CN113583266B - Method for freezing casting interlayer toughening fiber composite material - Google Patents
Method for freezing casting interlayer toughening fiber composite material Download PDFInfo
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Abstract
A method for freezing and casting interlayer toughening fiber composite material belongs to the technical field of preparation of structural composite materials. The application solves the problems of complex flow, higher equipment cost, low specific surface area and the like in the interlayer toughening fiber treatment process, and the method comprises the following steps: dispersing one-dimensional or two-dimensional nano material in water, and fully mixing with water-soluble polymer; fully soaking the woven fiber cloth in a water-soluble polymer solution containing nano materials, then carrying out directional freezing on a metal mold, and obtaining the fiber cloth loaded with aerogel after freeze drying; and (3) impregnating the aerogel-loaded fiber cloth in matrix resin in a vacuum state, fully impregnating the matrix resin into a plurality of layers of aerogel-loaded fiber cloth, and adopting a molding curing process to obtain the composite material. The method for growing aerogel on the fiber surface has simple process and low cost, can endow the fiber composite material with multiple functionalities, and lays a foundation for realizing the structural and functional integration of the composite material.
Description
Technical Field
The application belongs to the technical field of preparation of structural composite materials, and particularly relates to a method for freezing and casting an interlayer toughening fiber composite material.
Background
The specific strength and specific stiffness in the surface 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 light weight and high performance of the aerospace material, but the carbon fiber composite material is subjected to impact damage since being applied to high end for solving the light weight requirement, layering damage caused by low-speed impact and temperature impact on the laminated plate, microcrack generation and expansion, and the integral performance of a material structure is reduced. Therefore, the development of the toughened epoxy resin carbon fiber composite material is an important development trend in the future, and is also a technical field which is valued by military countries in the world.
The epoxy resin has high crosslinking density and is brittle, and the epoxy resin carbon fiber composite material layer and the layer only play roles in bonding and load transmission by the matrix resin, so the strength in the thickness direction is lower; meanwhile, the Poisson ratio between fiber layers is not matched, and the thermal expansion coefficients are greatly different, so that interlayer stress concentration areas are easy to generate, and layering damage is further 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 obstruct the application of the advanced composite material in the fields of weaponry and aerospace.
Disclosure of Invention
The application aims to solve the problems of complex flow, higher equipment cost, low specific surface area and the like in the existing 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 an aerogel network is constructed among the fiber cloth layers by adopting a freezing casting method, so that the composite structure has a better toughening effect, and the toughening structure has high designability.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
a method for freezing and casting interlayer toughening fiber composite material comprises the following specific steps:
step one: dispersing one-dimensional or two-dimensional nano material in water, and fully mixing with water-soluble polymer;
step two: fully soaking the woven fiber cloth in the water-soluble polymer solution containing the nano material obtained in the first step, then carrying out directional freezing on a metal mold, and carrying out freeze drying to obtain aerogel-loaded fiber cloth;
step three: and (3) impregnating the aerogel-loaded fiber cloth in matrix resin in a vacuum state, fully impregnating the matrix resin into a plurality of layers of aerogel-loaded fiber cloth, and adopting a molding curing process to obtain the composite material.
Further, in the first step, the nanomaterial is one or more of graphene oxide, reduced graphene oxide, carbon nanotubes, boron nitride nanoplatelets, and aluminum oxide nanoplatelets; the concentration of the extract in the solution is 0.5-20mg/mL.
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 2-100mg/mL.
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.
Further, the fiber cloth is extracted or untreated fiber cloth by polydopamine treatment, silane coupling agent treatment, plasma treatment and acidification treatment.
Further, in the second step, the freezing temperature is between-20 ℃ and-196 ℃, and the freeze-drying time is between 30 and 50 hours.
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.
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 molding and curing process is one or more of an autoclave molding process, an RTM molding process, a compression molding process, a vacuum assist process or a vacuum bag molding process.
Compared with the prior art, the application has the beneficial effects that:
(1) The process flow is simple, 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 'freeze casting method' only by one step; the grown ice crystal template can be simply removed by freeze drying and has no pollution to the environment, and the purpose of controllable preparation of the aerogel three-dimensional network structure can be achieved by simply controlling the reaction conditions, such as reactant concentration, freezing temperature and the like. Low requirement on reaction equipment and mild reaction condition.
(2) The interlaminar toughening fiber composite material prepared by the method has excellent I-type interlaminar fracture toughness, and the method for growing aerogel on the fiber surface is simple in process and low in cost, can endow the fiber composite material with multiple functionalities, and lays a foundation for realizing structural and functional integration of the composite material.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of graphene aerogel grown in situ on a carbon fiber cloth in example 1.
Detailed Description
The following description of the present application refers to the accompanying drawings and examples, but is not limited to the same, and modifications and equivalents of the present application can be made without departing from the spirit and scope of the present application.
Example 1:
the method for growing the composite graphene aerogel on the surface of the carbon fiber comprises the following steps:
step one: dispersing the two-dimensional graphene oxide nano-sheets in water, and fully mixing with sodium alginate powder under ultrasound, wherein the concentration of graphene oxide is 1mg/ml, and the concentration of sodium alginate is 10mg/ml;
step two: fully soaking a plurality of layers of unidirectional carbon fiber cloth in the mixed solution, and then carrying out directional freezing on a plane metal mold, wherein a plane metal plate part is in direct contact with liquid nitrogen, and then rapidly transferring the mixed solution to a freeze dryer for freeze drying for 48 hours at the temperature of minus 50 ℃ to obtain aerogel-loaded fiber cloth; the resulting graphene aerogel loading fiber of the cellular network structure is shown in fig. 1. The carbon fiber cloth is carbon fiber cloth which is pretreated and then is introduced with carboxyl, hydroxyl and amino.
Step three: and (3) impregnating the aerogel-loaded fiber cloth in matrix resin in a vacuum state, fully impregnating the matrix resin into a plurality of layers of aerogel-loaded fiber cloth, and obtaining the final composite material by using an autoclave molding process.
The embodiment has simple process flow, structural controllability 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 'freeze casting method' only by one step; the grown ice crystal template can be simply removed by freeze drying and has no pollution to the environment, and the purpose of controllable preparation of the aerogel three-dimensional network structure can be achieved by simply controlling the reaction conditions, such as reactant concentration, freezing temperature and the like. Low requirement on reaction equipment and mild reaction condition. The final composite material has a flexural strength of 800MPa and a tensile modulus (in the machine direction)>120GPa, shear modulus (longitudinal)>170MPa, type I interlayer shear strength of G IC ≈1.32KJ/m 2 Has good mechanical property and interlayer toughening effect.
Example 2:
the method for growing the composite graphene aerogel on the surface of the PBO fiber comprises the following steps:
step one: dispersing graphene nano sheets in water, and fully mixing the graphene nano sheets with chitosan macromolecules under ultrasound, wherein the concentration of the graphene nano sheets is 5mg/ml, and the concentration of the chitosan is 10mg/ml;
step two: fully soaking a plurality of layers of unidirectional carbon fiber cloth in the mixed solution, and then carrying out directional freezing on a wedge-shaped metal block mold, wherein part of metal blocks are in direct contact with liquid nitrogen, and obtaining aerogel-loaded fiber cloth after supercritical drying; the PBO fiber cloth is prepared by introducing carboxyl, hydroxyl and amino after pretreatment.
Step three: and (3) impregnating the aerogel-loaded fiber cloth in matrix resin in a vacuum state, fully impregnating the matrix resin into a plurality of layers of aerogel-loaded fiber cloth, and obtaining the final composite material by using an RTM (real time kinematic) forming process.
The embodiment has simple process flow, structural controllability 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 'freeze casting method' only by one step; the grown ice crystal template can be simply removed by freeze drying and has no pollution to the environment, and the purpose of controllable preparation of the aerogel three-dimensional network structure can be achieved by simply controlling the reaction conditions, such as reactant concentration, freezing temperature and the like. Low requirement on reaction equipment and mild reaction condition. The I-type interlayer shear strength of the finally obtained composite material is G IC ≈1.3KJ/m 2 The material is improved by 30 to 50 percent compared with the non-toughened composite material. In addition, the composite material has good radiation (ultraviolet) resistance.
Example 3:
the method for growing the composite carbon nano tube aerogel on the surface of the carbon fiber comprises the following steps:
step one: dispersing one-dimensional carbon nano tubes in water, and fully mixing the carbon nano tubes with polyvinyl alcohol powder under ultrasonic, wherein the concentration of the carbon nano tubes is 2mg/ml, and the concentration of the polyvinyl alcohol is 10mg/ml;
step two: fully soaking a plurality of layers of unidirectional carbon fiber cloth in the mixed solution, and then carrying out directional freezing on a plane metal plate mold, wherein a part of the plane metal plate is soaked in dry ice bath, and the fiber cloth/aerogel composite structure is obtained after freeze drying; the carbon fiber cloth is carbon fiber cloth which is pretreated and then is introduced with carboxyl, hydroxyl and amino.
Step three: the final composite material is obtained by impregnating and filling the laminated fiber cloth with epoxy resin by vacuum infusion and using a vacuum auxiliary molding process.
The embodiment has simple process flow, structural controllability 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 'freeze casting method' only by one step; the grown ice crystal template can be simply removed by freeze drying and has no pollution to the environment, and the purpose of controllable preparation of the aerogel three-dimensional network structure can be achieved by simply controlling the reaction conditions, such as reactant concentration, freezing temperature and the like. Low requirement on reaction equipment and mild reaction condition. The final composite material has a flexural strength of 700MPa and a tensile modulus (longitudinal direction)>110GPa, shear modulus (longitudinal)>170MPa, type I interlayer shear strength of G IC ≈1.5KJ/m 2 Has good mechanical property and interlayer 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:
step one: dispersing the two-dimensional boron nitride nano-sheets in water, and fully mixing with water-soluble phenolic resin under ultrasonic, wherein the concentration of the boron nitride nano-sheets is 5mg/ml, and the concentration of the water-soluble phenolic resin is 10mg/ml;
step two: fully soaking a plurality of layers of unidirectional carbon fiber cloth in the mixed solution, and then carrying out directional freezing on a closed metal mold, wherein the closed metal mold is placed in an ultralow temperature refrigerator, and the fiber cloth/aerogel composite structure is obtained after vacuum drying; the aramid fiber cloth is an aramid fiber cloth which is pretreated and then is introduced with carboxyl, hydroxyl and amino.
Step three: the final composite is obtained by impregnating and impregnating the laminated fiber cloth with epoxy resin by vacuum infusion and using a vacuum bag forming process.
The embodiment has simple process flow, structural controllability and low cost. Can be manufactured by a 'freeze casting method' with only one step"assembling an aerogel network comprising two-dimensional nanomaterial to a carbon fiber fabric surface in situ; the grown ice crystal template can be simply removed by freeze drying and has no pollution to the environment, and the purpose of controllable preparation of the aerogel three-dimensional network structure can be achieved by simply controlling the reaction conditions, such as reactant concentration, freezing temperature and the like. Low requirement on reaction equipment and mild reaction condition. The I-type interlayer shear strength of the finally obtained composite material is G IC ≈1.0KJ/m 2 Has good mechanical property and interlayer toughening effect. In addition, the composite material has significantly improved heat conducting properties.
While the preferred embodiment of the present application has been described in detail, the present application is not limited to the embodiment, and various equivalent modifications and substitutions can be made by those skilled in the art without departing from the spirit of the present application, and these equivalent modifications and substitutions are intended to be included in the scope of the present application as defined in the appended claims.
Claims (5)
1. A method for freezing and casting interlayer toughening fiber composite material is characterized in that: the method comprises the following specific steps:
step one: dispersing one-dimensional or two-dimensional nano material in water, and fully mixing with water-soluble polymer; the nano material is one or more of graphene oxide, reduced graphene oxide, carbon nanotubes and alumina nano sheets; the concentration of the water in the solution is 0.5-20mg/mL; the water-soluble polymer is one or more of sodium alginate, water-soluble phenolic resin, chitosan, gelatin and water-soluble starch; the concentration of the water in the solution is 2-100mg/mL;
step two: fully soaking the woven fiber cloth in the water-soluble polymer solution containing the nano material obtained in the first step, then carrying out directional freezing on a metal mold, and carrying out freeze drying to obtain aerogel-loaded fiber cloth; the fiber cloth is fiber cloth which is extracted or untreated by polydopamine treatment, silane coupling agent treatment, plasma treatment and acidification treatment; the metal mold is one of a planar metal plate, a wedge-shaped metal block and a three-dimensional sealable metal cavity;
step three: and (3) impregnating the aerogel-loaded fiber cloth in matrix resin in a vacuum state, fully impregnating the matrix resin into a plurality of layers of aerogel-loaded fiber cloth, and adopting a molding curing process to obtain the composite material.
2. The method of freeze casting an interlaminar toughened fibrous composite material as in 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.
3. The method of freeze casting an interlaminar toughened fibrous composite material as in claim 1 wherein: in the second step, the freezing temperature is-20 ℃ to-196 ℃ and the freeze-drying time is 30-50h.
4. The method of freeze casting an interlaminar toughened fibrous composite material as in claim 1 wherein: in the third step, the matrix resin is one or more of epoxy resin, benzoxazine resin, bismaleimide resin and polyimide resin.
5. The method of freeze casting an interlaminar toughened fibrous composite material as in claim 1 wherein: in the third step, the molding and curing process is one or more of an autoclave molding process, an RTM molding process, a compression molding process, a vacuum auxiliary process or a vacuum bag molding process.
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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 |
| 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 |
| CN114771052B (en) * | 2022-04-25 | 2022-10-04 | 叶金蕊 | Mixed-woven fiber cloth for high-voltage-resistant composite material and preparation method 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 |
| CN115214201B (en) * | 2022-06-15 | 2023-09-29 | 北京理工大学 | Carbon fiber/epoxy resin laminated plate and preparation method 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 |
| 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 |
| 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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| CN102924736A (en) * | 2012-10-30 | 2013-02-13 | 天津大学 | Preparation of carbon fiber/ carbon nano tube/ epoxy resin composite material and assisted by freezing and drying |
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| CN102924736A (en) * | 2012-10-30 | 2013-02-13 | 天津大学 | Preparation of carbon fiber/ carbon nano tube/ epoxy resin composite material and assisted by freezing and drying |
| CN103275525A (en) * | 2013-05-28 | 2013-09-04 | 天津大学 | Preparation method of fiber/carbon nano tube conductive network for modifying polymers |
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