CN105819860B - A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material and preparation method thereof - Google Patents
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic materials, are made of the raw material below according to parts by weight: 65-68 parts of titanium carbide powder, 32-40 parts of silicon carbide powder, 26-29 parts of silication titanium powder, 3-6 parts of alumina powder, 5-8 parts of nano indium oxide powder, 2-4 parts of molybdenum powder.The present invention also provides the preparation methods of the titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material.Titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material prepared by the present invention, bending strength and fracture toughness show well, and thermal shock resistance is excellent, are conducive to the application range for expanding silicon carbide ceramics.
Description
Technical field
The present invention relates to ceramic composite technical field, specifically a kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramics
Material and preparation method thereof.
Background technique
Ceramics development history be Chinese civilization history an important component part, China as four major acids ancient country it
One, brilliant contribution is made that for mankind's social progress and development, wherein the invention and development of ceramics have more unique meaning
Justice, each Chao Gedai has different artistic styles and different technical characteristics on Chinese history.With the development of modern science technology, closely
Occur many new ceramic kinds again over 100 years.They do not use or are rarely employed the traditional ceramics such as clay, feldspar, quartz
Raw material, but other special materials are used, or even be expanded to non-silicate, the range of non-oxidized substance, and occur many new
Technique." Ceramic " word is interpreted as various inorganic non-metal solid materials by the document of some countries of US and European
Common name.Therefore the meaning of ceramics actually much surmounts traditional concept narrow in the past.
Titanium carbide is typical transition metal carbide.Its bond type is blended in by ionic bond, covalent bond and metallic bond
In same crystal structure, therefore titanium carbide has many unique performances.The structure of crystal determine titanium carbide have high rigidity,
The essential characteristics such as high-melting-point, wear-resistant and electric conductivity.Titanium carbide ceramic is titanium, zirconium, develops most in chromium transition metal carbide
Wide material is widely answered in many fields such as machinery, electronics, chemical industry, environmental protection, fusion reactor, national defense industry
With.But the brittleness of titanium carbide ceramic is big, toughness is insufficient and heat shock resistance can be poor, these all limit its fortune to a certain extent
With.
Summary of the invention
The purpose of the present invention is to provide a kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material and preparation method thereof,
To solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made of the raw material below according to parts by weight: carbonization
65-68 parts of titanium powder, 32-40 parts of silicon carbide powder, 26-29 parts of silication titanium powder, 3-6 parts of alumina powder, nano indium oxide
5-8 parts of powder, 2-4 parts of molybdenum powder.
As a further solution of the present invention: it is made of the raw material below according to parts by weight: 66-67 parts of titanium carbide powder,
34-38 parts of silicon carbide powder, 27-28 parts of silication titanium powder, 4-5 parts of alumina powder, 6-7 parts of nano indium oxide powder, molybdenum powder
3-4 parts.
As further scheme of the invention: being made of the raw material below according to parts by weight: 67 parts of titanium carbide powder, carbon
36 parts of SiClx powder, 28 parts of silication titanium powder, 5 parts of alumina powder, 6 parts of nano indium oxide powder, 3 parts of molybdenum powder.
The preparation method of the titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, steps are as follows:
1) titanium carbide powder, silicon carbide powder and silication titanium powder are weighed, is put into ball grinder, using dehydrated alcohol as point
Dispersion media, ball milling 8-12h obtain the first dispersion liquid;
2) the first dispersion liquid is placed in vacuum oven, the dry 2-3h at 140-150 DEG C, to remove dehydrated alcohol,
Obtain the first mixed powder;
3) the first mixed powder is put into vacuum sintering furnace, and is sintered at 0.1-0.5Pa, 1230-1260 DEG C
Processing, sintering time 1-2h obtain sintering feed;
4) after crushing sintering feed, sintering feed powder is obtained, alumina powder, nano indium oxide powder and molybdenum powder are weighed,
And merge with sintering feed powder, it puts into ball grinder, using dehydrated alcohol as decentralized medium, ball milling 15-18h obtains second
Dispersion liquid;
5) the second dispersion liquid is placed in a vacuum drying oven, the dry 4-5h at 155-160 DEG C, to remove dehydrated alcohol,
Obtain the second mixed powder;
6) by the second mixed powder at 120Mpa isostatic pressing, obtain biscuit;
7) biscuit is put into vacuum sintering furnace, is sintered at 0.1-0.2Pa, 1680-1740 DEG C, sintering time is
1-2h obtains titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material.
Compared with prior art, the beneficial effects of the present invention are: titanium carbide-titanium carbide prepared by the present invention silicon-titanium silicide is multiple
Close ceramic material, bending strength 986-1050Mpa, fracture toughness 5.9-6.5Mpam1/2, bending strength and fracture toughness
Performance is good, and heat shock resistance number has reached 152-164 times, and thermal shock resistance is excellent, is conducive to expand silicon carbide ceramics
Application range.Titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material prepared by the present invention passes through addition nano indium oxide powder
And molybdenum powder, nano indium oxide powder, molybdenum powder and other components cooperate, and can enhance titanium carbide-titanium carbide silicon-titanium silicide composite ceramics
The mechanical property of material.
Specific embodiment
Technical solution of the present invention is described in more detail With reference to embodiment.
Embodiment 1
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made of the raw material below according to parts by weight: carbonization
65 parts of titanium powder, 32 parts of silicon carbide powder, 26 parts of silication titanium powder, 3 parts of alumina powder, 5 parts of nano indium oxide powder, molybdenum powder
2 parts.
The silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material preparation method, steps are as follows:
1) titanium carbide powder, silicon carbide powder and silication titanium powder are weighed, is put into ball grinder, using dehydrated alcohol as point
Dispersion media, ball milling 8h obtain the first dispersion liquid;
2) the first dispersion liquid is placed in vacuum oven, the dry 2h at 140 DEG C, to remove dehydrated alcohol, obtains the
One mixed powder;
3) the first mixed powder is put into vacuum sintering furnace, and is sintered at 0.1Pa, 1230 DEG C, is sintered
Time is 1h, obtains sintering feed;
4) after crushing sintering feed, sintering feed powder is obtained, alumina powder, nano indium oxide powder and molybdenum powder are weighed,
And merge with sintering feed powder, it puts into ball grinder, using dehydrated alcohol as decentralized medium, ball milling 15h obtains the second dispersion
Liquid;
5) the second dispersion liquid is placed in a vacuum drying oven, the dry 4h at 155 DEG C, to remove dehydrated alcohol, obtains the
Two mixed powders;
6) by the second mixed powder at 120Mpa isostatic pressing, obtain biscuit;
7) biscuit is put into vacuum sintering furnace, is sintered at 0.1Pa, 1680 DEG C, sintering time 1h, obtain carbon
Change titanium-silicon carbide-titanium silicide composite ceramic material.
Embodiment 2
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made of the raw material below according to parts by weight: carbonization
68 parts of titanium powder, 40 parts of silicon carbide powder, 29 parts of silication titanium powder, 6 parts of alumina powder, 8 parts of nano indium oxide powder, molybdenum powder
4 parts.
The silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material preparation method, steps are as follows:
1) titanium carbide powder, silicon carbide powder and silication titanium powder are weighed, is put into ball grinder, using dehydrated alcohol as point
Dispersion media, ball milling 12h obtain the first dispersion liquid;
2) the first dispersion liquid is placed in vacuum oven, the dry 3h at 150 DEG C, to remove dehydrated alcohol, obtains the
One mixed powder;
3) the first mixed powder is put into vacuum sintering furnace, and is sintered at 0.5Pa, 1260 DEG C, is sintered
Time is 2h, obtains sintering feed;
4) after crushing sintering feed, sintering feed powder is obtained, alumina powder, nano indium oxide powder and molybdenum powder are weighed,
And merge with sintering feed powder, it puts into ball grinder, using dehydrated alcohol as decentralized medium, ball milling 18h obtains the second dispersion
Liquid;
5) the second dispersion liquid is placed in a vacuum drying oven, the dry 5h at 160 DEG C, to remove dehydrated alcohol, obtains the
Two mixed powders;
6) by the second mixed powder at 120Mpa isostatic pressing, obtain biscuit;
7) biscuit is put into vacuum sintering furnace, is sintered at 0.2Pa, 1740 DEG C, sintering time 2h, obtain carbon
Change titanium-silicon carbide-titanium silicide composite ceramic material.
Embodiment 3
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made of the raw material below according to parts by weight: carbonization
67 parts of titanium powder, 36 parts of silicon carbide powder, 28 parts of silication titanium powder, 5 parts of alumina powder, 6 parts of nano indium oxide powder, molybdenum powder
3 parts.
The silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material preparation method, steps are as follows:
1) titanium carbide powder, silicon carbide powder and silication titanium powder are weighed, is put into ball grinder, using dehydrated alcohol as point
Dispersion media, ball milling 10h obtain the first dispersion liquid;
2) the first dispersion liquid is placed in vacuum oven, dry 2.5h is obtained at 145 DEG C with removing dehydrated alcohol
First mixed powder;
3) the first mixed powder is put into vacuum sintering furnace, and is sintered at 0.3Pa, 1250 DEG C, is sintered
Time is 2h, obtains sintering feed;
4) after crushing sintering feed, sintering feed powder is obtained, alumina powder, nano indium oxide powder and molybdenum powder are weighed,
And merge with sintering feed powder, it puts into ball grinder, using dehydrated alcohol as decentralized medium, ball milling 16h obtains the second dispersion
Liquid;
5) the second dispersion liquid is placed in a vacuum drying oven, the dry 5h at 158 DEG C, to remove dehydrated alcohol, obtains the
Two mixed powders;
6) by the second mixed powder at 120Mpa isostatic pressing, obtain biscuit;
7) biscuit is put into vacuum sintering furnace, is sintered at 0.2Pa, 1700 DEG C, sintering time 1.5, obtained
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 of the raw material below according to parts by weight: carbonization
65 parts of titanium powder, 38 parts of silicon carbide powder, 26 parts of silication titanium powder, 6 parts of alumina powder, 8 parts of nano indium oxide powder, molybdenum powder
3 parts.
The silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material preparation method, steps are as follows:
1) titanium carbide powder, silicon carbide powder and silication titanium powder are weighed, is put into ball grinder, using dehydrated alcohol as point
Dispersion media, ball milling 10h obtain the first dispersion liquid;
2) the first dispersion liquid is placed in vacuum oven, the dry 2h at 150 DEG C, to remove dehydrated alcohol, obtains the
One mixed powder;
3) the first mixed powder is put into vacuum sintering furnace, and is sintered at 0.5Pa, 1260 DEG C, is sintered
Time is 2h, obtains sintering feed;
4) after crushing sintering feed, sintering feed powder is obtained, alumina powder, nano indium oxide powder and molybdenum powder are weighed,
And merge with sintering feed powder, it puts into ball grinder, using dehydrated alcohol as decentralized medium, ball milling 18h obtains the second dispersion
Liquid;
5) the second dispersion liquid is placed in a vacuum drying oven, the dry 5h at 155 DEG C, to remove dehydrated alcohol, obtains the
Two mixed powders;
6) by the second mixed powder at 120Mpa isostatic pressing, obtain biscuit;
7) biscuit is put into vacuum sintering furnace, is sintered at 0.2Pa, 1690 DEG C, sintering time 2h, obtain carbon
Change titanium-silicon carbide-titanium silicide composite ceramic material.
Embodiment 5
A kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, is made of the raw material below according to parts by weight: carbonization
67 parts of titanium powder, 38 parts of silicon carbide powder, 29 parts of silication titanium powder, 5 parts of alumina powder, 5 parts of nano indium oxide powder, molybdenum powder
3 parts.
The silicon of titanium carbide-titanium carbide described in the present embodiment-titanium silicide composite ceramic material preparation method, steps are as follows:
1) titanium carbide powder, silicon carbide powder and silication titanium powder are weighed, is put into ball grinder, using dehydrated alcohol as point
Dispersion media, ball milling 11h obtain the first dispersion liquid;
2) the first dispersion liquid is placed in vacuum oven, the dry 3h at 145 DEG C, to remove dehydrated alcohol, obtains the
One mixed powder;
3) the first mixed powder is put into vacuum sintering furnace, and is sintered at 0.1Pa, 1250 DEG C, is sintered
Time is 1h, obtains sintering feed;
4) after crushing sintering feed, sintering feed powder is obtained, alumina powder, nano indium oxide powder and molybdenum powder are weighed,
And merge with sintering feed powder, it puts into ball grinder, using dehydrated alcohol as decentralized medium, ball milling 18h obtains the second dispersion
Liquid;
5) the second dispersion liquid is placed in a vacuum drying oven, dry 4.5h is obtained at 157 DEG C with removing dehydrated alcohol
Second mixed powder;
6) by the second mixed powder at 120Mpa isostatic pressing, obtain biscuit;
7) biscuit is put into vacuum sintering furnace, is sintered at 0.1Pa, 1740 DEG C, sintering time 2h, obtain carbon
Change titanium-silicon carbide-titanium silicide composite ceramic material.
Comparative example 1
Compared with Example 3, nano indium oxide powder and molybdenum powder are free of, other are same as Example 3.
Comparative example 2
Compared with Example 3, nano indium oxide powder is free of, other are same as Example 3.
Performance test
It makes a service test to embodiment 1-5 and comparative example 1-2, test result is as shown in table 1.
1 performance test table of table
Bending strength (MPa) | Fracture toughness (Mpam1/2) | Heat shock resistance number (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 test method of heat shock resistance are as follows: sample is first heated to 1000 DEG C, 30min is kept the temperature, is subsequently placed in air
Quenching until sample generates macroscopic cracking, records number repeatedly.
As can be seen from the above table, titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material prepared by the present invention, bending resistance are strong
Degree is 986-1050Mpa, fracture toughness 5.9-6.5Mpam1/2, bending strength and fracture toughness show well, heat resistanceheat resistant punching
It hits number to have reached 152-164 times, thermal shock resistance is excellent, is conducive to the application range for expanding silicon carbide ceramics.
Bending strength, fracture toughness and the thermal shock resistance of embodiment 3 are superior to comparative example 1 and comparative example 2, and right
Bending strength, fracture toughness and the thermal shock resistance of ratio 2 are superior to comparative example 1.Comparative example 1 compared with Example 3, no
Powder containing nano indium oxide and molybdenum powder, other are same as Example 3.Comparative example 2 compared with Example 3, is free of nano indium oxide
Powder, other are same as Example 3.Here, it can be seen that by addition nano indium oxide powder and molybdenum powder, nano indium oxide powder
End, molybdenum powder and other components cooperate, and can enhance titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material mechanical property.
Better embodiment of the invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be without departing from the purpose of the present invention
Various changes can be made.
Claims (3)
1. a kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material, which is characterized in that by below according to the raw material of parts by weight
Composition: 66-67 parts of titanium carbide powder, 27-28 parts of silication titanium powder, 4-5 parts of alumina powder, is received 34-38 parts of silicon carbide powder
Rice 6-7 parts of indium oxide powder, 3-4 parts of molybdenum powder.
2. titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material according to claim 1, which is characterized in that by pressing below
According to the raw material composition of parts by weight: 67 parts of titanium carbide powder, 36 parts of silicon carbide powder, 28 parts of silication titanium powder, alumina powder 5
Part, 6 parts of nano indium oxide powder, 3 parts of molybdenum powder.
3. a kind of titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material preparation method as described in claim 1-2 is any,
It is characterized in that, steps are as follows:
1) titanium carbide powder, silicon carbide powder and silication titanium powder are weighed, is put into ball grinder, is situated between using dehydrated alcohol as dispersion
Matter, ball milling 8-12h obtain the first dispersion liquid;
2) the first dispersion liquid is placed in vacuum oven, dry 2-3h is obtained at 140-150 DEG C with removing dehydrated alcohol
First mixed powder;
3) the first mixed powder is put into vacuum sintering furnace, and is sintered at 0.1-0.5Pa, 1230-1260 DEG C,
Sintering time is 1-2h, obtains sintering feed;
4) after crushing sintering feed, sintering feed powder is obtained, weighs alumina powder, nano indium oxide powder and molybdenum powder, and with
Sintering feed powder merges, and puts into ball grinder, and using dehydrated alcohol as decentralized medium, ball milling 15-18h obtains the second dispersion
Liquid;
5) the second dispersion liquid is placed in a vacuum drying oven, dry 4-5h is obtained at 155-160 DEG C with removing dehydrated alcohol
Second mixed powder;
6) by the second mixed powder at 120MP a isostatic pressing, obtain biscuit;
7) biscuit is put into vacuum sintering furnace, is sintered at 0.1-0.2Pa, 1680-1740 DEG C, sintering time 1-
2h obtains titanium carbide-titanium carbide silicon-titanium silicide composite ceramic material.
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CN103979538B (en) * | 2014-05-30 | 2015-09-30 | 四川理工学院 | A kind of method preparing micro-nano TiC/TiSi2 composite granule |
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