Effect of salt–fog spray environment on bending fatigue properties of 3D woven composites

Abstract

In this study, the effect of salt–fog spray corrosion environment on bending fatigue properties of three-dimensional (3D) woven composites was investigated. Three test environmental conditions, namely a normal environment, two cycles of salt–fog spray corrosion environment, and four cycles of salt–fog spray corrosion environment, were designed. In addition, the salt–fog spray corrosion mechanism, the bending fatigue properties, damage mechanisms, and failure modes of 3D woven composites were studied. The results showed that the bending strength and bending modulus decreased by 5.5 and 9.3%, and 2.27 and 3.45% after two and four salt–fog spray cycles, respectively, compared with that of the normal environment. The bending fatigue properties of 3D woven composites were related to the applied stress and salt–fog spray cycles. The salt–fog spray environment was responsible for the degradation of the interface bonding strength. The maximum reduction ratio of bending fatigue life after salt–fog spray treatment exceeded 70%. The brittle fracture characteristics of 3D woven composite yarn were more pronounced with an increase in salt–fog spray aging cycles.

Keywords

Salt–fog spray 3D woven composites fatigue mechanism bending fatigue

Introduction

Three-dimensional (3D) woven composites are gradually being used as structural parts for aircraft engine blades, offshore wind turbines, bridges, and other fields owing to their high load-bearing capacity, corrosion resistance, and excellent fatigue performance.^1–3 The performance degradation of composite structural parts subjected to the marine environment has become a major concern.^4–6

The integrity of the composites can be negatively affected in the marine environment. Studies have shown that the impact performance,⁷ bending strength,⁸ tensile strength,⁹ fracture toughness,¹⁰ and other mechanical properties of laminated and woven composites subjected to marine environments can be reduced. The crack initiation and propagation speed of the composites increase under fatigue load after seawater immersion, thus decreasing their fatigue life.^11,12 At present, there is a lack of research on crack initiation and propagation of 3D woven composites under marine environments. There is a similarity between the fatigue failure mechanism and the static failure mechanism of the 3D woven composites under normal environments,¹³ The resin-rich region of 3D woven composites is easy to promote crack initiation and propagation.¹⁴ The degradation of mechanical properties of laminated composites depends on the duration of seawater immersion. Hilal¹⁰ showed that the fracture toughness of laminated composites immersed in seawater for 21 and 35 days decreased by 31% and 48.55%, respectively, compared with that of dry samples. Alaattin¹⁵ studied the effect of seawater immersion time (1, 2, 4 months) on the tensile strength of glass fiber composites. The results showed that the composite bearing capacities significantly decreased as the seawater immersion time increased. Koshima¹⁶ studied the tensile–tensile, tensile–compressive, and compressive–compressive fatigue lifespans of carbon fiber reinforced plastic laminates at different seawater immersion times (0, 100, 225, and 385 days). The result showed that the fatigue life of the composites initially reduced significantly and then rose slightly. This phenomenon was attributed to the post-curing effect of the resin. Deniz¹⁷ showed that the fatigue life of glass–epoxy composite pipe initially increased and then decreased with the increase in seawater immersion time. This phenomenon occurred because a shorter seawater immersion time was conducive to eliminating the residual stress in the sample, while a longer immersion time destroyed the matrix and interface properties. The effect of the marine environment on the fatigue properties of composites is related to the contact mode between the specimen and environment. Siriruk¹⁸ studied the effect of marine environment on the tensile fatigue properties of carbon fiber–vinyl ester composites. The fatigue life of the samples completely immersed in seawater and one sided sample face exposed to sea water decreased by 85% and 50%, respectively, compared with the normal environment. Altunsaray¹⁹ showed that the seawater environment reduced the fatigue life of the composite, but sample thickness and material direction had no significant effect on the fatigue behavior of materials. Some researchers have studied the hygroscopic mechanism of woven composites by establishing a water diffusion model. Tang²⁰ studied water diffusion in woven composites using the micromechanical model. The result showed that the hygroscopic ability of the woven laminates was higher than that of the unidirectional laminates. The hygroscopic ability of the woven laminates was higher because an increase in yarn waviness promoted the propagation of water molecules inside the composite material. Yu²¹ studied the non-Fikian behavior of 3D woven composites using the two-stage water diffusion model. The model was divided into an initial fast diffusion model and a long-term slow diffusion model. Yuan²² established a mesoscale moisture absorption model of 3D woven composites. The study showed that the moisture absorption process exhibited the characteristics of a sandwich structure, and the resin-rich area on the surface rapidly absorbed moisture, which served as a water transport channel and abundant water storage, promoting internal diffusion of water. The above studies showed that marine environments significantly affect the fatigue properties of composites. The current research mainly focuses on the influence of marine environment on the quasi-static mechanical properties and bending fatigue properties of laminate composites, while the influence of marine environment on the degradation degree of bending fatigue performance of 3D woven composites needs to be studied. The failure mode and failure mechanism of 3D woven composites under bending fatigue load were different from those of laminates.^23–25 Differences were observed between the seawater immersion and salt–fog spray environments.²⁶ Salt spray corrosion environment is the environment that 3D woven composites may face when applied to military and marine equipment. 3D woven composites may subject to salt–fog spray corrosion environment and bending fatigue load in marine environment. The purpose of this study is to promote the application of 3D woven composite structural parts under marine environments. Thus, in this study, the effect of a salt–fog spray environment on the bending fatigue properties of 3D woven composites was studied. This work provides experimental data and corresponding theoretical guidance for the future design and application of 3D woven composites subjected to marine environment.

Materials

Figure 1 shows the structure of the 3D woven preform and yarn interweaving rule of composites, and the composites parameters are shown in Table 1. The matrix used 5284 epoxy resin provided by AVIC Composites Co., Ltd (Tianjin, China). Resin transfer molding technology was adopted in the composites process.

Figure 1.

3D woven preform stereogram and composites yarn path diagram (a) preform structure, (b) warp and weft yarn interweaving points on the surface of the preform and composites, and (c) warp and stuffer yarn paths diagrams.

Table 1.

Preforms weaving parameter.

Warp yarns tex	Stuffer yarns tex	Weft yarns tex	Warp and stuffer yarns density	Weft yarns density	Compaction thickness (mm)
T800-12k	T800-24k	T800-24k	4 ends/cm	4 picks/cm	3.8

Experimental method

The salt–fog spray test was conducted according to the standard GJB 150.11A-2009 and reference 26, and the alternating steps of 24 h salt–fog spray and 24 h drying were adopted, with a test cycle of 48 h. In the salt-fog spray stage, the salt-fog had a chemical composition of 5% NaCl solution with the pH value of between 6.5 and 7.2, and the test temperature was set at 35°C. In the drying stage, the drying temperature was set to 35°C and the relative humidity was set to 40% in the oven. The bending performance test environment was normal, with two and four salt–fog spray cycles. The bending performance test environment was normal, with two and four salt–fog spray cycles. Quasi-static bending and bending fatigue tests were conducted using the Instron 8801 (INSTRON, Boston, USA) fatigue testing machine according to ASTM D7264 and ASTM D7774−17, respectively. Figure 2 shows the salt–fog spray device, test device, and parameter setting for the bending performance test. There were three quasi-static bending and bending fatigue tests.

Figure 2.

Fatigue test salt–fog spray environment and fatigue test device.

Results and discussion

Salt-fog spray corrosion mechanism of composites

Figure 3(a) shows the hygroscopic mechanism and hygroscopic weight gain curve. Figure 3(b) shows the surface topography characteristics of samples under normal environments and four salt–fog spray cycles corrosion environments. Figure 3(a1)–(a3) show the erosion process of composites under a salt–fog spray environment, which was represented by three stages. In stage I, the sample was in a salt–fog spray environment. In stage II, molecules of water and sodium chloride entered the composite, mainly in the defect and resin-rich areas of composites; these areas were mainly concentrated at the interweaving point of warp and weft yarn on the sample surface. Water molecules continued to invade the interior of the composite material as the salt–fog spray treatment time increased. In stage III, the water molecules aggregation state was different due to the hydrophobicity of carbon fiber and hydrophilic characteristics of resin.²⁷ Water molecules and sodium chloride molecules aggregated in the cross-linked structure of the resin. The exposure of composite to salt spray corrosion destroyed the C–O and C–H bonds, thus damaging the polymer chain and branch chain. The fracture of the chemical bond reduced the strength of the resin, and water molecules caused plasticization and expansion of the resin, which damaged the interface adhesion between fiber and matrix.^28–30 Figure 3(a4) shows the hygroscopic weight gain curve of the composite material. The weight of the composites slightly increased as the salt–fog spray treatment time increased. The hygroscopic degree of the composite was close to saturation at the end of the fourth salt–fog spray cycle. Figure 3(b1)–(b2) shows the surface characteristics of the samples under normal environments and four salt–fog spray cycles. The white spots in the resin-rich area after salt–fog spray treatment were generated by plasticizing swelling.

Figure 3.

(a) Mechanism diagram of the effects of salt–fog spray duration on composite materials and curves of moisture absorption process and moisture absorption weight gain of salt–fog spray (b) surface effect diagram of the samples after normal environment and four cycles of moisture absorption.

Effects of salt–fog spray duration on quasi-static bending properties

Figure 4(a) shows the quasi-static bending stress–strain curves of 3D woven composites under three environments. The stress–strain curves were similar, and a linear growth stage was observed before the stress reached peak point A. The stuffer yarn was the main load-bearing component, and the warp yarn was the secondary load-bearing component. The stress from point b to point c was lower than the peak and was in a state of fluctuation. In this stage, the warp played the role of a truss, made the composites not easy to fail quickly, and exhibited good toughness behavior characteristics. The stress rapidly decreased after the value point c, which indicated that the bearing capacity of the yarn reached its limit. Figure 4(b) shows the bending strength and modulus of the composites under three environments. The strength and modulus of two and four salt–fog spray cycles decreased by 5.5% and 9.3%, respectively, compared with that of the standard environment, and their moduli decreased by 2.27% and 3.45%, respectively. Swelling and plastic deformation of the matrix occurred, microcracks were generated at the interface between matrix and fiber, the internal integrity of composites was damaged, and the interface performance decreased in the salt–fog spray environment. The yarn was subjected to external forces in advance as the salt–fog spray time increased, resulting in a significant decrease in the mechanical bending strength of the composite. The modulus of the composite slightly decreased after salt–fog spray environment treatment. The slight decrease in the modulus can be attributed to the corrosion resistance and hydrophobicity of the carbon fiber.

Figure 4.

3D woven composites quasi-static bending properties (a) stress–strain curve diagram (b) bending strength and modulus diagram.

Influence of salt–fog spray treatment time on bending fatigue life

The loads applied to 3D woven composites were 306, 270, 234, and 198 N. Figure 5 shows the relationship between stress and bending fatigue life of 3D woven composites. The bending fatigue limits of 3D woven composites in the normal environment, two salt–fog spray treatment cycles, and four salt–fog spray cycles were 198, 198, and 193.2 N, respectively. Compared with the flexural fatigue life under a normal environment and four stress conditions, the flexural fatigue life under two salt–fog spray cycle environments decreased by 25.25, 51.63, 20.01, and 7.53%. The bending fatigue life of the composite under four salt–fog spray cycles environment decreased by 58.83, 71.32, 55.97, and 27.86%. The bending fatigue life of 3D woven composites further decreased as the salt–fog spray treatment time increased, indicating that the damage of salt–fog spray corrosion to the interior of the composites significantly increased under the bending fatigue loading mode. The water ingress due to the capillary phenomenon significantly accelerated the progress of crack initiation and propagation of composites under bending fatigue load,¹¹ And the salt-fog spray has promoted the formation of cracks in the resin-rich area and the interfacial debonding of the fiber and resin.²⁶ Thus, Initial cracks and the reduction of interface performance may have adverse effects on the lifespan of 3D woven composites under the bending fatigue load. In a salt–fog spray environment, the crack initiation occurred earlier, the number of cracks increased, and water molecules caused swelling and deformation of the matrix, which facilitated the expansion of microcracks at the interface under the bending fatigue load. The decrease in interface properties directly led to the decrease in bending fatigue life. The bending fatigue life of the composites significantly decreased at 270 N load and slightly decreased at 198 N load. Under the same salt–fog spray environmental treatment conditions, the reduction range of bending fatigue property initially increased and then decreased as the applied load value decreased. The fatigue life of 3D woven composites sample is greatly affected by the loading load. With the increase of the loading load level, the damage evolution rate and internal damage degree of 3D woven composites mesoscopic components increases.^31,32 In this study, at a load of 270 N, the internal damage degree of composites was the greatest, the interface performance was more severe, and the reduction of bending fatigue life was the greatest. However, under the load of 198 N, the damage degree of the specimen was reduced, the damage evolution time of the specimen increased, and the reduction of bending fatigue life of the composite was reduced.

Figure 5.

Flexural stress-life curve of 3D woven composites.

Effect of salt–fog spray environment on bending modulus life

The evolution law of bending fatigue damage of 3D woven composites is shown in Figure 6. The bending modulus life curve is divided into three stages under a normal environment. In stage I, the bending modulus of the composites rapidly decreased. This stage accounted for approximately 10% of the total bending fatigue process. In stage I, the occurrence and propagation of microcracks in resin-rich regions near the warp path was the main failure mode, resin‐rich appear near the warp/weft weaving points, Jiao’s research³³ confirmed the locations of resin-rich regions. In stage II, the bending modulus curve was flat and stable. The flatness and stability of the curve were because the warp and weft yarn were closely intertwined, the single cell size was only 5 mm in the warp direction, and the interface crack did not spread easily. The speed of the warp yarn transmitting stress along the thickness and in-plane direction, and the extent of crack propagation along the warp path were the main factors that influenced the flexural fatigue life of the composites at this stage. This stage accounted for approximately 77% of the total process. At stage III, the interface crack was unable to expand, and the stuffer and warp yarn were directly subjected to external loads. The moduli of the stuffer and warp yarn rapidly decreased owing to the fracture of the carbon fiber. In addition, stage III accounted for approximately 13% of the total fatigue process. The proportion of the three stages in the salt–fog spray environment was close to that of the normal environment. The bending modulus life, initial modulus after salt–fog spray treatment was lower than that under a normal environment because water molecules destroyed the integrity of the sample. The matrix became swollen and soft with the continuous intrusion of water molecules, and the influence of matrix micro–deformation extended to the fiber/matrix interface, which eventually affected the yarn and decreased the initial modulus. The bending modulus value under a standard environment was relatively stable under a three–point bending fatigue load. However, the modulus after salt–fog spray treatment slightly fluctuated, which indicated that the internal damage area of the sample was unstable, and the crack growth was irregular. Salt–fog spray treatment intensified the microscopic damage inside the sample, resulting in a fluctuating and slowly decreasing trend in the second stage of the bending modulus curve of the sample. The bearing capacity of the yarn approached the limit when the damage accumulated to a certain extent, thus rapidly decreasing the bending modulus of the composites.

Figure 6.

The curve of bending modulus and life of laminated woven composites.

Failure mode and failure mechanism of 3D woven composites

Figure 7 shows the macro fracture morphology photos and fatigue failure mechanism diagram subjected to three environments and at 270 N loading conditions. During three-point bending, yarns in the beam length direction mainly carry tensile load at outer layers and carry compression load at inner layers, yarns in the beam thickness direction mainly carry shear load.³⁴ In Figure 7(a), The macroscopic failure topography characteristics revealed that the fracture failure mode changes under the three environments. The failure modes of the sample include breaking of the warp and stuffer yarns, cracking between the warp fiber bundles, cracking of the weft, separation of the interfacial interface between the warp and weft yarns, delamination of the interface between the stuffer and weft yarns, and breaking of the interfacial interface between the yarn and resin under a normal environment. The failure modes of the sample after two salt–fog spray cycles were as follows: breakage of the warp and stuffer yarns, cracking of the warp and weft yarns, separation of the warp and weft yarns interface, separation of the stuffer and weft yarns interface, cracking of the weft yarn. The failure modes of the sample after four cycles of salt–fog spray cycles were as follows: fracture of the warp and stuffer yarns, matrix fracture, and slight interface cracking throughout the thickness direction of the sample. This study showed that the failure mode of 3D woven composites under bending fatigue load is different the pure bending failure mode of metal materials.

Figure 7.

Bending fatigue failure mechanism of composite materials under salt–fog spray environment, (a) fracture failure morphology under three environments (b) normal environment, (c) twice salt–fog spray cycle treatment, (d) four salt–fog spray cycle treatment.

In this study, By combining the the experimental phenomenon, macroscopic fracture morphology characteristics and the failure mechanism of bending fatigue, the process of bending fatigue damage initiation to failure of 3D woven composites was described under normal environments and salt–fog spray corrosion environments. The bending fatigue failure mechanism was shown in Figure 7(b)–(d) The corners of the warp yarn paths were prone to crack initiation and propagation along the warp yarn paths under bending fatigue load, ultimately leading to composites failure,³⁵ In initial damage stage, The damage of 3D woven composites mainly occurs at the interweaving of the warp and weft yarns on the upper and lower surfaces and near the stuffer yarns under normal conditions, However, cracks are easy to occur in the resin-rich region near the warp and weft yarns interweaving of 3D woven composite samples after salt spray treatment, resulting in a significant decrease in bending fatigue performance, as shown in the first stage of stiffness degradation in Figure 6. In damage evolutiong stage, Compared to the damage process of 3D woven composites under normal environments, the interface performance of 3D woven composites after salt spray treatment decreases, and the yarns are more susceptible to external loads in advance, thus, the degree of yarn damage increases. In failure stage, the yarn fracture phenomenon along the thickness direction of the 3D woven composites becomes more obvious with the salt spray treatment cycles increases. This stage corresponds to the fracture morphology in Figure 7(a), which indicating that the salt spray environment has caused serious damage to the interior of the sample. In this study, the residual bending fatigue strength of 3D woven composites was tested under normal conditions, as shown in Table 2. Under the bending fatigue life conditions of 1/2, 2/3, and 5/6, the remaining strength is 94%, 91.7%, and 84.5% of the initial strength, respectively. The results showed that the reduction degree of residual strength of the specimen increases with the increase of the set number of bending fatigue cycles. Compared with the normal environment, the plasticizing effect and severe cracks were observed in the resin–rich area of the sample after salt–fog spray treatment, and the failure location occurred near the resin–rich area. The resin–rich area was more prone to crack, and microcracks were generated at the interface with the yarn after salt–fog spray treatment. Many cracks were generated with the progress of fatigue loading, resulting in more severe damage areas. The interface properties were severely damaged as the salt–fog spray treatment time increased, the yarn lost protection, and the stress time advanced, facilitating the brittle fracture of the yarn.

Table 2.

Residual strength test of 3D woven composites.

Ultimate strength (MPa)	Environment	Stress level (%)	Residual strength in a specific number of cycles
360	Normal environment	80	Half of the total number of cycles	Two-thirds of the total number of cycles	Five-sixths of the total number of cycles
360	Normal environment	80	338.4 MPa	330.12 MPa	304.2 MPa

To further illustrate the failure mode, Figure 8 shows the micromorphologies of the two samples after full fatigue loading under a normal environment and four cycles of salt–fog spray. Figure 8(a) shows the fracture morphology characteristics of the sample. The yarn on the fracture surface of the sample under a normal environment exhibited a cohesive state and was not completely broken. However, the yarn fracture of the sample after four salt–fog spray cycles became flat, and the characteristics of brittle fracture of the yarn were more pronounced. Figure 8(b) shows the comparison of the residual state of the resin after bending fatigue loading. The surface of the yarn after salt–fog spray treatment was relatively clean, and a large amount of resin fell off from the surface of the yarn. Figure 8(c) shows the surface state of the resin. The resin after salt–fog spray treatment was more likely to swell due to moisture absorption, and microcracks were more likely to occur under bending fatigue load and eventually lead to fall off. As shown in Figure 8(d), the samples exhibited better interface properties under normal conditions, while the samples treated with salt–fog spray were more likely to produce interface debonding and cracking between fiber bundles. The comparison of the microtopography of 3D woven composites in Figure 8 revealed that the interface properties of the samples after salt–fog spray treatment decreased, and the chance of resin falling off the fiber surface was high. The cracking phenomenon between fiber bundles increased the probability of fiber bundles being stressed in advance, thus decreasing the bending fatigue properties of composites.

Figure 8.

Failure micromorphology of 3D woven composites under a normal environment and after four cycles of salt–fog spray.

Conclusion

In this study, the effects of salt–fog spray duration on quasi-static bending and bending fatigue properties of 3D woven composites were studied, and the salt–fog spray corrosion mechanism, bending fatigue damage mechanism, and failure mode of 3D woven composites were analyzed. The main conclusions are as follows:

Compared with the standard environment, the quasi-static bending strength and modulus decreased with the increase in salt–fog spray treatment time. After two and four salt–fog spray cycles, the strength decreased by 5.5 and 9.3%, and the modulus decreased by 2.27 and 3.45%, respectively.

The bending fatigue properties of 3D woven composites decreased with increasing salt–fog spray treatment time. Under the same salt–fog spray environmental treatment conditions, as the applied load of bending fatigue decreased, the reduction range of bending fatigue performance initially increased and then decreased, and the maximum decrease in fatigue life exceeded 70%.

The bending modulus fatigue life curve of 3D woven composites was divided into three stages, and the bending modulus fluctuated and slowly decreased after salt–fog spray treatment in the second stage.

The macro and microfracture morphology revealed that the interface properties of 3D woven composites after salt–fog spray treatment were worse, the yarns were prone to premature damage, and more severe yarns broke and pulled out.

Footnotes

Declaration of conflicting interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and publication of this article.

Funding

This work was supported by Science and Technology on Advanced Functional Composites Laboratory, Aerospace Research Institute of Material and Processing Technology (No. 6142906210406), A Multi-Scale and High-Efficiency Computing Platform for Advanced Functional Materials, a scientific research program funded by Haihe Laboratory in Tianjin, China(Grants No. 22HHXCJC00007), National Science and Technology Major Project, China(No. 2017-Ⅶ-0011-0177), Science Center for Gas Turbine Project, China (No. P2022-B-IV-014-001). The authors acknowledge National Supercomputer Center in Tianjin, and the calculations were performed on Tianhe 3F.

ORCID iD

Shibo Zhao

Data Availability Statement

The datasets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request*.

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