CN105819860A - Titanium carbide-silicon carbide-titanium silicide composite ceramic material and preparation method thereof - Google Patents

Titanium carbide-silicon carbide-titanium silicide composite ceramic material and preparation method thereof Download PDF

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CN105819860A
CN105819860A CN201610124298.6A CN201610124298A CN105819860A CN 105819860 A CN105819860 A CN 105819860A CN 201610124298 A CN201610124298 A CN 201610124298A CN 105819860 A CN105819860 A CN 105819860A
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CN105819860B (en
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刘佩佩
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Zhuzhou Huachi New Materials Co., Ltd.
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刘佩佩
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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    • C04B2235/3891—Silicides, e.g. molybdenum disilicide, iron silicide
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    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/404—Refractory metals

Abstract

The invention discloses a titanium carbide-silicon carbide-titanium silicide composite ceramic material. The composite ceramic material comprises, by weight, 65-68 parts of titanium carbide powder, 32-40 parts of silicon carbide powder, 26-29 parts of titanium silicide powder, 3-6 parts of alumina powder, 5-8 parts of indium oxide nanopowder and 2-4 parts of molybdenum powder. The invention also provides a preparation method of the titanium carbide-silicon carbide-titanium silicide composite ceramic material. The titanium carbide-silicon carbide-titanium silicide composite ceramic material prepared in the invention has the advantages of good bending strength, good fracture toughness, and excellent thermal shock resistance, so development of the application range of silicon carbide ceramic is facilitated.

Description

A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material and preparation method thereof
Technical field
The present invention relates to ceramic composite technical field, specifically a kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material and preparation method thereof.
Background technology
The development history of pottery is an important ingredient of Chinese civilization history, and China is as one of four major acids ancient country, for the progress of human society With the contribution that development is made that brilliance, wherein invention and the development of pottery has more unique meaning, and on Chinese history, each Chao Gedai has different art Style and different technical characteristics.Along with the development of modern science technology, occur in that the most again many new ceramic kinds.They not in use by or It is rarely employed the traditional ceramics raw materials such as clay, Anhydrite, quartz, but uses other special materials, even expand non-silicate to, non-oxidized substance Scope, and occur in that much new technique." Ceramic " word is interpreted as various inorganic non-gold by the document of some countries of US and European Belong to the common name of solid material.Therefore the implication of pottery surmounts the most far away the narrowest traditional view.
Titanium carbide is typical transition metal carbide.Its of bonding is to be blended in same crystal structure by ionic bond, covalent bond and metallic bond, because of This titanium carbide has many unique performances.It is basic that the structures shape of crystal titanium carbide has high rigidity, high-melting-point, wear-resistant and electric conductivity etc. Feature.Titanium carbide ceramic is to develop the widest material in titanium, zirconium, chromium transition metal carbide, in machinery, electronics, chemical industry, environmental conservation, gathers Many fields such as temperature shift reactor, national defense industry are widely used.But the fragility of titanium carbide ceramic is big, toughness is not enough and heat shock resistance can be poor, this A little utilizations limiting it the most to a certain extent.
Summary of the invention
It is an object of the invention to provide a kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material and preparation method thereof, to solve above-mentioned background technology The problem of middle proposition.
For achieving the above object, the present invention provides following technical scheme:
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made up of according to the raw material of weight portion following: titanium carbide powder 65-68 part, carbon SiClx powder 32-40 part, titanium silicide powder 26-29 part, alumina powder 3-6 part, nano indium oxide powder 5-8 part, molybdenum powder 2-4 part.
As the further scheme of the present invention: be made up of according to the raw material of weight portion following: titanium carbide powder 66-67 part, silicon carbide powder 34-38 Part, titanium silicide powder 27-28 part, alumina powder 4-5 part, nano indium oxide powder 6-7 part, molybdenum powder 3-4 part.
As the present invention further scheme: be made up of according to the raw material of weight portion following: titanium carbide powder 67 parts, silicon carbide powder 36 parts, 28 parts of titanium silicide powder, alumina powder 5 parts, 6 parts of nano indium oxide powder, molybdenum powder 3 parts.
The preparation method of described titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, step is as follows:
1) weigh titanium carbide powder, silicon carbide powder and titanium silicide powder, put in ball grinder, using dehydrated alcohol as disperse medium, ball milling 8-12h, Obtain the first dispersion liquid；
2) the first dispersion liquid is placed in vacuum drying oven, at 140-150 DEG C, is dried 2-3h, to remove dehydrated alcohol, it is thus achieved that the first mixed powder Material；
3) being put in vacuum sintering furnace by the first mixed powder, and be sintered at 0.1-0.5Pa, 1230-1260 DEG C, sintering time is 1-2h, it is thus achieved that sintering feed；
4), after being pulverized by sintering feed, it is thus achieved that sintering feed powder, weigh alumina powder, nano indium oxide powder and molybdenum powder, and with sintering feed powder Merge, put into in ball grinder, using dehydrated alcohol as disperse medium, ball milling 15-18h, it is thus achieved that the second dispersion liquid；
5) the second dispersion liquid is placed in vacuum drying oven, at 155-160 DEG C, is dried 4-5h, to remove dehydrated alcohol, it is thus achieved that the second mixed powder Material；
6) by the second mixed powder isostatic pressing under 120Mpa, it is thus achieved that biscuit；
7) putting in vacuum sintering furnace by biscuit, be sintered at 0.1-0.2Pa, 1680-1740 DEG C, sintering time is 1-2h, it is thus achieved that carbonization Titanium-carborundum-titanium silicide composite ceramic material.
Compared with prior art, the invention has the beneficial effects as follows: titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material prepared by the present invention, bending resistance is strong Degree is 986-1050Mpa, and fracture toughness is 5.9-6.5Mpa m1/2, bending strength and fracture toughness all show well, and heat shock resistance number of times reaches 152-164 time, thermal shock resistance is excellent, is conducive to expanding the range of application of silicon carbide ceramics.Titanium carbide-titanium carbide silicon-silicon prepared by the present invention Change titanium composite ceramic material is by adding nano indium oxide powder and molybdenum powder, and nano indium oxide powder, molybdenum powder coordinate with other components, it is possible to strengthen carbon Change the mechanical property of titanium-carborundum-titanium silicide composite ceramic material.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in more detail.
Embodiment 1
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made up of according to the raw material of weight portion following: titanium carbide powder 65 parts, carbonization Si powder 32 parts, 26 parts of titanium silicide powder, alumina powder 3 parts, 5 parts of nano indium oxide powder, molybdenum powder 2 parts.
The preparation method of the silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material, step is as follows:
1) weigh titanium carbide powder, silicon carbide powder and titanium silicide powder, put in ball grinder, using dehydrated alcohol as disperse medium, ball milling 8h, Obtain the first dispersion liquid；
2) the first dispersion liquid is placed in vacuum drying oven, at 140 DEG C, is dried 2h, to remove dehydrated alcohol, it is thus achieved that the first mixed powder；
3) being put in vacuum sintering furnace by the first mixed powder, and be sintered at 0.1Pa, at 1230 DEG C, sintering time is 1h, it is thus achieved that Sintering feed；
4), after being pulverized by sintering feed, it is thus achieved that sintering feed powder, weigh alumina powder, nano indium oxide powder and molybdenum powder, and with sintering feed powder Merge, put into in ball grinder, using dehydrated alcohol as disperse medium, ball milling 15h, it is thus achieved that the second dispersion liquid；
5) the second dispersion liquid is placed in vacuum drying oven, at 155 DEG C, is dried 4h, to remove dehydrated alcohol, it is thus achieved that the second mixed powder；
6) by the second mixed powder isostatic pressing under 120Mpa, it is thus achieved that biscuit；
7) putting in vacuum sintering furnace by biscuit, be sintered at 0.1Pa, at 1680 DEG C, sintering time is 1h, it is thus achieved that titanium carbide-titanium carbide silicon- Titanium silicide composite ceramic material.
Embodiment 2
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made up of according to the raw material of weight portion following: titanium carbide powder 68 parts, carbonization Si powder 40 parts, 29 parts of titanium silicide powder, alumina powder 6 parts, 8 parts of nano indium oxide powder, molybdenum powder 4 parts.
The preparation method of the silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material, step is as follows:
1) weigh titanium carbide powder, silicon carbide powder and titanium silicide powder, put in ball grinder, using dehydrated alcohol as disperse medium, ball milling 12h, Obtain the first dispersion liquid；
2) the first dispersion liquid is placed in vacuum drying oven, at 150 DEG C, is dried 3h, to remove dehydrated alcohol, it is thus achieved that the first mixed powder；
3) being put in vacuum sintering furnace by the first mixed powder, and be sintered at 0.5Pa, at 1260 DEG C, sintering time is 2h, it is thus achieved that Sintering feed；
4), after being pulverized by sintering feed, it is thus achieved that sintering feed powder, weigh alumina powder, nano indium oxide powder and molybdenum powder, and with sintering feed powder Merge, put into in ball grinder, using dehydrated alcohol as disperse medium, ball milling 18h, it is thus achieved that the second dispersion liquid；
5) the second dispersion liquid is placed in vacuum drying oven, at 160 DEG C, is dried 5h, to remove dehydrated alcohol, it is thus achieved that the second mixed powder；
6) by the second mixed powder isostatic pressing under 120Mpa, it is thus achieved that biscuit；
7) putting in vacuum sintering furnace by biscuit, be sintered at 0.2Pa, at 1740 DEG C, sintering time is 2h, it is thus achieved that titanium carbide-titanium carbide silicon- Titanium silicide composite ceramic material.
Embodiment 3
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made up of according to the raw material of weight portion following: titanium carbide powder 67 parts, carbonization Si powder 36 parts, 28 parts of titanium silicide powder, alumina powder 5 parts, 6 parts of nano indium oxide powder, molybdenum powder 3 parts.
The preparation method of the silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material, step is as follows:
1) weigh titanium carbide powder, silicon carbide powder and titanium silicide powder, put in ball grinder, using dehydrated alcohol as disperse medium, ball milling 10h, Obtain the first dispersion liquid；
2) the first dispersion liquid is placed in vacuum drying oven, at 145 DEG C, is dried 2.5h, to remove dehydrated alcohol, it is thus achieved that the first mixed powder；
3) being put in vacuum sintering furnace by the first mixed powder, and be sintered at 0.3Pa, at 1250 DEG C, sintering time is 2h, it is thus achieved that Sintering feed；
4), after being pulverized by sintering feed, it is thus achieved that sintering feed powder, weigh alumina powder, nano indium oxide powder and molybdenum powder, and with sintering feed powder Merge, put into in ball grinder, using dehydrated alcohol as disperse medium, ball milling 16h, it is thus achieved that the second dispersion liquid；
5) the second dispersion liquid is placed in vacuum drying oven, at 158 DEG C, is dried 5h, to remove dehydrated alcohol, it is thus achieved that the second mixed powder；
6) by the second mixed powder isostatic pressing under 120Mpa, it is thus achieved that biscuit；
7) putting in vacuum sintering furnace by biscuit, be sintered at 0.2Pa, at 1700 DEG C, sintering time is 1.5, it is thus achieved that titanium carbide-titanium carbide silicon- Titanium silicide composite ceramic material.
Embodiment 4
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made up of according to the raw material of weight portion following: titanium carbide powder 65 parts, carbonization Si powder 38 parts, 26 parts of titanium silicide powder, alumina powder 6 parts, 8 parts of nano indium oxide powder, molybdenum powder 3 parts.
The preparation method of the silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material, step is as follows:
1) weigh titanium carbide powder, silicon carbide powder and titanium silicide powder, put in ball grinder, using dehydrated alcohol as disperse medium, ball milling 10h, Obtain the first dispersion liquid；
2) the first dispersion liquid is placed in vacuum drying oven, at 150 DEG C, is dried 2h, to remove dehydrated alcohol, it is thus achieved that the first mixed powder；
3) being put in vacuum sintering furnace by the first mixed powder, and be sintered at 0.5Pa, at 1260 DEG C, sintering time is 2h, it is thus achieved that Sintering feed；
4), after being pulverized by sintering feed, it is thus achieved that sintering feed powder, weigh alumina powder, nano indium oxide powder and molybdenum powder, and with sintering feed powder Merge, put into in ball grinder, using dehydrated alcohol as disperse medium, ball milling 18h, it is thus achieved that the second dispersion liquid；
5) the second dispersion liquid is placed in vacuum drying oven, at 155 DEG C, is dried 5h, to remove dehydrated alcohol, it is thus achieved that the second mixed powder；
6) by the second mixed powder isostatic pressing under 120Mpa, it is thus achieved that biscuit；
7) putting in vacuum sintering furnace by biscuit, be sintered at 0.2Pa, at 1690 DEG C, sintering time is 2h, it is thus achieved that titanium carbide-titanium carbide silicon- Titanium silicide composite ceramic material.
Embodiment 5
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made up of according to the raw material of weight portion following: titanium carbide powder 67 parts, carbonization Si powder 38 parts, 29 parts of titanium silicide powder, alumina powder 5 parts, 5 parts of nano indium oxide powder, molybdenum powder 3 parts.
The preparation method of the silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material, step is as follows:
1) weigh titanium carbide powder, silicon carbide powder and titanium silicide powder, put in ball grinder, using dehydrated alcohol as disperse medium, ball milling 11h, Obtain the first dispersion liquid；
2) the first dispersion liquid is placed in vacuum drying oven, at 145 DEG C, is dried 3h, to remove dehydrated alcohol, it is thus achieved that the first mixed powder；
3) being put in vacuum sintering furnace by the first mixed powder, and be sintered at 0.1Pa, at 1250 DEG C, sintering time is 1h, it is thus achieved that Sintering feed；
4), after being pulverized by sintering feed, it is thus achieved that sintering feed powder, weigh alumina powder, nano indium oxide powder and molybdenum powder, and with sintering feed powder Merge, put into in ball grinder, using dehydrated alcohol as disperse medium, ball milling 18h, it is thus achieved that the second dispersion liquid；
5) the second dispersion liquid is placed in vacuum drying oven, at 157 DEG C, is dried 4.5h, to remove dehydrated alcohol, it is thus achieved that the second mixed powder；
6) by the second mixed powder isostatic pressing under 120Mpa, it is thus achieved that biscuit；
7) putting in vacuum sintering furnace by biscuit, be sintered at 0.1Pa, at 1740 DEG C, sintering time is 2h, it is thus achieved that titanium carbide-titanium carbide silicon- Titanium silicide composite ceramic material.
Comparative example 1
Compared with Example 3, without nano indium oxide powder and molybdenum powder, other are same as in Example 3.
Comparative example 2
Compared with Example 3, without nano indium oxide powder, other are same as in Example 3.
Performance test
Making a service test embodiment 1-5 and comparative example 1-2, result of the test is as shown in table 1.
Table 1 performance test table
Bending strength (MPa) Fracture toughness (Mpa m1/2) Heat shock resistance number of times (secondary)
Embodiment 1 986 6.0 159
Embodiment 2 1028 5.9 152
Embodiment 3 1050 6.5 163
Embodiment 4 1049 6.2 164
Embodiment 5 1012 6.5 156
Comparative example 1 725 4.2 89
Comparative example 2 841 4.9 103
Note: the method for testing of heat shock resistance is: first sample is heated to 1000 DEG C, is incubated 30min, is subsequently placed in quenching in air, the most repeatedly, Until sample produces macroscopic cracking, record number of times.
As can be seen from the above table, titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material prepared by the present invention, bending strength is 986-1050Mpa, Fracture toughness is 5.9-6.5Mpa m1/2, bending strength and fracture toughness all show well, and heat shock resistance number of times has reached 152-164 time, heat resistanceheat resistant Impact property is excellent, is conducive to expanding the range of application of silicon carbide ceramics.
The bending strength of embodiment 3, fracture toughness and thermal shock resistance are superior to comparative example 1 and comparative example 2, and the bending resistance of comparative example 2 is strong Degree, fracture toughness and thermal shock resistance are superior to comparative example 1.Comparative example 1 compared with Example 3, without nano indium oxide powder and molybdenum powder, Other are same as in Example 3.Compared with Example 3, without nano indium oxide powder, other are same as in Example 3 for comparative example 2.The most permissible Finding out, by adding nano indium oxide powder and molybdenum powder, nano indium oxide powder, molybdenum powder coordinate with other components, it is possible to strengthen titanium carbide-titanium carbide The mechanical property of silicon-titanium silicide composite ceramic material.
Above the better embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the common skill of this area In the ken that art personnel are possessed, it is also possible on the premise of without departing from present inventive concept, various changes can be made.

Claims (4)

1. titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, it is characterised in that be made up of according to the raw material of weight portion following: titanium carbide Powder 65-68 part, silicon carbide powder 32-40 part, titanium silicide powder 26-29 part, alumina powder 3-6 part, nano indium oxide powder 5-8 part, Molybdenum powder 2-4 part.
Titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material the most according to claim 1, it is characterised in that by following according to weight portion Raw material forms: titanium carbide powder 66-67 part, silicon carbide powder 34-38 part, titanium silicide powder 27-28 part, alumina powder 4-5 part, nanometer Indium oxide powder 6-7 part, molybdenum powder 3-4 part.
Titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material the most according to claim 2, it is characterised in that by following according to weight portion Raw material forms: titanium carbide powder 67 parts, silicon carbide powder 36 parts, 28 parts of titanium silicide powder, alumina powder 5 parts, nano indium oxide powder 6 Part, molybdenum powder 3 parts.
4. the preparation method of the titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material as described in claim 1-3 is arbitrary, it is characterised in that Step is as follows:
1) weigh titanium carbide powder, silicon carbide powder and titanium silicide powder, put in ball grinder, using dehydrated alcohol as disperse medium, ball milling 8-12h, Obtain the first dispersion liquid；
2) the first dispersion liquid is placed in vacuum drying oven, at 140-150 DEG C, is dried 2-3h, to remove dehydrated alcohol, it is thus achieved that the first mixed powder Material；
3) being put in vacuum sintering furnace by the first mixed powder, and be sintered at 0.1-0.5Pa, 1230-1260 DEG C, sintering time is 1-2h, it is thus achieved that sintering feed；
4), after being pulverized by sintering feed, it is thus achieved that sintering feed powder, weigh alumina powder, nano indium oxide powder and molybdenum powder, and with sintering feed powder Merge, put into in ball grinder, using dehydrated alcohol as disperse medium, ball milling 15-18h, it is thus achieved that the second dispersion liquid；
5) the second dispersion liquid is placed in vacuum drying oven, at 155-160 DEG C, is dried 4-5h, to remove dehydrated alcohol, it is thus achieved that the second mixed powder Material；
6) by the second mixed powder isostatic pressing under 120Mpa, it is thus achieved that biscuit；
7) putting in vacuum sintering furnace by biscuit, be sintered at 0.1-0.2Pa, 1680-1740 DEG C, sintering time is 1-2h, it is thus achieved that carbonization Titanium-carborundum-titanium silicide composite ceramic material.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106380200A (en) * 2016-08-31 2017-02-08 周飞燕 High-toughness composite material and application of high-toughness composite material in ceramic cutter
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CN106380200A (en) * 2016-08-31 2017-02-08 周飞燕 High-toughness composite material and application of high-toughness composite material in ceramic cutter
CN113264775A (en) * 2020-01-29 2021-08-17 日本碍子株式会社 Dense composite material, method for producing same, joined body, and member for semiconductor manufacturing apparatus
CN113264775B (en) * 2020-01-29 2023-07-04 日本碍子株式会社 Compact composite material, method for producing the same, bonded body, and member for semiconductor manufacturing device
TWI825384B (en) * 2020-01-29 2023-12-11 日商日本碍子股份有限公司 Dense composite material, method for producing the same, joined body, and member for semiconductor manufacturing device

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