A C / TiC-Cu x Si y Composite material and preparation method thereof

Abstract

The present invention relates to a C / TiC-Cu x Si y Composite material and preparation method thereof. The method prepares C / TiC-Cu by combining precursor impregnation pyrolysis (PIP) with reactive melt infiltration (RMI). x Si y Composite materials, firstly, a porous low-density C / C-SiC substrate is prepared by PIP process, and then a titanium-copper alloy is used for reactive infiltration on the substrate to generate TiC and Cu in situ. x Si y Matrix phase. The titanium-copper alloy of the present invention has good wettability with the SiC substrate and low infiltration temperature. The prepared C / TiC-Cu x Si y The composite material has good mechanical and friction and wear properties.

Description

Technical Field

[0001] The present invention relates to a carbon fiber reinforced ceramic matrix composite material, in particular to a C / TiC-Cu x Si y Composite materials and methods for preparing the same. Background Art

[0002] Carbon fiber reinforced ceramic matrix composites are often used to prepare friction materials such as brake discs due to their excellent friction and wear properties, and have broad application prospects in aerospace, vehicle engineering, mechanical engineering and other fields.

[0003] TiC has the advantages of high hardness, high melting point and good thermal stability; metal Cu and its alloys have very good electrical and thermal conductivity and good plasticity. The carbon fiber reinforced ceramic matrix composites composed of the two combine the advantages of each and have application value as thermal conductive, electrical conductive and wear-resistant materials.

[0004] Patent CN110983208A discloses a C / C-SiC-Cu composite material, its preparation method, and its application. The method uses pressure infiltration to press a CuSn alloy into a C / C porous body containing SiC. Due to the poor wettability of Cu and SiC, the pressure infiltration method employed is demanding, difficult, and expensive, requiring high equipment requirements.

[0005] Patent CN201010300558.3 discloses a method for preparing a copper-silicon alloy-modified carbon / ceramic friction material. The method involves layering a C / C porous material onto a Cu and Si infiltration powder. The resulting composite is then composited through reactions between Si and C, and then Si and Cu, to produce a copper-silicon alloy-modified C / C-SiC friction material. However, the infiltration process temperature is between 1500°C and 1900°C, which is too high to achieve a reduction in the mechanical properties of the composite material. Furthermore, the resulting composite material contains a large amount of residual Si, which negatively impacts its performance. Summary of the Invention

[0006] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a C / TiC-Cu x Si y Composite materials and preparation methods thereof are used to improve the mechanical and friction and wear properties of composite materials.

[0007] In order to achieve the above object, the present invention provides the following technical solutions:

[0008] A C / TiC-Cu x Si y The preparation method of the composite material comprises the following steps:

[0009] (1) Depositing a pyrolytic carbon interface layer on the fiber surface of the carbon fiber preform: depositing a pyrolytic carbon interface layer on the fiber surface of the carbon fiber preform by chemical vapor deposition;

[0010] (2) Preparation of a porous low-density C / C-SiC substrate: A carbon fiber preform with a pyrolytic carbon interface layer was impregnated with polycarbosilane (PCS), and then cured and pyrolyzed to prepare a porous low-density C / C-SiC substrate;

[0011] (3) Preparation of C / TiC-Cu x Si y Composite material: C / TiC-Cu is prepared by reactive infiltration of porous low-density C / C-SiC substrate using titanium-copper alloy. x Si y Composite materials.

[0012] Preferably, the carbon fiber preform is a needle punched preform with a density of 0.45-0.65 g / cm 3 , and / or the carbon fiber preform is subjected to high temperature preheating treatment before performing step (1).

[0013] Preferably, the high temperature preheating treatment temperature is 1800-2000° C., and the holding time is 2-3 hours.

[0014] Preferably, the preform is carbonized by chemical vapor deposition, the carbon source used is propylene, the carrier gas is nitrogen, the deposition temperature is 800-1100° C., and the deposition time depends on the density of the carbon fiber preform after pyrolytic carbon deposition.

[0015] Preferably, the density of the carbon fiber preform after the deposition of pyrolytic carbon is 0.9-1.1 g / cm 3 .

[0016] Preferably, the impregnation temperature of the polycarbosilane (PCS) is 10-100°C, the impregnation pressure is 0.5-2MPa, and the impregnation time is 0.5-2h; the curing temperature of the curing is 100-350°C, the curing pressure is 0.5-2MPa, and the curing time is 0.5-2h; the temperature of the high-temperature pyrolysis treatment is 900-1200°C, and the pyrolysis time is 2-4h.

[0017] Preferably, the density of the porous low-density C / C-SiC substrate is 1.2-1.3 g / cm 3 .

[0018] Preferably, the atomic weight of Ti in the titanium-copper alloy accounts for 20-70%;

[0019] Preferably, the temperature of the reactive infiltration is 1200-1500° C., and the holding time is 1-2 hours.

[0020] The present invention also provides C / TiC-Cu prepared by the above method x Si y Composite materials.

[0021] The present invention prepares C / TiC-Cu by combining precursor impregnation pyrolysis (PIP) with reactive melt infiltration (RMI) x Si y The composite material has at least the following beneficial effects compared with the prior art:

[0022] Metal Cu and SiC have poor wettability. This patent improves the wettability of Cu alloy and SiC by reacting Ti in titanium-copper alloy with SiC.

[0023] The melting point of the titanium-copper alloy in this patent is about 1000℃, and the infiltration process temperature is 1200℃-1500℃, which greatly reduces the infiltration reaction temperature, helps to reduce the damage of the metal melt to the carbon fiber, and thus helps to improve the mechanical properties of the composite material; at the same time, the composite material matrix contains only TiC and Cu x Si y phase, without the presence of other impurities, and stable performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 The C / TiC-Cu prepared in Example 1 x Si y XRD patterns of composite materials;

[0025] Figure 2 The C / TiC-Cu prepared in Example 1 x Si y Microstructure morphology of composite materials. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0027] The present invention provides a C / TiC-Cu x Si y A method for preparing a composite material, comprising the following steps:

[0028] (1) Depositing a pyrolytic carbon interface layer on the fiber surface of the carbon fiber preform: depositing a pyrolytic carbon interface layer on the fiber surface of the carbon fiber preform by chemical vapor deposition;

[0029] (2) Preparation of a porous low-density C / C-SiC substrate: A carbon fiber preform with a pyrolytic carbon interface layer was impregnated with polycarbosilane (PCS), and then cured and pyrolyzed to prepare a porous low-density C / C-SiC substrate;

[0030] (3) Preparation of C / TiC-Cu x Si y Composite material: C / TiC-Cu is prepared by reactive infiltration of porous low-density C / C-SiC substrate using titanium-copper alloy. x Si y Composite materials.

[0031] The present invention firstly uses polycarbosilane to prepare a porous low-density C / C-SiC substrate from a carbon fiber preform after carbon deposition through a PIP process, and then uses a titanium-copper alloy to perform reactive infiltration to prepare a C / TiC-Cu substrate. x Si y Composite materials. The present invention found that titanium-copper alloys can only be well wetted in porous, low-density substrates containing SiC; however, they cannot be well wetted on either porous, low-density C / C substrates or porous, low-density substrates containing B4C, making it impossible to obtain a relatively dense infiltration composite material.

[0032] In addition, the present invention also found that the C / TiC-Cu x Si y The matrix phase of the composite material contains only TiC and Cu x Si y phase, without the presence of other impurities, so the obtained composite material has stable performance.

[0033] According to some preferred embodiments, the carbon fiber preform density is preferably 0.45-0.65 g / cm 3 , a high temperature preheating treatment of 1800-2000℃ / 2-3h is performed before carbon deposition; the carbon source used in the chemical vapor deposition process is propylene, the carrier gas is nitrogen, the deposition temperature is preferably 800-1100℃, and the deposition time depends on the density of the carbon fiber preform after the deposition of pyrolytic carbon; the density of the preform after the deposition of pyrolytic carbon is preferably 0.9-1.1g / cm 3 .

[0034] According to some preferred embodiments, the preparation process parameters of the porous low-density C / C-SiC substrate are preferably: impregnation temperature 10-100°C, impregnation pressure 0.5-2MPa, impregnation time 0.5-2h; curing temperature 100-350°C, curing pressure 0.5-2MPa, curing time 0.5-2h; high-temperature pyrolysis temperature 900-1200°C, pyrolysis time 2-4h; the density of the porous low-density C / C-SiC substrate is preferably 1.2-1.3g / cm 3 .

[0035] According to some preferred embodiments, the infiltration alloy infiltrant is a titanium-copper alloy, wherein the atomic weight of Ti is preferably 20-70%; the temperature of the reactive infiltration is preferably 1200-1500° C., and the holding time is preferably 1-2 h.

[0036] In order to more clearly illustrate the technical solutions and advantages of the present invention, the present invention is further described below with reference to embodiments.

[0037] Example 1

[0038] A C / TiC-Cu5Si composite material and a preparation method thereof, wherein the specific steps are as follows:

[0039] (1) Density is 0.6g / cm 3 The needle-punched carbon fiber preform is subjected to a high-temperature preheating treatment at 1800°C for 2 hours, and then a pyrolytic carbon interface layer is deposited thereon by chemical vapor deposition. The carbon source used is propylene, the carrier gas is nitrogen, and the deposition temperature is preferably 900°C. The density of the preform after pyrolytic carbon deposition is 1.05g / cm 3 .

[0040] (2) A carbon fiber preform with a pyrolytic carbon interface layer was impregnated with polycarbosilane (PCS), and then cured and pyrolyzed to prepare a porous low-density C / C-SiC substrate. The impregnation temperature was room temperature, the impregnation pressure was 1 MPa, and the impregnation time was 1.5 h; the curing temperature was 220 ° C, the curing pressure was 1 MPa, and the curing time was 1.5 h; the pyrolysis temperature was 1000 ° C, and the pyrolysis time was 3 h; the density of the prepared porous low-density C / C-SiC substrate was 1.22 g / cm 3 .

[0041] (3) Ti2Cu alloy was used to react infiltrate the porous low-density C / C-SiC substrate with the infiltration process parameters of 1500℃ / 1h to prepare C / TiC-Cu5Si composite material.

[0042] The density of the C / TiC-Cu5Si composite material obtained in this embodiment is 3.92 g / cm 3, the bending strength is 204MPa.

[0043] Example 2

[0044] A C / TiC-Cu3Si composite material and a preparation method thereof, wherein the specific steps are as follows:

[0045] (1) Density is 0.6g / cm 3 The needle-punched carbon fiber preform is subjected to a high-temperature preheating treatment at 1800°C for 2 hours, and then a pyrolytic carbon interface layer is deposited thereon by chemical vapor deposition. The carbon source used is propylene, the carrier gas is nitrogen, and the deposition temperature is preferably 900°C. The density of the preform after pyrolytic carbon deposition is 1.0 g / cm 3 .

[0046] (2) A carbon fiber preform with a pyrolytic carbon interface layer was impregnated with polycarbosilane (PCS), and then cured and pyrolyzed to prepare a porous low-density C / C-SiC substrate. The impregnation temperature was room temperature, the impregnation pressure was 1 MPa, and the impregnation time was 1.5 h; the curing temperature was 220 ° C, the curing pressure was 1 MPa, and the curing time was 1.5 h; the pyrolysis temperature was 1000 ° C, and the pyrolysis time was 3 h; the density of the prepared porous low-density C / C-SiC substrate was 1.28 g / cm 3 .

[0047] (3) Ti2Cu alloy was used to react infiltrate the porous low-density C / C-SiC substrate with the infiltration process parameters of 1450℃ / 1h to prepare C / TiC-Cu3Si composite material.

[0048] The density of the C / TiC-Cu3Si composite material obtained in this embodiment is 3.98 g / cm 3 , the bending strength is 196MPa.

[0049] Comparative Example 1

[0050] A C / TiC-Cu composite material and a preparation method thereof, wherein the specific steps are as follows:

[0051] (1) Density is 0.6g / cm 3 The needle-punched carbon fiber preform is subjected to a high-temperature preheating treatment at 1800°C for 2 hours, and then a pyrolytic carbon interface layer is deposited thereon by chemical vapor deposition. The carbon source used is propylene, the carrier gas is nitrogen, and the deposition temperature is preferably 900°C. The density of the preform after pyrolytic carbon deposition is 1.0 1g / cm 3 .

[0052] (2) A carbon fiber preform with a pyrolytic carbon interface layer was impregnated with bran, and then cured and pyrolyzed to prepare a porous low-density C / C substrate. The impregnation temperature was room temperature, the impregnation pressure was 1 MPa, and the impregnation time was 1.5 h; the curing temperature was 220 ° C, the curing pressure was 1 MPa, and the curing time was 1.5 h; the pyrolysis temperature was 900 ° C, and the pyrolysis time was 3 h; the density of the prepared porous low-density C / C substrate was 1.25 g / cm 3 .

[0053] (3) Ti2Cu alloy was used to perform reactive infiltration on the porous low-density C / C substrate with the infiltration process parameters of 1500℃ / 1h to prepare C / TiC-Cu composite material.

[0054] The density of the C / TiC-Cu composite material obtained in this embodiment is 1.65 g / cm 3 , the bending strength is 30MPa.

[0055] The specific embodiments of the present invention disclosed above are intended to facilitate understanding and implementation of the present invention. Those skilled in the art will appreciate that various substitutions, changes, and modifications are possible without departing from the spirit and scope of the present invention. The present invention should not be limited to the embodiments disclosed in this specification; the scope of protection of the present invention shall be determined by the scope defined in the claims.

Claims

1. A C / TiC-Cu x Si y The method for preparing a composite material is characterized in that: Preparation of C / TiC-Cu by combining precursor impregnation cracking (PIP) with reactive melt infiltration (RMI) x Si y The composite material comprises the following steps: (1) Depositing a pyrolytic carbon interface layer on the fiber surface of a carbon fiber preform by chemical vapor deposition; the carbon fiber preform is a needle-punched preform with a density of 0.45-0.65 g / cm 3 ; (2) a carbon fiber preform with a pyrolytic carbon interface layer deposited thereon is impregnated with polycarbosilane, and then cured and pyrolyzed to prepare a porous low-density C / C-SiC substrate; (3) The porous low-density C / C-SiC substrate was infiltrated with titanium-copper alloy to improve the wettability of Cu alloy and SiC through the reaction between Ti in titanium-copper alloy and SiC, and C / TiC-Cu was prepared. x Si y Composite material; the titanium-copper alloy has a Ti atomic weight of 20-70%; the reaction infiltration temperature is 1200-1500 ° C, and the holding time is 1-2 hours; the matrix of the composite material contains only TiC and Cu x Si y phase, without the existence of other mixed phases.

2. The preparation method according to claim 1, wherein: Before performing step (1), the carbon fiber preform is subjected to high-temperature preheating treatment, the high-temperature preheating treatment temperature is 1800-2000° C., and the insulation time is 2-3 hours.

3. The preparation method according to claim 1, wherein: In step (1), the carbon source used in the chemical vapor deposition method is propylene, the carrier gas is nitrogen, the deposition temperature is 800-1100° C., and the deposition time depends on the density of the carbon fiber preform after the pyrolytic carbon is deposited.

4. The preparation method according to claim 1, wherein: The density of the carbon fiber preform after deposition of pyrolytic carbon is 0.9-1.1g / cm 3 .

5. The preparation method according to claim 1, wherein: In step (2), the immersion temperature is 10-100°C, the immersion pressure is 0.5-2MPa, and the immersion time is 0.5-2h; the curing temperature is 100-350°C, the curing pressure is 0.5-2MPa, and the curing time is 0.5-2h; the high-temperature pyrolysis temperature is 900-1200°C, and the pyrolysis time is 2-4h.

6. The preparation method according to claim 1, wherein: In step (2), the density of the porous low-density C / C-SiC substrate is 1.2-1.3 g / cm 3 .

7. C / TiC-Cu prepared by the method according to any one of claims 1 to 6 x Si y Composite materials.

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