature had a visible impact on the inter-laminar shear strength (ILSS), deformation modes, and failure mechanism. The ILSS decreased as temperature increased, which was caused by the degradation of the matrix properties and fiber/matrix interface properties at high temperature. A finite element model was established to analyze the transient deformation process and the damage mechanism of the 3D orthogonal woven composite. This indicated that Z-binder yarns could improve the delamination resistance of 3D orthogonal woven composites, especially under high temperatures. The changes in failure modes of the 3D orthogonal woven composites was put down to thermal softening of the epoxy resin caused by high temperature and the undulation of the yarns.

Keywords

3-dimensional orthogonal composite inter-laminar shear strength high temperature;finite element model (FEM)

Carbon fiber reinforced plastics are attractive for use in a wide range of aeronautical structures due to their high performance in mechanics.^1–4 Compared with two-dimensional (2D) composites, three-dimensional orthogonal woven composites (3DOWCs) are increasingly being adopted in aeronautical structures and components^5–7 due to their superior inter-laminar fracture toughness.^8,9 In such applications, the composites are subjected to harsh environments featuring high-temperature exposure, which accelerates the decline in their mechanical and other properties.^5,6 Investigation of the degradation of 3DOWCs under high temperatures is vital in order to provide basic information relating to their safe usage.

Several studies that take into account the effects of temperature on the mechanical properties of composites are available in the literature.^10–15 Liu et al.¹³ reported that high temperatures caused a much greater decrease in bending strength than the tensile strength of 3D braided composites. Cao et al.¹⁴ compared the tensile properties of composites with those of hybrid carbon/glass fiber reinforced epoxy resin sheets at elevated temperatures. They found that the tensile strength of different sheets decreased significantly with increasing temperature and, further, that the hybridization of fibers could reduce the scatter of the strengths of composites. Wang et al.¹⁵ investigated the effects of elevated temperature on the mechanical properties of pultruded composites. Their results showed that the ultimate strength at 300 ℃ was reduced by 50% of that under 25 ℃. The above research revealed the mechanical properties of the composites were sensitive to high-temperature environments. Moreover, Hawileh et al.¹⁰ captured brittle fiber ruptures and sheet splitting during tensile tests under elevated temperatures; and Liu et al.¹² found that the failure mode of the composites with a sandwich structure changed from node failure to fiber micro-buckling with increasing temperatures. Their studies showed that high temperatures had a visible impact on the failure modes of the composites. At the same time, 2D composites were found to be prone to suffering delamination damage at elevated temperatures.^14,16 Compared with 2D plain woven composites (2DPWCs), 3DOWCs can improve delamination resistance at room temperature (25 ℃) due to the additional yarns, known as binders, which interlace through the fabric thickness.^17–19 However, to date, little work has been carried out on high-temperature shear properties and understanding the failure mechanism of 3DOWCs.

This study aimed to understand how elevated temperatures affected the shear property of 3DOWCs. Double-notch shear tests were performed to investigate the ILSS of the 3DOWCs at temperatures ranging from 25 ℃ to 150 ℃. The effects of high temperature on ILSS, damage modes, and failure mechanisms were studied and analyzed. Furthermore, a finite element model (FEM) was created to reveal the failure mechanism of the 3DOWCs. In addition, the results of the 3DOWCs and 2DPWCs were compared in this work.

Materials and experiments

Materials

Carbon fibers T700S-12K-CF and T300S-6K-CF (Toray Inc., Japan) were used to weave the 3D orthogonal woven fabric (Figure 1(a)) on a 3D weaving machine in Xi'an Polytechnic University, China. The first and last two layers were composed of T700S-12K-CF, and the other layers and Z-binder yarns comprised T300-6K-CF. T700S-12K-CF plain woven fabric (Dezhou Jiatong Composites Co., LTD, China) was used to make the plain woven preform (Figure 1(b)). The parameters of the 3D orthogonal woven preform and the 2D plain woven preform are shown in Table 1.

Figure 1.

Schematic diagram of the preforms: (a) the 3D orthogonal woven preform, and (b) the 2D plain woven preform.

Table 1.

Parameters of the 3D orthogonal and 2D plain woven preform

Reinforced structure	Preformed unit density/(yarn/cm)			Layers
Reinforced structure	Warp	Weft	Z-binder yarn	Layers
3D orthogonal woven preform	5	5	5	11
2D plain woven preform	1.3	1.3	–	18

JC-02A, JC-02B, and JC-02C (Changshu Jiafa Chemical Co., Ltd, China) were mixed in a weight ratio of 100:85:1 and used as the matrix with the vacuum assisted resin transfer molding process to make composites. The tensile strength and tensile modulus of the epoxy resin were 65 MPa and 2.2 GPa, respectively. The elongation rate of the epoxy resin was 5%. The glass transition temperature (T_g) of epoxy resin was 120℃. The curing cycle of the epoxy resin was 90℃ for 2 h, 110℃ for 1 h, and 135℃ for 6 h. The curing processes are detailed in research by Fan et al.²⁰

The cross-section microscope pictures of the 3DOWCs and 2DPWCs are shown in Figure 2. Figure 2(a) shows the profile of the Z-binder yarn in the 3DOWCs.

Figure 2.

The cross-section microscope pictures of the composites: (a) the 3D orthogonal woven composite, and (b) the 2D plain woven composite.

The utilized weighting method calculated the fiber volume fraction according to the following equation:²¹

V_{f} = 1 - \frac{G_{c} - G_{p}}{ρ r} \times 100 %

(1)

where V_f is the fiber volume fraction (%), G_c is the weight of the composite (g), G_P is the weight of the preform (g), and ρ_r is the density of resin (g/cm³). The fiber volume fractions of 3DOWCs and 2DPWCs were 56.8% and 56.3%, respectively.

Test methods

Inter-laminar shear test

A previous study showed that complex fractures are prone to occur in the short-beam shear test.²² However, Mahmood et al.²³ reported results with fractures occurring in a single plane using the double-notch shear test. Therefore, the shear behaviors of the composites were investigated with the double-notch shear test method. Specimens with dimensions 79.5 × 12.7 × 4 mm³ and a notch depth of 2 mm (the two notches were 6.4 mm apart) were prepared according to ASTM D3846.²⁴ The double-notch shear test is very sensitive to the accuracy of the notches cut, therefore, they were made using a laser cutting machine employing small depth increments to control the precision and reduce micro-cracks. An additional benefit is that the cooling liquid used in laser cutting can effectively avoid the damage caused by overheated cutting. The schematic diagram of the double-notch shear test apparatus is shown in Figure 3. In this study, four temperature cases (25℃, 90℃, 120℃, and 150℃) were considered for the shear test of the composites.

Figure 3.

Schematic diagram of the double-notch shear test.

The experiments were carried out using a universal test machine (Shenzhen Suns Technology Co., Ltd, China) with a thermal chamber. The measuring range of the load cell tester was 0–50 kN. The chamber was able to heat the specimens to the defined temperatures. After temperature stabilization inside the chamber, a minimum soaking period of 30 min was determined to guarantee the thermal equilibrium of the test specimens. The test speed was set at 1.3 mm/min through the displacement-controlled model. The average value of each coupon obtained was based on three repeated shear tests.

Compression test

The compression tests were conducted on pure resin using a universal testing machine. The dimensions of the compression sample were 10 × 10 × 15 mm³. The compressive speed was set as 2 mm/min. The test temperatures were 25℃, 90℃, 120℃, and 150℃ respectively, which were consistent with the inter-laminar shear test temperatures.

Fracture morphology

The fracture morphologies of specimens were observed with the VHX-5000 Ultra-Field Microscopy System (KEYENCE International Trading (Shanghai) Co., Ltd.). The fiber/matrix interface morphologies were observed using a scanning electron microscope (SEM) (Quanta-450-FEG, FEI Co., America). To be observable by SEM, the sample surface needs to be coated with an ultrathin coating of electrically conductive material, gold in our case.

Finite element model

The shear properties of the 3DOWCs were simulated under 25℃ and 150℃ conditions to reveal the influence of temperature and Z-binder yarns on the shear properties of 3DOWCs. Detailed information about the model follows.

Multi-scale geometrical model

In the FEM, the representative unit cell (RUC) incorporated microstructural details to predict the mechanical behavior of the fiber reinforced composites.^25,26 However, the RUC model could not be used to simulate the double-notch shear test. Based on the microstructure geometry of the 3D orthogonal woven preform and the epoxy resin, the multi-scale (micro-, meso-, and macro-scale) geometrical models were established as shown in Figure 4. The composites are composed of the enormous carbon fiber filaments and the resin matrix. To simplify the model, the fiber tow, which was comprised of the fiber filaments and the resin, was utilized to create the geometrical model of the RUC in a meso-unit cell scale. The matrix model was obtained through Boolean operations in the commercial ABAQUS²⁷ software package. According to the dimensions of the specimen, the full-size model of the composite was obtained through duplicating the meso-unit cell. Though a full-size model would have required considerable time to simulate the shear process due to the large number of elements, Liu et al.²⁸ proved that the ideal size of a geometrical model did not affect the compressive properties of composites with the same repeated structure, hence, we used a small-scale model to represent the full-size model to complete the shear test simulation, as shown in Figure 4.

Figure 4.

The multi-scale microstructural geometrical models of the 3DOWCs.

Material model

Carbon fiber is considered to be temperature-independent material.²⁹ Table 2 presents the mechanical parameters of carbon fiber at 25℃. The compression property of the resin at different temperatures is shown in Figure 5. The compression property of the resin is heavily dependent on temperature (Figure 5), therefore, the resin was assumed to be temperature-dependent in the FEM. This is consistent with other research.^30,31 The parameters in Table 3 were calculated according to the method mentioned in the work of Haque et al.⁵ The details are as follows. The reduction in the elastic properties of the epoxy resin-based fiber tow after thermal exposure was extracted from the initial slopes of the load-displacement curves from the experimental compression data. All elastic properties, except for Poisson's ratio, were moderated by the reduction factor, which was obtained by comparing the compression modulus of the specimen under high temperatures with that of a pristine specimen. In the present work, the resin matrix was assumed to be an elastic-plastic material. The carbon fiber tows were regarded as a transversely isotropic unidirectional composite. To simulate the fracture of the composite, the ductile and shear failure criteria³² were utilized to control the damage of the fiber tow and epoxy resin, respectively. The interfaces between fiber tow and resin were assumed to be an ideal case, in that the surfaces of the fiber tow and resin were combined with the tie constraint.

Figure 5.

Stress–strain curves of epoxy resin at elevated temperatures.

Table 2.

Elastic parameters of the carbon fibers at 25℃

	Carbon fiber
Longitudinal modulus, E₁₁ (GPa)	230
Transversal modulus, E₂₂ (GPa)	30
Shear modulus, G₁₃ (GPa)	12.5
Shear modulus, G₂₃ (GPa)	15
Poisson's ratio, ν₁₂	0.3

Table 3.

The elastic parameters of the epoxy resin-based fiber tow under different temperatures

	25℃	90℃	120℃	150℃
Longitudinal modulus, E₁₁ (GPa)	161.66	161.39	161.20	161
Transversal modulus, E₂₂ (GPa)	9.49	6.41	3.66	0.137
Shear modulus, G₁₃ (GPa)	3.65	2.38	1.32	0.047
Shear modulus, G₂₃ (GPa)	3.48	2.34	1.33	0.049
Poisson's ratio, ν₁₂	0.3	0.3	0.3	0.3

Double-notch shear testing model of 3DOWCs

The double-notch shear testing model of the 3DOWCs is presented in Figure 6. The mesh schemes of each component are illustrated in Figure 6(b). Internal defects such as voids were not considered. The plate, warp yarns, and weft yarns were meshed with the linear hexahedral element (C3D8R). Two types of mesh (C3D8R and C3D6R) were adopted for meshing the Z-binder yarns. Considering the complexity and irregularity of the geometrical structure, a linear tetrahedral element (C3D4) was chosen for the resin matrix.

Figure 6.

Schematic of the double-notch shear test model: (a) the geometrical model, and (b) detailed information about the model.

Results

Figure 7 shows the stress–strain curves of all composites through inter-laminar shear tests at various temperatures. The shear stress of all specimens decreased with increasing temperature (Figure 7), which indicates temperature had a visible impact on the shear property of the composites. All the curves increase linearly during the initial stage, but with different slopes. At temperature above the T_g of epoxy resin, the curves initially rise more slowly. When the stress reaches a certain point, the curves all transition to the nonlinear phase, implying some initial damage such as fiber fracture, micro-buckling, and delamination has occurred in specimens. Subsequently, when the stress reaches a peak value, it suddenly drops at temperatures below the T_g, which indicates apparent brittle failure. The drop in the stress is more gradual at temperatures above the T_g.

Figure 7.

The shear stress–strain curves of the composites at different temperatures.

Compared with 2DPWCs, the 3DOWCs were capable of bearing higher shear stress. Moreover, when the stress increased to peak stress, the curves of the 2DPWCs suddenly dropped. However, the yield phenomenon indicating ductile damage³³ was observed for the 3DOWCs tested at temperatures above the T_g. Given the results presented, the 2DPWCs appear to have been prone to delamination in the shear test. The 3DOWCs suffered delamination at temperatures below the T_g, however, when temperatures were above the T_g, ductile damage occurred in the 3DOWCs.

Figures 8 and 9 show the failure modes of the composites at different temperatures. The fracture surface in the double-notch shear tests included one of the stacked fabric layers; the surface lay on a plane across the inter-laminar planes at a right angle. Figures 8(a) and (b) illustrate the inter-laminar shear failure of the 2DPWCs when the temperature was below the T_g of the resin. However, inter-laminar shear failure accompanied by apparent fiber bridging (Figure 8(d)) was apparent when the temperature was higher than the T_g of the resin.

Figure 8.

Fracture morphologies of the 2DPWCs at elevated temperatures.

Figure 9.

Fracture morphologies of the 3DOWCs at elevated temperatures.

Figure 9 shows the failure morphologies of the 3DOWCs. It can be seen that the damage modes of the composites change from fiber breakage and matrix damage to buckling failure at the double-notch locations when the temperature increases from 25℃ to temperatures that are higher than the T_g of the resin matrix.

Discussions

The effect of the matrix on the shear property

This paper compared the ILSS and the shear modulus in the linear phases of all specimens at different temperatures in Figure 10. The ILSS and shear modulus of all specimens declined with the rise of temperature.

Figure 10.

The ILSS and shear modulus (G) of the composites at elevated temperatures.

The compression test results (Figure 5) indicated the degradation of the epoxy resin under high temperatures: the curves fell gradually as temperature increased, which was due to molecular chain relaxation in the resin.³⁴ Carbon fiber filaments are temperature-independent, therefore, the degradation of the resin gave rise to the decline in the ILSS and shear modulus of the composites, illustrated in Figure 10. When the temperature exceeded the T_g, the thermal softening effect became particularly serious, which caused a significant reduction in the ILSS and shear modulus of the composites, reducing the structure's resistance to deformation. The epoxy resin could not transfer stress well at high temperatures. Therefore, degradation of the epoxy resin also contributed to the yield phenomenon observed in the 3DOWCs specimens under high temperatures.

In order to investigate the effect of temperature on the degradation mechanism of composites, SEM was used to examine the fiber/matrix interfaces of specimens at different temperatures. Figure 11 shows the microstructural failure morphologies of the 2DPWCs after the shear test at elevated temperatures. Figure 11(a) illustrates that a significant amount of residual resin matrix bonded to the fiber filaments, indicating that the interface between the fibers and resin was ideal at 25℃. There is less resin adhered to fibers and large gap between fibers, as depicted in Figure 11(d). Furthermore, there is large gap between fibers. This indicates that fiber/matrix interfacial debonding was the primary failure mechanism. Figure 11 shows that the amount of resin bonding to the fibers apparently reduced with the rise in temperature, indicating lower fiber to matrix adhesion and weak bonding. Hence, the reduction of the interface properties was a significant factor in the decrease of the ILSS of the composite under high temperatures.

Figure 11.

SEM images of fiber/matrix interfaces at elevated temperatures.

As discussed above, the thermal softening of the matrix resin and the deterioration of the fiber/matrix interface were two key factors resulting in the continual reduction in the ILSS and shear modulus of the composites. This yield phenomenon was also due to the significant thermal softening of the epoxy resin matrix at temperatures near or above the T_g.

The effect of reinforced structure on shear property

As evident from Figure 10, the ILSS and shear modulus of the 3DOWCs were higher than those of the 2DPWCs. The ILSS retention rates of the composites are summarized in Table 4. The ILSS retention rates of the 2DPWCs and the 3DOWCs at 90℃ were 83.21% and 84.66%, respectively; the difference between the two rates, 1.45%, indicating the difference was negligible in the case of temperatures below the T_g of the resin matrix. This phenomenon suggests that enhancement of the Z-binder yarns was not apparent at temperatures below the T_g. However, compared with the 2DPWCs, the ILSS retention rate of the 3DOWCs was significantly enhanced when the temperatures were equal to or higher than the T_g of the resin matrix. Since the temperature was close to the T_g of the resin matrix, the resulting accelerated relaxation process of the resin molecular chain induced weak interface adhesion and softened the resin.³⁴ In this case, the shear stress could not effectively propagate along the shear surface and caused buckling deformation of the 3DOWCs.

Table 4.

ILSS retention rate of the composites

	Retention Rate/%
	90℃	120℃	150℃
2D-CF/epoxy composite	83.21	30.41	11.83
3D-CF/epoxy composite	84.66	41.20	19.66

Figures 8 and 9 show the failure modes of the two kinds of composites at different temperatures. The reason for the difference in failure modes between the 2DPWCs and the 3DOWCs is that the addition of Z-binder yarns improved the integrity of the 3D orthogonal woven preform. The failure mode transition can be explained as follows. At temperatures below the T_g of the resin matrix, the molecular chain mobility of the resin matrix is inhibited.³⁵ In this case, the epoxy resin stress transfer was perfect. However, after it had attained peak value, the shear stress dropped suddenly, and brittle failure was observed under the shear test, as shown in Figures 8(a) and (b) and Figures 9(a) and (b). The resin matrix experienced severe thermal softening when the temperatures were approaching or above the T_g of the resin matrix, which caused degradation of the matrix properties (Figure 5). In this case, the properties of the epoxy resin protected and unified the fibers; the stress transferred between the fibers also reduced. As a result, the fibers were misaligned but in a continually wavy stage. Therefore, fiber bridging was observed in the 2DPWCs tested at temperatures close to or above the T_g. Moreover, the addition of Z-binder yarns in the 3DOWCs along the thickness direction, accompanied by the weak load-bearing property of the fibers, resulted in ductile damage.

To get a better understanding of the changes observed in the failure modes, the failure process of the 3DOWCs calculated in the small-scale model is presented in Figure 12. This shows the primary damage processes of the 3DOWC, the 3D orthogonal woven preform, and epoxy resin at 25℃. Six representative moments were chosen to illustrate the stress transfer process. Before strain reached around 4.0%, stress concentration occurred in the warp yarns. This was because the warp yarns were parallel with the loading direction; they had a chief role in load carrying. Figure 12(c) shows that damage occurred in the intermediate warp yarns when the strain was about 4.0%, implying fiber fracture occurred in the specimen. After that, the stress concentration area transferred to the Z-binder yarns. This means the warp and Z-binder yarns resisted shear deformation with the rise in shear strain. This is the primary reason that the 3DOWCs showed apparent nonlinear behavior in the test results shown in Figure 7. Figure 12 also shows the failure process of the matrix under the shear test. According to the stress contour in the resin, stress was primarily concentrated in the intermediate area. This failure of the resin was due to the shear damage of the corresponding Z-binder yarns. Taking the process as a whole, the 3DOWC underwent fiber breakage, resin damage, and destructive damage in sequence.

Figure 12.

The primary damage processes of the 3DOWCs at 25℃: (a) ε = 1.8%; (b) ε = 3.6%; (c) ε = 4.0%; (d) ε = 8.0%; (e) ε = 12.0%; and (f) ε = 12.4%.

As discussed (see Figure 5), the resin matrix lost its load-bearing capacity at temperatures above the T_g of the resin. Moreover, the reinforcement of the composites was the main load-bearing component and its stress state and damage had a significant impact on the overall mechanical behavior of the composites. Figure 13 depicts the stress distribution and propagation of the warp and Z-binder yarns at 150℃. Only buckling of the warp yarns is observed in Figure 13. This phenomenon could be attributed to the difference between the transversal modulus and the shear modulus of the yarns caused by the softened resin matrix (Table 3). The transversal and shear modulus of the fiber tows were 0.137 GPa and 0.047 GPa, respectively, at 150℃ (Table 3). Thus, the 3DOWCs were prone to suffering ductile damage at high temperature, as shown in Figure 9(d). In addition, the shear stress of the Z-binder yarns increased with increasing shear deformation and was concentrated in the double-notch location. This indicates that the Z-binder yarns helped resist the shear load at high temperatures where the resin matrix and the fiber/matrix performance degraded. It was the effect of the shear load on the Z-binder yarns that changed the tension effect. Accordingly, the 3DOWCs showed higher ILSS and shear modulus than the 2DPWCs at 150℃ (Figure 7). The ILSS retention rate of the 3DOWCs was higher than that of the 2DPWCs under high temperatures (Table 4).

Figure 13.

The primary damage processes of the 3DOWCs at 150℃: (a) ε = 0.6%; (b) ε = 1.2%; (c) ε = 1.8%; (d) ε = 2.4%; (e) ε = 3.0%; and (f) ε = 3.6%.

Briefly, some initial damage such as micro-buckling, fiber fracture, and delamination occurred in the specimens, which resulted in the nonlinear stage. The changes in the failure modes were attributed to the thermal softening of the epoxy resin caused by high temperatures. The Z-binder yarns did certainly but not obviously improve the shear property of the 3DOWCs at temperatures below the T_g, while their strengthening effect was significant in the case of temperatures that were close to or above the T_g.

Conclusions

This paper investigated the inter-laminar shear properties of 3DOWCs by experimental and numerical methods. In the double-notch shear test for characterization of the inter-laminar shear properties of 3DOWCs, the ILSS decreased with increasing temperatures ranging from 25℃ to 150℃; this was associated with degradation of the epoxy resin and the fiber/matrix interface performance. Compared with 2DPWCs, the 3DOWCs exhibited a higher ILSS retention rate. Moreover, there was a somewhat different temperature dependence between the failure modes of the 3DOWCs and 2DPWCs. Buckling damage was only observed for the 3DOWCs specimens tested at temperatures above the T_g due to the strengthening effect of the Z-binder yarns; this was confirmed by the experimental and FEM results. The 2DPWCs composites always suffered delamination failure due to the weak interface bonding. The 3DOWCs may be used as components for the engine exposure to high-temperature environment.

Footnotes

Declaration of conflicting interests

The authors declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Funding

The authors disclosed receipt of the following financial support for the research, authorship, and/or publication of this article: The authors acknowledge the financial support from National Natural Science Foundation, China (Grant Nos. 51603163, 51703179), Science and Technology Project of Shaanxi, China (Grant Nos. 2018JQ5214, 2019JQ–182), Scientific Research Program Funded by Shaanxi Provincial Education Department, China (Grant No. 18JS041), the sponsorship of Research Fund for the Doctoral Program of Xi'an Polytechnic University (Grant No. BS201910), Thousand Talents Program of Shaanxi Province, and Sanqin Scholar Foundation of Shaanxi Province, China.

ORCID iD

Wei Fan

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