CN112111131A - Carbon fiber-epoxy resin composite material with improved MXene and improving method - Google Patents

Carbon fiber-epoxy resin composite material with improved MXene and improving method Download PDF

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CN112111131A
CN112111131A CN202011022148.7A CN202011022148A CN112111131A CN 112111131 A CN112111131 A CN 112111131A CN 202011022148 A CN202011022148 A CN 202011022148A CN 112111131 A CN112111131 A CN 112111131A
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mxene
carbon fiber
composite material
epoxy resin
resin composite
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CN112111131B (en
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应国兵
刘璐
孙铖
胡聪
张晨
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Hohai University HHU
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/02Ingredients treated with inorganic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/42Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • C08G59/4215Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/62Alcohols or phenols
    • C08G59/621Phenols
    • C08G59/623Aminophenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general

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  • Reinforced Plastic Materials (AREA)
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Abstract

The invention relates to a method for improving a carbon fiber-epoxy resin composite material interface by MXene, which comprises the following steps: preparing MXene colloidal solution, preparing MXene functionalized carbon fiber composite material and preparing MXene functionalized carbon fiber-epoxy resin composite material, wherein the strong polarity of the MXene surface is favorable for the combination with the carboxyl on the surface of the carbon fiber treated by acid and the bonding with a resin matrix, wherein Ti is contained in the composite material3C2TxThe carbon fibers and epoxy resin may be "bridged".

Description

Carbon fiber-epoxy resin composite material with improved MXene and improving method
Technical Field
The invention relates to a composite material, in particular to a carbon fiber-epoxy resin composite material with improved MXene and an improving method.
Background
Carbon fibers have excellent properties such as high strength, high fatigue resistance, high corrosion resistance, and light weight, and thus are ideal structural materials for polymer-based composite materials. In general, the mechanical properties of composite materials are affected not only by the inherent properties of carbon fibers and epoxy resins, but also by their interfacial bonding properties. However, the non-polarity and lack of chemically active groups on the surface of carbon fibers limits their natural wettability and adsorption to most polymers. Therefore, improving the interfacial properties of carbon fibers has become an important research hotspot in polymer science. In the past few years, carbon fiber multi-scale reinforcement has been increasingly explored by various methods, such as bridging agent molecular grafting and incorporation of various nanomaterials, such as carbon nanotubes, graphene, and graphene oxide. However, these preparation routes have disadvantages in large scale preparation, high raw material costs and complex processing.
Disclosure of Invention
The invention aims to provide a novel improvement method for improving the wettability of fibers and improving the surface free energy of the fibers. In order to achieve the purpose, the carbon fiber-epoxy resin composite material improved by MXene is adopted, and the MXene has a large number of oxygen-containing functional groups on the surface, has excellent wettability with epoxy resin and is an excellent material for modifying the epoxy resin. The strong polarity of MXene surface facilitates the bonding with the carboxyl groups on the surface of the acid-treated carbon fiber and the bonding with the resin matrix, wherein Ti3C2TxThe carbon fibers and epoxy resin may be "bridged".
The technical scheme adopted by the invention is as follows: the method for improving the interface of the carbon fiber-epoxy resin composite material by MXene comprises the following steps
Preparation of MXene colloidal solution
1) Sintering M, Al and C powder to form a ceramic block material, and grinding the prepared ceramic block material to obtain ceramic powder;
2) placing the ceramic powder material in a mixed solution of hydrochloric acid and lithium fluoride or hydrofluoric acid for corrosion, washing a corrosion product by clear water for multiple times, preparing a suspension by using deionized water, and performing ultrasonic layering and centrifugation to obtain an MXene colloidal solution;
preparation of MXene functionalized carbon fiber composite material
1) Removing the surface sizing agent of the carbon fiber by using acetone, acidifying the carbon fiber in concentrated nitric acid at the temperature of 60-100 ℃ for 1-6 hours, and cleaning the carbon fiber to be neutral;
2) soaking the acidified carbon fiber in MXene colloidal solution for 5-60 min, and taking out;
3) washing off redundant MXene on the surface of the fiber by using water, and carrying out vacuum drying on the washed fiber to obtain an MXene functionalized carbon fiber composite material;
preparation of MXene functionalized carbon fiber-epoxy resin composite material
1) Uniformly mixing methyl tetrahydrophthalic anhydride and E51 resin to obtain a mixed solution;
2) and (3) placing the mixed solution on the surface of the fiber prepared in the step (3), curing for 1-6 h at 70-120 ℃, heating to 120-160 ℃, curing for 2-10 h, and cooling with a furnace to obtain the fiber.
Further, the step 2) of preparing the MXene colloidal solution is specifically (1) adding 1g of prepared ceramic powder into 5-25 ml of a mixed solution of 9-12 mol/ml hydrochloric acid and 0.2-2 g of lithium fluoride, or adding 5-25 ml of an aqueous solution with 10-70 wt.% HF content, adding a magnetic rotor, and stirring for 12-96 hours in an oil bath environment at 20-70 ℃ to obtain a suspension;
(2) washing the corroded suspension of the mixture with 5-100 ml of deionized water, centrifuging, pouring out the supernatant, and repeating for multiple times until the pH value of the supernatant is more than or equal to 6;
(3) after the pH value of the supernatant is more than or equal to 6, continuously using 5-100 ml of deionized water for washing and centrifuging, pouring out the supernatant, and repeating for 3-5 times;
(4) and adding 5-40 ml of deionized water into the mixture finally cleaned, performing ultrasonic layering treatment under the protection of argon atmosphere, keeping the temperature below 35 ℃ in the ultrasonic process, performing centrifugal treatment on the mixed solution after ultrasonic treatment, and taking the upper layer solution, namely the single-layer MXene colloidal solution.
Further, the concentration of the MXene colloidal solution is determined by using a suction filtration method.
Further, the mixed solution in the MXene functionalized carbon fiber-epoxy resin composite material preparation step also comprises tris- (dimethylaminomethyl) phenol, and the mixed solution is obtained by uniformly mixing the E51 resin, the methyl tetrahydrophthalic anhydride and the tris- (dimethylaminomethyl) phenol and performing vacuum defoaming for 10-60 min. Tris- (dimethylaminomethyl) phenol is used as an accelerator for accelerating curing, and the addition amount of tris- (dimethylaminomethyl) phenol is 0.1-0.5%, preferably 0.3%.
Furthermore, the mass ratio of the selected E51 type resin to the methyl tetrahydrophthalic anhydride is 100: 70-100, and the preferred ratio is 100: 85.
Further, the ceramic powder is Mn+1AlCnThe ceramic powder is prepared by mixing a ceramic powder,nand =1,2,3, M is a transition metal element.
Further, said Mn+1AlCnThe preparation steps of the ceramic powder are as follows: mixing M, Al and C powders in a molar ratio of (A), (B), (Cn+1):1.2:nn=1,2, 3) mixing uniformly, preparing high-purity ternary lamellar M through pressureless sintering at 1000-1800 DEG Cn+1AlCnn=1,2, 3) ceramic block material, M to be producedn+1AlCnGrinding the ceramic material to obtain Mn+1AlCnCeramic powder.
Further, said Mn+1AlCnM in the ceramic powder is Ti, Nb, V, Cr or Ta.
Furthermore, the fineness of the ceramic powder is 100-1200 meshes.
Furthermore, the addition amount of MXene in the MXene functionalized carbon fiber composite material is 0-50% by mass.
Further, the carbon fiber is acidified in concentrated nitric acid for 1-6 hours at the temperature of 60-100 ℃, and the optimal parameter is 4 hours at the temperature of 80 ℃.
Further, soaking the carbon fiber subjected to nitric acid acidification in the MXene colloidal solution for 5-60 min, preferably for 30 min.
The invention also provides the carbon fiber-epoxy resin composite material prepared by the method for improving the interface of the carbon fiber-epoxy resin composite material by MXene.
The beneficial effects produced by the invention comprise: the method for improving the carbon fiber-epoxy resin interface by MXene provided by the invention has the advantages of simple process and low cost, and can change the surface appearance of the carbon fiber, increase the number of functional groups on the surface of the carbon fiber and increase the wettability of the carbon fiber and the epoxy resin. The surface free energy of the functionalized fiber can be improved by more than 134 percent, and the interfacial shear force with the epoxy resin can be increased by more than 186 percent.
Specifically, the present invention has the following outstanding advantages over the prior art:
(1) the invention effectively changes the surface appearance of the carbon fiber, so that the surface is rougher; meanwhile, a large number of oxygen-containing functional groups on the surface of MXene are utilized, so that the surface polarity of the carbon fiber is increased, the wettability of the fiber is improved, and the surface free energy of the fiber is increased.
(2) The method has easily controlled conditions, can accurately quantify the addition amount of single-layer MXene, and can prepare the composite materials with different MXene addition ratios.
(3) The carbon fiber-epoxy resin composite material prepared by the method has the advantages of obviously improved interface strength and excellent mechanical property.
Drawings
Fig. 1(a) and (b) are photographs of an MXene functionalized carbon fiber composite material obtained in embodiment 1 of the method of the present invention.
Fig. 2 shows the wetting angle and the surface free energy of the MXene functionalized carbon fiber composite material prepared by the embodiment 2 of the method of the present invention.
FIG. 3 shows the improvement of the shear properties of the carbon fiber-epoxy interface in example 3 of the process of the present invention.
Detailed Description
The present invention is explained in further detail below with reference to the drawings and the specific embodiments, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Example 1
The method for improving the interface of the carbon fiber-epoxy resin composite material by MXene comprises the following steps:
firstly, preparing single-layer MXene:
(1) uniformly mixing Ti, Al and C powder according to the molar ratio of 3:1.2:2, and preparing high-purity ternary layered Ti at 1350 ℃ by a pressureless sintering process3AlC2Ceramic bulk material, Ti to be produced3AlC2Drilling powder by a drilling machine to obtain Ti3AlC2Ceramic powder. Prepared Ti3AlC2Sieving the ceramic powder with a 325-mesh sieve;
(2) 1g of prepared Ti3AlC2Adding ceramic powder into 20ml of mixed solution of 9mol/ml hydrochloric acid and 1.6g of lithium fluoride, adding a magnetic rotor, stirring for 24 hours in an oil bath environment at 35 ℃, and removing Ti3AlC2An Al atomic layer;
(3) washing the corroded suspension of the mixture with 40ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6;
(4) after the pH value of the supernatant is more than or equal to 6, continuously using 40ml of deionized water for washing and centrifuging, pouring out the supernatant, and repeating for 3-5 times;
(5) and finally, cleaning the finished mixture, adding 20ml of deionized water, and performing ultrasonic layering treatment under the protection of argon atmosphere. The temperature was kept below 35 ℃ during sonication. And centrifuging the mixed solution after ultrasonic treatment to obtain a supernatant solution which is a monolayer MXene colloidal solution. The concentration of MXene in the colloidal solution was determined using suction filtration.
Preparation of MXene functionalized carbon fiber composite material
(1) Removing the surface sizing agent of the carbon fiber by using acetone;
(2) putting the cleaned carbon fiber in concentrated nitric acid, and acidifying for 4 hours at the temperature of 80 ℃;
(3) washing the acidified carbon fiber with deionized water until the pH value is more than or equal to 6;
(4) and soaking the acidified carbon fiber in MXene colloidal solution for 15min, taking out, washing with deionized water, and vacuum drying for storage.
Thirdly, preparing the MXene functionalized carbon fiber-epoxy resin composite material:
(1) calculating the mass of the E51 resin and the methyl tetrahydrophthalic anhydride according to the ratio of 100 parts of the E51 resin to 85 parts of the methyl tetrahydrophthalic anhydride;
(2) in order to accelerate the curing speed, 0.3% by mass of tris- (dimethylaminomethyl) phenol;
(3) uniformly mixing E51 resin, methyl tetrahydrophthalic anhydride and tris- (dimethylaminomethyl) phenol, and defoaming for 30min in vacuum;
(4) and (3) dropwise adding the mixed solution on the surface of the fiber after vacuum treatment, firstly curing at 90 ℃ for 1h, then heating to 110 ℃ for curing for 4h, and cooling along with the furnace to obtain the MXene functionalized carbon fiber-epoxy resin composite material.
Example 2
The preparation method of the epoxy resin/MXene composite material comprises the following steps:
firstly, preparing single-layer MXene:
(1) uniformly mixing Ti, Al and C powder according to the molar ratio of 3:1.2:2, and preparing high-purity ternary layered Ti at 1400 ℃ by a pressureless sintering process3AlC2Ceramic bulk material, Ti to be produced3AlC2Drilling powder by a drilling machine to obtain Ti3AlC2Ceramic powder. Prepared Ti3AlC2Sieving the ceramic powder with a 325-mesh sieve;
(2) 1g of prepared Ti3AlC2Adding ceramic powder into 10ml of mixed solution of hydrochloric acid with the concentration of 12mol/ml and 1g of lithium fluoride, adding a magnetic rotor, stirring for 24 hours in an oil bath environment at 38 ℃, and removing Ti3AlC2An Al atomic layer;
(3) washing the corroded suspension of the mixture with 50ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6.2;
(4) after the pH value of the supernatant is more than or equal to 6.2, continuously using 50ml of deionized water for washing and centrifuging, pouring out the supernatant, and repeating for 3-5 times;
(5) and finally, cleaning the finished mixture, adding 50ml of deionized water, and performing ultrasonic layering treatment under the protection of argon atmosphere. The temperature was kept below 30 ℃ during sonication. And centrifuging the mixed solution after ultrasonic treatment to obtain a supernatant solution which is a monolayer MXene colloidal solution. The concentration of MXene in the colloidal solution was determined using suction filtration.
Preparation of MXene functionalized carbon fiber composite material
(1) Removing the surface sizing agent of the carbon fiber by using acetone;
(2) putting the cleaned carbon fiber into concentrated nitric acid, and acidifying for 2 hours at the temperature of 100 ℃;
(3) washing the acidified carbon fiber with deionized water until the pH value is more than or equal to 6;
(4) and soaking the acidified carbon fiber in MXene colloidal solution for 60min, taking out, washing with deionized water, and vacuum drying for storage.
Thirdly, preparing the MXene functionalized carbon fiber-epoxy resin composite material:
(1) calculating the mass of the E51 resin and the methyl tetrahydrophthalic anhydride according to the ratio of 100 parts of the E51 resin to 90 parts of the methyl tetrahydrophthalic anhydride;
(2) in order to accelerate the curing speed, 0.3% by mass of tris- (dimethylaminomethyl) phenol;
(3) uniformly mixing E51 resin, methyl tetrahydrophthalic anhydride and tris- (dimethylaminomethyl) phenol, and defoaming in vacuum for 60 min;
(4) and (3) dropwise adding the mixed solution on the surface of the fiber after vacuum treatment, curing for 2h at 100 ℃, heating to 130 ℃, curing for 5h, and cooling along with the furnace to obtain the MXene functionalized carbon fiber-epoxy resin composite material.
Example 3
The method for improving the interface of the carbon fiber-epoxy resin composite material by MXene comprises the following steps:
firstly, preparing single-layer MXene:
(1) uniformly mixing Ti, Al and C powder according to the molar ratio of 3:1.2:2, and preparing high-purity ternary layered Ti at 1450 ℃ by a pressureless sintering process3AlC2Ceramic bulk material, Ti to be produced3AlC2Drilling powder by a drilling machine to obtain Ti3AlC2Ceramic powder. Prepared Ti3AlC2Sieving the ceramic powder with a 325-mesh sieve;
(2) 1g of prepared Ti3AlC2Adding ceramic powder into 15ml of mixed solution of hydrochloric acid with the concentration of 10mol/ml and 1.4g of lithium fluoride, adding a magnetic rotor, stirring for 24 hours in an oil bath environment at 35 ℃, and removing Ti3AlC2An Al atomic layer;
(3) washing the corroded suspension of the mixture with 40ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6.5;
(4) after the pH value of the supernatant is more than or equal to 6.5, continuously using 40ml of deionized water for washing and centrifuging, pouring out the supernatant, and repeating for 5-8 times;
(5) and finally, cleaning the finished mixture, adding 20ml of deionized water, and performing ultrasonic layering treatment under the protection of argon atmosphere. The temperature was kept below 35 ℃ during sonication. And centrifuging the mixed solution after ultrasonic treatment to obtain a supernatant solution which is a monolayer MXene colloidal solution. The concentration of MXene in the colloidal solution was determined using suction filtration.
Preparation of MXene functionalized carbon fiber composite material
(1) Removing the surface sizing agent of the carbon fiber by using acetone;
(2) putting the cleaned carbon fiber in concentrated nitric acid, and acidifying for 8 hours at the temperature of 85 ℃;
(3) washing the acidified carbon fiber with deionized water until the pH value is more than or equal to 6.5;
(4) and soaking the acidified carbon fiber in MXene colloidal solution for 30min, taking out, washing with deionized water, and vacuum drying for storage.
Thirdly, preparing the MXene functionalized carbon fiber-epoxy resin composite material:
(1) calculating the mass of the E51 resin and the methyl tetrahydrophthalic anhydride according to the ratio of 100 parts of the E51 resin to 85 parts of the methyl tetrahydrophthalic anhydride;
(2) in order to accelerate the curing speed, 0.5% by mass of tris- (dimethylaminomethyl) phenol;
(3) uniformly mixing E51 resin, methyl tetrahydrophthalic anhydride and tris- (dimethylaminomethyl) phenol, and defoaming for 30min in vacuum;
(4) and (3) dropwise adding the mixed solution on the surface of the fiber after vacuum treatment, curing for 2h at 90 ℃, heating to 110 ℃, curing for 4h, and cooling along with the furnace to obtain the MXene functionalized carbon fiber-epoxy resin composite material.
Fig. 1 is a photograph of the MXene functionalized carbon fiber composite material prepared in embodiment 1 of the method of the present invention, and it can be seen that the carbon fiber in the method of the present invention obtains good MXene functionalization, and MXene has an obvious grafting characteristic.
Fig. 2(a) and (b) show the wetting angle and the surface free energy of the MXene functionalized carbon fiber composite material prepared in embodiment 1 of the method of the present invention, respectively, and it can be seen from the figure that the surface MXene functionalization of the carbon fiber in the method of the present invention can significantly change the surface wetting angle and the surface free energy of the carbon fiber, which is the key to influence the characteristics of the carbon fiber as a reinforcement.
Fig. 3 shows that the embodiment 1 of the method improves the shear property of the carbon fiber-epoxy resin interface, and it can be clearly seen that the MXene functionalized carbon fiber composite material prepared by the method has obviously different shear properties at the carbon fiber-epoxy resin interface, and the higher the shear property is, the better the performance of the MXene functionalized carbon fiber composite material will be. The abscissa content in the figure is the content relative to the base material.
The wetting angle, surface free energy and shear performance of the functionalized carbon fiber composite materials of example 2 and example 3 are similar to the detection data in example 1.
In the description of the present application, it is to be understood that the terms "central," "longitudinal," "lateral," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings for the convenience of description and simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be considered limiting of the claimed invention.
The above description is only a preferred embodiment of the present invention, and the present invention is not limited to the content of the embodiment. It will be apparent to those skilled in the art that various changes and modifications can be made within the technical scope of the present invention, and any changes and modifications made are within the protective scope of the present invention.

Claims (10)

1. A method for improving the interface of a carbon fiber-epoxy resin composite material by MXene is characterized by comprising the following steps: comprises the following steps
Preparation of MXene colloidal solution
1) Sintering M, Al and C powder to form a ceramic block material, and grinding the prepared ceramic block material to obtain ceramic powder;
2) placing the ceramic powder material in a mixed solution of hydrochloric acid and lithium fluoride or hydrofluoric acid for corrosion, washing a corrosion product by clear water for multiple times, preparing a suspension by using deionized water, and performing ultrasonic layering and centrifugation to obtain an MXene colloidal solution;
preparation of MXene functionalized carbon fiber composite material
1) Removing a surface sizing agent from the carbon fiber by using acetone, acidifying the carbon fiber in concentrated nitric acid, and cleaning the carbon fiber to be neutral;
2) soaking the acidified carbon fiber in MXene colloidal solution for a set time and then taking out;
3) washing off redundant MXene on the surface of the fiber by using water, and carrying out vacuum drying on the washed fiber to obtain an MXene functionalized carbon fiber composite material;
preparation of MXene functionalized carbon fiber-epoxy resin composite material
1) Uniformly mixing methyl tetrahydrophthalic anhydride and E51 resin to obtain a mixed solution;
2) and (4) placing the mixed solution on the surface of the fiber prepared in the step (3), curing for a set time at a first temperature, then heating to cure, and then cooling along with a furnace to obtain the fiber.
2. The method for improving the interface of the carbon fiber-epoxy resin composite material by the MXene according to claim 1, wherein: the step 2) of preparing the MXene colloidal solution is specifically that (1) 1g of prepared ceramic powder is added into a mixed solution of 5-25 ml of 9-12 mol/ml hydrochloric acid and 0.2-2 g of lithium fluoride, or added into 5-25 ml of an aqueous solution with 10-70 wt.% HF content, a magnetic rotor is added, and the mixture is stirred in an oil bath environment at the temperature of 20-70 ℃ for 12-96 hours to obtain a suspension;
(2) washing the corroded suspension of the mixture with 5-100 ml of deionized water, centrifuging, pouring out the supernatant, and repeating for multiple times until the pH value of the supernatant is more than or equal to 6;
(3) after the pH value of the supernatant is more than or equal to 6, continuously using 5-100 ml of deionized water for washing and centrifuging, pouring out the supernatant, and repeating for 3-5 times;
(4) and adding 5-40 ml of deionized water into the mixture finally cleaned, performing ultrasonic layering treatment under the protection of argon atmosphere, keeping the temperature below 35 ℃ in the ultrasonic process, performing centrifugal treatment on the mixed solution after ultrasonic treatment, and taking the upper layer solution, namely the single-layer MXene colloidal solution.
3. The method for improving the interface of the carbon fiber-epoxy resin composite material by the MXene according to claim 1, wherein: the concentration of the MXene colloidal solution was determined using a suction filtration method.
4. The method for improving the interface of the carbon fiber-epoxy resin composite material by the MXene according to claim 1, wherein: the mixed liquid in the MXene functionalized carbon fiber-epoxy resin composite material preparation step also comprises tri- (dimethylaminomethyl) phenol, and the mixed liquid is obtained by uniformly mixing E51 resin, methyl tetrahydrophthalic anhydride and tri- (dimethylaminomethyl) phenol and defoaming in vacuum for 10-60 min.
5. The method for improving the interface of the carbon fiber-epoxy resin composite material by the MXene according to claim 4, wherein: and preparing the mixed solution by using 80-90 parts of methyl tetrahydrophthalic anhydride per 100 parts of E51 resin.
6. The method for improving the interface of the carbon fiber-epoxy resin composite material by the MXene according to claim 1, wherein: the ceramic powder is Mn+1AlCnThe ceramic powder is prepared by mixing a ceramic powder,nand =1,2,3, M is a transition metal element.
7. The method for improving the interface of the carbon fiber-epoxy resin composite material by the MXene according to claim 6, wherein: the M isn+1AlCnThe preparation steps of the ceramic powder are as follows: mixing M, Al and C powders in a molar ratio of (A), (B), (Cn+1):1.2:nn=1,2, 3) mixing uniformly, preparing high-purity ternary lamellar M through pressureless sintering at 1000-1800 DEG Cn+1AlCnn=1,2, 3) ceramic block material, M to be producedn+1AlCnGrinding the ceramic material to obtain Mn+1AlCnCeramic powder.
8. The method for improving MXene interface of carbon fiber-epoxy resin composite material according to claim 6 or 7, characterized by: the M isn+1AlCnM in the ceramic powder is Ti, Nb, V, Cr or Ta.
9. The method for improving the interface of the carbon fiber-epoxy resin composite material by the MXene according to claim 1, wherein: the fineness of the ceramic powder is 100-1200 meshes.
10. The carbon fiber-epoxy resin composite material prepared by the method for improving the interface of the carbon fiber-epoxy resin composite material by MXene according to claim 1.
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Cited By (7)

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CN112812496A (en) * 2021-01-04 2021-05-18 中国科学院兰州化学物理研究所 Mxene-V2C modified carbon fiber fabric self-lubricating material and preparation method thereof
CN112812496B (en) * 2021-01-04 2021-11-12 中国科学院兰州化学物理研究所 Mxene-V2C modified carbon fiber fabric self-lubricating material and preparation method thereof
KR20220103311A (en) * 2021-01-15 2022-07-22 성균관대학교산학협력단 Enhancement structure of the interfacial strength between carbon fiber and epoxy resin composites and manufacturing methode of the same
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CN113248746A (en) * 2021-06-04 2021-08-13 北京化工大学 Method for improving high-modulus carbon fiber composite material interface performance
CN113248746B (en) * 2021-06-04 2022-07-05 北京化工大学 Method for improving high-modulus carbon fiber composite material interface performance
CN113445306A (en) * 2021-07-18 2021-09-28 陕西科技大学 Preparation method of modified carbon fiber based on two-dimensional nano material
CN113652858A (en) * 2021-08-26 2021-11-16 浙江理工大学绍兴柯桥研究院有限公司 MXene coated carbon fiber and preparation method thereof
CN113912983A (en) * 2021-11-09 2022-01-11 珠海三臻新材料科技有限公司 Modified MXene/carbon fiber/epoxy resin composite material and preparation method thereof
CN113912983B (en) * 2021-11-09 2023-06-02 珠海三臻新材料科技有限公司 Modified MXene/carbon fiber/epoxy resin composite material and preparation method thereof
CN115073886A (en) * 2022-07-13 2022-09-20 哈尔滨工业大学 Preparation method of MXene/CNT composite sponge reinforced resin matrix composite material
CN115073886B (en) * 2022-07-13 2024-03-15 哈尔滨工业大学 Preparation method of MXene/CNT composite sponge reinforced resin matrix composite material

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