Static and fatigue tensile properties of cross-ply carbon fiber-reinforced epoxy matrix composite laminates with thin ply thickness

doi:10.21203/rs.3.rs-2345897/v1

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Static and fatigue tensile properties of cross-ply carbon fiber-reinforced epoxy matrix composite laminates with thin ply thickness

https://doi.org/10.21203/rs.3.rs-2345897/v1

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The static and tensile fatigue properties of cross-ply high-strength polyacrylonitrile (PAN)-based carbon (T800SC) fiber-reinforced epoxy matrix composites (CFRPs) with thin ply thickness were studied. The fiber orientations of the CFRP specimens were set to cross-ply with [0/90]_10S (subscript S means symmetry), [(0)₅/(90)₅]_2S, and [(0)₁₀/(90)₁₀]_S. The static and tensile fatigue characteristics of cross-ply CFRPs with thick ply thickness with [0/90]_2S and [(0)₂/(90)₂]_S were also investigated for comparison. Under static loading, the tensile strength and failure strain of thinnest 90° ply CFRP specimens were higher than those of other 90° ply thickness ones. But, the tensile modulus and Poisson’s ratios were comparable among the cross-ply CFRP with thin and thick ply thickness specimens. Under fatigue loading, the fatigue response of thinnest 90° ply CFRP specimens were higher than those of other 90° ply thickness ones for lower fatigue cycle testing (< 10⁵ cycles). Though, for higher fatigue cycle testing (> 10⁵ cycles), the fatigue responses decreased with a decrease in the 90° ply thickness and the fatigue characteristics of the thinnest 90° ply CFRP specimen were lower than those of other cross-ply CFRP thin and thick ply thickness specimens.

Physical sciences/Engineering

Physical sciences/Materials science

CFRP

cross-ply

ply thickness

static

fatigue

tensile properties

Carbon fiber-reinforced polymer matrix composites (CFRPs) have gained in aerospace, automotive, and sporting goods industries^1–5. CFRP laminates are impacted by the buildup of damage (e.g., matrix cracking, delamination), and strong CFRPs can be developed when achieving an increase in the damage resistance^6–10. The fracture behavior in the CFRP laminates includes matrix cracking, which can be delamination, fiber-matrix debonding, and fiber fracture and splitting. Transverse microcracking via the thickness of the ply occurs, and the delamination damage follows. Many theoretical and practical studies have been performed on CFRP laminates’ fracture behavior, including delamination induced by transverse cracks^11–18. Laws and Dvorak re-ported the transverse cracking in cross-ply composite laminates based on statistical fracture mechanics. The crack density as a function of the applied load was also assessed¹¹. Lim and Hong investigated the effect of transverse cracks on the thermo-mechanical property degradation of cross-ply composite laminates¹². Lee and Daniel proposed a simplified shear lag analysis using a progressive damage scheme for cross-ply composite laminates under uniaxial tensile loading. Closed-form solutions for stress distributions, transverse crack density and reduced stiffnesses of damaged plies could be obtained as a function of the applied load¹³. Takeda and Ogihara evaluated the microscopic fracture mechanisms focusing on the transverse crack in CFRP cross-ply laminates^14–16.

Ply thickness significantly impacts the increase in damage accumulation and thinner plies have higher transverse strength or (i.e., resistance to matrix cracking)^{6–10, 19–21}. Sasayama et al.¹⁹ developed thin-ply prepregs using a novel spread technique of carbon fiber tows. CFRP laminates with thin ply thickness have high damage resistance properties compared with standard prepregs^19–21. Nevertheless, there are still few studies on CFRP laminates with thin ply thickness, and there are no studies investigating the relationship between ply thickness and static and tensile fatigue properties of CFRP laminate with thin ply thickness with various-stacking sequences. Static and fatigue tensile fracture behavior of cross-ply CFRP laminates with thin ply thickness should be further studied for the applicability of thin-ply prepregs for industrial structures.

Cross-ply laminates have been extensively investigated via theoretical and experimental studies because this is a basic laminate configuration^12–16. In this work, static and tensile fatigue tests of cross-ply high-strength polyacrylonitrile (PAN)-based carbon (T800SC) fiber-reinforced epoxy matrix composite laminates with thin ply thickness with three stacking sequences ([0/90]_10S, [(0)₅/(90)₅]_2S, and [(0)₁₀/(90)₁₀]_S.) were conducted to examine their fracture behavior. In situ static and tensile fatigue tests using a digital microscope were performed to obtain practical knowledge of the fracture mechanism of tensile properties. The relationship between the crack density, number of cracks, and tensile properties were examined according to the obtained damage observation.

Materials

A promising and cost-effective method is to use a tow-spreading technology developed by the Industrial Technology Center in Fukui Prefecture¹⁹. CFRP laminates were produced using an epoxy matrix-based thin-ply unidirectional (UD) prepreg (fiber: T800SC-24000-10E, matrix: 180°C-cured-type epoxy). The T800SC carbon fiber is a high-strength PAN-based carbon fiber. The Industrial Technology Center of Fukui Prefecture supplied thin-ply UD prepreg. Thin-ply UD prepreg with nominal thick-nesses of 0.032 mm (fiber area weight (FAW): 30 g/m², resin content (RC): 38%) was used. Thick-ply UD prepreg (fiber: T800SC, matrix: 180°C-cured-type epoxy), which Industrial Technology Center of Fukui Prefecture also supplied, with nominal thick-nesses of 0.160 mm (FAW: 150 g/m², RC: 38%) was also used for comparison.

Specimen preparation

The prepreg sheets were cut into a suitable size and fiber orientation. The sheets were placed on a vacuum molding board. CFRP laminates were made using a hand lay-up and vacuum bagging method (no bleeder). The fiber orientations of the CFRP laminates were set to cross-ply with thin ply thickness with [0/90]_10S (subscript 10 and S mean repeating and symmetry), [(0)₅/(90)₅]_2S, and [(0)₁₀/(90)₁₀]_S. Cross-ply CFRPs with thick ply thickness with [0/90]_2S and [(0)₂/(90)₂]_S were also fabricated for comparison. The cross-ply CFRPs with thin ply thickness with [0/90]_10S, [(0)₅/(90)₅]_2S, and [(0)₁₀/(90)₁₀]_S and cross-ply CFRPs with thick ply thickness with [0/90]_2S and [(0)₂/(90)₂]_S were designated as NA, NB, NC, WB, and WC, respectively. The fiber volume fraction of the cross-ply CFRPs with thin and thick ply thickness was 52.3%. The prepreg sheets were pressed at 490 kPa and cured at 180°C for 4 h (the heating rate was 1°C/min) using an autoclave (ACA Series, Ashida Mfg. Co., Ltd.) in the laboratory. The nominal thickness of the CFRP laminates was about 1.28 mm.

The fabricated CFRP laminates were cut into 10 mm × 10 mm pieces using a rotary cutting machine (Refine cutter RCA-234, Refine Tec Ltd.) at 2,500 rpm with an abrasive cutting wheel (GC150NB, Heiwa Technica Co., Ltd.). The CFRP samples were embedded in epoxy resin and subsequently polished by an automatic polishing machine (Automet 2000, Buhler Ltd.) with polycrystalline diamond suspensions of 6 µm and 3 µm and alumina suspension of 0.05 µm to produce cross-sections of the CFRP samples for morphological observation. The cross-sectional morphology of the CFRP samples was also observed using a digital microscope (dual objective zoom lens (20 × to 2000 ×) VH-ZST in VHX-6000, Keyence).

The CFRP laminates were cut into rectangular straight-side tensile test specimens with dimensions of 200 mm in length (gage length, L, of 100 mm) and 10 mm in width. Plain-woven fabric glass fiber-reinforced plastic (50 mm in length, 10 mm in width, and 1 mm in thickness) tapered tabs were affixed to the tensile test specimen to minimize damage from the grips on the tensile testing machine. The fiber axis in the sample was oriented in line with the length of the tensile test specimen (outer 0° direction specimen). The edges of the tensile test specimens were polished to remove scratches to eliminate the effect of stress concentrations caused by surface roughness from the edges. Similar specimen preparation procedures of other composites have been observed in the literature^4,22,23.

Static test

Static tensile tests of CFRP specimens were conducted using a universal testing machine (Autograph AG-series, Shimadzu Corp.) with a load cell of 50 kN. The specimen was set up in the testing machine. A crosshead speed of 1.0 mm/min was applied, and all tests were performed in the laboratory environment at room temperature (at 23°C ± 3°C and 50% ± 5% relative humidity). The static tensile test gives a load (P) as a function of the extension (U^*) curve up to failure. The tensile stress (σ_L) and tensile strain (ε_L) were calculated as follows:

$${\sigma }_{L}=\frac{P}{S}$$

$${\epsilon }_{L}=\frac{{U}^{*}}{{L}^{*}}$$

$${\nu }_{LT}=-\frac{{\epsilon }_{T\left(gauge\right)}}{{\epsilon }_{L\left(gauge\right)}}$$

where S is the total cross-sectional area of the CFRP specimens, which can be computed from the width and thickness as determined using a micrometer. L^* is the distance between targets (reference marks). The targets were marked on the specimens (L^* ≈ 50 mm). The extension (U^*) was measured using a non-contact video extensometer (DVE-201, Shimadzu Corp.). The DVE-201 extensometers perform precise, non-contact elongation measurements using CCD cameras to capture digital images of test specimens. The longitudinal (tensile) strain (ε_L(gauge)) and transverse strain (ε_T(gauge)) were also determined using strain gauges. Similar static test procedures of other composites have been observed in the literature^4,22,23. Five specimens were tested for each instance.

Fatigue test

Uniaxial fatigue tests of CFRP specimens were performed under sinusoidal waveform loading by a servo-hydraulic testing machine (MTS Landmark, MTS) with a 50-kN load cell at a frequency of 10 Hz. The stress ratio of the minimum stress to the maximum stress was 0.1. The fatigue tests were terminated after 1 × 10⁷ cycles. All tests were performed in the laboratory environment at room temperature (at 23°C ± 3°C and 50% ± 5% relative humidity). Similar fatigue test procedures of other composites have been observed in the literature^{5, 24–26}.

In situ static and fatigue tests

Figure 1 shows the experimental set-up for in situ static and tensile fatigue tests. In situ static and tensile fatigue tests using a digital microscope (long-focal-distance, high-performance zoom lens (50 ×–500 ×) VH-Z50L in VHX-6000, Keyence) with a XYZ stage were performed using a servo-hydraulic testing machine (MTS Landmark, MTS) with a 50-kN load cell. The CFRP specimens used for in situ observation were directly polished by an automatic polishing machine using a specimen fixing tool.

An automatic procedure was used for observation. The testing machine was paused when the loads or cycles reached a setting value. XYZ stages were moved automatically to obtain the photos. Following the observation, the XYZ stage was also moved to safety, and the loads or fatigue cycles were restarted. The observation tests were repeated until the setting end loads or cycles. For the static tensile test, the displacement after a predetermined load (100 MPa increment before 600 MPa and 50 MPa increment after 600 MPa) was stopped to allow the in situ digital microscope observation.

Two testing procedures were applied for the tensile fatigue test, and the observation cycles were set to 10⁴. (1) To obtain the transverse crack onset stress under fatigue loading at 10⁵ cycles. (2) To obtain the fatigue damage propagation behavior at same applied maximum stress. In (1) method, the low cyclic stress (95 MPa) was applied to 10⁵ cycles. When the transverse crack was not observed, the cyclic stress increased 32 MPa, and then the cyclic stress was applied to 10⁵ cycles. This procedure was used until a transverse crack was observed. In the (2) method, applied maximum stress was selected to 1.05 GPa (all specimens were failed between 10⁶ and 10⁷ cycles) for each specimen.

Morphologies

Figure 2 shows the digital microscope images of through-thickness-edge-sectional view for the cross-ply CFRP with thin and thick ply thickness samples. Each layer was observed, and the CFRP samples presented matrix-rich regions in the gaps between the layers. There were no noticeable voids in any cross-ply CFRP with thin and thick ply thickness samples.

Static tensile properties

For the cross-ply CFRP with thin and thick ply thickness specimens, the stress-strain response was linearly proportional to failure. The tensile modulus (E_L) and Poisson’s ratio (ν_LT) were computed using a least square method of tensile stress-strain and the longitudinal strain-transverse strain curves. The average tensile modulus, Poisson’s ratio, tensile strength (σ_L.ult.ave) and failure strain (ε_L.ult.ave) of the CFRP specimens are summarized in Table 1. The tensile strength and failure strain of thinnest 90° ply CFRP (NA) specimens were higher than those of thin 90° ply (NB and NC) ones. For the identical 90° ply thickness specimens, the tensile strength and failure strain of cross-ply CFRP with thin ply thickness (NB and NC) specimens were slightly higher than those of cross-ply CFRP with thick ply thickness (WB and WC) ones. Though, the tensile modulus and Poisson’s ratios were comparable among all cross-ply CFRP with thin and thick ply thickness specimens.

Table 1

Static and tensile fatigue properties of the CFRP specimens.
	NA	NB	NC	WB	WC
Static tensile properties
Tensile modulus E_L.ave (GPa)	93.9 (4.4)	93.0 (3.1)	93.7 (7.1)	93.4 (3.6)	93.8 (3.3)
Poisson’s ratio ν_LT.ave	0.042 (0.001)	0.040 (0.005)	0.043 (0.009)	0.041 (0.006)	0.043 (0.002)
Tensile strength σ_L.ult.ave (GPa)	1.730 (0.131)	1.719 (0.105)	1.645 (0.068)	1.658 (0.103)	1.584 (0.041)
Failure strain ε_L.ult.ave (%)	1.878 (0.068)	1.817 (0.053)	1.747 (0.080)	1.731 (0.054)	1.715 (0.064)
Fatigue tensile properties
Intercept a (GPa)	2.143	1.873	1.776	1.844	1.781
Slope b	−0.182	−0.130	−0.103	−0.116	−0.104
() indicate standard deviations

Fatigue tensile properties

Figure 3 indicates the relation between the applied maximum stress, σ_max, and the number of cycles to failure, N_f, also defined as the S-N curves for the cross-ply CFRP with thin ply thickness (NA, NB, and NC) specimens. The S-N curves for the cross-ply CFRP with thick ply thickness (WB and WC) specimens are also presented in this figure. The horizontal lines show the static tensile strengths. For lower fatigue cycle testing (< 10⁵ cycles), the trends of fatigue response were comparable to static properties among thin, thick ply thickness, and stacking sequences. The fatigue response of thin-nest 90° ply CFRP specimens were higher than those of other 90° ply thickness ones for lower fatigue cycle testing (< 10⁵ cycles). However, for higher fatigue cycle testing (> 10⁵ cycles), the fatigue responses decreased with a decrease in the 90° ply thickness. The fatigue properties (slope and fatigue limit stress, etc.) of the NA specimen were lower than those of other cross-ply CFRP with thin ply thickness (NB, NC) and cross-ply CFRP with thick ply thickness (WB and WC) specimens.

Static tensile properties

Figure 4 shows the digital microscope images of the NA, NB, and NC specimens obtained from the in situ static tensile tests just before fracture. The transverse matrix cracking through the thickness of the ply, delamination damage, and fiber breakage were observed in the specimens.

Figure 5 shows the relationship between the transverse crack onset stress and the stress first noticed in the transverse crack on an in situ static test. The 90° ply thickness or the thickness of the center ply, including the transverse crack density, i.e., the number of cracks per unit length and the applied stress, is shown in Fig. 5. The transverse crack onset stress increased with a decrease in the 90° ply thickness. The onset stress of the NA specimen (900 MPa) was more than two times higher than that of the NC specimen (400 MPa) (750 MPa in the NB specimen).

In this literature, the transverse crack onset stress or strain has been computed using a finite element method analysis with Drucker-Prager elastoplastic damage model in the matrix, the cohesive zone model in fiber-matrix and 0°–90° layer inter-faces. The results showed that the transverse crack onset strain of thin-90°-ply was higher than that of thick-90°-ply. A similar finite element method (FEM) analysis was performed in this study and the results are shown in the Supplementary Information^27,28. Comparable findings have been observed experimentally and analytically in the literature²⁷.

The crack density increased quickly in the initial stage and then saturated a value. The critical crack density also increased with a decrease in the 90° ply thickness. For NA (thinnest 90° ply) specimens, the constraint effects of 0° layers were large. The onset of transverse matrix cracking through the thickness of the ply, delamination damage, and fiber breakage was suppressed. Therefore, the tensile strength and failure strain of the NA specimen were higher than those of other cross-ply ones.

Fatigue tensile properties

S-N curves

The S-N curves can be described using a semi-log model. The semi-log model^29–34 is given by

$${\sigma }_{max}=a+b \text{l}\text{o}\text{g}\left({N}_{f}\right)$$

where a and b are experimental constants. The least squares fitting of the fatigue trends with the semi-log model is demonstrated in Fig. 3. The intercept, a, and slope, b, are summarized in Table 1. The intercept, a, and absolute value of the slope, |b|, in-creased with a decrease in the 90° ply thickness. The trend, a, depended on the static tensile strength. A higher |b| indicates enormous fatigue degradation. Consequently, the fatigue characteristics of the NA specimens were lower than those of NB, NC and cross-ply CFRP with thick ply thickness (WB and WC) specimens.

Transverse crack onset stress under fatigue loading

Figure 6 displays the relationship between the transverse crack onset stress under fatigue loading (first observed in the transverse crack on the in situ fatigue test) and the 90° ply thickness (center 90° ply thickness). The transverse crack onset stress under fatigue loading increased with a decrease in the 90° ply thickness, though the onset stress was lower than in the static case. The onset stress of the NA specimen (477 MPa) was higher than that of the NC specimen (349 MPa) (381 MPa in the NB specimen).

Fatigue damage propagation behavior

Figure 7 presents the digital microscope images of the NA, NB, and NC specimens obtained from the in situ fatigue tensile tests at the number of cycles, N = 990000 cycles. The transverse matrix cracking via the thickness of the ply, delamination damage, and fiber breakage increased with the number of cycles for all specimens. Figure 8 displays the relationship between the transverse crack density and the number of cycles. The crack density increased in the initial number of cycles and then saturated to value. The saturated crack densities that were similar to the static case and the saturated number of cycles increased with a decrease in the 90° ply thickness.

Figure 8 also includes the relationship between the number of cycles and the phase variations between the load and the displacement in cycles. The phase difference decreased in the initial number of cycles and then saturated a value (0.02 rad). The phase differences were caused by the viscoelastic nature of 90° ply and changed with the 90° ply transverse crack and saturated the 0° ply behavior. The 90° ply transverse cracks increased with an increase in the number of cycles and decreasing the phase differences. The saturated phase differences were comparable among the NA, NB, and NC specimens, and the saturated number of cycles increased with a decrease in the 90° ply thickness.

For NA (thinnest 90° ply) specimens, the onset of transverse matrix cracking through the thickness of the ply and increasing transverse crack were suppressed. However, the damage to fibers started near the transverse cracks, and the larger saturated crack density (number of transverse cracks and several positions of the trans-verse crack) caused a lot of damage to fibers at 0° ply and rapidly grew the delamination damage and fiber breakage because of thin 0° ply thickness under fatigue loading. Therefore, the fatigue characteristics of the NA specimens were lower than those of other cross-ply ones.

Under static loading, the tensile strength and failure strain of thinnest 90° ply CFRP specimens were higher than those of other 90° ply thickness ones. However, the tensile modulus and Poisson’s ratios were similar among the cross-ply CFRP with thin and thick ply thickness specimens. For the thinnest 90° ply CFRP specimens, the constraint effects of 0° layers were large. The onset of transverse matrix cracking via the thickness of the ply, delamination damage, and fiber breakage was suppressed.

Under fatigue loading, the trends of fatigue response were similar to static properties among thin, thick ply thickness and stacking sequences for lower fatigue cycle testing (< 10⁵ cycles). The fatigue response of thinnest 90° ply CFRP specimens were higher than those of other 90° ply thickness ones for lower fatigue cycle testing (< 10⁵ cycles). The fatigue responses did, however, decrease with a reduction in the 90° ply thickness for higher fatigue cycle testing (> 10⁵ cycles), and the fatigue properties (slope and fatigue limit stress, etc.) of the thinnest 90° ply CFRP specimen were lower than those of other cross-ply CFRP with thin ply thickness and cross-ply CFRP with thick ply thickness specimens. For the thinnest 90° ply CFRP specimens, the onset of transverse matrix cracking through the thickness of the ply and increasing transverse crack were suppressed. However, the damage to fibers began near the transverse cracks, and the larger saturated crack density (number of transverse cracks and sever-al positions of the transverse crack) resulted in considerable damage to fibers 0° ply and rapidly grew the delamination damage and fiber breakage because of thin 0° ply under fatigue loading.

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No competing interests reported.

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Static and fatigue tensile properties of cross-ply carbon fiber-reinforced epoxy matrix composite laminates with thin ply thickness

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Abstract

Figures

Introduction

Experimental Procedure

Materials

Specimen preparation

Static test

Fatigue test

In situ static and fatigue tests

Results

Morphologies

Static tensile properties

Fatigue tensile properties

Discussion

Static tensile properties

Fatigue tensile properties

S-N curves

Transverse crack onset stress under fatigue loading

Fatigue damage propagation behavior

Conclusions

References

Additional Declarations

Supplementary Files

Status:

Version 1