Microstructure,mechanical properties and heat-resistance properties of bismaleimide composites modified synergistically by alumina and two kinds of thermoplastic resins

Abstract

Al₂O₃-PES-SPEEK/MBAE composites has been prepared, polymer matrix (MBAE) was obtained with 4,4’-diamino diphenyl methane bismaleimide (BMI) as reaction monomer, 3,3’-diallyl bisphenol A (BBA) and bisphenol A diallyl ether (BBE) as the reactive diluent, and two kinds of thermal plastic resins (polyether sulfone PES and sulfonated poly(ether ether ketone) SPEEK) as the reinforcements, nano-alumina (Al₂O₃) prepared by Sol–Gel method as the filler. The microstructure of SPEEK, Al₂O₃ and the composites were characterized, the mechanical properties and heat resistance of the composites were also studied and analyzed. The results reveal that there are sulfonic acid groups in SPEEK structure and the microstructure is more loose, and the degree of sulfonation is about 41.3%. Al₂O₃ is a nano-sized short-fibrous crystal with hydroxyl groups on its surface. The micromorphology of Al₂O₃-PES-SPEEK/MBAE composites show that the proper amount of PES, SPEEK and Al₂O₃ are uniformly dispersed in the matrix resin, which improves the fracture surface morphology of the composite, the shape of the section is fish scale and the fracture cracks are irregular and divergent, and the composites are ductile fracture. The mechanical properties indicate that the flexural strength, flexural modulus and impact strength of the composite is the maximum value 172.9 MPa, 4.7 GPa and 21.4 kJ/m², which is 73.1%, 74.1% and 125.3%, higher than the matrix resin, respectively, when the PES content is 3 wt%, 2 wt% SPEEK and 3 wt% Al₂O₃ in the composite. At this time, the thermal decomposition temperature of the composite material is 453.5°C, which is 15.4°C higher than that of the matrix resin, and the mechanical properties and heat-resistance properties of the Al₂O₃-PES-SPEEK/MBAE composite are significantly improved.

Keywords

Polyether sulfone sulfonated poly(ether ether ketone)alumina bismaleimide mechanical properties and heat-resistance properties

Introduction

Bismaleimide (BMI) is a kind of thermosetting resin with excellent high-temperature resistance, moist heat resistance and corrosion resistance.^1

–5 However, the unmodified BMI monomer structure contains a large number of rigid groups such as an imide ring and a benzene ring, resulting in high brittleness of the cured product and restricting in further applications in the fields of aerospace, electronics, and the like.^6

–10 Polyethersulfone (PES) is a high performance thermoplastic resin with excellent comprehensive properties, excellent mechanical properties, heat resistance and aging resistance.^11
–13 Due to the good interfacial compatibility between PES and BMI resin, PES can be used to further improve the toughness of BMI resin.¹⁴ The polyetheretherketone (PEEK) molecular chain contains a large amount of benzene ring, ether bond and carbonyl group and gives it excellent heat resistance, mechanical properties, corrosion resistance and abrasion resistance.^15

–18 However, PEEK is difficult to disperse in the polymer matrix and has poor interfacial compatibility, so it needs to be modified to enhance the compatibility between the two phases.¹⁹ After PEEK is sulfonated with concentrated sulfuric acid, a sulfonic acid group can be introduced into the PEEK macromolecular chain structure to obtain a sulfonated polyetheretherketone (SPEEK), thereby solving the problem of compatibility of the PEEK with the resin matrix.²⁰ Nano-Al₂O₃ is often used as an inorganic filler to improve the mechanical, thermal and electrical insulation properties of materials, due to its excellent properties such as high hardness, high-temperature resistance and electrical insulation.^21

–25

At present, most of the BMI resins are modified with a single reinforcement such as only SPEEK and PES are used for modification,^26,27 but it is never reported that inorganic component and two kinds of thermoplastic resins synergistically improved its performances. In the paper, polymer matrix (MBAE) was synthesized, which BMI was used as reactive monomer, 3,3’-diallyl bisphenol A (BBA) and bisphenol A bisallyl ether (BBE) as reactive diluent. And Al₂O₃-PES-SPEEK/MBAE multiphase composite was prepared, which thermoplastic resin PES and SPEEK were used as reinforcements, and Al₂O₃ by sol–gel method (Sol–Gel) as a filler, at the same time, to study the microstructure, mechanical properties and heat resistance of the composites.

Experimental

Materials

Polyethersulfone (PES, molecular weight 30,000, intrinsic viscosity 0.32 dl/g) and polyetheretherketone (PEEK, molecular weight 40,000, intrinsic viscosity 0.35 dl/g) were all obtained from Changchun Jida Plastic Engineering Research. N, N’-4,4’-diphenylmethane bismaleimide (BMI), 3,3’-diallyl bisphenol A (BBA) and bisphenol A bisallyl ether (BBE) were manufactured by Laizhou Laiyun Chemical production. Concentrated sulfuric acid (98 wt%) was purchased from Sinopharm Chemical Reagent. Isopropanol (analytical grade) and Aluminum isopropoxide (chemically pure) were obtained from Tianjin Fuyu Fine Chemical.

Measurements

The infrared characteristic peaks of PEEK, SPEEK and Al₂O₃ were characterized by infrared spectroscopy (FTIR, EQUINOX-55, Bruker). The test range is 400–4000 cm⁻¹.

Microscopic morphology of the SPEEK and composites are characterized by Scanning electron microscopy (SEM, SU8020, Hitachi High-Tech Company, Japan). Before the test, the composite material is cut in liquid nitrogen and the surface of the sample is sprayed with gold.

The microstructure of Al₂O₃ was observed by a transmission electron microscope (TEM, JEM-2100, JEOL, Japan).

The impact strength of composite materials is measured by charpy impact testing machine (TCJ-4, Jinan Huaxing Experimental Equipment, China) according to GB/T1043.1-2008 (China).²⁸ The pendulum energy is 2 J, the span is 6 cm, the length is (80 ± 0.5) mm, the width is (10 ± 0.1) mm, and the thickness is (4 ± 0.1) mm. Five parallel samples of each sample were averaged and the test samples were unnotched.

Bending strength test (universal material testing machine, CSS-4430, Shanghai Taiji Instrument & Meter Technology): Refer to GB/T2567-2008 to test the flexural strength of composite materials. The sample length is (80 ± 0.5) mm, the width is (10 ± 0.1) mm, the thickness is (4 ± 0.1) mm, and the speed is 2 mm/min. Five parallel samples of each sample were averaged and the test samples were unnotched.

Thermogravimetric analyzer (TGA, STA449F3, Netzsch, Germany): The test temperature range is 200–800°C, nitrogen protection during the test, the heating rate is 20°C/min, the sample quality is 5–10 mg.

Experimental procedure

(1) Modification of PEEK

5 g PEEK and 200 ml concentrated sulfuric acid were added into a three-necked flask and heated in a 50°C oil bath under N₂ atmosphere, and stirred for 48 h. During this process, the reaction system prevented from coming into water or air. The reacted solution was slowly poured into 800 ml ice water mixture and quickly stirred, and the dark yellow reactant gradually precipitated as a white polymer, kept for 12 h, filtered and washed with deionized water until pH value was about 7. The filtrate was dried under vacuum to give SPEEK.

(2) Preparation of Al₂O₃ with Sol–Gel method

Aluminum isopropoxide (20 g), isopropanol (100 ml) and deionized water (40 ml) were mixed and stirred in a water bath at 80°C for 2 h to sufficiently hydrolyze aluminum isopropoxide. The isopropanol and deionized water were removed by reduced pressure distillation, and the solid was dried at 120°C and calcined at 700°C for 3 h to obtain Al₂O₃.

(3) Preparation of Al₂O₃-PES-SPEEK/MBAE composite material

8 g BBA, 6 g BBE and Al₂O₃ were mixed in the three-necked bottle and ultrasonically dispersed at 80°C for 20 min, and then SPEEK was added and stirred until SPEEK completely dissolved. PES was slowly added into above the mixed solution to sufficiently dissolve at 170°C and 20 g BMI was added at 130°C, degassing for 30 min to obtain a glue, when the BMI resin was uniformly dispersed and the color of the solution became burgundy. The glue was poured into preheated molds and placed in a vacuum oven for gradient heating, and the curing conditions: 130°C/1 h, 150°C/2 h, 180°C/1 h, 200°C/2 h, 220°C/1 h. After curing, the Al₂O₃-PES-SPEEK/MBAE composite material can be obtained by demolding. For the convenience of analysis, the sample numbers are shown in Table 1.

Table 1.

Number and component of sample.

No.	Component	Mass fraction/wt%
No.	Component	PES	SPEEK	Al₂O₃
A	MBAE	0	0	0
B0–B5	Al₂O₃-PES-SPEEK/MBAE	3	2	0–5

Results and discussions

Microstructure of PEEK, SPEEK and PES

The infrared spectra of PEEK and SPEEK were shown in Figure 1. There are distinct sulfone acid group characteristic peaks in the SPEEK infrared spectrum, in which the absorption peak at 1251cm⁻¹ belongs to the asymmetric stretching vibration peak of O═S═O in sulfonic acid group, and 1076cm⁻¹ is symmetrical stretching vibration peak of O═S═O bond. It can be seen that the 1015 cm⁻¹ in the infrared spectrum of the SPEEK is the stretching vibration absorption peak of the S═O bond in –SO₃H. The absorption peak at 707 cm⁻¹, is caused by the symmetric stretching vibration of the S–O–C bond, and it can be preliminarily determined that the SPEEK has successfully introduced the sulfonic acid group.²⁹ It is confirmed that the introduction of sulfonic acid group did not change the basic structure of PEEK, and PEEK has been successfully sulfonated.³⁰

Figure 1.

FTIR spectrum of PEEK and SPEEK.

Figure 2 shows the SEM image and energy spectrum (EDS) of PEEK and SPEEK. It can be seen from Figure 2(a) that PEEK structure is tight within a certain range and there are a little holes, Figure 2(c) demonstrates the microcosmic morphology of SPEEK, which is quite different from PEEK. It has irregular shape with certain gaps, and the surface structure is loose and not tight. The main reasons are probable that sulfonated PEEK increases the activity of the benzene ring in the main chain with the introduction of the sulfonic acid group, improving the surface polarity of PEEK and the binding force between SPEEK and the matrix resin.³¹ From the results of the energy spectrum of Figure 2(b) and (d), there is no sulfur element in the energy spectrum of PEEK, and sulfur element appears in the energy spectrum of SPEEK. The sulfur of SPEEK is calculated by analyzing the content of each element of the energy spectrum of SPEEK.³² The SPEEK sulfonation degree was 41.3%. At the same time, the SPEEK sulfonation degree was calculated to be 42.4% with titration method. The analysis result of the two methods was basically consistent.

Figure 2.

SEM images and energy spectrum (EDS) result of PEEK and SPEEK. (a) PEEK, (b) EDS spectrum of PEEK, (c) SPEE, (d) EDS spectrum of SPEEK.

Figure 3 is the SEM and energy spectrum test results of PES. It can be seen that the surface of PES is uneven and has many fine pores. The sulfur content of PES is 19.29 wt% and higher than that of SPEEK. It indicates that the molecular structure of PES contains more sulfone groups, and the group has a certain polarity,³³ which is beneficial to form cross-linking with the resin matrix, thereby improving the dispersion in the matrix.³⁴

Figure 3.

SEM image and energy spectrum result of PES. (a) PES, (b) EDS spectrum of PES.

Micromorphology of Al₂O₃ and Al₂O₃-PES-SPEEK /MBAE composites

Figure 4 are infrared spectrum of SPEEK, PES, Al₂O₃ and Al₂O₃-PES-SPEEK/MBAE composites. It is known that Al₂O₃ exhibits weak hydroxyl absorption peaks at 3727 cm⁻¹ and 3701 cm⁻¹. It shows that there is a little amount of hydroxyl groups on the surface of Al₂O_3. ³⁵ In Al₂O₃-PES-SPEEK/MBAE composite, the peaks at 1104 cm⁻¹ and 1254 cm⁻¹ are symmetry and asymmetric stretching vibration absorption peaks of O═S═O bond in PES and SPEEK, the peak at 1781 cm⁻¹ is characteristic peak of the carbonyl group, at 599 cm⁻¹ is a six-coordinated Al–O stretching vibration peak. These results prove that Al₂O₃ is doped into the composite.

Figure 4.

FTIR spectrums of SPEEK, PES, Al₂O₃ and Al₂O₃-PES-SPEEK/MBAE composites.

Figure 5 is a TEM image of Al₂O₃. It is known that Al₂O₃ is a short-fiber crystal with a dimension of 5 nm diameter and 50 nm length. The structure has a large specific surface area and a small volume effect and chemical bonding with the matrix resin. These factors can improve comprehensive properties of the composite material.³⁶

Figure 5.

TEM photograph of Al₂O₃.

Figure 6 indicates cross-sectional SEM images of the matrix (MBAE), PES/MBAE, SPEEK/MBAE, PES-SPEEK/MBAE and Al₂O₃-PES-SPEEK/MBAE composite, respectively. From Figure 6(a), it can be seen that the fracture surface of the matrix MBAE is basically regular, and development direction of the broken crack is single, it is typical brittle fracture. The reason may be that the internal structure of the resin is regular and the fracture crack is developed in accordance with the stress direction, when the material is subjected to an external force.³⁷ In Figure 6(b), it can be seen that the fracture morphology of PES/MBAE composite has changed, the fracture crack becomes short and divergent, which is a ductile fracture.³⁸ At the same time, PES is dispersed in the matrix and the phase interface is clearly, PES exhibits a honeycomb structure with a size about 50 μm, and the large-sized honeycomb structure becomes a defect in the material, which is detrimental to the overall performance of the composite material. Figure 6(c) displays that the fracture surface of the SPEEK/MBAE composite has a rugged appearance, long and smooth fracture crack disappears. The SPEEK also exists in the matrix based on the two-phase, and SPEEK has good compatibility with the matrix, the phase interface is ambiguous and the size of porous SPEEK becomes smaller, the threshing phenomenon is difficult to occur during the fracture process, and the toughness of the material is remarkably improved. Figure 6(d) indicates that the cross-sectional morphology of PES-SPEEK/MBAE composites is very obvious under the action of PES and SPEEK. PES and SPEEK are dispersed in the matrix and show multiphase structure, PES and SPEEK are reinforcements, the size of PES is reduced and is more uniform in MBAE matrix. This may be the interaction between the two phases of PES and SPEEK to improve PES molecules compatibility with the substrate, and SPEEK plays a bridging role between the PES and the substrate, which makes the interface between the PES and the substrate more stable. And the other hand, PES and SPEEK will hinder the development of broken cracks and change its direction and consume most of the energy to enhance the overall performance of the material, when the composite is subjected to external stress.

Figure 6.

SEM images of (a) MBAE, (b) PES/MBAE, (c) SPEEK/MBAE, (d) PES-SPEEK/MBAE, (e) 3 wt% Al₂O₃-PES-SPEEK/MBAE and (f) 4 wt% Al₂O₃-PES-SPEEK/MBAE composites.

Figure 6(e) shows that Al₂O₃ dispersed uniformly in the matrix, and the direction of the crack is divergent to form a fish scale-like cross-section. The porous structure and the smaller size of the SPEEK basically disappeared, and the PES size of the honeycomb structure becomes smaller about 3 µm. This phenomenon suggests that Al₂O₃ has good compatibility with the matrix and can improve the dispersibility of PES and SPEEK in the matrix resin to achieve the aim of further toughening. Figure 6(f) suggests that the dispersibility is weakened and agglomeration occurs, when the content of Al₂O₃ is more than 4 wt%, the size of PES becomes bigger approximately 20 µm. The properties of PES-SPEEK/MBAE composite will be decreased.

3.3 Mechanical properties of Al₂O₃-PES-SPEEK/MBAE composites

The bending strength and bending modulus of the Al₂O₃-PES-SPEEK/MBAE composite are shown in Figure 7, and Figure 8 is the impact strength. It can be seen that the bending strength, bending modulus and impact strength of the PES-SPEEK/MBAE composite are 165.3 MPa, 4.5 GPa and 19.9 kJ/m², respectively, when the PES content is 3 wt% and the SPEEK is 2 wt% (sample B0). Compared with the matrix material (sample A, 99.9 MPa, 2.7 GPa, and 9.5 kJ/m²), they have been increased 5.5%, 66.7%, and 109.5%, respectively. The main reason is maybe that PES and SPEEK are thermoplastic resin and have better compatibility with the matrix, the interface effect between two phases can absorb most of energy, when the material is subjected to external stress.³⁷ So, the mechanical properties of the material have improved significantly.

Figure 7.

Flexural strength and flexural modulus of Al₂O₃-PES-SPEEK/MBAE composites.

Figure 8.

Impact strength of Al₂O₃-PES-SPEEK/MBAE composites.

The bending strength, bending modulus and impact strength of Al₂O₃-PES-SPEEK/MBAE composites (samples B1–B5) increased first and then decreased with the increase of Al₂O₃ doping amount in Figure 7 and Figure 8, and the sample B3 (3 wt% Al₂O₃) reached the maximum value of 172.9 MPa, 4.7 GPa and 21.4 kJ/m², which was 73.1%, 74.1% and 125.3% higher than the matrix resin (sample A), respectively, and 4.6%, 4.4% and 7.5% higher than those of sample B0. The reason is probable that the surface of Al₂O₃ has a hydroxyl group, which has strong interfacial bonding force with the resin matrix and it can be uniformly dispersed in the matrix, when Al₂O₃ doping amount is less than 3 wt%. Additionally, the crack extension direction changes, a large number of microcracks will generate and simultaneously absorb fracture energy to improve the mechanical properties of the materials, and there are an interaction among Al₂O₃, PES and SPEEK.^39,40 However, agglomeration phenomenon will occur and the size of Al₂O₃ become larger, the dispersibility deteriorates, when the content of Al₂O₃ is more than 3 wt%. So, proper Al₂O₃ will help to improve the mechanical properties of the materials.

Thermal stability of Al₂O₃-PES-SPEEK/MBAE composite

The thermogravimetric curves of Al₂O₃-PES-SPEEK/MBAE composites is shown in Figure 9, and it can be seen that the thermal decomposition temperature (T_d ) is between 438°C and 455°C, its heat resistance is good. Thermal weight loss of the materials is significantly between 425°C and 600°C, which is caused by the decomposition of the aromatic ring backbone of the material.

Figure 9.

Thermal loss curve of Al₂O₃-PES-SPEEK/MBAE composites.

As shown in Table 2, the thermal decomposition temperature of the material increases first and then decreases with the increase of the Al₂O₃ doping amount. When the Al₂O₃ content is 3 wt% (sample B3), the thermal decomposition temperature of the material reaches 453.5°C and increased by 15.4°C, compared with the matrix resin (sample A, 438.1°C). The main reason is that Al₂O₃ has a high thermal decomposition temperature and excellent heat resistance, it is beneficial to improve the heat resistance of the composite. And the surface of Al₂O₃ has more hydroxyl group and there is an interaction between Al₂O₃ and the matrix, the interaction can form good interface with the matrix. Al₂O₃ can uniformly disperse in the matrix to form strong interface with the matrix and limit polymer chains vibration, when Al₂O₃ doping amount is less than 3 wt%. This corresponds to the microscopic morphology analysis. However, the interaction force between the Al₂O₃ particles is enhanced, which is higher than the interaction between the particles and the matrix, thereby causing agglomeration, increasing the particle size, and causing compatibility among PES, SPEEK and the matrix reduction and destruction of the network-like structure in the system, resulting in a decrease in the regularity of the internal structure of the material, a large number of defects and heat concentration, which lowers the thermal decomposition temperature, when the Al₂O₃ doping amount is more than 3 wt%.

Table 2.

Decomposition temperature of Al₂O₃-PES-SPEEK/MBAE composites.

Sample numbers	T _d/°C	T _d ⁵/°C	T _d ¹⁰/°C
A	438.1	452.3	461.1
B0	442.5	457.7	466.4
B1	445.6	461.3	472.3
B2	449.8	465.8	476.5
B3	453.5	468.2	479.5
B4	449.7	465.4	476.4
B5	446.8	461.7	472.8

Conclusions

Sulfonated polyetheretherketone (SPEEK) was obtained by sulfonation of polyetheretherketone (PEEK) with concentrated sulfuric acid. FTIR spectroscopy, SEM images and EDS spectrum show that there exist obvious sulfonic acid groups in the SPEEK and the microstructure was more loose, and the degree of sulfonation was 41.3%. The Al₂O₃ prepared by the sol–gel method is a nano-sized short-fiber crystal having a hydroxyl group on its surface.

When PES, SPEEK and Al₂O₃ synergistically modify the matrix (MBAE), the cross-section morphology is fish scale, the crack is irregular, Al₂O₃ particles is uniformly dispersed in the matrix, the dispersion of PES and SPEEK in the matrix is increased, and the PES size of the honeycomb structure is increased. As the size becomes smaller, the porous structure of SPEEK disappears, and the Al₂O₃-PES-SPEEK/MBAE composite exhibits ductile fracture.

When the content of PES, SPEEK and Al₂O₃ is 3 wt%, 2 wt% and 3 wt%, the flexural strength, flexural modulus and impact strength of Al₂O₃-PES-SPEEK/MBAE composites are 172.9 MPa, 4.7 GPa and 21.4 kJ/m², which is 73.1%, 74.1% and 125.3% higher than the matrix resin, respectively. At this time, the thermal decomposition temperature of the composite material is 453.5°C, which is 15.4°C higher than that of the matrix resin, and the mechanical properties and heat resistance of the material are greatly improved.

Footnotes

Acknowledgements

The authors would like to express their appreciation to the project support by the Harbin technology bureau subject leader (Grant No. 2015RAXXJ029), and thank Yuyang Shang for helping in the experiment and polishing the article.

Data availability

All data included in this study are available upon request by contact with the corresponding author.

Declaration of conflicting interests

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

Funding

The author(s) received no financial support for the research, authorship, and/or publication of this article.

ORCID iD

Yufei Chen

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Microstructure,mechanical properties and heat-resistance properties of bismaleimide composites modified synergistically by alumina and two kinds of thermoplastic resins

Abstract

Keywords

Introduction

Experimental

Materials

Measurements

Experimental procedure

Results and discussions

Microstructure of PEEK, SPEEK and PES

Micromorphology of Al2O3 and Al2O3-PES-SPEEK /MBAE composites

3.3 Mechanical properties of Al2O3-PES-SPEEK/MBAE composites

Thermal stability of Al2O3-PES-SPEEK/MBAE composite

Conclusions

Footnotes

Acknowledgements

Data availability

Declaration of conflicting interests

Funding

ORCID iD

References

Micromorphology of Al₂O₃ and Al₂O₃-PES-SPEEK /MBAE composites

3.3 Mechanical properties of Al₂O₃-PES-SPEEK/MBAE composites

Thermal stability of Al₂O₃-PES-SPEEK/MBAE composite