CN103360041B - Carbon/lithium disilicate composite ceramic material and preparation method thereof - Google Patents

Carbon/lithium disilicate composite ceramic material and preparation method thereof Download PDF

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CN103360041B
CN103360041B CN201310307820.0A CN201310307820A CN103360041B CN 103360041 B CN103360041 B CN 103360041B CN 201310307820 A CN201310307820 A CN 201310307820A CN 103360041 B CN103360041 B CN 103360041B
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ceramic material
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CN103360041A (en
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覃春林
甘笑雨
温广武
王春雨
王鑫宇
宋亮
夏龙
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Harbin Institute of Technology
Harbin Institute of Technology Weihai
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Abstract

The invention relates to a carbon/lithium disilicate composite ceramic material and a preparation method thereof. The preparation method comprises the steps: taking SiO2, Li2O, P2O5, ZnO, CaO, K2O and carbon power as raw materials, by mass: 67.6-73.6% of SiO2, 16.9-18.7% of Li2O, 2.3-5.3% of P2O5, 0.8-3.1% of ZnO, 1.1-2.3% of CaO, 1.8-5.3% of K2O, and 0.2-0.9% of the carbon powder; carrying out crystallization heat treatment of a glass mixture composed of the above oxides at the temperature of 1400 DEG C-1500 DEG C to obtain a basic glass body, mixing and ball-milling with the carbon powder, then carrying out hot-pressing sintering, demolding at the high temperature, and cooling along with a furnace to obtain the carbon/lithium disilicate composite ceramic material. The material has relatively good mechanical properties, relatively high strength and good chemical stability, has better wear-resistant performance and better self-lubricating performance which are different from other lithium disilicate composite materials, and is suitable for being used as a dressing material of diamond blades and diamond grinding wheels.

Description

A kind of carbon/bis-lithium silicate composite ceramic material and preparation method thereof
Technical field
The present invention relates to a kind of composite ceramic material and preparation method thereof, specifically relate to carbon/bis-lithium silicate composite ceramic material that a kind of two lithium silicates are principal crystalline phase and preparation method thereof.
Background technology
In today of scientific and technological high speed development, stupalith is widely used in fields such as military, machinery, aerospace and the energy, is day by day improving in the demand of all respects such as wear resisting property, corrosion resistance nature, resistance to elevated temperatures, rigidity, hardness, intensity for material.Within the time of nearly decades, Crystallization Mechanism, technology of preparing and the composition designing technique of investigators to devitrified glass carried out long exploratory development.Two lithium silicate devitrified glasses are a kind of two lithium silicate (Li to separate out 2si 2o 5) be the general designation of a series of devitrified glasses of main crystalline phase, the devitrified glass of this series has many advantages, for example low melting point and the coefficient of expansion are adjustable, so be widely used in biomedical sector and Electronic Packaging field, especially have especially higher utility value in gear division field.Preparation two lithium silicate devitrified glasses often adopt scorification, hot pressing sintering method and vacuum heating-press sintering preparation technology at present, common use zirconium white and rare earth element are as the wild phase of two lithium silicates, as Chinese patent CN200710072597.0 and CN200910043711.6.But the research for carbon/bis-lithium silicate composite ceramic material have not been reported.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of preparation method simple, energy-conserving and environment-protective, production cost is lower, there is good mechanical property, chemical stability is good, carbon/bis-lithium silicate composite ceramic material that abrasion resistance properties and self-lubricating property are good and preparation method thereof.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of carbon/bis-lithium silicate composite ceramic material, is characterized in that: it is with SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust are raw material, and the mass percent of each component is: SiO 267.6～73.6%, Li 2o 16.9～18.7%, P 2o 52.3～5.3%, ZnO 0.8～3.1%, CaO 1.1～2.3%, K 2o 1.8～5.3%, carbon dust 0.2～0.9%; At 1400oC-1500oC, the glass mixture of above-mentioned oxide compound composition is carried out to crystallization and thermal treatment, obtains parent glass body, with after carbon dust mixing and ball milling by hot pressed sintering, the high temperature demoulding furnace cooling, obtain carbon/bis-lithium silicate composite ceramic material.
The preparation method of above-mentioned carbon/bis-lithium silicate of the present invention composite ceramic material, is characterized in that: it comprises following step:
1) take in proportion SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust, by SiO 2, Li 2o, P 2o 5, ZnO, CaO and K 2o dusty raw materials is through mixing and ball milling, ball milling 6-12 hour post-drying, the glass mixture that obtains mixing;
2) corundum crucible being put into resistance furnace is heated to 1400-1500oC and takes out rapidly, then by step 1) in glass mixture put into the corundum crucible that is heated to 1400-1500oC, then at once the corundum crucible that glass mixture is housed is reentered in resistance furnace, insulation 30-40min, then take out, pour in distilled water and quench, obtain parent glass body;
3) by step 2) in the parent glass body that obtains wear into tiny glass powder, then, after 2 hours, dry with carbon dust mixing and ball milling, put into subsequently mould, carry out precompressed;
4) directly the mould that raw material powder is housed after precompressed is put into hot pressing furnace, under air atmosphere, be heated to 820-850oC, under passive state, be incubated 1h, be forced into subsequently 32-40Mpa, insulation 1-2h, then the high temperature demoulding furnace cooling, obtain the carbon/bis-lithium silicate composite ceramic material taking two lithium silicates as principal crystalline phase.
Matrix material prepared by the present invention has good mechanical property, and intensity is higher, and chemical stability is good, and grey black is opaque, and carbon content accounts for 0.2-0.9wt%, in the time of cutting, can engender resistance to cutting energy; The preparation method of this material is simple to operation, and energy-conserving and environment-protective are pollution-free, does not introduce heavy metal ion and toxic substance, and lower to equipment requirements, production cost is lower.Carbon/bis-lithium silicate composite ceramic material prepared by the present invention also has good abrasion resistance properties and self-lubricating property, is suitable for using as the trim materials of diamond blade and diamond wheel.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but should not limit the scope of the invention with this.
Embodiment 1: a kind of carbon/bis-lithium silicate composite ceramic material, it is with SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust are raw material, and the mass percent of each composition is SiO 268.4%, Li 2o 17.1%, P 2o 54.9%, ZnO 3.1%, CaO 2.1%, K 2o 3.9%, unformed carbon dust 0.5%; At 1400oC-1500oC, the glass mixture of above-mentioned oxide compound composition is carried out to crystallization and thermal treatment, obtains parent glass body, with after carbon dust mixing and ball milling by hot pressed sintering, the high temperature demoulding furnace cooling, obtain carbon/bis-lithium silicate composite ceramic material.
The preparation method of above-mentioned carbon/bis-lithium silicate of the present invention composite ceramic material, it comprises following step:
(1) take in proportion SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust, by SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o dusty raw materials is through mixing and ball milling, ball milling 6-12 hour post-drying, the glass mixture that obtains mixing;
(2) quenching of glass: corundum crucible is put into resistance furnace and be heated to 1400oC and take out rapidly, then by step 1) in glass mixture put into the corundum crucible that is heated to 1400oC, then at once the corundum crucible that glass mixture is housed is reentered in resistance furnace, insulation 40min, then take out, pour in distilled water and quench, obtain parent glass body;
(3) by step 2) in the parent glass body that obtains wear into tiny glass powder, then, after 2 hours, dry with carbon dust mixing and ball milling, put into subsequently mould, carry out precompressed;
(4) after precompressed, directly the mould that raw material powder is housed is put into hot pressing furnace, under air atmosphere, be heated to 820oC and be incubated 1h under passive state, be forced into subsequently 32MPa insulation 1h, then the high temperature demoulding furnace cooling, just obtain the carbon/bis-lithium silicate composite ceramic material taking two lithium silicates as principal crystalline phase.
Prepared material bending strength is 141.535MPa, and Vickers' hardness is 730.76, and void content is 1.0137*10 -5%.
Embodiment 2: a kind of carbon/bis-lithium silicate composite ceramic material, it is with SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust are raw material, and the mass percent of each composition is SiO 267.6%, Li 2o 16.9%, P 2o 55.3%, ZnO 2.4%, CaO 2.3%, K 2o 5.3%, Graphite Powder 99 0.2%; At 1400oC-1500oC, the glass mixture of above-mentioned oxide compound composition is carried out to crystallization and thermal treatment, obtains parent glass body, with after carbon dust mixing and ball milling by hot pressed sintering, the high temperature demoulding furnace cooling, obtain carbon/bis-lithium silicate composite ceramic material.
The preparation method of above-mentioned carbon/bis-lithium silicate of the present invention composite ceramic material, it comprises following step:
(1) take in proportion SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust, by SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o dusty raw materials is through mixing and ball milling, ball milling 6-12 hour post-drying, the glass mixture that obtains mixing;
(2) quenching of glass: corundum crucible is put into resistance furnace and be heated to 1400oC and take out rapidly, then by step 1) in glass mixture put into the corundum crucible that is heated to 1400oC, then at once the corundum crucible that glass mixture is housed is reentered in resistance furnace, insulation 35min, then take out, pour in distilled water and quench, obtain parent glass body;
(3) by step 2) in the parent glass body that obtains wear into tiny glass powder, then, after 2 hours, dry with carbon dust mixing and ball milling, put into subsequently mould, carry out precompressed;
(4) after precompressed, directly the mould that raw material powder is housed is put into hot pressing furnace, under air atmosphere, be heated to 820oC and be incubated 1h under passive state, be forced into subsequently 32MPa insulation 1h, then the high temperature demoulding furnace cooling, just obtain the carbon/bis-lithium silicate composite ceramic material taking two lithium silicates as principal crystalline phase.
Prepared material bending strength is: bending strength is 139.459MPa, and Vickers' hardness is 717.31, and void content is 1.1425*10 -5%.
Embodiment 3: a kind of carbon/bis-lithium silicate composite ceramic material, it is with SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust are raw material, and the mass percent of each composition is SiO 271.8%, Li 2o 18.0%, P 2o 53.1%, ZnO 2.4%, CaO 1.6%, K 2o 2.4%, Graphite Powder 99 0.7%; At 1400oC-1500oC, the glass mixture of above-mentioned oxide compound composition is carried out to crystallization and thermal treatment, obtains parent glass body, with after carbon dust mixing and ball milling by hot pressed sintering, the high temperature demoulding furnace cooling, obtain carbon/bis-lithium silicate composite ceramic material.
The preparation method of above-mentioned carbon/bis-lithium silicate of the present invention composite ceramic material, it comprises following step:
(1) take in proportion SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust, by SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o dusty raw materials is through mixing and ball milling, ball milling 6-12 hour post-drying, the glass mixture that obtains mixing;
(2) quenching of glass: corundum crucible is put into resistance furnace and be heated to 1400oC and take out rapidly, then by step 1) in glass mixture put into the corundum crucible that is heated to 1400oC, then at once the corundum crucible that glass mixture is housed is reentered in resistance furnace, insulation 35min, then take out, pour in distilled water and quench, obtain parent glass body;
(3) by step 2) in the parent glass body that obtains wear into tiny glass powder, then, after 2 hours, dry with carbon dust mixing and ball milling, put into subsequently mould, carry out precompressed;
(4) after precompressed, directly the mould that raw material powder is housed is put into hot pressing furnace, under air atmosphere, be heated to 820oC and be incubated 1h under passive state, be forced into subsequently 32MPa insulation 1h, then the high temperature demoulding furnace cooling, just obtain the carbon/bis-lithium silicate composite ceramic material taking two lithium silicates as principal crystalline phase.
Prepared material bending strength is: bending strength is 148.540MPa, and Vickers' hardness is 754.38, and void content is 1.1023*10 -5%.
Embodiment 4: a kind of carbon/bis-lithium silicate composite ceramic material, it is with SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust are raw material, and the mass percent of each composition is SiO 273.2%, Li 2o 18.3%, P 2o 52.8%, ZnO 1.6%, CaO 1.3%, K 2o 1.8%, Graphite Powder 99 0.9%; At 1400oC-1500oC, the glass mixture of above-mentioned oxide compound composition is carried out to crystallization and thermal treatment, obtains parent glass body, with after carbon dust mixing and ball milling by hot pressed sintering, the high temperature demoulding furnace cooling, obtain carbon/bis-lithium silicate composite ceramic material.
The preparation method of above-mentioned carbon/bis-lithium silicate of the present invention composite ceramic material, it comprises following step:
(1) take in proportion SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust, by SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o dusty raw materials is through mixing and ball milling, ball milling 6-12 hour post-drying, the glass mixture that obtains mixing;
(2) quenching of glass: corundum crucible is put into resistance furnace and be heated to 1500oC and take out rapidly, then by step 1) in glass mixture put into the corundum crucible that is heated to 1500oC, then at once the corundum crucible that glass mixture is housed is reentered in resistance furnace, insulation 35min, then take out, pour in distilled water and quench, obtain parent glass body;
(3) by step 2) in the parent glass body that obtains wear into tiny glass powder, then, after 2 hours, dry with carbon dust mixing and ball milling, put into subsequently mould, carry out precompressed;
(4) after precompressed, directly the mould that raw material powder is housed is put into hot pressing furnace, under air atmosphere, be heated to 820oC and be incubated 1h under passive state, be forced into subsequently 32MPa insulation 1h, then the high temperature demoulding furnace cooling, just obtain the carbon/bis-lithium silicate composite ceramic material taking two lithium silicates as principal crystalline phase.
Prepared material bending strength is: bending strength is 143.268MPa, and Vickers' hardness is 715.20, and void content is 1.2074*10 -5%.
Embodiment 5: a kind of carbon/bis-lithium silicate composite ceramic material, it is with SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust are raw material, and the mass percent of each composition is SiO 273.6%, Li 2o 18.7%, P 2o 52.3%, ZnO 0.8%, CaO 1.1%, K 2o 2.8%, Graphite Powder 99 0.7%; At 1400oC-1500oC, the glass mixture of above-mentioned oxide compound composition is carried out to crystallization and thermal treatment, obtains parent glass body, with after carbon dust mixing and ball milling by hot pressed sintering, the high temperature demoulding furnace cooling, obtain carbon/bis-lithium silicate composite ceramic material.
The preparation method of above-mentioned carbon/bis-lithium silicate of the present invention composite ceramic material, it comprises following step:
(1) take in proportion SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and carbon dust, by SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o dusty raw materials is through mixing and ball milling, ball milling 6-12 hour post-drying, the glass mixture that obtains mixing;
(2) quenching of glass: corundum crucible is put into resistance furnace and be heated to 1500oC and take out rapidly, then by step 1) in glass mixture put into the corundum crucible that is heated to 1500oC, then at once the corundum crucible that glass mixture is housed is reentered in resistance furnace, insulation 35min, then take out, pour in distilled water and quench, obtain parent glass body;
(3) by step 2) in the parent glass body that obtains wear into tiny glass powder, then, after 2 hours, dry with carbon dust mixing and ball milling, put into subsequently mould, carry out precompressed;
(4) after precompressed, directly the mould that raw material powder is housed is put into hot pressing furnace, under air atmosphere, be heated to 820oC and be incubated 1h under passive state, be forced into subsequently 32MPa insulation 1h, then the high temperature demoulding furnace cooling, just obtain the carbon/bis-lithium silicate composite ceramic material taking two lithium silicates as principal crystalline phase.
Prepared material bending strength is: bending strength is 144.769MPa, and Vickers' hardness is 746.914, and void content is 1.0318*10 -5%.

Claims (2)

1. a carbon/bis-lithium silicate composite ceramic material, is characterized in that: it is with SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and amorphous carbon powder or Graphite Powder 99 are raw material, and the mass percent of each component is: SiO 267.6～73.6%, Li 2o 16.9～18.7%, P 2o 52.3～5.3%, ZnO 0.8～3.1%, CaO 1.1～2.3%, K 2o 1.8～5.3%, amorphous carbon powder or Graphite Powder 99 0.2～0.9%; At 1400oC-1500oC, the glass mixture of above-mentioned oxide compound composition is carried out to crystallization and thermal treatment, obtain parent glass body, with after amorphous carbon powder or Graphite Powder 99 mixing and ball milling by hot pressed sintering, the high temperature demoulding furnace cooling, obtain carbon/bis-lithium silicate composite ceramic material.
2. a preparation method for carbon/bis-lithium silicate composite ceramic material claimed in claim 1, is characterized in that: it comprises following step:
(1) take in proportion SiO 2, Li 2o, P 2o 5, ZnO, CaO, K 2o and amorphous carbon powder or Graphite Powder 99, by SiO 2, Li 2o, P 2o 5, ZnO, CaO and K 2o dusty raw materials is through mixing and ball milling, ball milling 6-12 hour post-drying, the glass mixture that obtains mixing;
(2) corundum crucible being put into resistance furnace is heated to 1400-1500oC and takes out rapidly, then the glass mixture in step (1) is put into the corundum crucible that is heated to 1400-1500oC, then at once the corundum crucible that glass mixture is housed is reentered in resistance furnace, insulation 30-40min, then take out, pour in distilled water and quench, obtain parent glass body;
(3) the parent glass body obtaining in step (2) is worn into tiny glass powder, then, after 2 hours, dry with amorphous carbon powder or Graphite Powder 99 mixing and ball milling, put into subsequently mould, carry out precompressed;
(4) directly the mould that raw material powder is housed after precompressed is put into hot pressing furnace, under air atmosphere, be heated to 820-850oC, under passive state, be incubated 1h, be forced into subsequently 32-40Mpa, insulation 1-2h, then the high temperature demoulding furnace cooling, obtain the carbon/bis-lithium silicate composite ceramic material taking two lithium silicates as principal crystalline phase.
CN201310307820.0A 2013-07-22 2013-07-22 Carbon/lithium disilicate composite ceramic material and preparation method thereof Expired - Fee Related CN103360041B (en)

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