Method for preparing carbon fiber / epoxy resin composite material by utilizing regulation and control of intercalation interface of graphene oxide nanosheet

Abstract

The invention discloses a method for preparing a carbon fiber / epoxy resin composite material by utilizing regulation and control of an intercalation interface of a graphene oxide nanosheet, and belongs to the technical field of carbon fiber / epoxy resin composite materials. The preparation method comprises the following steps: pretreating carbon fibers to prepare aminated carbon fibers; preparing a carbon fiber / graphene oxide nanosheet hybrid material; and preparing the graphene oxide nanosheet intercalation interface regulated carbon fiber / epoxy resin composite material. According to the method for preparing the carbon fiber / epoxy resin composite material by utilizing graphene oxide nanosheet intercalation interface regulation, the interface compatibility of the carbon fiber and the epoxy resin matrix is regulated by taking the graphene oxide nanosheet as an intercalation, the mechanical and thermodynamic properties of the composite material can be improved, the method is simple and easy to implement, and the method is suitable for industrial production. And the method is suitable for different types of carbon fiber / epoxy resin systems.

Description

Technical Field

[0001] The present invention belongs to the technical field of carbon fiber / epoxy resin composites; specifically, it relates to a method for preparing carbon fiber / epoxy resin composites by modulating the interface through the intercalation of graphene oxide nanosheets. Background Art

[0002] Carbon fiber / epoxy resin composite is a new type of composite material with epoxy resin as the matrix and carbon fiber as the reinforcing material, which has properties such as high strength, high stiffness, fatigue resistance, corrosion resistance, good heat resistance, and strong designability, and is widely used in the fields of aerospace, automotive manufacturing, high-speed railway trains, medical equipment, etc.

[0003] Epoxy resin has good thermal conductivity and can maintain its excellent properties within a certain temperature range. Carbon fiber can provide the required high stiffness and high strength for the composite material, making it lighter, stronger, and having excellent fatigue resistance, ensuring the stable performance of the composite material under long-term cyclic loading. However, carbon fiber / epoxy resin composites are easily affected by the interfacial compatibility between carbon fiber and epoxy resin matrix, and there are prominent problems such as large brittleness of the bonding layer, easy peeling and delamination, which seriously affect the stability of the structural strength of the composite material and the safety of practical applications. Generally speaking, the orientation and stacking mode of carbon fiber in the composite material will directly affect the mechanical properties of the composite material, and its strength, stiffness, and toughness can be changed by changing its orientation and stacking mode; the interfacial bonding between carbon fiber and resin matrix can also be improved by means of chemical treatment, surface coating, etc. on the surface of carbon fiber; the curing conditions of epoxy resin (such as temperature, pressure, and curing time, etc.) have an important influence on the properties of the composite material, and appropriately adjusting the curing conditions can improve the mechanical properties and heat resistance of the composite material. However, there are still certain limitations in the prior art for improving the properties of carbon fiber / epoxy resin composites. Therefore, it is very necessary to develop an effective method to regulate the interfacial interaction between carbon fiber and epoxy resin matrix to improve the performance stability of the composite material.

[0004] Graphene is a multifunctional two-dimensional nanomaterial with high surface area, high mechanical strength, and excellent thermal and electrical conductivity, etc., which can be used to improve the interfacial bonding between carbon fiber and epoxy resin matrix, and regulate the stiffness, strength, toughness, electrical conductivity, thermal conductivity, etc. of the composite material. By using graphene oxide nanosheets as intercalants to modulate the interfacial compatibility between carbon fiber and epoxy resin matrix, the mechanical and thermodynamic properties of the composite material can be improved, and the method is simple and feasible, and is applicable to different types of carbon fiber / epoxy resin systems. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets.

[0006] To solve the above technical problem, the technical solution adopted by the present invention is:

[0007] A method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets, comprising the following steps:

[0008] Step a, carbon fiber pretreatment: The carbon fiber is surface-modified with polymer molecules to prepare amino-functionalized carbon fiber, so that active groups capable of combining with graphene oxide nanosheets are obtained on its surface;

[0009] Step b, preparation of carbon fiber / graphene oxide nanosheet hybrid material: By adjusting the hybridization ratio of the amino-functionalized carbon fiber obtained by the surface modification treatment in step a and the activated graphene oxide nanosheets, a carbon fiber / graphene oxide nanosheet hybrid material is prepared by reacting at room temperature;

[0010] Step c, preparation of carbon fiber / epoxy resin composites with modulated intercalation interface of graphene oxide nanosheets: The carbon fiber / graphene oxide nanosheet hybrid material prepared in step b is mixed with an epoxy resin matrix in a certain proportion. After removing bubbles by vacuum pumping, it is cured at high temperature in a curing furnace and then naturally cooled to obtain carbon fiber / epoxy resin composites with modulated intercalation interface of graphene oxide nanosheets.

[0011] The method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets according to the present invention, step a includes the following steps:

[0012] Step a1, weigh 5 - 50 g of carbon fiber in a beaker, add 50 mL each of a silver nitrate solution with a molar concentration of 0.01 mol / L and a potassium persulfate solution with a molar concentration of 0.1 mol / L under stirring conditions, place it in a water bath at 70 - 90 °C, and keep reacting for 2 h to generate carboxylic acid groups on the surface of the carbon fiber. Centrifuge 3 times, collect the final precipitate, and dry it at room temperature to obtain carboxylated carbon fiber for later use;

[0013] Step a2, under magnetic stirring conditions, dissolve the carboxylated carbon fiber obtained in step a1 in 100 mL of dimethyl sulfoxide solution, add 5 g of polyetherimide, keep reacting at room temperature for 48 h, then centrifuge 3 times, collect the final precipitate, and dry it at room temperature to obtain amino-functionalized carbon fiber.

[0014] The method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets according to the present invention, step b includes the following steps:

[0015] Step b1: Under the condition of magnetic stirring, 0.1 - 1 g of graphene oxide nanosheets are dissolved in 100 mL of dimethyl sulfoxide solution, and ultrasonic oscillation is carried out at room temperature for 4 h to obtain a uniformly dispersed graphene oxide nanosheet dispersion for later use;

[0016] Step b2: Under the condition of magnetic stirring, 1 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and 0.5 g of N-hydroxysuccinimide are jointly added to the graphene oxide nanosheet dispersion obtained in step b1, and the reaction is maintained at room temperature for 2 h to obtain an activated graphene oxide nanosheet dispersion for later use;

[0017] Step b3: Under the condition of magnetic stirring, the amino-functionalized carbon fiber obtained in step a and the activated graphene oxide nanosheet dispersion obtained in step b2 are mixed in a mass ratio of 1:10 - 60, the reaction is maintained at room temperature for 24 h, centrifuged 3 times, and the final precipitate is collected and dried at room temperature to obtain a carbon fiber / graphene oxide nanosheet hybrid material.

[0018] Furthermore, the mass ratio of the amino-functionalized carbon fiber obtained in step a of the present invention to the activated graphene oxide nanosheet dispersion obtained in step b2 can be 1:10, 1:20, 1:40, or 1:60.

[0019] For the method for preparing a carbon fiber / epoxy resin composite by intercalation interface control of graphene oxide nanosheets according to the present invention, step c includes the following steps:

[0020] Step c1: Epoxy resin E51 and curing agent H256 are mixed in a mass ratio of 32 - 100:1 to form an epoxy resin matrix for bonding, and are mixed with the carbon fiber / graphene oxide nanosheet hybrid material obtained in step b in a mass ratio of 32:68 for later use;

[0021] Step c2: The epoxy resin matrix and carbon fiber / graphene oxide nanosheet hybrid material mixture obtained in step c1 are fed by a vacuum pump to remove air bubbles, and are sent to a preheated mold (mold size 6 mm × 3 mm × 200 mm) in a curing furnace, and molded under a molding temperature of 90 - 150 °C and a molding strength of 10 MPa, with a pressure holding time of 2 - 3 h. After natural cooling at room temperature, a carbon fiber / epoxy resin composite with intercalation interface control of graphene oxide nanosheets is obtained.

[0022] Furthermore, in step c1 of the present invention, the mass of epoxy resin E51 is 1 - 5 g.

[0023] Adopting the technical solution provided by the present invention, compared with the existing well-known technologies, it has the following beneficial effects:

[0024] 1. A method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets, which uses graphene oxide nanosheets as intercalants to modulate the interfacial compatibility between carbon fibers and epoxy resin matrix, effectively improving the mechanical and thermodynamic properties of the composites.

[0025] 2. The method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets according to the present invention has a simple and easy preparation method, is suitable for industrial production, and can be applied to different types of carbon fiber / epoxy resin systems.

[0026] 3. The carbon fiber / epoxy resin composites prepared by the method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets according to the present invention have excellent wear resistance, fatigue resistance, corrosion resistance and impact resistance, and are applicable to multiple fields such as rubber materials, tire manufacturing, aerospace, corrosion-resistant electronic devices, and preparation of special environment sensors. Description of the Drawings

[0027] Figure 1 It is the scanning electron microscope image of the aminated carbon fiber obtained in Example 1;

[0028] Figure 2 It is the atomic force microscope image of the graphene oxide nanosheets in Example 1;

[0029] Figure 3 It is the scanning electron microscope image of the carbon fiber / epoxy resin composites with the intercalation interface of graphene oxide nanosheets modulated obtained in Example 1. Detailed Embodiments

[0030] The present invention will be further described below in conjunction with specific embodiments.

[0031] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments; based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0032] In the present invention, unless otherwise specified, the raw materials used are all commercially available products in the art.

[0033] Example 1

[0034] A method for preparing carbon fiber / epoxy resin composites by modulating the intercalation interface of graphene oxide nanosheets provided in this example includes the following steps:

[0035] Step a, carbon fiber pretreatment: Use polymer molecules to modify the surface of carbon fibers to prepare amino-functionalized carbon fibers, so that active groups capable of combining with graphene oxide nanosheets are obtained on the surface;

[0036] Step b, preparation of carbon fiber / graphene oxide nanosheet hybrid material: By adjusting the hybridization ratio of the amino-functionalized carbon fibers treated by surface modification in step a and the activated graphene oxide nanosheets, react at room temperature to obtain a carbon fiber / graphene oxide nanosheet hybrid material;

[0037] Step c, preparation of graphene oxide nanosheet intercalated interface-regulated carbon fiber / epoxy resin composite: Mix the carbon fiber / graphene oxide nanosheet hybrid material prepared in step b with an epoxy resin matrix in proportion. After removing air bubbles by vacuum pumping, cure at high temperature in a curing furnace, and after natural cooling, obtain a graphene oxide nanosheet intercalated interface-regulated carbon fiber / epoxy resin composite.

[0038] For the method for preparing a carbon fiber / epoxy resin composite by regulating the intercalated interface of graphene oxide nanosheets according to this embodiment, step a includes the following steps:

[0039] Step a1, Weigh 10 g of carbon fibers (Jilin Carbon Co., Ltd., average diameter 7 µm) in a beaker. Under stirring conditions, add 50 mL each of a silver nitrate solution with a molar concentration of 0.01 mol / L and a potassium disulfate solution with a molar concentration of 0.1 mol / L, place it in a water bath at 80 °C, and keep reacting for 2 h to generate carboxylic acid groups on the surface of the carbon fibers. Centrifuge (centrifugation speed is 10,000 rpm, centrifugation time is 15 min) 3 times, collect the final precipitate, and dry it at room temperature to obtain carboxylated carbon fibers for use;

[0040] Step a2, Under magnetic stirring (stirring speed is 500 rpm), dissolve the carboxylated carbon fibers obtained in step a1 in 100 mL of dimethyl sulfoxide solution, add 5 g of polyetherimide, keep reacting at room temperature for 48 h, then centrifuge (centrifugation speed is 10,000 rpm, centrifugation time is 15 min) 3 times, collect the final precipitate, and dry it at room temperature to obtain amino-functionalized carbon fibers, as Figure 1 shown.

[0041] For the method for preparing a carbon fiber / epoxy resin composite by regulating the intercalated interface of graphene oxide nanosheets according to this embodiment, step b includes the following steps:

[0042] Step b1, Under magnetic stirring (stirring speed is 500 rpm), add graphene oxide nanosheets (Hangzhou Gaoxi Technology Co., Ltd., thickness 1 nm, size 1 - 5 µm, as Figure 21 g was dissolved in 100 mL of dimethyl sulfoxide solution and ultrasonically oscillated at room temperature for 4 h to obtain a uniformly dispersed graphene oxide nanosheet dispersion for later use;

[0043] Step b2: Under the condition of magnetic stirring (stirring speed: 500 rpm), 1 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and 0.5 g of N-hydroxysuccinimide were jointly added to the graphene oxide nanosheet dispersion obtained in step b1, and the reaction was maintained at room temperature for 2 h to obtain an activated graphene oxide nanosheet dispersion for later use;

[0044] Step b3: Under the condition of magnetic stirring (stirring speed: 500 rpm), the amino-functionalized carbon fiber obtained in step a was mixed with the activated graphene oxide nanosheet dispersion obtained in step b2 at a mass ratio of 1:10, and the reaction was maintained at room temperature for 24 h. Then, centrifugation was performed 3 times (centrifugation speed: 10,000 rpm, centrifugation time: 15 min), and the final precipitate was collected and dried at room temperature to obtain a carbon fiber / graphene oxide nanosheet hybrid material.

[0045] For the method for preparing a carbon fiber / epoxy resin composite by modulating the intercalation interface of graphene oxide nanosheets according to this example, step c includes the following steps:

[0046] Step c1: 4.7 g of epoxy resin E51 (Shanghai Macklin Biochemical Co., Ltd.) was mixed with a curing agent H256 at a mass ratio of 100:1 to form an epoxy resin matrix for bonding, and then mixed with the carbon fiber / graphene oxide nanosheet hybrid material obtained in step b at a mass ratio of 32:68 for later use;

[0047] Step c2: The epoxy resin matrix and the carbon fiber / graphene oxide nanosheet hybrid material mixture obtained in step c1 were fed through a vacuum pump to remove air bubbles, and then sent to a preheated mold (mold size: 6 mm × 3 mm × 200 mm) in a curing furnace. Molding was carried out at a molding temperature of 120 °C and a molding pressure of 10 MPa, and the pressure holding time was 3 h. After natural cooling at room temperature, a carbon fiber / epoxy resin composite with modulated intercalation interface of graphene oxide nanosheets was obtained, as Figure 3 shown.

[0048] Example 2.

[0049] The method for preparing a carbon fiber / epoxy resin composite by modulating the intercalation interface of graphene oxide nanosheets provided in this example includes the following steps:

[0050] Step a: Carbon fiber pretreatment: The carbon fiber was surface-modified with polymer molecules to prepare amino-functionalized carbon fiber, so that active groups capable of combining with graphene oxide nanosheets were obtained on its surface;

[0051] Step b: Preparation of carbon fiber / graphene oxide nanosheet hybrid material: By adjusting the hybridization ratio of the surface-modified amino-functionalized carbon fibers and activated graphene oxide nanosheets in step a, the carbon fiber / graphene oxide nanosheet hybrid material is prepared by reacting at room temperature;

[0052] Step c: Preparation of graphene oxide nanosheet intercalated interface-regulated carbon fiber / epoxy resin composite: The carbon fiber / graphene oxide nanosheet hybrid material prepared in step b is mixed with an epoxy resin matrix in a certain proportion. After removing air bubbles by vacuum pumping, it is cured at a high temperature in a curing furnace and then cooled naturally to obtain the graphene oxide nanosheet intercalated interface-regulated carbon fiber / epoxy resin composite.

[0053] A method for preparing a carbon fiber / epoxy resin composite by regulating the intercalated interface of graphene oxide nanosheets according to this embodiment, step a includes the following steps:

[0054] Step a1: Weigh 10 g of carbon fibers (Jilin Carbon Co., Ltd., average diameter 7 µm) in a beaker. Under stirring conditions, add 50 mL each of a silver nitrate solution with a molar concentration of 0.01 mol / L and a potassium persulfate solution with a molar concentration of 0.1 mol / L, place it in a water bath at 80 °C, and keep reacting for 2 h to generate carboxylic acid groups on the surface of the carbon fibers. Centrifuge (centrifugation speed: 10000 rpm, centrifugation time: 15 min) 3 times, collect the final precipitate, and dry it at room temperature to obtain carboxylated carbon fibers for use;

[0055] Step a2: Under magnetic stirring (stirring speed: 500 rpm), dissolve the carboxylated carbon fibers obtained in step a1 in 100 mL of dimethyl sulfoxide solution, add 5 g of polyetherimide, keep reacting at room temperature for 48 h, then centrifuge (centrifugation speed: 10000 rpm, centrifugation time: 15 min) 3 times, collect the final precipitate, and dry it at room temperature to obtain amino-functionalized carbon fibers.

[0056] A method for preparing a carbon fiber / epoxy resin composite by regulating the intercalated interface of graphene oxide nanosheets according to this embodiment, step b includes the following steps:

[0057] Step b1: Under magnetic stirring (stirring speed: 500 rpm), dissolve 0.5 g of graphene oxide nanosheets (Hangzhou Graphene Technology Co., Ltd., thickness 1 nm, size 1 - 5 µm) in 100 mL of dimethyl sulfoxide solution, and ultrasonically oscillate at room temperature for 4 h to obtain a uniformly dispersed graphene oxide nanosheet dispersion for use;

[0058] Step b2: Under the condition of magnetic stirring (stirring speed is 500 rpm), 1 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and 0.5 g of N-hydroxysuccinimide are jointly added to the graphene oxide nanosheet dispersion obtained in step b1, and the reaction is maintained at room temperature for 2 h to obtain an activated graphene oxide nanosheet dispersion for later use;

[0059] Step b3: Under the condition of magnetic stirring (stirring speed is 500 rpm), the amino-functionalized carbon fiber obtained in step a and the activated graphene oxide nanosheet dispersion obtained in step b2 are mixed at a mass ratio of 1:20, and the reaction is maintained at room temperature for 24 h, centrifuged (centrifugation speed is 10000 rpm, centrifugation time is 15 min) 3 times, the final precipitate is collected and dried at room temperature to obtain a carbon fiber / graphene oxide nanosheet hybrid material.

[0060] A method for preparing a carbon fiber / epoxy resin composite material by controlling the intercalation interface of graphene oxide nanosheets according to this embodiment, step c includes the following steps:

[0061] Step c1: 4 g of epoxy resin E51 (Shanghai Macklin Biochemical Co., Ltd.) and the curing agent H256 are mixed at a mass ratio of 80:1 to form an epoxy resin matrix for bonding, and are mixed with the carbon fiber / graphene oxide nanosheet hybrid material obtained in step b at a mass ratio of 32:68 for later use;

[0062] Step c2: The epoxy resin matrix and the carbon fiber / graphene oxide nanosheet hybrid material mixture obtained in step c1 are fed by a vacuum pump to remove air bubbles, and are sent to a preheated mold (mold size 6 mm×3 mm×200 mm) in a curing furnace, and are molded under a molding temperature of 120 °C and a molding strength of 10 MPa, and the pressure holding time is 3 h. After natural cooling at room temperature, a carbon fiber / epoxy resin composite material with regulated intercalation interface of graphene oxide nanosheets is obtained.

[0063] Example 3.

[0064] A method for preparing a carbon fiber / epoxy resin composite material by controlling the intercalation interface of graphene oxide nanosheets provided in this embodiment includes the following steps:

[0065] Step a: Carbon fiber pretreatment: The carbon fiber is surface-modified with polymer molecules to prepare amino-functionalized carbon fiber, so that active groups capable of combining with graphene oxide nanosheets are obtained on its surface;

[0066] Step b: Preparation of carbon fiber / graphene oxide nanosheet hybrid material: By adjusting the hybridization ratio of the amino-functionalized carbon fiber and the activated graphene oxide nanosheets treated by surface modification in step a, a carbon fiber / graphene oxide nanosheet hybrid material is prepared by reacting at room temperature;

[0067] Step c: Preparation of graphene oxide nanosheet intercalated interface regulated carbon fiber / epoxy resin composite: The carbon fiber / graphene oxide nanosheet hybrid material prepared in step b is mixed with an epoxy resin matrix in a certain proportion. After removing air bubbles by vacuum pumping, it is cured at a high temperature in a curing furnace and then cooled naturally to obtain the graphene oxide nanosheet intercalated interface regulated carbon fiber / epoxy resin composite.

[0068] For the method for preparing a carbon fiber / epoxy resin composite by using graphene oxide nanosheet intercalated interface regulation according to this embodiment, step a includes the following steps:

[0069] Step a1: Weigh 10 g of carbon fibers (Jilin Carbon Co., Ltd., average diameter 7 µm) in a beaker. Under stirring conditions, add 50 mL each of a silver nitrate solution with a molar concentration of 0.01 mol / L and a potassium persulfate solution with a molar concentration of 0.1 mol / L, place it in a water bath at 80 °C, and keep reacting for 2 h to generate carboxylic acid groups on the surface of the carbon fibers. Centrifuge (centrifugation speed: 10000 rpm, centrifugation time: 15 min) 3 times, collect the final precipitate, and dry it at room temperature to obtain carboxylated carbon fibers for use.

[0070] Step a2: Under magnetic stirring (stirring speed: 500 rpm), dissolve the carboxylated carbon fibers obtained in step a1 in 100 mL of dimethyl sulfoxide solution, add 5 g of polyetherimide, keep reacting at room temperature for 48 h, then centrifuge (centrifugation speed: 10000 rpm, centrifugation time: 15 min) 3 times, collect the final precipitate, and dry it at room temperature to obtain amino-functionalized carbon fibers.

[0071] For the method for preparing a carbon fiber / epoxy resin composite by using graphene oxide nanosheet intercalated interface regulation according to this embodiment, step b includes the following steps:

[0072] Step b1: Under magnetic stirring (stirring speed: 500 rpm), dissolve 0.17 g of graphene oxide nanosheets (Hangzhou Graphene Technology Co., Ltd., thickness 1 nm, size 1 - 5 µm) in 100 mL of dimethyl sulfoxide solution, and ultrasonically oscillate at room temperature for 4 h to obtain a uniformly dispersed graphene oxide nanosheet dispersion for use.

[0073] Step b2: Under magnetic stirring (stirring speed: 500 rpm), add 1 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and 0.5 g of N-hydroxysuccinimide to the graphene oxide nanosheet dispersion obtained in step b1, and keep reacting at room temperature for 2 h to obtain an activated graphene oxide nanosheet dispersion for use.

[0074] Step b3: Under the condition of magnetic stirring (stirring speed: 500 rpm), mix the amino-functionalized carbon fiber obtained in step a with the activated graphene oxide nanosheet dispersion obtained in step b2 at a mass ratio of 1:40, keep the reaction at room temperature for 24 h, centrifuge 3 times (centrifugation speed: 10,000 rpm, centrifugation time: 15 min), collect the final precipitate, and dry it at room temperature to obtain the carbon fiber / graphene oxide nanosheet hybrid material.

[0075] In the method for preparing a carbon fiber / epoxy resin composite by regulating the intercalation interface of graphene oxide nanosheets according to this embodiment, step c includes the following steps:

[0076] Step c1: Mix 4.7 g of epoxy resin E51 (Shanghai Macklin Biochemical Co., Ltd.) with a curing agent H256 at a mass ratio of 100:1 to form an epoxy resin matrix for bonding, and mix it with the carbon fiber / graphene oxide nanosheet hybrid material obtained in step b at a mass ratio of 32:68 for standby.

[0077] Step c2: Remove the bubbles from the mixture of the epoxy resin matrix and the carbon fiber / graphene oxide nanosheet hybrid material obtained in step c1 by vacuum pumping, send it to a preheated mold (mold size: 6 mm×3 mm×200 mm) in a curing furnace, and carry out molding under a molding temperature of 120°C and a molding pressure of 10 MPa for a holding time of 3 h. After natural cooling at room temperature, obtain the carbon fiber / epoxy resin composite with regulated intercalation interface of graphene oxide nanosheets.

[0078] Physical and chemical data analysis of the carbon fiber / epoxy resin composite with regulated intercalation interface of graphene oxide nanosheets in the above embodiment.

[0079] Main experimental equipment: FM-Nanoview6800 atomic force microscope (Suzhou Feishiman Precision Instruments Co., Ltd.), Regulus 8100 scanning electron microscope (Hitachi, Japan), FA620 interface detector (Japan), GT-7000-A2X electronic universal testing machine (Taiwan, China), 9250HV drop hammer impact tester (Instron Corporation, USA).

[0080] Comparison of mechanical properties:

[0081] Item Example 1 Example 2 Example 3 Contact Angle (degree) 41.3 49.4 51.3 Surface Energy (mN / m) 63.2 56.5 51.2 Interfacial Shear Strength (MPa) 74.7 68.8 67.6 Flexural Modulus (GPa) 60.2 61.3 54.1 Stress (MPa) 810.3 692.0 710.5

[0082] As described above, these are only the preferred embodiments of the present invention. The foregoing embodiments are only used to illustrate the technical solutions of the present invention and do not impose any formal restrictions on the present invention; although the present invention has been described in detail with reference to the foregoing embodiments, any person of ordinary skill in the art can still modify the technical solutions disclosed in the foregoing embodiments or perform equivalent replacements for some of the technical features without departing from the principles and spirit of the present invention; however, any simple modifications, equivalent changes and decorations made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solutions of the present invention still fall within the scope of the technical solutions of the present invention; the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a carbon fiber / epoxy resin composite material by regulating the intercalation interface of graphene oxide nanosheets, characterized in that: The steps include: Step a, carbon fiber pretreatment: using polymer molecules to modify the surface of carbon fiber to prepare amino carbon fiber, so that the surface of the carbon fiber obtains active groups that can combine with graphene oxide nanosheets; Step b, preparation of carbon fiber / graphene oxide nanosheet hybrid material: adjusting the hybrid ratio of the amino carbon fiber surface-modified in step a and the activated graphene oxide nanosheet, and reacting at room temperature to obtain the carbon fiber / graphene oxide nanosheet hybrid material; Step c, preparation of carbon fiber / epoxy resin composite material with graphene oxide nanosheet intercalation interface regulation: the carbon fiber / graphene oxide nanosheet hybrid material prepared in step b is mixed with an epoxy resin matrix in proportion, the material is fed by a vacuum pump to remove bubbles, and then cured at high temperature in a curing furnace. After natural cooling, a carbon fiber / epoxy resin composite material with graphene oxide nanosheet intercalation interface regulation is obtained.

2. The method for preparing a carbon fiber / epoxy resin composite material by controlling the intercalation interface of graphene oxide nanosheets according to claim 1, characterized in that: Step a includes the following steps: Step a1, weigh 5-50g of carbon fiber in a beaker, add 50mL of a silver nitrate solution with a molar concentration of 0.01mol / L and a potassium disulfate solution with a molar concentration of 0.1mol / L under stirring, place in a water bath at 70-90°C, keep reacting for 2h to generate carboxylic acid groups on the surface of the carbon fiber, centrifuge 3 times, collect the final precipitate, dry at room temperature, and obtain carboxylated carbon fiber for standby use; Step a2: Under magnetic stirring, dissolve the carboxylated carbon fiber obtained in step a1 in 100 mL of dimethyl sulfoxide solution, add 5 g of polyetherimide, keep the reaction at room temperature for 48 hours, centrifuge 3 times, collect the final precipitate, and dry it at room temperature to obtain amino carbon fiber.

3. The method for preparing a carbon fiber / epoxy resin composite material by controlling the intercalation interface of graphene oxide nanosheets according to claim 1, characterized in that: Step b comprises the following steps: Step b1, under the condition of magnetic stirring, dissolve 0.1-1g of graphene oxide nanosheets in 100mL of dimethyl sulfoxide solution, and ultrasonically oscillate at room temperature for 4h to obtain a uniformly dispersed graphene oxide nanosheet dispersion for standby use; Step b2, under magnetic stirring, add 1 g of 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and 0.5 g of N-hydroxysuccinimide to the graphene oxide nanosheet dispersion obtained in step b1, and keep the reaction at room temperature for 2 hours to obtain an activated graphene oxide nanosheet dispersion for standby use; Step b3, under the condition of magnetic stirring, the amino carbon fiber obtained in step a and the activated graphene oxide nanosheet dispersion obtained in step b2 are mixed in a mass ratio of 1:10-60, the reaction is maintained at room temperature for 24 hours, centrifuged 3 times, the final precipitate is collected, and dried at room temperature to obtain a carbon fiber / graphene oxide nanosheet hybrid material.

4. The method for preparing a carbon fiber / epoxy resin composite material by controlling the intercalation interface of graphene oxide nanosheets according to claim 3, characterized in that: The mass ratio of the amination carbon fiber obtained in step a described in step b3 to the activated graphene oxide nanosheet dispersion obtained in step b2 is 1:10, 1:20, 1:40, or 1:

60.

5. The method for preparing a carbon fiber / epoxy resin composite material by controlling the intercalation interface of graphene oxide nanosheets according to claim 1, characterized in that: Step c comprises the following steps: Step c1, mixing epoxy resin E51 and curing agent H256 in a mass ratio of 32-100:1 to form an epoxy resin matrix for bonding, and mixing it with the carbon fiber / graphene oxide nanosheet hybrid material obtained in step b in a mass ratio of 32:68 for standby use; Step c2, the epoxy resin matrix and the carbon fiber / graphene oxide nanosheet hybrid material mixture obtained in step c1 are sent through a vacuum pump to remove bubbles, and sent to a preheated mold (mold size 6 mm×3 mm×200 mm) in a curing furnace, and molded at a molding temperature of 90-150°C and a molding strength of 10 MPa. The holding time is 2-3 hours, and after natural cooling at room temperature, a carbon fiber / epoxy resin composite material with graphene oxide nanosheet intercalation interface regulation is obtained.

6. The method for preparing a carbon fiber / epoxy resin composite material by controlling the intercalation interface of graphene oxide nanosheets according to claim 5, characterized in that: The mass of the epoxy resin E51 described in step c1 is 1-5g.

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