CN112830805A - Preparation method of carbon-ceramic wear-resistant composite material - Google Patents

Preparation method of carbon-ceramic wear-resistant composite material Download PDF

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CN112830805A
CN112830805A CN202110065574.7A CN202110065574A CN112830805A CN 112830805 A CN112830805 A CN 112830805A CN 202110065574 A CN202110065574 A CN 202110065574A CN 112830805 A CN112830805 A CN 112830805A
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composite material
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仝永刚
王斌
胡永乐
韩坤
沈宏继
华熳煜
张晓瑜
刘洋
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Changsha University of Science and Technology
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Abstract

The invention discloses a carbon-ceramic wear-resistant composite material and a preparation method thereofxCuy(x, y represent atomic ratio of alloy), TiC, C and a small amount of Cu phase. The preparation method comprises (1) preparing and pretreating C/C porous body; (2) preparing an interface protective coating on the surface of the carbon fiber of the C/C porous body; (3) densifying the C/C porous body with the interface protective coating to obtain a porous C/C preform; (4) preparing a Ti-Cu binary alloy; (5) and carrying out high-temperature infiltration treatment on the Ti-Cu binary alloy and the porous C/C prefabricated body to obtain the C/C-TiC-Cu composite material. The preparation method of the invention is simple, has high efficiency,the addition of TiC ceramic phase improves the frictional wear performance of the whole composite material, and TixCuyThe introduction of the alloy phase can effectively regulate and control the frictional wear performance of the composite material.

Description

Preparation method of carbon-ceramic wear-resistant composite material
Technical Field
The invention relates to a preparation method of a carbon-ceramic wear-resistant composite material, in particular to a ceramic matrix composite material taking carbon fiber as a reinforcing phase and titanium carbide and titanium-copper alloy as matrixes and a preparation method thereof.
Background
The carbon-ceramic friction material has the advantages of low density, high temperature resistance, high strength, stable friction performance, small abrasion loss, large brake ratio, long service life and the like; the carbon-ceramic composite material is often used for producing brake discs due to excellent friction and wear properties, has wide application prospects in emergency braking systems of high-speed trains, racing cars, high-grade cars and the like, and is considered to be the most promising friction braking material at present.
The titanium carbide ceramic has high melting point, small density, hardness higher than that of silicon carbide and other ceramics, excellent abrasion resistance and wide application prospect in the fields of abrasion-resistant materials, cutting tools, mechanical abrasion-resistant parts and the like.
The copper-based powder metallurgy material has the characteristics of stable friction factor, excellent wear resistance and heat resistance, good environmental adaptability, small damage to a brake disc and the like, and is widely used for domestic and foreign high-speed trains; when the brake is used for high-speed braking, the copper matrix is softened, so that damage to mating parts can be effectively reduced, the surface of the brake disc is free from scratches, hot spots, scratches and the like, and the brake disc is excellent in performance.
The invention combines the advantages of the carbon-ceramic composite material and the copper-based powder metallurgy material, overcomes the defects of the carbon-ceramic composite material and the copper-based powder metallurgy material, adopts Ti-Cu binary alloy as an impregnant and carbon fiber as a reinforcing phase by a reaction infiltration method, and prepares a novel C/C-TiC-Cu composite material at a low temperature.
Disclosure of Invention
The invention aims to provide a novel C/C-TiC-Cu composite material and a low-temperature and high-efficiency preparation method thereof, and the technical problem is solved by the invention through the following scheme:the phase composition of the composite material is TixCuy(x and y represent the atomic ratio of alloy), TiC, C and a small amount of Cu phase, wherein the composite material takes carbon fiber as a reinforcing phase and TixCuyTiC and C as matrix, containing small amount of Cu phase, carbon fiber reinforcement 10-40 vol%, carbon matrix 10-20 vol%, TiC matrix 10-50 vol%, and TixCuyThe volume fraction of the matrix is 10-40%, and the volume fraction of Cu is 5-10%.
The invention also discloses a preparation method of the composite material, which comprises the following steps.
1. Preparing and pretreating a C/C porous body.
The preparation of the C/C porous body is to make carbon fiber or carbon fiber cloth into a three-dimensional weaving structure, a two-dimensional carbon cloth laminated structure or a needle-punched carbon fiber felt structure; the pretreatment of the C/C porous body is carried out by subjecting the C/C porous body to a vacuum of 5.0X 10-2The Pa-3Pa temperature is 1200-1800 ℃ for 2-4 h.
2. Preparing an interface protective coating on the surface of the carbon fiber of the C/C porous body.
The method for preparing the interface protective coating on the surface of the carbon fiber of the C/C porous body comprises the steps of firstly generating a layer of pyrolytic carbon or boron nitride interface layer on the surface of the carbon fiber by a chemical vapor deposition method, wherein the thickness of the pyrolytic carbon or boron nitride interface layer is 40-300 nm; then, with TiC14-CH4-H2The mixture is used as a carbon source and a titanium source, a chemical vapor deposition process is adopted, heat treatment is carried out for 3-6h at the temperature of 950-1050 ℃, and a titanium carbide protective coating with controllable thickness is deposited and generated on the surface of the C/C porous body interface layer.
3. And densifying the C/C porous body with the interface protective coating to obtain the porous C/C preform.
The method for densifying the C/C porous body is to carry out chemical vapor deposition densification on the C/C porous body at 960-1050 ℃ in an inert gas atmosphere by taking propylene as a carbon source; then, carrying out graphitization heat treatment on the C/C porous body, namely carrying out heat treatment on the C/C porous body for 2-4h at 2100-2300 ℃ in vacuum or inert atmosphere to finally obtain the porous C/C preform.
And 4, preparing the Ti-Cu binary alloy.
The Ti-Cu binary alloy is prepared by adopting an electric arc melting method or an induction melting method, and the used raw materials are a titanium metal block and a copper metal block with the purity of more than or equal to 99.9 percent; the Ti-Cu binary alloy prepared by the design has the Ti atom content of 20-70%.
5. And carrying out high-temperature infiltration treatment on the Ti-Cu binary alloy and the porous C/C prefabricated body to obtain the C/C-TiC-Cu composite material.
The high-temperature infiltration treatment is to adopt a reaction infiltration method to take the prepared Ti-Cu binary alloy as an osmotic agent, place the Ti-Cu binary alloy on the porous C/C prefabricated body, heat up the Ti-Cu binary alloy to be above the melting point of the Ti-Cu binary alloy by 100 ℃ at the speed of 5-20 ℃/min under the vacuum or inert gas atmosphere, and preserve the heat for 1-5 h.
Preferably, by controlling TiC14-CH4-H2The mass percentages of the components in the mixture and the chemical vapor deposition time can effectively control the thickness of the titanium carbide protective coating.
Preferably, the Ti-Cu alloy is prepared by an arc melting method or an induction melting method, and the used raw materials are a titanium metal block and a copper metal block with the purity of more than or equal to 99.9 percent; the Ti-Cu binary alloy is designed to have a Ti atom content of 20-70% based on the in-situ reaction and reaction kinetics of the alloy and carbon.
According to the invention, carbon fibers and Cu are introduced into the TiC phase ceramic matrix, the brittleness of the TiC body ceramic is overcome by using the toughening effect of the carbon fibers, and the toughness and the frictional wear performance of the material are improved.
Compared with the prior art, the preparation method has the advantages that.
(1) The C/C-TiC-Cu composite material provided by the invention has the advantages that the titanium carbide ceramic phase with high melting point, small density and excellent wear resistance is introduced, so that the overall friction and wear resistance of the composite material is improved.
(2) The C/C-TiC-Cu composite material is prepared by introducing TixCuyThe matrix can effectively regulate and control the overall frictional wear performance of the composite material and can effectively reduce the damage to mating parts.
(3) Aiming at the problems that when titanium carbide is introduced into the porous C/C prefabricated body, the melting point of a titanium simple substance is too high, and experimental conditions are difficult to achieve, the Ti-Cu binary low-melting-point alloy is used as a infiltrant, so that the reaction temperature of 600-800 ℃, the production efficiency is improved, and resources are saved.
(4) The pyrolytic carbon or boron nitride interface layer and the titanium carbide interface protective coating with controllable thickness prepared by the invention ensure that the C/C-TiC-Cu composite material has good frictional wear performance and mechanical property, and the bending strength of the material can reach 273.641 MPa.
(5) The process adopted by the invention can form the friction pair in net size, and has the advantages of simple preparation process, low requirement on equipment, high production efficiency and lower preparation cost.
Drawings
FIG. 1 is an optical photograph of the C/C-TiC-Cu composite material obtained in example 1 of the present invention.
FIG. 2 is an XRD pattern of the C/C-TiC-Cu composite material prepared in example 1 of the present invention.
FIG. 3 is a scanning electron microscope image of a cross section of the C/C-TiC-Cu composite material prepared in example 1 of the present invention.
FIG. 4 is a three-point bending stress-displacement curve of the C/C-TiC-Cu composite material prepared in example 1 of the present invention.
FIG. 5 is an XRD pattern of the C/C-TiC-Cu composite material prepared in example 2 of the present invention.
FIG. 6 is a scanning electron microscope image of a cross section of the C/C-TiC-Cu composite material prepared in example 2 of the present invention.
Detailed Description
The technical solution of the present invention will be clearly and completely described below, and it should be apparent that the described embodiments are a part of the embodiments of the present invention, and not all of the embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless otherwise specified, the starting materials described in the examples of the present application are all commercially available.
Example 1
The method comprises the following steps: preparing and pretreating a C/C porous body.
Adopting continuous carbon fiber to weave weftless carbon cloth or carding to form thin net tyre, adopting three-dimensional needling weaving method to prepare the obtained C/C porous body, placing the porous body into vacuum degree of 5.0 x 10-2Pa, and the temperature is 1300 ℃ for 2 h.
Step two: preparing an interface protective coating on the surface of the carbon fiber of the C/C porous body.
Firstly, generating a pyrolytic carbon interface layer on the surface of carbon fiber by using a chemical vapor deposition method on the C/C porous body prepared in the step one, wherein the thickness of the pyrolytic carbon interface layer is 50 nm; then, with TiC14-CH4-H2The mixture is used as a carbon source and a titanium source, a chemical vapor deposition process is adopted, heat treatment is carried out for 3 hours at the temperature of 950 ℃, and a titanium carbide protective coating with the thickness of 50nm is deposited and generated on the surface of the interface layer of the C/C porous body.
Step three: and densifying the C/C porous body with the interface protective coating to obtain the porous C/C preform.
Performing chemical vapor deposition densification on the C/C porous body in the second step by taking propylene as a carbon source under the condition of the temperature of 1050 ℃ in the argon atmosphere; then, the C/C porous body is subjected to graphitization heat treatment, namely, the C/C porous body is subjected to heat treatment at 2300 ℃ for 2 hours under an argon atmosphere, and finally, a porous C/C preform is obtained.
Step four: preparing a Ti-Cu binary alloy;
the Ti-Cu binary alloy is prepared by an electric arc melting method, and the used raw materials are a titanium metal block and a copper metal block with the purity of more than or equal to 99.9 percent; the Ti-Cu binary alloy is designed to have the Ti atom content of 66.7 percent based on the in-situ reaction and the reaction kinetics of the alloy and carbon.
Step five: and carrying out high-temperature infiltration treatment on the Ti-Cu binary alloy and the porous C/C prefabricated body to obtain the C/C-TiC-Cu composite material.
And taking a Ti-Cu binary alloy with the Ti atom content of 66.7% as an infiltration agent, placing the Ti-Cu binary alloy on the porous C/C prefabricated body, heating to 1100 ℃ at the speed of 20 ℃/min under the argon atmosphere, preserving the heat for 2h, and cooling along with the furnace to obtain the C/C-TiC-Cu composite material.
C/C-The section of the TiC-Cu composite material is shown in FIG. 3 by scanning electron microscope, wherein the dark phase belongs to carbon fiber, the gray phase belongs to TiC phase, and the bright silver phase belongs to TixCuyA substrate; FIG. 1 is an optical photograph of the C/C-TiC-Cu composite material prepared in example 1; FIG. 2 is an XRD pattern of the C/C-TiC-Cu composite material prepared in example 1. FIG. 4 is a three-point bending stress-displacement curve diagram of the C/C-TiC-Cu composite material prepared in this example 1, and the bending strength is as high as 273.641 MPa.
Example 2
The method comprises the following steps: preparing and pretreating a C/C porous body.
Adopting continuous carbon fiber to weave weftless carbon cloth or carding to form thin net tyre, adopting three-dimensional needling weaving method to prepare the obtained C/C porous body, placing the porous body into vacuum degree of 5.0 x 10-2Pa, and the temperature is 1200 ℃ for 3 h.
Step two: preparing an interface protective coating on the surface of the carbon fiber of the C/C porous body.
Firstly, generating a pyrolytic carbon interface layer on the surface of carbon fiber by using a chemical vapor deposition method on the C/C porous body prepared in the step one, wherein the thickness of the pyrolytic carbon interface layer is 100 nm; then, with TiC14-CH4-H2The mixture is used as a carbon source and a titanium source, a chemical vapor deposition process is adopted, heat treatment is carried out for 4 hours at the temperature of 1000 ℃, and a titanium carbide protective coating with the thickness of 80nm is deposited and generated on the surface of the interface layer of the C/C porous body.
Step three: and densifying the C/C porous body with the interface protective coating to obtain the porous C/C preform.
Performing chemical vapor deposition densification on the C/C porous body in the second step at 1050 ℃ in an argon atmosphere by taking propylene as a carbon source; then, the C/C porous body is subjected to graphitization heat treatment, namely, the C/C porous body is subjected to heat treatment at 2200 ℃ for 2 hours under an argon atmosphere, and finally, a porous C/C preform is obtained.
Step four: and (3) preparing a Ti-Cu binary alloy.
The Ti-Cu binary alloy is prepared by an electric arc melting method, and the used raw materials are a titanium metal block and a copper metal block with the purity of more than or equal to 99.9 percent; the Ti-Cu binary alloy is designed to have a Ti atom content of 50% based on the in-situ reaction and reaction kinetics of the alloy and carbon.
Step five: and carrying out high-temperature infiltration treatment on the Ti-Cu binary alloy and the porous C/C prefabricated body to obtain the C/C-TiC-Cu composite material.
And taking a Ti-Cu binary alloy with the Ti atom content of 50% as an infiltration agent, placing the Ti-Cu binary alloy on the porous C/C prefabricated body, heating to 1100 ℃ at the speed of 15 ℃/min under the argon atmosphere, preserving the heat for 2h, and cooling along with the furnace to obtain the C/C-TiC-Cu composite material.
The scanning electron micrograph of the cross section of the C/C-TiC-Cu composite material prepared in this example 2 is shown in FIG. 6, in which the dark phase belongs to carbon fibers, the gray phase belongs to TiC phase, and the bright silver phase belongs to TixCuyA substrate; FIG. 5 is an XRD pattern of the C/C-TiC-Cu composite material prepared in this example.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention; accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (8)

1. The preparation method of the carbon-ceramic wear-resistant composite material is characterized by comprising the following steps:
(1) preparing and pretreating a C/C porous body;
(2) preparing an interface protective coating on the surface of the carbon fiber of the C/C porous body;
(3) densifying the C/C porous body with the interface protective coating to obtain a porous C/C preform;
(4) preparing a Ti-Cu binary alloy;
(5) and carrying out high-temperature infiltration treatment on the Ti-Cu binary alloy and the porous C/C prefabricated body to obtain the C/C-TiC-Cu composite material.
2. The preparation method of the carbon-ceramic wear-resistant composite material as claimed in claim 1, wherein the preparation method comprises the following steps: what is needed isThe phase composition of the composite material is TixCuy(x and y represent the atomic ratio of alloy), TiC, C and a small amount of Cu phase, wherein the composite material takes carbon fiber as a reinforcing phase and TixCuyTiC and C as matrix, containing small amount of Cu phase, carbon fiber reinforcement 10-40 vol%, carbon matrix 10-20 vol%, TiC matrix 10-50 vol%, and TixCuyThe volume fraction of the matrix is 10-40%, and the volume fraction of Cu is 5-10%.
3. The method of claim 1, wherein: preparing the C/C porous body in the step (1) by making carbon fibers or carbon fiber cloth into a three-dimensional woven structure, a two-dimensional carbon cloth laminated structure or a needled carbon fiber felt structure; the pretreatment of the C/C porous body in the step (1) is carried out by subjecting the C/C porous body to a vacuum of 5.0X 10-2Pa-3Pa, and the temperature is 1200-1800 ℃ for 2-4 h.
4. The method of claim 1, wherein: the method for preparing the interface protective coating on the surface of the carbon fiber of the C/C porous body in the step (2) is that firstly, a layer of pyrolytic carbon or boron nitride interface layer is generated on the surface of the carbon fiber by adopting a chemical vapor deposition method, and the thickness is 40-300 nm; then, with TiC14-CH4-H2The mixture is used as a carbon source and a titanium source, a chemical vapor deposition process is adopted, heat treatment is carried out for 3-6h at the temperature of 950-; by controlling TiC14-CH4-H2The mass percentages of the components in the mixture and the chemical vapor deposition time can effectively control the thickness of the titanium carbide protective coating.
5. The method of claim 1, wherein: in the step (3), propylene is used as a carbon source, and the C/C porous body is subjected to chemical vapor deposition densification at the temperature of 960-1050 ℃ in an inert gas atmosphere; then, carrying out graphitization heat treatment on the C/C porous body, namely carrying out heat treatment on the C/C porous body for 2-4h at 2100-2300 ℃ in vacuum or inert atmosphere to finally obtain the porous C/C preform.
6. The method of claim 1, wherein: the Ti-Cu binary alloy in the step (4) is prepared by adopting an electric arc melting method or an induction melting method, and the used raw materials are a titanium metal block and a copper metal block with the purity of more than or equal to 99.9 percent; the Ti-Cu binary alloy is designed to have a Ti atom content of 20-70% based on the in-situ reaction and reaction kinetics of the alloy and carbon.
7. The method of claim 1, wherein: and (5) the high-temperature infiltration treatment in the step (5) is high-temperature infiltration treatment, namely, a reaction infiltration method is adopted to take the prepared Ti-Cu binary alloy as a penetrating agent, the Ti-Cu binary alloy is placed on the porous C/C prefabricated body, the temperature is increased to be above the melting point of the Ti-Cu binary alloy by 100-200 ℃ at the speed of 5-20 ℃/min under the vacuum or inert gas atmosphere, and the temperature is kept for 1-5h to obtain the C/C-TiC-Cu composite material.
8. The carbon-ceramic wear-resistant composite material as claimed in claim 1, wherein: the material is applied to the field of friction braking.
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