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Mechanical properties of epoxy resin toughened with cornstarch

  • Zhi Wang EMAIL logo , Haopeng Lv and Yuxiang Yang
Published/Copyright: November 3, 2022
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e-Polymers
From the journal e-Polymers Volume 22 Issue 1

Abstract

We investigated the effect of starch modification on the mechanical properties of phenolic epoxy resin (EP). Corn starch admixture of 2.5, 5, 7.5, and 10 wt% were added into the EP. The tensile strength, elongation at break, and elastic modulus of different corn starch contents were compared. The containing of corn starch showed a positive effect on the toughness of the epoxy but showed little effect on strength when the additive content was less than 10 wt%. The strength and elastic modulus increased first and then decreased with the increase in starch content and reached their maximum values at a content of 2.5 wt%. The enhancement effect might be due to corn starch’s mechanical properties, dispersibility, and interfacial interaction. With the increase in starch content, starch granules quickly contact each other, causing self-aggregation sedimentation and a decrease in strength and elastic modulus. The scanning electron micrographs of the toughened EP specimens showed ductile failure because of the starch particles. The surface morphology of the blend resin specimens was full of staggered and stepped cracks caused by the shearing damage, which is shown by obvious plastic fracture characteristics with plastic deformation ability. The initiation of micro-cracks in the EP matrix was induced by the incorporation of starch particles, which caused localized stepped shear damage in the matrix. More energy would be absorbed during this process, and the toughness of the EP would be enhanced. It is recommended that the best corn starch content should be 2.5 wt% to obtain excellent strength and good toughness.

Keywords: corn starch; elastic modulus; mechanical properties; modified epoxy resin; toughened

1 Introduction

With a high strength-to-weight ratio, excellent adhesion, electrical insulation properties, low shrinkage deformation, and stable physical and chemical properties, epoxy resin (EP) is widely utilized as a high-performance thermosetting resin for many industrial applications (1,2). However, there are still disadvantages such as considerable internal stress, poor impact resistance, low-temperature brittleness, and relatively low toughness for EP to be modified. The toughening improvement of EP has been widely discussed in the last 10 years.

There are three main strategies for improving the toughness of EP: one is to incorporate high toughness polymer into EP, such as rubber elastomer (3,4), glass beads (5,6,7), and the other is to incorporate nanoparticles into EP, which can balance the contradiction between toughening and strengthening to achieve the purpose of toughening without declining strength and modulus, such as nano-SiO2 (8,9,10,11), nano-TiO2 (12), core-shell polymers (13), and silica nanoparticles (14). The toughness of the EP can also be enhanced by interpenetrating the network through its continuous permeability, such as in EP-acrylate systems (15,16,17,18) and EP polyurethane systems (19,20). The polymer structure can also be toughened by changing the crosslinked network chemical structure with a high net chain molecular, such as mixed with polyether ketone (21) and polyetherimide (22,23).

Nanoparticles have a small diameter (1–100 nm) and a large surface area, with solid interfacial interactions. Adding it to EP, the nanoparticles produce a stress concentration effect, reducing the overall internal stress of the material, thereby absorbing energy, and changing the fracture behavior of EP from brittle to ductile fracture (24,25,26,27,28). Singh et al. (29) dispersed SiO2 nanoparticles with a particle size of 15 nm in EP and studied the effect of SiO2 nanoparticles on the thermodynamic properties of epoxy nanocomposites. The results show that the tensile strength of nano-SiO2 with a mass fraction of 4% is increased by 44%. Ning et al. (30) prepared five polymer nanoparticles with different compositions and morphologies using methyl methacrylate, butyl acrylate, and ethylene dimethacrylate as raw materials. The results show that the fracture toughness and fracture energy are increased by 220% and 851%, respectively, after adding 10% by mass polymer nanoparticles. Baghdadi et al. (31) functionalized Fe3O4 nanoparticles with polydopamine, (3-glycidyloxypropyl)trimethoxysilane and (3-aminopropyl)trimethoxysilane, and Fe3O4/epoxy nanocomposite. The material’s mechanical properties were improved overall, with a 34% increase in tensile strength and a 13% increase in fracture toughness. These modifiers have an excellent effect on the toughening of EPs. However, the use of modifiers can be affected by many factors, such as price, toxicity, toughening effect, and agglomeration. The introduction of corn starch as a modifier is a newer application of biomaterials in composites. Starch is considered a cheap, completely nontoxic, readily available biomaterial that is very different from most amine or bromine-containing curing agents. The average diameter of the starch particles is about 10–25 mm, which can be considered a relatively suitable particle size. The smaller specific surface area relative to the nanoparticles means a little reunion phenomenon. Starch was used as one of the reactants for sustainable hyperbranched EPs. The starch additive can produce novel epoxy thermosetting materials with good toughness, excellent adhesion strength, and good biomedical properties. Duarah and Karal (32) and Wang et al. (33) modified the starch’s surface to improve the interfacial adhesion between the glass fiber and the EP, which showed a better bonding effect.

The present work aims to investigate corn starch content’s influence on the mechanical properties of EPs. We will carry on a uniaxial tensile test and scanning electron microscopy (SEM) observation of fracture surface morphology to reveal the mechanism of corn starch toughening EP. Five different contents of reinforced epoxy, 0, 2.5, 5, 7.5, and 10 wt%, will be introduced for the tensile mechanical properties. Section 2 briefly introduces the fracture mechanic techniques employed in this study.

2 Materials and methods

A two-component epoxy formulation was adopted as the experiment material. The EPs consisted of a phenolic resin (component A) and an Ethylenediamine curing agent (component B) supplied by Shanghai Jiahui Building Materials Co. Ltd, Shanghai, China. The corn starch particles provided by Shandong Jincheng shareholding Co. Ltd, were added as a toughening agent to the resin matrix. The starch used in this study was corn germ starch, and the starch granules were measured to be about 5–20 µm in diameter. Its amylose content is 20–26%, the rest was amylopectin, and the particle roundness was good. The corn starch particles had a mean particle size of about 12 μm, with a narrow range of particle-size distribution and roundness. The particle size and excellent dispersion of these corn starch particles remain unchanged during further mixing and blending operations.

Neat epoxy and corn starch-modified epoxy were selected to compare the properties of the polymers. According to the Chinese standard GB/T 2567-2008, a standard tensile dumbbell specimen with a length of 200 mm, a thickness of 4 mm, and an effective tensile length of more than 50 mm were prepared. The phenolic resin and the curing agent were mixed at a ratio of 2:1 for neat specimens. And then, the stoichiometric amount of the toughening agent was added to the mixture for modified samples, which were poured into release-coated molds and cured for 72 h at room temperature. We selected four corn starch contents of 2.5, 5, 7.5, and 10 wt% to study the influence of corn starch content on the mechanical properties.

The specimens were tested at a displacement rate of 1 mm·min−1 according to the Chinese standard GB/T 2567-2008 test method. The strain in the gauge length was measured using a clip-on extensometer, and the elastic modulus, E, was calculated.

The fracture surfaces of the specimens were investigated using SEM. A Keysight “8500B” scanning microscope was used, and all samples were coated with a thin layer of sputtered gold before analysis to prevent charging. An acceleration voltage of 1 kV was used.

3 Results and discussion

Figure 1 shows the failure performance of the specimens with different starch contents. There was no apparent necking phenomenon during the loading process when the corn starch content was less than 10 wt%: the smaller the corn starch content, the more brittle the specimens. Micro-cracks appeared in the middle of the modified epoxy specimens when the load reached 70% of the peak value. The cracks gradually expanded with the increase in the deformation and finally broke through the samples. These micro-cracks developed significantly when the starch content was 10 wt% compared with unmodified EP specimens. The corn starch particles presented as the second phase in the EP matrix correspond to introducing defects in the resin matrix. Stress concentration occurred around the corn starch particles, which would cause the initiation of cracks during the tensile process. High surface stress levels and semi-elliptical surface defects of cured EP specimens would induce cracks.

Figure 1 Failure modes of the specimens with different starch content: (a) 0 wt%, (b) 2.5 wt%, (c) 5 wt%, and (d) 10 wt%.
Figure 1

Failure modes of the specimens with different starch content: (a) 0 wt%, (b) 2.5 wt%, (c) 5 wt%, and (d) 10 wt%.

The mechanical properties of corn starch-modified EP composites could be characterized by a tensile test, which would visually indicate the toughening effect of corn starch. Tensile strength and elastic modulus test results are shown in Figure 2. The strength and elastic modulus increased first and then decreased with the increase in starch content and reached their maximum values of 22.19 MPa and 1.146 GPa at a content of 2.5 wt%, which were 9% and 33% higher than that of standard EP sample. The enhancement effect might be due to corn starch’s mechanical properties, dispersibility, and interfacial interaction. However, the strength decreased and was lower than that of the pure EP when the starch content exceeded 2.5 wt%. With the increase in starch content, starch particles were prone to contact each other and caused self-aggregation and sedimentation. When the starch content reached 10 wt%, the strength and elastic modulus decreased significantly.

Figure 2 Plot of relative tensile strength (a) and elastic modulus (b) vs corn starch content.
Figure 2

Plot of relative tensile strength (a) and elastic modulus (b) vs corn starch content.

Admixture materials are generally known to affect mechanical properties depending on their compatibility with the epoxy matrix, the surface area of contact, particle size, shape, and content, and the intrinsic strength of the corn starch phase. Figure 3 represents the stress vs strain curves of both neat EP and 2.5, 5, 7.5, and 10 wt% corn starch-modified EP. The results confirmed the better effect of corn starch toughening EPs which possessed relatively high strength and great plastic deformation ability. The elongation at break reached its average maximum value of 78.53% at a corn starch content of 2.5 wt%, which was 49.83% higher than that of neat EP. The modified epoxy exhibited a ductile deformation with the appearance of relatively high yield stress. It could be assumed that the shear stress might be the dominant mechanism of deformation in such systems, which will be seen in the later SEM analysis.

Figure 3 Plot of relative stress vs strain for corn starch modified specimens.
Figure 3

Plot of relative stress vs strain for corn starch modified specimens.

It is well known that particle agglomeration is considered one of the most critical factors affecting the performance of EP (34). Corn starch particles with diameters of 5–20 µm were used in this study to avoid particle aggregation. The micron-scale particles could effectively prevent the emergence of agglomeration (Figure 4), especially for mixed materials with a corn starch content of less than 5 wt%.

Figure 4 Micrographs of tensile fractured surfaces of specimens: (a) neat epoxy, 250× magnification; (b) neat epoxy, 1,000× magnification; (c) 2.5 wt% corn starch, 250× magnification; (d) 2.5 wt% corn starch, 1,000× magnification; (e) 5 wt% corn starch, 250× magnification; (f) 5 wt% corn starch, 1,000× magnification; (g) 7.5 wt% corn starch, 250× magnification; (h) 7.5 wt% corn starch, 1,000× magnification; (i) 10 wt% corn starch, 250× magnification; and (j) 10 wt% corn starch, 1,000× magnification.
Figure 4

Micrographs of tensile fractured surfaces of specimens: (a) neat epoxy, 250× magnification; (b) neat epoxy, 1,000× magnification; (c) 2.5 wt% corn starch, 250× magnification; (d) 2.5 wt% corn starch, 1,000× magnification; (e) 5 wt% corn starch, 250× magnification; (f) 5 wt% corn starch, 1,000× magnification; (g) 7.5 wt% corn starch, 250× magnification; (h) 7.5 wt% corn starch, 1,000× magnification; (i) 10 wt% corn starch, 250× magnification; and (j) 10 wt% corn starch, 1,000× magnification.

As shown in Figure 4, the fracture section of the neat EP was smoother than that of the blended resin. There were few gentle step-like fractures, and more of the fractures were neatly arranged on the fracture plane, which shows a typical brittle fracture characteristic for neat EP. In contrast, the surface morphology of the blend resin specimens was very complicated and full of staggered and stepped cracks. The step formation was probably caused by the shearing of the EP in the interface between corn particles and EP during the stretching process. The presence of many steps indicated that such a shear fracture occurs quickly, and the process of fracturing had prominent plastic fracture characteristics with plastic deformation ability. It could be best explained microscopically that starch was effective in improving the toughness of EPs.

We can see from Figure 4d, f, and h that the starch particles are usually concentrated at the edges of the steps, while fewer particles appear on the step plane. There is a direct causal relationship between the distribution of the corn starch particles and the formation of the steps. Stress concentration occurs around the starch, which would induce initial cracks during the stretching process. Crack initiation begins around corn starch particles with the continued stretching process, and propagation eventually forms through the fracture surface and stepped lines. This phenomenon is most evident at the fracture surface of the specimen with a corn starch content of 2.5 wt% (Figure 4c and d). With the increase in corn starch content, the starch particles’ average distance becomes shorter, making the micro-cracks quickly propagate with each other. This finding is also consistent with the results of the mechanical property analysis.

We can see from Figure 4c, e, g, and i that the altitude difference between adjacent steps and local shear fracture strength decreases with the increase in corn starch content. It is also evident that the number of localized shear steps increases as the presence of micro-cracks becomes more common as the number of starch particles grows. Macroscopically, the amount of micro-crack shear failure increases, resulting in an overall strength decrease and a toughness increase. When the content of corn starch particles reaches 10 wt%, there is no obvious step on the fracture surface, and the strength comes from the minimum value. The plastic deformation ability reaches the maximum value (Figure 4i). There is a particular gap between the corn starch particles and the EP matrix. The hole had been formed during stretching because of the weak interface binding, which would quickly result in interface debonding. In this case, the epoxy matrix failed to efficiently transfer stress to the starch particles through the interface between the starch and the EP. The tensile strength of the corn starch particles cannot contribute to the overall strength effectively; the presence of corn starch particles causes more pores in the matrix, and the toughness will be improved eventually. With the increase in starch content, the proportion of EP in the same cross-section becomes smaller and smaller, which makes the bearing capacity of the fracture surface smaller and smaller. Therefore, the tensile strength of starch/EP has dropped dramatically with the increase in starch content.

As shown in Figure 5, the starch particles are present in three forms on the fracture surface of the specimens, some of the particles remain intact. They offer a bright granular morphology; some particles completely peel and show a pits state. Some particles are broken into two pieces, one of which is still embedded in the fracture surface and shows a darker granular morphology. According to the statistical results of all the images, it can be found that the proportion of intact particles decreases linearly with the increase in starch content (Figure 6). With the addition of starch content, the probability of occurrence of transgranular fracture increases significantly. The strength of the EP decreases because of the low power of the corn starch.

Figure 5 Scanned electron micrographs showing the presence of starch particles.
Figure 5

Scanned electron micrographs showing the presence of starch particles.

Figure 6 Effect of starch content on the complete particles in fracture surface.
Figure 6

Effect of starch content on the complete particles in fracture surface.

4 Conclusion

This study aims to reveal the mechanism of corn starch toughening EP. Five corn starch admixture contents were designed for the modified EP materials. The tensile strength, elongation, Young’s modulus, and micrographs of tensile fractured surfaces were investigated. Based on the obtained results, we can draw some conclusions:

  1. The strength and elastic modulus increase first and then decrease with the addition of starch content and reach the maximum values of 22.19 MPa and 1.146 GPa at a range of 2.5 wt%, which are 9 and 33% higher than that of pure EP. The elongation at break reaches its average maximum value of 78.53% at a corn starch content of 2.5 wt%, which is 49.83% higher than that of pure EP. It is recommended that the best corn starch content should be 2.5 wt%.

  2. Microscopic observation shows that incorporating starch particles induce micro-cracks initiation in the EP matrix. Many localized shear-type stepped failures in the matrix can be observed, which means more energy would be absorbed during this process. The toughness of EP can be improved correspondingly.

  3. The starch particles are present in three typical forms in the fracture surface of the specimens: complete particles, peeled particles, and broken particles. According to the statistical results, we can find that the proportion of intact particles decreases linearly with starch content. With the addition of starch content, the probability of transgranular fracture occurring increases significantly. The strength of the EP decreases because of the low strength of the corn starch.

Acknowledgments

Thanks are due to Jun Xu for assistance with experiments and valuable discussion.

  1. Funding information: This work was supported by the Henan Science and Technology Research Project (Project 212102310402), the National Natural Science Foundation of China (Project 51404212), Basic Research Incubation Program for Young Teachers (Natural Science) of Zhengzhou University (Project JC202032026).

  2. Author contributions: Zhi Wang: writing – original draft, writing – review and editing, methodology, and formal analysis; Haopeng Lv: writing – original draft and investigation; Yuxiang Yang: investigation.

  3. Conflict of interest: Authors state no conflict of interest.

  4. Data availability statement: All relevant data are presented in the manuscript file.

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Received: 2022-08-13
Revised: 2022-10-03
Accepted: 2022-10-04
Published Online: 2022-11-03

© 2022 Zhi Wang et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  24. Experiment and analysis of mechanical properties of carbon fiber composite laminates under impact compression
  25. A machine learning investigation of low-density polylactide batch foams
  26. A comparison study of hyaluronic acid hydrogel exquisite micropatterns with photolithography and light-cured inkjet printing methods
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  31. Synergistic effects of PEG middle-blocks and talcum on crystallizability and thermomechanical properties of flexible PLLA-b-PEG-b-PLLA bioplastic
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  50. Study on composting and seawater degradation properties of diethylene glycol-modified poly(butylene succinate) copolyesters
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  66. Optoelectronic investigation and spectroscopic characteristics of polyamide-66 polymer
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  80. State of the art of geopolymers: A review
  81. Mechanical, thermal, and tribological characterization of bio-polymeric composites: A comprehensive review
  82. The influence of ionic liquid pretreatment on the physicomechanical properties of polymer biocomposites: A mini-review
  83. Influence of filler material on properties of fiber-reinforced polymer composites: A review
  84. Rapid Communications
  85. Pressure-induced flow processing behind the superior mechanical properties and heat-resistance performance of poly(butylene succinate)
  86. RAFT polymerization-induced self-assembly of semifluorinated liquid-crystalline block copolymers
  87. RAFT polymerization-induced self-assembly of poly(ionic liquids) in ethanol
  88. Topical Issue: Recent advances in smart polymers and their composites: Fundamentals and applications (Guest Editors: Shaohua Jiang and Chunxin Ma)
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https://doi.org/10.1515/epoly-2022-0075
Keywords for this article
corn starch; elastic modulus; mechanical properties; modified epoxy resin; toughened
Creative Commons
BY 4.0

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