CN117209296A - C/TiC-Cu x Si y Composite material and preparation method thereof - Google Patents
C/TiC-Cu x Si y Composite material and preparation method thereof Download PDFInfo
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- CN117209296A CN117209296A CN202210967455.5A CN202210967455A CN117209296A CN 117209296 A CN117209296 A CN 117209296A CN 202210967455 A CN202210967455 A CN 202210967455A CN 117209296 A CN117209296 A CN 117209296A
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000010949 copper Substances 0.000 claims abstract description 38
- 230000008595 infiltration Effects 0.000 claims abstract description 24
- 238000001764 infiltration Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000005336 cracking Methods 0.000 claims abstract description 13
- IUYOGGFTLHZHEG-UHFFFAOYSA-N copper titanium Chemical compound [Ti].[Cu] IUYOGGFTLHZHEG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 29
- 239000004917 carbon fiber Substances 0.000 claims description 29
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 28
- 238000000151 deposition Methods 0.000 claims description 25
- 239000002296 pyrolytic carbon Substances 0.000 claims description 23
- 238000007598 dipping method Methods 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229920003257 polycarbosilane Polymers 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- 238000000197 pyrolysis Methods 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 6
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 230000001419 dependent effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 8
- 239000011159 matrix material Substances 0.000 abstract description 7
- 238000005470 impregnation Methods 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000002783 friction material Substances 0.000 description 3
- 239000011226 reinforced ceramic Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000009715 pressure infiltration Methods 0.000 description 2
- 229910016347 CuSn Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a C/TiC-Cu x Si y Composite materials and methods of making the same. The method prepares C/TiC-Cu by combining precursor impregnation cracking (PIP) with reactive infiltration (RMI) x Si y The composite material is prepared into porous low-density C/C-SiC base material through PIP process, and then titanium copper alloy is adopted to perform reaction infiltration on the base material to generate TiC and Cu in situ x Si y A matrix phase. The titanium copper alloy has good wettability with SiC base material and low infiltration temperature, and the prepared C/TiC-Cu x Si y The composite material has good mechanical and frictional wear properties.
Description
Technical Field
The invention relates to a carbon fiber reinforced ceramic matrix composite material, in particular to a C/TiC-Cu composite material x Si y Composite materials and methods of making the same.
Background
The carbon fiber reinforced ceramic matrix composite is often used for preparing friction materials such as brake discs and the like with excellent friction and wear properties, and has wide application prospects in the fields of aerospace, vehicle engineering, mechanical engineering and the like.
TiC has the advantages of high hardness, high melting point, good thermal stability and the like; the metal Cu and the alloy thereof have very good electric conduction, heat conduction and plasticity, and the carbon fiber reinforced ceramic matrix composite material composed of the metal Cu and the alloy thereof integrates the respective advantages, and has application value as a heat conduction, electric conduction, wear resistance and other materials.
Patent CN110983208A discloses a C/C-SiC-Cu composite material, a method for preparing the same and application thereof, and CuSn alloy is pressed into a C/C porous body deposited with SiC by a pressure infiltration method. Because of poor wettability of Cu and SiC, the adopted pressure infiltration method has high requirements on equipment, great difficulty and high cost.
Patent CN201010300558.3 discloses a preparation method of a copper-silicon alloy modified carbon/ceramic friction material, wherein a C/C porous material is paved on Cu and Si infiltration powder, and the copper-silicon alloy modified C/C-SiC friction material is prepared by compounding Si, C and Si with Cu. However, the infiltration process temperature is 1500-1900 ℃, and the mechanical property of the composite material can be reduced when the infiltration process temperature is too high; meanwhile, the prepared composite material contains a large amount of residual Si simple substance phase, thereby being unfavorable for the performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the C/TiC-Cu with good wettability and low preparation process temperature x Si y The composite material and the preparation method thereof are used for improving the mechanical property, the friction and the wear performance of the composite material.
In order to achieve the above object, the present invention provides the following technical solutions:
C/TiC-Cu x Si y The preparation method of the composite material comprises the following steps:
(1) Depositing a pyrolytic carbon interface layer on the fiber surface of the carbon fiber preform: depositing a pyrolytic carbon interface layer on the surface of the carbon fiber preform fiber by adopting a chemical vapor deposition method;
(2) Preparing a porous low-density C/C-SiC substrate: impregnating a carbon fiber preform deposited with a pyrolytic carbon interface layer by adopting Polycarbosilane (PCS), and then carrying out curing and high-temperature pyrolysis treatment to prepare a porous low-density C/C-SiC substrate;
(3) Preparation of C/TiC-Cu x Si y Composite material: adopting titanium copper alloy to perform reaction infiltration on a porous low-density C/C-SiC base material to prepare C/TiC-Cu x Si y A composite material.
Preferably, the carbon fiber preform is a needled preform with a density of 0.45-0.65g/cm 3 And/or performing high-temperature preheating treatment on the carbon fiber preform before performing the step (1).
Preferably, the high-temperature preheating treatment temperature is 1800-2000 ℃, and the heat preservation time is 2-3h.
Preferably, the carbon deposition treatment is carried out on the preform by adopting a chemical vapor deposition method, wherein the carbon source is propylene, the carrier gas is nitrogen, the deposition temperature is 800-1100 ℃, and the deposition time is dependent on the density of the carbon fiber preform after the pyrolytic carbon deposition.
Preferably, the density of the carbon fiber preform after depositing pyrolytic carbon is 0.9-1.1g/cm 3 。
Preferably, the impregnating temperature of the Polycarbosilane (PCS) is 10-100 ℃, the impregnating pressure is 0.5-2MPa, and the impregnating time is 0.5-2h; the curing temperature of the curing is 100-350 ℃, the curing pressure is 0.5-2MPa, and the curing time is 0.5-2h; the high-temperature cracking treatment temperature is 900-1200 ℃, and the cracking time is 2-4h.
Preferably, the porous low density C/C-SiC substrate has a density of 1.2 to 1.3g/cm 3 。
Preferably, the titanium-copper alloy comprises 20-70% of Ti in atomic weight;
preferably, the temperature of the reaction infiltration is 1200-1500 ℃, and the heat preservation time is 1-2h.
The invention also provides the C/TiC-Cu prepared by the method x Si y A composite material.
The invention prepares C/TiC-Cu by a method combining precursor impregnation cracking (PIP) and reaction infiltration (RMI) x Si y Compared with the prior art, the composite material has at least the following beneficial effects:
the wettability of metal Cu and SiC is poor, and the wettability of Cu alloy and SiC can be improved through the reaction of Ti in the titanium-copper alloy and SiC.
The melting point of the titanium-copper alloy in the patent is about 1000 ℃, and the infiltration process temperature is 1200-1500 ℃, so that the infiltration reaction temperature is greatly reduced, the damage of a metal melt to carbon fibers is reduced, and the improvement of the mechanical property of the composite material is facilitated; meanwhile, the composite material matrix only contains TiC and Cu x Si y The phase has no other impurity phase and stable performance.
Drawings
FIG. 1 is a C/TiC-Cu prepared in example 1 x Si y XRD pattern of the composite material;
FIG. 2 is a C/TiC-Cu prepared in example 1 x Si y And (5) a microstructure morphology diagram of the composite material.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the embodiments described below will be clearly and completely described in conjunction with the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are some, but not all, embodiments of the present invention, and all other embodiments obtained by persons of ordinary skill in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
The invention provides a C/TiC-Cu x Si y The preparation method of the composite material comprises the following steps:
(1) Depositing a pyrolytic carbon interface layer on the fiber surface of the carbon fiber preform: depositing a pyrolytic carbon interface layer on the surface of the carbon fiber preform fiber by adopting a chemical vapor deposition method;
(2) Preparing a porous low-density C/C-SiC substrate: impregnating a carbon fiber preform deposited with a pyrolytic carbon interface layer by adopting Polycarbosilane (PCS), and then carrying out curing and high-temperature pyrolysis treatment to prepare a porous low-density C/C-SiC substrate;
(3) Preparation of C/TiC-Cu x Si y Composite material: adopting titanium copper alloy to perform reaction infiltration on a porous low-density C/C-SiC base material to prepare C/TiC-Cu x Si y A composite material.
The preparation method comprises the steps of firstly preparing a porous low-density C/C-SiC base material from a carbon fiber preform subjected to carbon precipitation by adopting polycarbosilane through a PIP process, and then preparing C/TiC-Cu by adopting titanium copper alloy for reaction infiltration on the basis of the porous low-density C/C-SiC base material x Si y A composite material. The invention discovers that the titanium-copper alloy can be well wetted only in the porous low-density base material containing the SiC matrix; whether in a porous low density C/C substrate or in a B-containing substrate 4 The porous low-density base material of C cannot be well wetted, so that a relatively dense infiltration composite material cannot be obtained.
In addition, the invention also discovers that the C/TiC-Cu prepared by the invention x Si y The composite matrix phase contains only TiC and Cu x Si y The phase is free from other impurity phases, so that the obtained composite material has stable performance.
According to some preferred embodiments, the carbon fiber preform density is preferably 0.45-0.65g/cm 3 High-temperature pre-treatment at 1800-2000 deg.c/2-3 hr before carbon depositionHeat treatment; 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 is determined according to the density of the carbon fiber preform after the pyrolytic carbon is deposited; the density of the preform after depositing pyrolytic carbon is preferably 0.9-1.1g/cm 3 。
According to some preferred embodiments, the preparation process parameters of the porous low density C/C-SiC substrate are preferably: the dipping temperature is 10-100 ℃, the dipping pressure is 0.5-2MPa, and the dipping time is 0.5-2h; curing temperature is 100-350 ℃, curing pressure is 0.5-2MPa, and curing time is 0.5-2h; high-temperature cracking temperature is 900-1200 ℃ and cracking time is 2-4h; the porous low density C/C-SiC substrate preferably has a density of 1.2 to 1.3g/cm 3 。
According to some preferred embodiments, the infiltration alloying agent is a titanium copper alloy, wherein the atomic weight of Ti is preferably 20-70%; the temperature of the reaction infiltration is preferably 1200-1500 ℃, and the heat preservation time is preferably 1-2h.
In order to more clearly illustrate the technical scheme and advantages of the present invention, the present invention will be further described below with reference to examples.
Example 1
C/TiC-Cu 5 The Si composite material and the preparation method thereof specifically comprise the following steps:
(1) For a density of 0.6g/cm 3 Performing high-temperature preheating treatment of 1800 ℃/2h on the needled carbon fiber preform, and then depositing a pyrolytic carbon interface layer by adopting a chemical vapor deposition method, wherein the carbon source is propylene, the carrier gas is nitrogen, and the deposition temperature is preferably 900 ℃; the density of the preform after depositing pyrolytic carbon is 1.05g/cm 3 。
(2) And (3) dipping the carbon fiber preform deposited with the pyrolytic carbon interface layer by adopting Polycarbosilane (PCS), and then carrying out curing and pyrolysis treatment to prepare the porous low-density C/C-SiC substrate. The dipping temperature is room temperature, the dipping pressure is 1MPa, and the dipping time is 1.5h; the curing temperature is 220 ℃, the curing pressure is 1MPa, and the curing time is 1.5h; the high-temperature cracking temperature is 1000 ℃, and the cracking time is 3 hours; the density of the prepared porous low-density C/C-SiC base material is 1.22g/cm 3 。
(3) Adopts Ti 2 The Cu alloy carries out reaction infiltration on the porous low-density C/C-SiC base material, and the infiltration technological parameter is 1500 ℃/1h, thus preparing the C/TiC-Cu 5 Si composite material.
Through testing, the C/TiC-Cu obtained in the embodiment 5 Si composite material density of 3.92g/cm 3 The bending strength was 204MPa.
Example 2
C/TiC-Cu 3 The Si composite material and the preparation method thereof specifically comprise the following steps:
(1) For a density of 0.6g/cm 3 Performing high-temperature preheating treatment of 1800 ℃/2h on the needled carbon fiber preform, and then depositing a pyrolytic carbon interface layer by adopting a chemical vapor deposition method, wherein the carbon source is propylene, the carrier gas is nitrogen, and the deposition temperature is preferably 900 ℃; the density of the preform after depositing pyrolytic carbon is 1.0g/cm 3 。
(2) And (3) dipping the carbon fiber preform deposited with the pyrolytic carbon interface layer by adopting Polycarbosilane (PCS), and then carrying out curing and pyrolysis treatment to prepare the porous low-density C/C-SiC substrate. The dipping temperature is room temperature, the dipping pressure is 1MPa, and the dipping time is 1.5h; the curing temperature is 220 ℃, the curing pressure is 1MPa, and the curing time is 1.5h; the high-temperature cracking temperature is 1000 ℃, and the cracking time is 3 hours; the density of the prepared porous low-density C/C-SiC base material is 1.28g/cm 3 。
(3) Adopts Ti 2 The Cu alloy carries out reaction infiltration on the porous low-density C/C-SiC base material, and the infiltration technological parameter is 1450 ℃/1h, thus preparing the C/TiC-Cu 3 Si composite material.
Through testing, the C/TiC-Cu obtained in the embodiment 3 Si composite material density of 3.98g/cm 3 The bending strength was 196MPa.
Comparative example 1
A C/TiC-Cu composite material and a preparation method thereof specifically comprises the following steps:
(1) For a density of 0.6g/cm 3 The needled carbon fiber preform is subjected to high-temperature preheating treatment of 1800 ℃/2h, and then a chemical vapor deposition method is adopted to carry out pyrolytic carbon interfaceDepositing a layer, wherein the carbon source is propylene, the carrier gas is nitrogen, and the deposition temperature is preferably 900 ℃; the density of the preform after depositing pyrolytic carbon is 1.0g/cm 3 。
(2) The carbon fiber preform deposited with the pyrolytic carbon interface layer is immersed in bran , and then solidified and subjected to pyrolysis treatment to prepare the porous low-density C/C substrate. The dipping temperature is room temperature, the dipping pressure is 1MPa, and the dipping time is 1.5h; the curing temperature is 220 ℃, the curing pressure is 1MPa, and the curing time is 1.5h; the high-temperature cracking temperature is 900 ℃, and the cracking time is 3 hours; the density of the prepared porous low-density C/C substrate is 1.25g/cm 3 。
(3) Adopts Ti 2 And (3) carrying out reaction infiltration on the porous low-density C/C base material by the Cu alloy, wherein the infiltration technological parameter is 1500 ℃/1h, and preparing the C/TiC-Cu composite material.
Through testing, the density of the C/TiC-Cu composite material obtained in the embodiment is 1.65g/cm 3 The bending strength was 30MPa.
The above-disclosed embodiments of the present invention are intended to aid in understanding the contents of the present invention and to enable the same to be carried into practice, and it will be understood by those of ordinary skill in the art that various alternatives, variations and modifications are possible without departing from the spirit and scope of the invention. The invention should not be limited to what has been disclosed in the examples of the specification, but rather by the scope of the invention as defined in the claims.
Claims (10)
1. The preparation method of the C/TiC-CuxSiy composite material is characterized by comprising the following steps:
(1) Depositing a pyrolytic carbon interface layer on the surface of the carbon fiber preform fiber by adopting a chemical vapor deposition method;
(2) Impregnating a carbon fiber preform deposited with a pyrolytic carbon interface layer by adopting polycarbosilane, and then curing and high-temperature cracking to prepare a porous low-density C/C-SiC substrate;
(3) Adopting titanium copper alloy to perform reaction infiltration on a porous low-density C/C-SiC base material to prepare C/TiC-Cu x Si y A composite material.
2. The method of manufacturing according to claim 1, characterized in that: in the step (1), the carbon fiber preform is a needled preform with a density of 0.45-0.65g/cm 3 。
3. The method of manufacturing according to claim 1, characterized in that: and (3) carrying out high-temperature preheating treatment on the carbon fiber preform before the step (1), wherein the high-temperature preheating treatment temperature is 1800-2000 ℃, and the heat preservation time is 2-3h.
4. The method of manufacturing according to claim 1, characterized in that: in the step (1), the carbon source adopted in the chemical vapor deposition method is propylene, the carrier gas is nitrogen, the deposition temperature is 800-1100 ℃, and the deposition time is dependent on the density of the carbon fiber preform after depositing pyrolytic carbon.
5. The method of manufacturing according to claim 1, characterized in that: the density of the carbon fiber preform after depositing pyrolytic carbon is 0.9-1.1g/cm 3 。
6. The method of manufacturing according to claim 1, characterized in that: in the step (2), the dipping temperature of the dipping is 10-100 ℃, the dipping pressure is 0.5-2MPa, and the dipping time is 0.5-2h; the curing temperature of the curing is 100-350 ℃, the curing pressure is 0.5-2MPa, and the curing time is 0.5-2h; the high-temperature pyrolysis temperature is 900-1200 ℃, and the pyrolysis time is 2-4h.
7. The method of manufacturing according to claim 1, characterized in that: in step (2), the porous low density C/C-SiC substrate has a density of 1.2 to 1.3g/cm 3 。
8. The method of manufacturing according to claim 1, characterized in that: in the step (3), the atomic weight of Ti in the titanium-copper alloy is 20-70%.
9. The method of manufacturing according to claim 1, characterized in that: in the step (3), the temperature of the reaction infiltration is 1200-1500 ℃, and the heat preservation time is 1-2h.
10. A C/TiC-CuxSiy composite material prepared according to the method of any one of claims 1 to 9.
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