Preparation method of HfZrB2 coating on surface of carbon fiber

Abstract

The invention discloses a preparation method of HfZrB2 coating on the surface of carbon fiber. The method is a low-temperature precursor solution impregnation and pyrolysis. The method is characterized by sequentially including preparation of a coating solution, carbon fiber surface activation treatment, coating, drying and heat treatment, and through the method, the high-temperature-resistant andoxidation-resistant HfZrB2 carbon fiber coating is obtained. The process is simple, the requirements of equipment and an operation environment are simple, no special equipment is needed, the feasibility is high, raw materials are cheap and easy to obtain, the method is easy to achieve, saves energy and is environmentally friendly, the high-temperature-resistant and anti-oxidation coating which isuniform, dense and good in adhesion and has the thickness within 2 micrometers can be prepared on the surface of the carbon fiber, the original mechanical properties of the carbon fiber are retained,the high temperature oxidation resistance of the carbon fiber is improved, and the interfacial compatibility between the fiber and a matrix is improved.

Description

technical field [0001] The invention belongs to the technical field of inorganic non-metallic materials, in particular to a carbon fiber surface HfZrB 2 Coating preparation method. Background technique [0002] Carbon fiber has excellent properties such as high modulus, high strength, low density, low thermal expansion, high temperature resistance, oxidation resistance, no creep, high thermal conductivity, and corrosion resistance. It can be used as a reinforcement for composite materials, making carbon fiber in ceramics, resins, It is widely used in composite materials with metal, carbon and other materials as the matrix. However, carbon fiber has been oxidized in the air above 400°C, and its oxidation resistance is poor, resulting in a decrease in the performance of the material. Moreover, the carbon fiber without surface treatment has low surface activity, poor wettability with some substrates, and poor bonding ability. Poor, it will also lead to a decrease in the perfo...

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Problems solved by technology

In the past, the synthesis route of hafnium boride and zirconium boride is mainly: the synthesis of HfB 2 with ZrB 2 The required powder raw materials are mixed in a certain proportion, and react at high temperature to form HfB 2 with ZrB 2 , this method is not suitable for preparing coatings on the surface of carbon fibers, and the synthesis reaction temperature is high and the impurities are high; CVD process prepares HfB 2 with ZrB 2 , looking for a suitable HfB 2 with ZrB 2 Precursor and the precursor is highly toxic, the synthesis reaction temperature is high, the process is complicated, special equipment is required, and it is not suitable for uniform coating on the surface of multi-dimensional fibers; the organic polymer cracking method needs to prepare the precursor polymer first, and then high temperature Cleavage of HfB 2 with ZrB 2 , this method is complicated to operate and is not suitable for preparing a dense interfacial phase coating on the fiber surface

In 2009, Chinese invention patent CN101428812A disclosed a method for preparing high-purity hafnium boride powder, which uses hafnium dioxide, boron carbide, graphite, and amorphous boron as raw materials, and is based on carbothermal / boron at 1500-1600°C A method for preparing hafnium boride powder by thermal reduction reaction. This method has high reaction temperature and high energy consumption, and is not suitable for preparing coatings on the surface of carbon fibers.

In 2014, Chinese invention patent CN103757603 A disclosed a preparation method of zirconium diboride coating, which is based on ZrCl 4 、BCl 3 and H 2 As source gas, Ar gas or N 2 As a carrier gas and protective gas, zirconium diboride coating is prepared by chemical vapor deposition method. The preparation process is complicated, the conditions are harsh, the temperature is high, the energy consumption is high, special equipment is required, and it is not suitable for uniform coating on the surface of multi-dimensional fibers.

In 2017, the Chinese invention patent CN 107523778 A disclosed the preparation method of hafnium boride composite coating, which uses hafnium oxide / boron carbide / aluminum composite powder as raw material according to a certain ratio, and uses thermal spraying in situ reaction to synthesize boron Hafnium compound coating mainly involves the plating of boride on metal, ceramic and other base materials, and is not suitable for preparing dense interfacial phase coating on the fiber surface

In 2015, Chinese invention patent CN 105331921 A disclosed a spraying powder, thermal spraying in-situ synthesis of zirconium boride-zirconium carbide based ceramic coating and its preparation method, which is composed of aluminum powder, zirconium hydride powder and boron carbide Zirconium boride composite coating is synthesized by thermal spraying in-situ reaction according to a certain ratio of powder as raw material. The preparation method of zirconium boride composite coating mainly involves the plating of boride on metal, ceramics and other substrate materials. To prepare a dense interfacial phase coating on the fiber surface

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