CN113583266A - Method for freezing and casting interlayer toughening fiber composite material - Google Patents
Method for freezing and casting interlayer toughening fiber composite material Download PDFInfo
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Abstract
A method for freezing and casting an interlaminar toughening fiber composite material belongs to the technical field of preparation of structural composite materials. The invention solves the problems of complex flow, higher equipment cost, low specific surface area and the like of an interlaminar toughening fiber treatment process, and the method comprises the following steps: dispersing one-dimensional or two-dimensional nano materials in water, and fully mixing the nano materials with water-soluble polymers; fully soaking the woven fiber cloth in a water-soluble polymer solution containing a nano material, then performing directional freezing on a metal mold, and performing freeze drying to obtain aerogel-loaded fiber cloth; and (3) soaking the aerogel-loaded fiber cloth in matrix resin in a vacuum state to enable the matrix resin to fully soak the multiple layers of aerogel-loaded fiber cloth, and obtaining the composite material by adopting a forming and curing process. The method for growing the aerogel on the surface of the fiber has simple process and low cost, can endow the fiber composite material with various functionalities, and lays a foundation for realizing the structural and functional integration of the composite material.
Description
Technical Field
The invention belongs to the technical field of preparation of structural composite materials, and particularly relates to a method for freezing and casting an interlaminar toughening fiber composite material.
Background
The specific strength and specific rigidity in the plane of the carbon fiber reinforced resin (CFRP) composite material are higher than those of the traditional carbon fiber material, the carbon fiber composite material is increasingly applied along with the development requirement of lightweight and high performance of aerospace materials, but the carbon fiber composite material is applied at high end for solving the lightweight requirement, the encountered technical key is impact damage, the laminated plate is subjected to layering damage caused by low-speed impact and temperature impact, microcracks are generated and expanded, and the overall performance of a material structure is reduced. Therefore, the development of toughened epoxy resin carbon fiber composite materials is an important development trend in the future and is also a technical field which is valued by various military and strong countries in the world.
The epoxy resin is brittle due to high crosslinking density, and the epoxy resin carbon fiber composite material layers only have the functions of bonding and load transmission by virtue of matrix resin, so that the strength in the thickness direction is low; meanwhile, the Poisson ratio mismatch and the thermal expansion coefficient of the fiber layers are greatly different, so that an interlayer stress concentration area is easily generated, and further layering damage is generated. In order to increase the interlaminar fracture toughness of the composite, it is desirable to improve the delamination resistance of the laminate, thereby improving the overall performance of the composite. However, the traditional interlayer toughening fiber treatment process has the problems of complex process flow, high equipment cost, low specific surface area and the like, and the problems seriously hinder the application of the advanced composite material in the fields of weaponry and aerospace.
Disclosure of Invention
The invention aims to solve the problems of complex flow, higher equipment cost, low specific surface area and the like of the conventional interlayer toughening fiber treatment process, and provides a simple method for freezing and casting an interlayer toughening fiber composite material. According to the method, the fiber cloth is fully soaked in the water-soluble polymer solution containing the nano material, and the aerogel network is constructed between the fiber cloth layers by adopting a freeze casting method, so that the composite structure has a better toughening effect, and the toughening structure has high designability.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for freezing and casting an interlaminar toughening fiber composite material comprises the following specific steps:
the method comprises the following steps: dispersing one-dimensional or two-dimensional nano materials in water, and fully mixing the nano materials with water-soluble polymers;
step two: fully soaking the woven fiber cloth in the water-soluble polymer solution containing the nano material obtained in the step one, then performing directional freezing on a metal mold, and performing freeze drying to obtain aerogel-loaded fiber cloth;
step three: and (3) soaking the aerogel-loaded fiber cloth in matrix resin in a vacuum state to enable the matrix resin to fully soak the multiple layers of aerogel-loaded fiber cloth, and obtaining the composite material by adopting a forming and curing process.
Further, in the first step, the nano material is one or more of graphene oxide, reduced graphene oxide, carbon nanotubes, boron nitride nanosheets and aluminum oxide nanosheets; the concentration of the compound in the solution is 0.5-20 mg/mL.
Further, in the first step, the water-soluble polymer is one or more of sodium alginate, polyvinyl alcohol, water-soluble phenolic resin, chitosan, gelatin, carboxymethyl cellulose and water-soluble starch; the concentration of the compound in the solution is 2-100 mg/mL.
Further, in the second step, the fiber of the woven fiber cloth is one or more of p-PBO fiber, carbon fiber, aramid fiber, polyester fiber, polyamide fiber, polyvinyl alcohol fiber, polyacrylonitrile fiber, polypropylene fiber, polyvinyl chloride fiber or glass fiber.
Further, the fiber cloth is extracted or untreated by polydopamine treatment, silane coupling agent treatment, plasma treatment and acidification treatment.
Further, in the second step, the freezing temperature is-20 ℃ to-196 ℃, and the freeze-drying time is 30-50 h.
Further, in the second step, the metal mold is one of a planar metal plate, a wedge-shaped metal block and a three-dimensional sealable metal cavity.
Further, in the third step, the matrix resin is one or more of epoxy resin, benzoxazine resin, bismaleimide resin and polyimide resin.
Further, in the third step, the forming and curing process is one or more of an autoclave forming process, an RTM forming process, a compression molding process, a vacuum assist or a vacuum bag forming process.
Compared with the prior art, the invention has the beneficial effects that:
(1) the process flow is simple, and the method has controllability and low cost. The aerogel network containing one-dimensional or two-dimensional nano materials can be assembled on the surface of the carbon fiber fabric in situ by a freezing casting method only by one step; the grown ice crystal template can be simply removed by freeze drying without pollution to the environment, and the aim of controllably preparing the aerogel three-dimensional network structure can be fulfilled by simply controlling reaction conditions such as reactant concentration, freezing temperature and the like. Low requirements on reaction equipment and mild reaction conditions.
(2) The interlaminar toughened fiber composite material prepared by the invention has excellent I-type interlaminar fracture toughness, the method for growing the aerogel on the surface of the fiber has simple process and low cost, can endow the fiber composite material with multiple functionalities, and lays a foundation for realizing the structural function integration of the composite material.
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Fig. 1 is a Scanning Electron Microscope (SEM) image of in-situ growth of graphene aerogel on carbon fiber cloth in example 1.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments, but the present invention is not limited thereto, and modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
the method for growing the composite graphene aerogel on the surface of the carbon fiber comprises the following steps:
the method comprises the following steps: dispersing two-dimensional graphene oxide nanosheets in water, and fully mixing the graphene oxide nanosheets with sodium alginate powder under ultrasonic, wherein the concentration of graphene oxide is 1mg/ml, and the concentration of sodium alginate is 10 mg/ml;
step two: fully soaking a plurality of layers of unidirectional carbon fiber cloth in the mixed solution, then directionally freezing on a plane metal mold, wherein the plane metal plate part is directly contacted with liquid nitrogen, and then quickly transferring to a freeze dryer for freeze drying for 48 hours at-50 ℃ to obtain aerogel-loaded fiber cloth; the produced graphene aerogel-loaded fiber with a honeycomb network structure is shown in fig. 1. The carbon fiber cloth is pretreated and then introduced with carboxyl, hydroxyl and amino.
Step three: and (3) soaking the aerogel-loaded fiber cloth in matrix resin in a vacuum state to enable the matrix resin to fully soak the multiple layers of aerogel-loaded fiber cloth, and obtaining the final composite material by using an autoclave molding process.
The method has the advantages of simple process flow, controllable structure and low cost. The aerogel network containing the nano material can be assembled on the surface of the carbon fiber fabric in situ by a freezing casting method only by one step; the grown ice crystal template can be simply removed by freeze-drying without environmental pollution, byThe aim of controllably preparing the aerogel three-dimensional network structure can be achieved by singly controlling reaction conditions such as reactant concentration, freezing temperature and the like. Low requirements on reaction equipment and mild reaction conditions. The resulting composite had a flexural strength of 800MPa, tensile modulus (longitudinal)>120GPa, shear modulus (longitudinal)>170MPa, I type interlaminar shear strength GIC≈1.32KJ/m2Has good mechanical property and interlaminar toughening effect.
Example 2:
the method for growing the composite graphene aerogel on the surface of the PBO fiber comprises the following steps:
the method comprises the following steps: dispersing graphene nano sheets in water, and fully mixing the graphene nano sheets with chitosan macromolecules under ultrasonic, wherein the concentration of the graphene nano sheets is 5mg/ml, and the concentration of the chitosan is 10 mg/ml;
step two: fully soaking a plurality of layers of unidirectional carbon fiber cloth in the mixed solution, then performing directional freezing on a wedge-shaped metal block die, wherein part of metal blocks are directly contacted with liquid nitrogen, and performing supercritical drying to obtain aerogel-loaded fiber cloth; the PBO fiber cloth is the PBO fiber cloth which is pretreated and then introduced with carboxyl, hydroxyl and amino.
Step three: and (3) soaking the aerogel-loaded fiber cloth in matrix resin in a vacuum state to enable the matrix resin to fully soak multiple layers of aerogel-loaded fiber cloth, and obtaining the final composite material by using an RTM (resin transfer molding) process.
The method has the advantages of simple process flow, controllable structure and low cost. The aerogel network containing the two-dimensional nano material can be assembled on the surface of the carbon fiber fabric in situ by a freezing casting method only by one step; the grown ice crystal template can be simply removed by freeze drying without pollution to the environment, and the aim of controllably preparing the aerogel three-dimensional network structure can be fulfilled by simply controlling reaction conditions such as reactant concentration, freezing temperature and the like. Low requirements on reaction equipment and mild reaction conditions. The final composite material has an I-type interlaminar shear strength of GIC≈1.3KJ/m2Is improved by 30 to 50 percent compared with the composite material without toughening.In addition, the composite material has good radiation (ultraviolet) resistance.
Example 3:
a method for growing composite carbon nanotube aerogel on the surface of carbon fiber is carried out according to the following steps:
the method comprises the following steps: dispersing one-dimensional carbon nanotubes in water, and fully mixing the one-dimensional carbon nanotubes and polyvinyl alcohol powder under ultrasonic, wherein the concentration of the carbon nanotubes is 2mg/ml, and the concentration of the polyvinyl alcohol is 10 mg/ml;
step two: fully soaking the multilayer unidirectional carbon fiber cloth in the mixed solution, and then directionally freezing on a plane metal plate mould, wherein the plane metal plate is partially soaked in a dry-ice bath, and obtaining a fiber cloth/aerogel composite structure after freezing and drying; the carbon fiber cloth is pretreated and then introduced with carboxyl, hydroxyl and amino.
Step three: the final composite material is obtained by vacuum infusion to impregnate and fill the laminated fiber cloth with the epoxy resin and by using a vacuum auxiliary forming process.
The method has the advantages of simple process flow, controllable structure and low cost. The aerogel network containing the two-dimensional nano material can be assembled on the surface of the carbon fiber fabric in situ by a freezing casting method only by one step; the grown ice crystal template can be simply removed by freeze drying without pollution to the environment, and the aim of controllably preparing the aerogel three-dimensional network structure can be fulfilled by simply controlling reaction conditions such as reactant concentration, freezing temperature and the like. Low requirements on reaction equipment and mild reaction conditions. The resulting composite had a flexural strength of-700 MPa, tensile modulus (longitudinal)>110GPa, shear modulus (longitudinal)>170MPa, I type interlaminar shear strength GIC≈1.5KJ/m2Has good mechanical property and interlaminar toughening effect. In addition, the composite material has significantly improved electrical conductivity.
Example 4:
the method for growing the composite boron nitride aerogel on the aramid fiber comprises the following steps:
the method comprises the following steps: dispersing two-dimensional boron nitride nanosheets in water, and fully mixing the two-dimensional boron nitride nanosheets with water-soluble phenolic resin under ultrasound, wherein the concentration of the boron nitride nanosheets is 5mg/ml, and the concentration of the water-soluble phenolic resin is 10 mg/ml;
step two: fully soaking a plurality of layers of unidirectional carbon fiber cloth in the mixed solution, and then directionally freezing on a closed metal mold, wherein the closed metal mold is placed in an ultra-low temperature refrigerator, and vacuum drying is carried out to obtain a fiber cloth/aerogel composite structure; the aramid fiber cloth is pretreated and then introduced with carboxyl, hydroxyl and amino.
Step three: and (3) impregnating and filling the laminated fiber cloth with epoxy resin by vacuum infusion, and obtaining the final composite material by using a vacuum bag forming process.
The method has the advantages of simple process flow, controllable structure and low cost. The aerogel network containing the two-dimensional nano material can be assembled on the surface of the carbon fiber fabric in situ by a freezing casting method only by one step; the grown ice crystal template can be simply removed by freeze drying without pollution to the environment, and the aim of controllably preparing the aerogel three-dimensional network structure can be fulfilled by simply controlling reaction conditions such as reactant concentration, freezing temperature and the like. Low requirements on reaction equipment and mild reaction conditions. The final composite material has an I-type interlaminar shear strength of GIC≈1.0KJ/m2Has good mechanical property and interlaminar toughening effect. In addition, the composite material has remarkably improved heat-conducting property.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A method for freezing and casting interlayer toughening fiber composite material is characterized in that: the method comprises the following specific steps:
the method comprises the following steps: dispersing one-dimensional or two-dimensional nano materials in water, and fully mixing the nano materials with water-soluble polymers;
step two: fully soaking the woven fiber cloth in the water-soluble polymer solution containing the nano material obtained in the step one, then performing directional freezing on a metal mold, and performing freeze drying to obtain aerogel-loaded fiber cloth;
step three: and (3) soaking the aerogel-loaded fiber cloth in matrix resin in a vacuum state to enable the matrix resin to fully soak the multiple layers of aerogel-loaded fiber cloth, and obtaining the composite material by adopting a forming and curing process.
2. The method of freeze casting an interlaminar toughening fiber composite of claim 1, wherein: in the first step, the nano material is one or more of graphene oxide, reduced graphene oxide, a carbon nano tube, a boron nitride nano sheet and an aluminum oxide nano sheet; the concentration of the compound in the solution is 0.5-20 mg/mL.
3. The method of freeze casting an interlaminar toughening fiber composite of claim 1, wherein: in the first step, the water-soluble polymer is one or more of sodium alginate, polyvinyl alcohol, water-soluble phenolic resin, chitosan, gelatin, carboxymethyl cellulose and water-soluble starch; the concentration of the compound in the solution is 2-100 mg/mL.
4. The method of freeze casting an interlaminar toughening fiber composite of claim 1, wherein: in the second step, the fiber of the woven fiber cloth is one or more of PBO fiber, carbon fiber, aramid fiber, polyester fiber, polyamide fiber, polyvinyl alcohol fiber, polyacrylonitrile fiber, polypropylene fiber, polyvinyl chloride fiber or glass fiber.
5. The method of freeze casting an interlaminar toughening fiber composite of claim 4, wherein: the fiber cloth is extracted or not treated by polydopamine treatment, silane coupling agent treatment, plasma treatment and acidification treatment.
6. The method of freeze casting an interlaminar toughening fiber composite of claim 1, wherein: in the second step, the freezing temperature is-20 ℃ to-196 ℃, and the freeze-drying time is 30-50 h.
7. The method of freeze casting an interlaminar toughening fiber composite of claim 1, wherein: in the second step, the metal mold is one of a plane metal plate, a wedge-shaped metal block and a three-dimensional sealable metal cavity.
8. The method of freeze casting an interlaminar toughening fiber composite of claim 1, wherein: in the third step, the matrix resin is one or more of epoxy resin, benzoxazine resin, bismaleimide resin and polyimide resin.
9. The method of freeze casting an interlaminar toughening fiber composite of claim 1, wherein: in the third step, the forming and curing process is one or more of an autoclave forming process, an RTM forming process, a compression molding process, a vacuum auxiliary or vacuum bag forming process.
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Cited By (12)
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| CN113914093A (en) * | 2021-12-14 | 2022-01-11 | 山东非金属材料研究所 | Anti-ultraviolet PBO fiber modified based on polydopamine layer-by-layer self-assembly bionic structure and preparation method thereof |
| CN114163775A (en) * | 2022-01-14 | 2022-03-11 | 安徽工程大学 | Composite material with composite reinforcement structure and preparation method thereof |
| CN114536877A (en) * | 2022-02-21 | 2022-05-27 | 杭州安士城消防器材有限公司 | Fire-proof equipment |
| CN114590794A (en) * | 2022-03-09 | 2022-06-07 | 中国科学技术大学 | Compressible carbon nanofiber aerogel, and preparation method and application thereof |
| CN114874755A (en) * | 2022-05-10 | 2022-08-09 | 武汉理工大学 | Aerogel-based phase change composite material for electronic component thermal management and preparation method and application thereof |
| CN115214201A (en) * | 2022-06-15 | 2022-10-21 | 北京理工大学 | Carbon fiber/epoxy resin laminated plate and preparation method thereof |
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| CN115449185A (en) * | 2022-09-21 | 2022-12-09 | 华南理工大学 | Glass fiber reinforced epoxy resin composite material and preparation method and application thereof |
| CN115505255A (en) * | 2022-09-22 | 2022-12-23 | 浙江大学 | Boron nitride polymer composite material and preparation method and application thereof |
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| CN113914093B (en) * | 2021-12-14 | 2022-03-01 | 山东非金属材料研究所 | Anti-ultraviolet PBO fiber modified based on polydopamine layer-by-layer self-assembly bionic structure and preparation method thereof |
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| CN115214201A (en) * | 2022-06-15 | 2022-10-21 | 北京理工大学 | Carbon fiber/epoxy resin laminated plate and preparation method thereof |
| CN115395026A (en) * | 2022-08-12 | 2022-11-25 | 陕西科技大学 | Fe monatomic-loaded N-doped carbon aerogel electrocatalyst and preparation method and application thereof |
| CN115395026B (en) * | 2022-08-12 | 2024-03-15 | 天津市顺红洋科技有限公司 | Fe single-atom-supported N-doped carbon aerogel electrocatalyst and preparation method and application thereof |
| CN115449185A (en) * | 2022-09-21 | 2022-12-09 | 华南理工大学 | Glass fiber reinforced epoxy resin composite material and preparation method and application thereof |
| CN115449185B (en) * | 2022-09-21 | 2023-05-23 | 华南理工大学 | Glass fiber reinforced epoxy resin composite material and preparation method and application thereof |
| CN115505255A (en) * | 2022-09-22 | 2022-12-23 | 浙江大学 | Boron nitride polymer composite material and preparation method and application thereof |
| CN115678109A (en) * | 2022-11-22 | 2023-02-03 | 齐鲁工业大学 | Preparation method of nano-cellulose-carbon fiber composite preform and composite material |
| CN116043548A (en) * | 2023-01-30 | 2023-05-02 | 青岛大学 | Flexible fabric/gel composite material and preparation method and application thereof |
| CN116043548B (en) * | 2023-01-30 | 2024-05-24 | 青岛大学 | Flexible fabric/gel composite material and preparation method and application thereof |
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