An ultrahigh-strength continuous fiber-reinforced liquid crystal polymer composite and a method for preparing the same

By combining continuous fibers with LCP powder and using hot pressing technology, the problem of insufficient strength of LCP composites in large components was solved, and a high-strength continuous fiber reinforced liquid crystal polymer composite material was prepared, which is suitable for aerospace and other fields.

CN117885407BActive Publication Date: 2025-11-04SHANGHAI PRET CHEM NEW MATERIALS CO LTD +1
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Patent Information

Application Number
CN202311843299.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-29
Publication Date
2025-11-04
Estimated Expiration
2043-12-29

AI Technical Summary

Technical Problem

Pure LCP resin or chopped fiber reinforced LCP composites have insufficient strength in large components, and LCP materials crystallize quickly, making it difficult to injection mold large components.

Method used

Continuous fibers are used as the reinforcing phase and combined with LCP powder. Taking advantage of the solid-phase polymerization characteristics of LCP materials, continuous fiber-reinforced LCP composite materials are prepared by hot pressing. The specific steps include plasma surface treatment of fiber cloth, impregnation with compatibilizer, layering and stacking, hot static pressing and heat treatment.

Benefits of technology

A high-strength continuous fiber reinforced liquid crystal polymer composite material was prepared, which is suitable for large components and improves the tensile strength and modulus of the material.

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Abstract

The application discloses a kind of super-high-strength continuous fiber reinforced liquid crystal polymer composite material and preparation method thereof. After using fiber cloth and liquid crystal polymer prepolymer powder hot isostatic pressing, the mechanical properties of the composite material are improved by heat treatment process, and the tensile strength of the obtained continuous fiber reinforced liquid crystal polymer composite material is greater than 1800MPa, which can be used for large structural parts.
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Description

TECHNICAL FIELD

[0001] The present application relates to a kind of compositions, specifically relates to a kind of super high strength continuous fiber reinforced liquid crystal polymer composite material and its preparation method, belong to composite material field. BACKGROUND

[0002] Resin-based composite material is an important cornerstone of modern industry and high-tech development, is one of the indispensable basic materials of national security and national economy.In recent years, with the vigorous development of China's aerospace industry, resin-based advanced composite material based on space application develops rapidly, and there is a great demand for the preparation technology of high-performance, lightweight and large-size resin-based composite material components.

[0003] Thermotropic liquid crystal polymer (LCP) is a kind of high-performance polymer material, which is usually known for its high strength, high modulus, excellent melt processing forming characteristics, inherent flame retardancy, low water absorption, chemical corrosion resistance, good radiation resistance and high and low temperature impact resistance and many other uses at high temperature, so it has a wide application in aerospace, special industry and other fields.But for large components, the strength of pure LCP resin or short fiber reinforced LCP composite material is still insufficient;And because the crystallization rate of LCP material is fast, it is difficult to injection mold large components.

[0004] The design idea of the present application is to use continuous fibers as reinforcing phase, which is combined with LCP powder, and then hot-pressed to prepare continuous fiber reinforced LCP composite material by using the solid phase polymerization characteristics of LCP material. SUMMARY

[0005] The purpose of the present application is to provide a kind of high-strength continuous fiber reinforced liquid crystal polymer composite material and its preparation method, in order to prepare large components.

[0006] The purpose of the present application can be realized by the following technical solutions:

[0007] A kind of super high strength continuous fiber reinforced liquid crystal polymer composite material is composed of continuous fiber cloth, compatibilizer and liquid crystal polymer, and its preparation method is as follows:

[0008] (1) the fiber cloth is subjected to plasma surface treatment, and then impregnated with compatibilizer containing epoxy functional group;

[0009] (2) The surface treated fiber cloth and liquid crystal polymer prepolymer powder are layered and stacked in a mold cavity, and then pre-pressed and formed by a hot isostatic pressing process. The hot isostatic pressing process is performed in an inert gas medium for 1-10 minutes, the inert gas is at least one of nitrogen, argon and carbon dioxide, and the oxygen content is below 20 PPM. If the oxygen content is too high, the small molecule content in the prepared liquid crystal polymer composite material is too high, there is a gap between the fiber cloth and the liquid crystal polymer, and the tensile strength is too low.

[0010] The treatment temperature used in the hot isostatic pressing process is in the range of the melting point of the liquid crystal polymer to the melting point of the liquid crystal polymer plus 20°C.

[0011] (3) The fiber cloth and liquid crystal polymer prepolymer powder laminated body after the hot isostatic pressing process is heat treated to obtain a continuous fiber reinforced liquid crystal polymer composite material. The laminated body is in a vacuum or inert gas medium during the heat treatment, and the oxygen content is controlled to be below 20 ppm.

[0012] The heat treatment is performed in an inert gas stream or vacuum condition for 4-12 hours, the inert gas is at least one of nitrogen, argon and carbon dioxide, and the gas flow is greater than 10 mL / min; the vacuum condition is a vacuum degree less than or equal to 100 Pa, preferably less than 20 Pa. If the gas flow is too small or the vacuum degree is insufficient, the small molecule content in the prepared liquid crystal polymer composite material is too high, and the tensile strength is too low. The treatment temperature used in the heat treatment is in the range of 100°C below the melting point of the liquid crystal polymer to 20°C below the melting point of the liquid crystal polymer.

[0013] The compatibilizer containing an epoxy functional group in the present application is a bisphenol A type unsaturated polyester, i.e. a bisphenol A type epoxy resin.

[0014] In the ultra-high strength continuous fiber reinforced liquid crystal polymer composite material in the present application, the fiber cloth accounts for greater than or equal to 25% and less than 65% of the weight ratio of the composite material.

[0015] The fiber cloth in the present application refers to one or both of glass fiber and carbon fiber woven, with a thickness of 10-50 microns.

[0016] The glass fiber in the present application can be selected as E-glass fiber, i.e. alkali-free glass, which is an aluminoborosilicate glass fiber. It has good electrical insulation performance and better strength, with a diameter of 5-20 microns.

[0017] The carbon fiber in the present application refers to high-strength high-modulus fiber with a carbon content of more than 90%, which can be selected as high-strength carbon fiber obtained by carbonization of polyacrylonitrile fiber, viscose-based fiber and pitch-based fiber, with a diameter of 5-15 microns.

[0018] The liquid crystal polymer in the present application is a liquid crystalline polyester or polyester amide using an aromatic compound as a raw material monomer, and is preferably a wholly aromatic liquid crystalline polyester or polyester amide using only an aromatic compound as a raw material monomer.

[0019] A typical example of the liquid crystal polymer of the present application is a liquid crystalline polyester formed by polymerizing an aromatic hydroxyl carboxylic acid and at least one compound selected from the group consisting of an aromatic hydroxyl amine, an aromatic diamine, an aromatic dicarboxylic acid, and an aromatic diol.

[0020] Part or all of the aromatic hydroxyl carboxylic acid, the aromatic hydroxyl amine, the aromatic diamine, the aromatic dicarboxylic acid, and the aromatic diol can be independently a polymerizable derivative thereof, respectively.

[0021] As the polymerizable derivative of the compound having a hydroxyl group such as the aromatic hydroxyl carboxylic acid, the aromatic hydroxyl amine, the aromatic diamine, and the aromatic diol, an acylate formed by acylating the hydroxyl group to an acyloxy group can be exemplified.

[0022] In the combination of each repeating unit constituting the liquid crystal polymer:

[0023] The aromatic hydroxyl carboxylic acid is selected from the repeating unit of p-hydroxybenzoic acid and 6-hydroxy-2-naphthoic acid; the aromatic dicarboxylic acid is selected from the repeating unit of terephthalic acid, isophthalic acid, and 2,6-naphthalene dicarboxylic acid, and is preferably selected from the repeating unit of terephthalic acid and isophthalic acid; the aromatic diol is selected from the repeating unit of hydroquinone, 2,6-naphthalene diol, and 4,4'-dihydroxybiphenyl, and is preferably selected from the repeating unit of hydroquinone and 4,4'-dihydroxybiphenyl; the aromatic hydroxyl amine is selected from the repeating unit of p-aminophenol and p-aminonaphthol, and is preferably selected from the repeating unit of p-aminophenol; and the aromatic diamine is selected from the repeating unit of p-phenylenediamine, 4,4'-diphenyl, and 2,6-naphthalene diamine.

[0024] The liquid crystal polymer of the present application contains at least the repeating unit of the aromatic hydroxyl carboxylic acid.

[0025] The liquid crystal polymer prepolymer powder in the present application refers to a liquid crystal polymer oligomer having a melt viscosity of 10 Pa·s or less. DETAILED DESCRIPTION

[0026] The present application will be further illustrated by the following examples and comparative examples, and the present application should not be limited to the specific contents illustrated by the following examples without violating the purpose of the present application.

[0027] Product performance test method:

[0028] The melting point (Tm) of the product was measured using a differential scanning calorimeter (DSC 8000, PerkinElmer, USA).m ), tested by referring to the method of ASTM D3418. The melt viscosity (MV) of the present application is tested by using a capillary rheometer (RH 2200, Malvern, UK), tested by referring to the method of ASTM D3835. The tensile strength and tensile modulus of the present application are tested by using a universal testing machine, tested by referring to the method of GBT 3354. The bending strength and bending modulus of the present application are tested by using a universal testing machine, tested by referring to the method of GB / T 3356. The heat distortion temperature of the present application is tested by using a heat distortion Vicat tester, tested by referring to the method of GB / T 1634.

[0029] Example 1:

[0030] First, p-hydroxybenzoic acid, 6-hydroxy-2-naphthoic acid and acetic anhydride are reacted at a constant temperature of 120-130°C for 1 hour, then the temperature is raised to 185-195°C within 2 hours, and then reacted at a constant temperature for 0.5-1 hour, and the acetylation reaction is completed. Then, the acetic ester obtained by acetylation is subjected to a melt polycondensation reaction, and the polymerization temperature is raised to a predetermined temperature within 3 hours to continuously carry out the polymerization reaction. Then, the temperature is kept constant, and the reactants become a prepolymer 1 with a certain molecular weight. When the torque of the stirrer rises to a predetermined level, nitrogen is immediately introduced to terminate the polymerization reaction. The nitrogen gas pressure is increased to 2 kg / cm 2 , and the liquid crystal polymer prepolymer 1 is obtained. The melting point and melt viscosity of the obtained liquid crystal polymer prepolymer 1 are measured. The monomer ratio for preparing the above-mentioned liquid crystal polymer is as follows: p-hydroxybenzoic acid 73 mol%, 6-hydroxy-2-naphthoic acid 27 mol%. The melting point is about 280°C, and the viscosity is about 7 Pa·s.

[0031] The carbon fiber cloth (TZ700S, Weihai Tuozhan Fiber Co., Ltd.) is subjected to plasma surface treatment, and the treatment conditions are as follows: the treatment medium is nitrogen gas, the gas flow rate is 50 mL / min, the plasma generation power is 300 W, and the treatment time is 80 s. After the treatment, the carbon fiber cloth is immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain a surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and the liquid crystal polymer prepolymer 1 powder are layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder is 55:45. Then, the mold cavity is replaced with nitrogen, and the mold cavity is sealed. Then, the temperature is slowly raised to 285°C, and the hot isostatic pressing process is carried out in a nitrogen medium for 3 minutes, and the oxygen content is controlled to be below 20 PPM.

[0032] After that, the temperature of the mold cavity is decreased to 250°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the static pressure process is started. After the temperature is decreased to 250°C, nitrogen is discharged, and vacuum is applied, with the vacuum degree being about 50 Pa, and the oxygen content being controlled to be less than 20 ppm. The whole heat treatment process lasts for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material is obtained, and its performance is shown in Table 1.

[0033] Example 2:

[0034] First, p-hydroxybenzoic acid, 6-hydroxy-2-naphthoic acid, and hydroquinone are reacted with acetic anhydride at 120-130°C for 1 hour, then increased to 185-195°C within 2 hours, and then reacted at constant temperature for 0.5-1 hour, and the acetylation reaction is completed. Then, the acetic ester obtained by the acetylation reaction is subjected to melt polycondensation reaction with terephthalic acid, and the polymerization temperature is increased to the predetermined temperature within 3 hours, so that the polymerization reaction is continuously carried out. Then, the temperature is kept constant, and the reactants become a prepolymer 2 with a certain molecular weight. When the torque of the stirrer reaches a predetermined level, nitrogen is introduced to terminate the polymerization reaction. The nitrogen gas pressure is increased to 2 kg / cm 2 The liquid crystal polymer prepolymer 2 obtained is subjected to melting point and melt viscosity determination. The monomer ratio for preparing the above liquid crystal polymer is as follows: p-hydroxybenzoic acid 42 mol%, 6-hydroxy-2-naphthoic acid 22 mol%, hydroquinone 18 mol%, and terephthalic acid 18 mol%. The melting point is about 340°C, and the viscosity is about 8 Pa·s.

[0035] The carbon fiber cloth (TZ700S, Weihai Tuozhan Fiber Co., Ltd.) is subjected to plasma surface treatment, and the treatment conditions are as follows: the treatment medium is nitrogen, the gas flow is 50 mL / min, the plasma generation power is 300 W, and the treatment time is 80 s. After the treatment, the carbon fiber cloth is immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and the liquid crystal polymer prepolymer 2 powder are layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder is 55:45. Then, the mold cavity is replaced with nitrogen, and the mold cavity is sealed. Then, the temperature is slowly increased to 345°C, and the heat and static pressure process is carried out in a nitrogen medium for 3 minutes, with the oxygen content being controlled to be less than 20 PPM.

[0036] After that, the temperature of the mold cavity is decreased to 260°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the static pressure process is started. After the temperature is decreased to 260°C, nitrogen is discharged, and vacuum is applied, with the vacuum degree being about 50 Pa, and the oxygen content being controlled to be less than 20 ppm. The whole heat treatment process lasts for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material is obtained, and its performance is shown in Table 1.

[0037] Example 3:

[0038] First, p-hydroxybenzoic acid, 4-aminophenol, and diphenylolpropane are acetylated with acetic anhydride at 120-130°C for 1 hour, then the temperature is raised to 185-195°C in 2 hours, and the acetylation reaction is continued for 0.5-1 hour. Then, the acetylated product is subjected to melt polycondensation with isophthalic acid, and the temperature is raised to a predetermined temperature in 3 hours to continuously perform the polycondensation reaction. Then, the temperature is kept constant, and the reaction product is converted into a prepolymer 3 having a certain molecular weight. When the torque of the stirrer reaches a predetermined value, nitrogen is introduced to terminate the polycondensation reaction. The nitrogen pressure is increased to 2 kg / cm 2 The liquid crystal polymer prepolymer 3 is discharged, and the liquid crystal polymer prepolymer 3 thus obtained is subjected to measurement of the melting point and the melt viscosity. The monomer ratio for preparing the above liquid crystal polymer is as follows: p-hydroxybenzoic acid 50 mol%, 4-aminophenol 8 mol%, diphenylolpropane 21 mol%, and isophthalic acid 21 mol%. The melting point thereof is about 370°C, and the viscosity thereof is about 9 Pa-s.

[0039] The carbon fiber cloth (TZ700S, Weihai Tuozhan Fiber Co., Ltd.) is subjected to plasma surface treatment under the following conditions: nitrogen gas is used as the treatment medium, the gas flow rate is 50 mL / min, the plasma generation power is 300 W, and the treatment time is 80 s. After the treatment, the carbon fiber cloth is immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain a surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and the liquid crystal polymer prepolymer 3 powder are layered and stacked in a mold cavity to 10 layers, wherein the weight ratio of the carbon fiber cloth to the liquid crystal polymer prepolymer 1 powder is 55:45. Then, the mold cavity is replaced with nitrogen, and the mold cavity is sealed. Then, the temperature is slowly raised to 375°C, and the hot isostatic pressing process is performed in a nitrogen medium for 3 minutes, with the oxygen content controlled to be below 20 PPM.

[0040] Subsequently, the temperature of the mold cavity is lowered to 260°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process is started. After the temperature is lowered to 260°C, nitrogen is continuously introduced on one side of the mold cavity, and the nitrogen is discharged on the other side of the mold cavity. The nitrogen flow rate is about 20 mL / min, and the oxygen content is controlled to be below 20 ppm. The entire hot treatment process lasts for 12 hours, and a carbon fiber-reinforced liquid crystal polymer composite material is finally obtained. The performance of the material is shown in Table 1.

[0041] Example 4:

[0042] The glass fiber cloth (EWR800, China Jushi Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the glass fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodu Chemical Industry (Kunshan) Co., Ltd.) to obtain the glass fiber cloth subjected to surface treatment. Then, the glass fiber cloth subjected to surface treatment and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the glass fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, the mold cavity was sealed, and then slowly heated to 385°C, and the hot isostatic pressing process was performed in a nitrogen medium for 1 minute, and the oxygen content was controlled to be below 20 PPM.

[0043] Then, the temperature of the mold cavity was reduced to 270°C, and the hot treatment of the glass fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 270°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 10 hours, and finally the glass fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0044] Example 5:

[0045] The carbon fiber glass fiber mixed woven cloth (WP3911, Weihai Guangwei Composite Material Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber woven cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodu Chemical Industry (Kunshan) Co., Ltd.) to obtain the carbon fiber woven cloth subjected to surface treatment. Then, the carbon fiber woven cloth subjected to surface treatment and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the carbon fiber woven cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, the mold cavity was sealed, and then slowly heated to 380°C, and the hot isostatic pressing process was performed in a nitrogen medium for 1 minute, and the oxygen content was controlled to be below 20 PPM.

[0046] Then, the temperature of the mold cavity was reduced to 270°C, and the hot treatment of the glass fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 270°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 10 hours, and finally the glass fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0047] Example 6:

[0048] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was performed in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0049] Then, the temperature of the mold cavity was reduced to 260°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 260°C, the nitrogen was discharged, and a vacuum was applied, and the vacuum degree was about 50 Pa, and the oxygen content was controlled to be below 20 ppm. The entire heat treatment process lasted for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0050] Example 7:

[0051] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was performed in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0052] Then, the temperature of the mold cavity was reduced to 260°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 260°C, the nitrogen was discharged, and a vacuum was applied, and the vacuum degree was about 50 Pa, and the oxygen content was controlled to be below 20 ppm. The entire heat treatment process lasted for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0053] Example 8:

[0054] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, and the treatment time was 80 s. After the treatment, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain a surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed. Then, the temperature was slowly increased to 375°C, and the hot isostatic pressing process was performed in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0055] Then, the temperature of the mold cavity was reduced to 300°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 300°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity. The nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The entire hot treatment process lasted for 4 hours, and finally a carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0056] Example 9:

[0057] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, and the treatment time was 80 s. After the treatment, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain a surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed. Then, the temperature was slowly increased to 375°C, and the hot isostatic pressing process was performed in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0058] Then, the temperature of the mold cavity was reduced to 300°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 300°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity. The nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The entire hot treatment process lasted for 4 hours, and finally a carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0059] Comparative Example 1:

[0060] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 360°C, and the hot isostatic pressing process was carried out in a nitrogen medium for 10 minutes, and the oxygen content was controlled to be below 20 PPM.

[0061] Then, the temperature of the mold cavity was reduced to 300°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 300°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0062] Comparative Example 2:

[0063] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was carried out in a nitrogen medium for 30 minutes, and the oxygen content was controlled to be below 20 PPM.

[0064] Then, the temperature of the mold cavity was reduced to 300°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 300°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0065] Comparative Example 3:

[0066] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 1 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 395°C, and the hot isostatic pressing process was performed in a nitrogen medium for 1 minute, and the oxygen content was controlled to be below 20 PPM.

[0067] Then, the temperature of the mold cavity was reduced to 260°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 260°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 4 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0068] Comparative Example 4:

[0069] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 1 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 320°C, and the hot isostatic pressing process was performed in a nitrogen medium for 2 minutes, and the oxygen content was controlled to be below 20 PPM.

[0070] Then, the temperature of the mold cavity was reduced to 260°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 260°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 4 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0071] Comparative Example 5:

[0072] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guoduo Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was carried out in an air medium for 3 minutes.

[0073] After that, the temperature of the mold cavity was reduced to 270°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 270°C, nitrogen was continuously introduced and discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0074] Comparative Example 6:

[0075] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guoduo Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was carried out in an air medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0076] After that, the temperature of the mold cavity was reduced to 270°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 270°C, nitrogen was continuously introduced and discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 8 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0077] Comparative Example 7:

[0078] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, and the treatment time was 80 s. After the treatment, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain a surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 1 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed. Then, the temperature was slowly increased to 285°C, and the hot isostatic pressing process was performed in a nitrogen medium for 5 minutes, with the oxygen content controlled to be below 20 PPM.

[0079] Then, the temperature of the mold cavity was reduced to 220°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 220°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity. The nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The entire hot treatment process lasted for 24 hours, and finally a carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0080] Comparative Example 8:

[0081] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, and the treatment time was 80 s. After the treatment, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain a surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 1 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed. Then, the temperature was slowly increased to 285°C, and the hot isostatic pressing process was performed in a nitrogen medium for 5 minutes, with the oxygen content controlled to be below 20 PPM.

[0082] Then, the temperature of the mold cavity was reduced to 220°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 220°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity. The nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The entire hot treatment process lasted for 24 hours, and finally a carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0083] Comparative Example 9:

[0084] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was performed in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0085] Then, the temperature of the mold cavity was reduced to 270°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 270°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 2 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 12 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0086] Comparative Example 10:

[0087] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was performed in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0088] Then, the temperature of the mold cavity was reduced to 270°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminate after the isostatic pressing process was started. After the temperature was reduced to 270°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 2 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 12 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0089] Comparative Example 11:

[0090] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was carried out in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0091] Then, the temperature of the mold cavity was reduced to 330°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 330°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 4 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0092] Comparative Example 12:

[0093] The carbon fiber cloth (TZ700S, Weihai Taideng Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, the treatment time was 80 s, and after the treatment was completed, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain the surface-treated carbon fiber cloth. Then, the surface-treated carbon fiber cloth and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the fiber cloth to the liquid crystal polymer prepolymer 1 powder was 55:45. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C, and the hot isostatic pressing process was carried out in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0094] Then, the temperature of the mold cavity was reduced to 330°C, and the heat treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 330°C, nitrogen was continuously introduced, and nitrogen was discharged on the other side of the mold cavity, and the nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole heat treatment process lasted for 4 hours, and finally the carbon fiber reinforced liquid crystal polymer composite material was obtained, and its performance is shown in Table 1.

[0095] Comparative Example 13:

[0096] The carbon fiber cloth (TZ700S, Weihai Taiding Fiber Co., Ltd.) was subjected to plasma surface treatment, and the treatment conditions were as follows: the treatment medium was nitrogen, the gas flow was 50 mL / min, the plasma generation power was 300 W, and the treatment time was 80 s. After the treatment, the carbon fiber cloth was immersed in bisphenol A diglycidyl ether (YD114, Guodou Chemical (Kunshan) Co., Ltd.) to obtain a carbon fiber cloth subjected to surface treatment. Then, the carbon fiber cloth subjected to surface treatment and liquid crystal polymer prepolymer 3 powder were layered and stacked to 10 layers in a mold cavity, and the weight ratio of the carbon fiber cloth to the liquid crystal polymer prepolymer 1 powder was 70:30. Then, the mold cavity was replaced with nitrogen, and the mold cavity was sealed, and then slowly heated to 375°C. The hot isostatic pressing process was performed in a nitrogen medium for 3 minutes, and the oxygen content was controlled to be below 20 PPM.

[0097] Then, the temperature of the mold cavity was reduced to 260°C, and the hot treatment of the carbon fiber cloth and the liquid crystal polymer prepolymer powder laminated body after the isostatic pressing process was started. After the temperature was reduced to 260°C, nitrogen was continuously introduced, and nitrogen was discharged from the other side of the mold cavity. The nitrogen flow was about 20 mL / min, and the oxygen content was controlled to be below 20 ppm. The whole hot treatment process lasted for 12 hours, and finally a composite material was obtained.

[0098] Table 1 summarizes the properties of the liquid crystal polymer composite materials of the examples and the comparative examples

[0099]

[0100] The properties of the continuous fiber reinforced liquid crystal polymer composite materials prepared in Examples 1-9 and Comparative Examples 1-12 are shown in Table 1. During the hot isostatic pressing process, the liquid crystal polymer prepolymer powder infiltrates into the interstices between the fiber cloth fibers, fully contacts and combines with the fiber cloth, and itself is fused into the continuous phase matrix of the composite material. After high temperature heat treatment, the degree of polymerization of the liquid crystal polymer prepolymer is increased to the desired molecular weight. Comparing Comparative Example 3 with Comparative Example 1, if the temperature during the hot isostatic pressing process is too low, the liquid crystal polymer will weakly combine with the fiber cloth, and the matrix itself will not be fully fused, resulting in a poor overall strength of the obtained composite material. Comparing Comparative Example 3 with Comparative Examples 2-5, it can be seen that if the hot isostatic pressing temperature is too high, the time is too long, or the oxygen content is too high, the mechanical properties of the obtained composite material will be poor, which is due to the high temperature decomposition or oxidation of the liquid crystal polymer prepolymer during this process. Comparing Comparative Example 3 with Comparative Examples 6 and 9, if the inert gas flow is too small or the vacuum degree is not enough, the mechanical properties of the liquid crystal polymer composite material will not be significantly improved during the heat treatment process, and will not meet the requirements of ultra-high strength, and may even decrease. Comparing Comparative Example 3 with Comparative Examples 7 and 8, if the heat treatment temperature is too low or the time is not enough, the properties of the composite material will not be improved. Similarly, in Comparative Examples 10 and 11, if the heat treatment temperature is too high or the time is too long, the properties of the composite material will not be improved, and may even be damaged. Comparing Comparative Example 3 with Comparative Example 12, if the fiber cloth content is too low, the overall strength of the obtained composite material will not meet the required requirements.

[0101] The continuous fiber reinforced liquid crystal polymer composite material of the present application is easy to prepare and has high strength, and can be used for large structural parts.

Claims

1. A method for preparing an ultra-high strength continuous fiber reinforced liquid crystal polymer composite material, characterized in that: The composite material is composed of continuous fiber cloth, compatibilizer, and liquid crystal polymer, and its preparation method is as follows: (1) The fiber cloth is subjected to plasma surface treatment and then impregnated with a compatibilizer containing epoxy functional groups; (2) The surface-treated fiber cloth and liquid crystal polymer prepolymer powder are layered and stacked in the mold cavity, and then pre-pressed by hot static pressing process; The hot static pressing process is carried out in an inert gas medium, and the oxygen content is controlled to be below 20 ppm; (3) Heat-treat the fiber cloth after static pressing and the liquid crystal polymer prepolymer powder laminate to obtain a continuous fiber reinforced liquid crystal polymer composite material. During the heat treatment process, the laminate is placed in a vacuum or inert gas medium, and the oxygen content is controlled to be below 20 ppm; The fiber cloth accounts for 25%-65% of the weight of the composite material; the fiber cloth is woven from one or both of glass fiber and carbon fiber; the liquid crystal polymer is a fully aromatic polyester or polyesteramide; the hot static pressing process temperature is within the range of the melting point of the liquid crystal polymer to 20°C above the melting point of the liquid crystal polymer; the heat treatment process temperature is within the range of 230°C to 320°C. The prepared composite material has a tensile strength ≥1800 MPa.

2. The method for preparing an ultra-high strength continuous fiber reinforced liquid crystal polymer composite material according to claim 1, characterized in that: The epoxy-functionalized compatibilizer is a bisphenol A type unsaturated polyester.

3. A continuous fiber reinforced liquid crystal polymer composite material, which is manufactured by the method for preparing ultra-high strength continuous fiber reinforced liquid crystal polymer composite material according to claim 1 or 2.

4. A molded article comprising the continuous fiber-reinforced liquid crystal polymer composite material of claim 3.

Citation Information

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