Interlaminar shear and flexural properties of three-dimensional braided glass fiber/polylactic acid composites

doi:10.21203/rs.3.rs-3573035/v1

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Interlaminar shear and flexural properties of three-dimensional braided glass fiber/polylactic acid composites

https://doi.org/10.21203/rs.3.rs-3573035/v1

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To address the problem of environmental pollution caused by the transitional use of petroleum-based composites, a green and environmentally friendly thermoplastic resin compound molding process is proposed. In this study, continuous glass fiber (GF) reinforced polylactic acid (PLA) composites were prepared. The coupling agent KH550 was used to modify the preforms to enhance the interfacial properties. The three-dimensional (3D) braiding technology and hot pressing were adopted to produce the samples. Then, the crystallinity, transverse shear stress, interlaminar shear, and bending properties of samples were tested. Finally, the effects of GF content, preform thickness, cutting edge, and KH550 concentration on the longitudinal bending properties of composites were investigated. The results showed that GF improved the crystallinity of PLA, and the bending performance was better at a GF content of 40% and a preform thickness of 9 mm. The cutting edge has little effect on the mechanical properties of the composites and can be cut according to the requirements. The best mechanical properties are achieved at a KH550 concentration of 40%.

Three-dimensional braiding

Hot pressing

Coupling agent

The advancement of technology has promoted the consumption of resources and the environmental degradation caused by the transitional use of petroleum resources has become increasingly serious. The green material that is environmentally friendly, biodegradable, and recyclable is essential[1, 2]. Polylactic acid (PLA) is considered one of the good alternatives to petroleum-based materials, with biocompatible and degradable features[3]. Meanwhile, PLA is a renewable resource that can be extracted from crops such as corn and sugar beets, and the cost is lower compared to other materials[4]. The above advantages of PLA make this thermoplastic resin have a wide range of applications, such as aerospace, automotive parts, biomedical, food packaging, sensors, and other areas that have ample prospects for development[5–9]. Although PLA has poor mechanical properties and the samples are brittle[10], this phenomenon can be improved by introducing reinforcements that can carry external loads and improve the mechanical properties of the composite. The main materials currently used to reinforce PLA are natural fibers (NF)[11], carbon fibers (CF)[12], and glass fibers (GF)[13]. In particular, GF is relatively low cost and improves the mechanical properties of the composite while improving the crystallinity of PLA.[14].

Betanzos et al.[15] prepared GF fibers by melt stretching and molded them with PLA films. The results show that the strength of the composite reinforced by GF will be increased by 30%. Yu et al.[16] adopted melt impregnation equipment to prepare GF/PLA composite filaments to prepare GF-reinforced PLA composites by 3D printing. According to the results, the tensile strength of the reinforced specimens can reach 200 MPa and the bending strength can reach more than 300 MPa. Moslehi et al.[17] obtained short-cut GF by recycling old wind turbine blades, shredding them, and blending them into PLA to produce filaments that can be used for 3D printing, while treating the GF with coupling agents. The results showed that the strength of the composites was improved by more than 30%, the elongation at the break by a factor of 3, and the impact strength by a factor of 2 Wang et al.[18] used the ring spinning method to blend PLA and GF and then combined the strands, and then prepared the composite sheets by molding. The bending strength of the composites was tested to reach 293 MPa at a GF content of 40%. Ahmed et al.[19] used quaternary phosphate-based GF to reinforce PLA to obtain composites that can be used in the field of medical devices. The composites prepared by adopting this approach have little difference in bending strength with human bones and can be used for internal fracture fixation field applications. The mass loss was 14% after 6 weeks of degradation in deionized water. Zhu et al.[20] prepared composites of phosphate GF-reinforced PLA with different fiber interlayer structures by a molding process. The unidirectional fiber-reinforced composites were observed to have the best bending strength and modulus, while the short-cut fibers performed the worst.

From the above, it can be seen that GF can enhance the mechanical properties of PLA composites effectively and that short-cut GF was relatively poor. Prefabricated systems are also mostly dipped and twisted. Nevertheless, the three-dimensional braiding technique is rarely used. The three-dimensional braided material has relatively excellent strength and stiffness, high impact resistance, excellent axial performance, and high freedom of design, allowing the preparation of different styles of prefabricated bodies according to actual needs[21–23]. Wang et al.[24] adopted resin transfer molding method to investigate the mechanical properties of composite tubes prepared with different three-dimensional braided structures. The results show that the mechanical properties of the three-dimensional five-way structure are better than other structures. Zhou et al.[25] explored the damage mechanisms of different weave structures and weave angles, and adopted digital image techniques as well as CT scans to determine the criteria. According to the results, the three-dimensional five-way structure is more resistant to delamination due to the presence of the axial yarn. Simultaneously, specimens with smaller weave angles have higher fiber orientation, a shorter damage process, and less deformation than bigger weave angles. In this study, the prefabricated body was prepared by a four-step three-dimensional five-way structure with continuous GF and PLA, and the prefabricated body was modified with coupling agent KH550. The composite material is prepared by hot pressing. The effects of GF content, preform thickness, cutting edges, and coupling agent modification on the interlaminar shear and bending properties and crystallinity of the composites were investigated.

2.1 Materials

PLA fiber(Diameter 0.3 mm, Density1.25 g/cm3), provided by Nantong Xindike Monofilament Technology Co.; GF fiber(Wire density 130tex, Density2.4 g/cm3), provided by Shandong Future New Materials Co.; Hot melt tubes and elastic leads, commercially available; γ-aminopropyltriethoxysilane(C9H23NO3Si, Analytical Reagent) purchased from Shandong Urso Chemical Technology Co.; Anhydrous ethanol(C2H6O, Analytical Reagent) from Tianjin Huihang Chemical Technology Co.; Acetone(C3H6O) From Tianjin Windship Chemical Reagent Technology Co.; Mold release agent is provided by Qingdao Dehui Company.

2.2 Three-dimensional braided prefabricated equipment

The prefabricated bodies were designed as shown in Table 1, Fig. 1 shows the physical picture of the 3D braided prefabricated body.

Table 1

Design parameters of the prefabricated body
Serial number	Fiber content /%	Main yarn /m×n	Length /mm	Width /mm	Thickness /mm	Flower nodes length /mm	Braided corners /°
1	30	6×9	260	15	9	6 ± 0.5	20 ± 3
2	35	6×9	260	15	9	6 ± 0.5	20 ± 3
3	40	6×9	260	15	9	6 ± 0.5	20 ± 3
4	40	5×9	260	15	8	6 ± 0.5	20 ± 3
5	40	4×9	260	15	7	6 ± 0.5	20 ± 3
6	40	6×15	260	25	9	6 ± 0.5	20 ± 3

2.3 Coupling agent modification

Surface treatment of the preform using γ-aminopropyltriethoxysilane (KH550) in the following manner: KH550 was dispersed in anhydrous ethanol solvent and prepared into KH550/ethanol solutions with mass fractions of 3%, 4%, and 5%. Then, the prefabricated body was immersed in the solution for 1.5h and then removed and placed in an oven at 45°C for 12h for drying treatment, which was removed and set aside. The reaction process of KH550 with GF is shown in Fig. 2[26].

2.4 Hot pressing process for fabricating the composite

The mold for the hot pressing process used in this experiment consists of 3 parts: upper mold, middle mold, and lower mold, with good internal sealing. The prefabricated body in the mold cavity is uniformly heated and well-sealed, which prevents the loss of the PLA resin matrix. Compounding conditions[15, 18] are shown in Fig. 3. Sandpaper was taken to polish the mold before the experiment, and wiped with ethanol and acetone, left for 10min after cleaning. Apply the release agent twice, 10min apart. The prefabricated body is laid flat in the mold cavity and placed in the hydraulic press after the mold is installed, setting the temperature to 190°C and starting to warm up, during which a pre-pressure of 2 MPa is applied. After the temperature reaches the set value, 5MPa molding pressure is applied and the constant pressure is maintained for 60min. After reaching the time required for the experiment, the composite plate is removed after the circulating water has cooled to room temperature.

2.5 Characterization

2.5.1 Experimental equipment

The instruments and equipment used in this study are shown in Table 2

Table 2

Experimental equipment
Equipment name	Model specification	Manufacturers
Differential Scanning Calorimeter	DSC200F3	NETZSCH Germany
Rotational rheometer	DHR-2	TA Instruments, Inc.
Three-dimensional braiding machine	YSB-6X40	Self-study at Tiangong University
Mold	/	Self-design
Four column hydraulic press	YRD32-200T	Shandong Ludi Heavy Industry Machinery Co.
Electronic balance	CP124C	Olds Instruments (Changzhou) Co.
Universal material testing machine	AG-250KNE	Shimadzu Corporation, Japan
Cold-field scanning electron microscope	Regulus 8100	Hitachi, Japan

2.5.2 Differential Scanning Calorimetry (DSC)

The sample mass was 10 mg, and the sample was heated from room temperature to 230°C at a heating rate of 10°C/min under a nitrogen atmosphere with a gas flow rate of 50 mL/min, and kept for 5 min to eliminate the thermal history. Then the temperature was cooled down to 0°C at a cooling rate of 10°C/min and finally heated to230°C at a heating rate of 10°C/min, recording the secondary temperature rise curve.

\(X\text{c}=\frac{{\Delta H\text{m}-\Delta H\text{c}\text{c}}}{{\omega \Delta H0}} \times 100\%\) 1

Where X_C is the crystallinity of PLA in the composite,%; ΔH_m is the enthalpy of melting of PLA in the composite, J/g; ΔH_cc is the enthalpy of cold crystallization of PLA in the composite, J/g; ω is the mass fraction of PLA in the composite,%; ΔH₀ is the melting enthalpy of the complete crystallization of PLA, and its value is 93.6 J/g[27].

2.5.3 Interlayer shear strength

The test was conducted at room temperature with a specimen size of 25mm x 8mm x 4mm and a span of 16mm, with a loading speed set at 1mm/min. The calculation criteria were as follows:

\(ILSS=0.75 \times \frac{{{F_{max}}}}{{b \times h}}\) 2

Where ILSS is the interlaminar shear strength of the composite specimen, MPa; F_max is the maximum load of the specimen, N; b and h are the width and thickness measurements of the specimen, respectively, mm.

2.5.4 3-Point bending test

The bending property is one of the most important mechanical properties of composite materials, which reflects the ability of composite materials to resist damage by external bending loads. This experiment takes three-point bending, and the three-point bending strength and modulus are calculated as follows:

Bending strength

\({\sigma _f}=\frac{{3Pl}}{{2b{h^2}}}\) 3

Where σf is the bending strength, MPa; P is the breaking load, N; l is the span, mm; b is the specimen width, mm; h is the specimen thickness, mm.

Bending modulus

\({E_f}=\frac{{{l^3}\Delta P}}{{4b{h^3}\Delta S}}\) 4

Where E_f is the bending modulus of elasticity, MPa; ΔP is the load increment of the initial straight section on the load-deflection curve, N; ΔS is the deflection increment at the span center point corresponding to the load increment ΔP, mm.

2.5.5 3-point bending test samples

To investigate the effects of glass fiber content, preform thickness, cutting edges, and coupling agent modification on the bending properties of 3D braided composites, experiments were designed as shown in Table 3. Where NB represents the uncut edge bending experimental specimen and CB represents the cutting edge bending experimental specimen; the middle number represents the mass fraction of glass fiber in the preform; L represents the number of hanging rows, which represents the thickness of the preform; the number plus m indicates the content of KH550.

Table 3

Bending specimen parameters specifications
Serial number	GF content /%	KH550 content /%	Width /mm	Thickness /mm
NB-30-6L	30	-	14.95	4.2
NB-35-6L	35	-	14.94	4.17
NB-40-6L	40	-	14.96	4.13
NB-40-4L	40	-	15.00	3.96
NB-40-5L	40	-	14.95	3.95
CB-40-6L	40	-	14.94	4.11
NB-40-6L-3m	40	3%	14.92	3.97
NB-40-6L-4m	40	4%	14.96	3.88
NB-40-6L-5m	40	5%	14.97	3.93

3.1 DSC Analysis

Figure 4 shows the DSC curves of the GF/PLA composites for the second warming, and Table 4 presents the DSC-related data of PLA in the composites The increase of GF mass fraction promotes the crystallinity of PLA. GF, as a heterogeneous nucleating agent, can guide the arrangement of PLA molecules, improve the crystallization ability, and facilitate the improvement of the mechanical properties of the composites. the introduction of KH550 further enhances the crystallinity and enables the formation of more nucleation sites between GF and PLA. However, the excessive amount of KH550 will affect the interfacial effect and reduce the mechanical properties of the composites.[28, 29].

Table 4

GF/PLA composite secondary heating DSC parameters
Serial number	T_g/℃	T_c/℃	ΔH_cc/(J/g)	T_m℃	ΔH_m/(J/g)	X_c/%
PLA fiber	56.3	110.8	32.4	165.2	34.84	2.61
NB-30-8L	57.9	111.9	11.8	165.1	15.6	5.8
NB-35-8L	57.8	112.8	12.86	166.2	17.64	7.86
NB-40-8L	63.1	116	17.35	166.9	23.12	10.27
NB-40-8L-3m	63	108.5	6.72	167.5	19.54	22.82
NB-40-8L-4m	63	108.8	5.13	167.8	18.42	23.64
NB-40-8L-5m	61.5	107.6	4.14	160.5	14.09	17.71

3.2 Interlaminar shear strength and damage morphology

3.2.1 Interlaminar shear strength

Figure 5(a) shows the shear load-deflection curve of the transverse short beam of GF/PLA composite. The unmodified specimens have relatively low shear strength, micro-cracks, and pores inside the composites, and the curves are nonlinear at small load loading. The toughness of the modified composites was improved and the curves decreased more gently after reaching the maximum load compared to the unmodified specimens. The increase of the coupling agent can reduce the cross-linking density of PLA, reduce the performance of the matrix and make the load difficult to transfer efficiently when subjected to external forces[30].

Figure 5(b) illustrates the interlaminar shear strength of the GF/PLA composite. After 4% KH550 modification, the shear strength of composite material increased most significantly, reaching 36.68%. Amino and silyl alcohol groups are formed after KH550 alcohol dissolution and react with hydroxyl groups in GF, improving the interface between GF and PLA. However, with the modification of 5% KH550, the shear strength decreases due to the increase in PLA stress concentration.

3.2.2 SEM images

Figures 6 show the SEM images of the transverse short beam shear fractures of the four GF/PLA composites[31]. Among them, Fig. 6(a) shows the unmodified composite, and it can be seen that the GF surface is smoother with less PLA resin bonding residue. Figures 6(b), 6(c), and 6(d) show the composites modified with 3%, 4%, and 5% KH550, respectively. With the increase of coupling agent concentration, the PLA resin retained on the surface of GF fibers gradually increased, a phenomenon that indicates the chemical reaction between KH550 and the hydroxyl groups in GF fibers. Meanwhile, the primary amine bond in KH550 improves the surface properties of PLA and further enhances the interfacial properties between GF and PLA. The agglomeration phenomenon of KH550 can be seen in Fig. 5(d), which is due to the high concentration of coupling agent that cannot fully react with GF, which in turn leads to the accumulation of agglomerated polymer on the fiber surface and will affect the mechanical properties of the composite[32, 33].

(a)Nmod GF/PLA, (b)3mod GF/PLA, (c)4mod GF/PLA, (d)5mod GF/PLA

3.3 3-Point bending

Table 5 shows the results of the three-point bending experiment.

Table 5

Bending properties of composite materials test results
Serial number	GF content /%	Thickness /mm	KH550 content /%	Max. load /N	Displacement at max. load /mm	Bending strength /MPa	Bending modulus /GPa
NB-30-6L	30	9	-	295	2.66	107.41	9.79
NB-35-6L	35	9	-	330.42	2.92	121.92	11.05
NB-40-6L	40	9	-	421.25	2.93	158.25	11.6
NB-40-4L	40	7	-	277.5	2.52	113.26	10.07
NB-40-5L	40	8	-	307.08	3.28	126.2	10.7
CB-40-6L	40	9	-	390.42	4.22	148.28	10.84
NB-40-6L-3m	40	9	3	447.92	3.86	182.6	12.7
NB-40-6L-4m	40	9	4	475	4.38	202.49	12.36
NB-40-6L-5m	40	9	5	343.75	2.87	142.95	10.6

3.3.1 Effect of GF content on bending properties

Figure 7(a) shows the longitudinal bending load-deflection curves for the three composites with 30%, 35%, and 40% GF content. Specimens with 30% GF content showed a rapid decrease in a curve, which resulted in a more brittle composite due to the low GF content. With the increase of GF content, the decrease of the curve slows down relatively and the maximum load point is also increased, and the toughness of the composite is improved. Figure 7(b) shows the bending strength and bending modulus of composites. At 35% GF content, the longitudinal bending strength and bending modulus are increased by 13.51% and 12.87% compared to 30%. When the GF content reaches 40%, the bending strength and bending modulus are improved by 47.33% and 18.49%. The improvement in mechanical properties is attributed to the increase in GF content in the composite. In the prefabricated body, the increase of GF content in the axial yarn part will enhance the load-bearing capacity of the composite in the longitudinal direction and better stress transfer, thus improving the bending resistance.[34, 35].

3.3.2 Effect of prefabricated body thickness on bending properties

Figure 8(a) shows the longitudinal bending load-deflection curves for three composites with prefabricated body thicknesses of 7 mm, 8 mm, and 9 mm. Figure 8(b) shows the histogram of longitudinal bending strength and bending modulus. Compared with the 7mm specimens, the longitudinal bending strength and bending modulus of the 8mm specimens increased by 11.42% and 6.26%; the 9mm specimens increased by 39.72% and 15.19% respectively. After the three-dimensional braided structure is hot-pressed, there is porosity inside, which can be improved by increasing the thickness of the prefabricated body. The prefabricated body thickness increases, resulting in increased Z-yarn and increased longitudinal carrying capacity. The Z-yarn can bind the prefabricated body as a whole, to some extent preventing the tendency of failure between matrix and interface and the continued expansion of interlayer cracks[36, 37].

3.3.3 Effect of cutting edge on bending properties

In practical applications, various specifications of composite materials may be prepared due to different requirements, in which the trimming process is unavoidable [38, 39]. Figure 9(a) shows the bending load-deflection curves of the cut-edge and uncut-edge composite specimens. The modulus difference between the two curves is small and the decreasing trend is flat, which proves that the cutting edge has little effect on the toughness of the composite. Figure 9(b) shows the histogram of longitudinal bending strength versus bending modulus. Compared with the uncut specimens, the longitudinal bending strength and bending modulus of the cut specimens were reduced by 6.3% and 6.55%, respectively. Although cutting the edges causes the woven structure formed by the stranded fiber bundles to be loose, which affects the mechanical properties of the composite, it has little effect on the overall molding structure. Meanwhile, the presence of axial yarns in the three-dimensional five-way structure mitigates the effect of cut edges on the bending properties of the composite.

3.3.4 Effect of modification on bending properties of composite materials

Figure 10(a) presents the longitudinal bending load-deflection curves of four GF/PLA composite specimens with coupling agent KH550 content of 3%, 4%, 5%, and unmodified. It can be seen that the specimens with 3%mod and 4%mod show an increase in the maximum load point compared to the unmodified composites. However, the 3%mod curve shows a rapid decrease after the maximum load point, due to the excessive brittleness of the composite[32, 40]. Because some of the GF in the modified composite is more tightly bonded to PLA, the interface damage is mitigated when subjected to longitudinal bending pressure.

Figure 10(b) shows the histogram of bending strength and bending modulus. Compared to the unmodified specimens, the longitudinal bending strength and bending modulus of the 3%mod specimens increased by 15.39% and 9.48%; the specimens with 4% mod improved by 27.96% and 6.55%, respectively. KH550 improves the interfacial properties of GF/PLA and enhances the bending strength. Meanwhile, the primary amine contained in the side chain of KH550 allows PLA to acquire certain surface energy and entangle with the internal molecular chain of PLA, further improving the interfacial binding properties. The longitudinal bending strength and bending modulus of the specimens with 5% mod were reduced by 9.67% and 8.62%. High KH550 content will prevent some coupling agents from reacting with GF and form agglomerates between GF and PLA, weakening the transfer of external forces between the resin matrix and the reinforcement and affecting the interfacial bonding between the two, resulting in lower bending performance[41, 42].

In this study, continuous GF and PLA were used to prepare the prefabricated body by three-dimensional braiding process, the coupling agent KH550 was taken to modify the prefabricated body, and the composites were prepared by the hot pressing molding process. The crystallinity of PLA was enhanced by DSC testing of the composite. The results of the interlaminar shear performance tests showed that the composite modified with 4% KH550 had better shear strength improvement and 5% KH550 had a decrease in shear strength, which was also confirmed by SEM images. Regarding the bending performance, the GF is 40%, and the bending strength is better when the thickness of the prefabricated body is 9mm. The cutting-edge process has little effect on the bending strength and can be trimmed according to actual needs. The 4% mod KH550 modification is better and the 5% mod KH550 bending strength is reduced.

Author Contributions: Author 1: Conceptualization；Author 2:Writing - Original Draft, Data Curation；Author 3:Investigation

Institutional Review Board Statement: Not applicable.

Informed Consent Statement: Not applicable.

Data Availability Statement: The data presented in this study are available on request from the corresponding author.

Conflicts of Interest: The authors declare no conflict of interest.

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No competing interests reported.

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Interlaminar shear and flexural properties of three-dimensional braided glass fiber/polylactic acid composites

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Abstract

Figures

1 Introduction

2 Materials and Methods

2.1 Materials

2.2 Three-dimensional braided prefabricated equipment

2.3 Coupling agent modification

2.4 Hot pressing process for fabricating the composite

2.5 Characterization

2.5.1 Experimental equipment

2.5.2 Differential Scanning Calorimetry (DSC)

2.5.3 Interlayer shear strength

2.5.4 3-Point bending test

2.5.5 3-point bending test samples

3 Results and discussion

3.1 DSC Analysis

3.2 Interlaminar shear strength and damage morphology

3.2.1 Interlaminar shear strength

3.2.2 SEM images

3.3 3-Point bending

3.3.1 Effect of GF content on bending properties

3.3.2 Effect of prefabricated body thickness on bending properties

3.3.3 Effect of cutting edge on bending properties

3.3.4 Effect of modification on bending properties of composite materials

4 Conclusions

Declarations

References

Additional Declarations

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