CN102515725A - Preparation method of fused quartz ceramic material containing boron carbide and silicon nitride - Google Patents
Preparation method of fused quartz ceramic material containing boron carbide and silicon nitride Download PDFInfo
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- CN102515725A CN102515725A CN2011103540351A CN201110354035A CN102515725A CN 102515725 A CN102515725 A CN 102515725A CN 2011103540351 A CN2011103540351 A CN 2011103540351A CN 201110354035 A CN201110354035 A CN 201110354035A CN 102515725 A CN102515725 A CN 102515725A
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Abstract
The invention relates to a preparation method of a fused quartz ceramic material containing boron carbide and silicon nitride, which belongs to the field of high temperature structure ceramic material. The ceramic material comprises the following raw materials in percentage by weight: 97-98% of fused quartz fine powder as well as 1-3% of mixed fine powder of boron carbide and silicon nitride (mass ratio of 1:1). The preparation method comprises the following steps of: mixing the fused quartz fine powder, the boron carbide fine powder and the silicon nitride fine powder in a dry way; and then adding polyvinyl alcohol solution bonding agent to be mixed with the fine powder in a wet way; screening, stirring and ageing the mixture so as to obtain a blank material for molding blank, wherein the blank molding pressure is no less than 50 MPa; preserving the heat of the dried blank at 1100 DEG C for 1-2 hours; and then preserving the heat of the blank at 1250-1400 DEG C for 1-3 hours; and sintering the blank at high temperature so as to obtain the fused quartz ceramic material containing boron carbide and silicon nitride. The ceramic material provided by the invention has the advantages of small thermal expansion and low crystallization degree. According to the invention, a safe and reliable high temperature structure material can be provided in the fields like domestic glass smelting, iron and steel, military industry, aerospace and the like.
Description
Technical field
The invention belongs to the high-temperature structural ceramics field, be specifically related to a kind of fused quartz ceramic preparation methods that contains norbide and silicon nitride.
Background technology
The fused quartz ceramic material is to be raw material with fine fused quartz particle, according to the material of ceramic process method preparation.Fused quartz particle in the fused quartz ceramic material still is unstable high-energy state material; Has the trend that easy crystallization is a cristobalite under the fused quartz certain temperature; And the cristobalite after the crystallization because of the crystal formation of cristobalite changes, and is followed bigger volume change under the high temperature working conditions or during the thermal shocking of experience high temperature difference; Cause fused quartz ceramic material production crackle, even damage because of crack propagation causes the material cracking.
At present, domestic how tame research institution has carried out the research that the sintering, crystallization behavior, crystallization of fused quartz and fused quartz ceramic material suppress, and each experimental study method is to be employed in the approach of introducing the foreign substances additive in the fused quartz ceramic admixtion basically.Some investigators adopt single S i
3N
4, B
4C etc. are incorporated in the fused quartz ceramic matrix as additive; Obtain certain crystallization and suppressed effect; But when being elevated to more than 1300 ℃ temperature, significantly crystallization phenomenon still can occur, therefore need further to improve and suppress the crystallization effect and improve the sintering degree along with temperature.
The present invention adopts norbide and silicon nitride subparticle to be incorporated in the fused quartz ceramic material powder as the crystallization suppressant additive; Behind moulding and high temperature sintering, make the fused quartz ceramic material that contains norbide and silicon nitride; With independent introducing norbide or the fused quartz ceramic material of introducing silicon nitride separately relatively; Or with the check sample of not introducing the crystallization suppressant additive relatively; This stupalith has advantages such as intensity height, crystallization degree is low, thermal expansivity is little, is the higher fused quartz ceramic material of a kind of security reliability standard.The present invention can be fields such as China's glass smelting, iron and steel and Non-ferrous Metallurgy, electronics, military project guided missile, spacecraft a kind of new type high temperature structured material is provided, and obtains more extensively effectively to reach the application of safe reliability.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency of the prior art, the fused quartz ceramic preparation methods that contains norbide and silicon nitride of a kind of low-thermal-expansion, low crystallization degree is provided.
Technical scheme of the present invention and technical characterictic are:
The present invention is a kind of fused quartz ceramic preparation methods that contains norbide and silicon nitride; It is characterized in that this stupalith weight percent raw materials used and raw material is: fused quartz fine powder 97～99%, the mixing fine powders 1～3% of norbide and silicon nitride.This ceramic material may further comprise the steps: the blank preparation; Blank forming; Body drying; Base substrate burns till.
Particle diameter＜the 0.065mm of the used fused quartz fine powder of this stupalith, the weight percent of fused quartz fine powder purity is: SiO
2>=99.9%.
The mixing fine powders weight percent of used norbide of this stupalith and silicon nitride is: norbide fine powder 50%, silicon nitride fine powder 50%.
The particle diameter of the used norbide fine powder of this stupalith is＜0.074mm that the weight percent of norbide fine powder purity is: B
4C>=95.0%.
The particle diameter of the used silicon nitride fine powder of this stupalith is＜0.074mm that the weight percent of norbide fine powder purity is: Si
3N
4>=90.0%.
The blank preparation method of this stupalith is: do after fused quartz fine powder, norbide fine powder, silicon nitride fine powder are measured by proportioning and mixed 3～10 minutes; Polyvinyl alcohol solution bonding 6% (the weight percent that under continuous whipped state, progressively adds mass concentration 2% then; Add); Continue to mix and cross 40 mesh sieves after 10～15 minutes, the continued of sieving stirs and was placed on ageing mixture in the airtight plastics bag in 2～5 minutes, but obtains the blank of voltage supply power moulding behind the ageing mixture through 4～6 hours.
The blank forming method of this stupalith is: mix and adopt hydropress to be shaped to base substrate through the blank of ageing mixture above-mentioned, blank forming pressure is >=50MPa.
The body drying method of this stupalith was: base substrate after the moulding is obtained the dry base substrate that Gong to burn till 60 ℃～90 ℃ dryings 2～3 hours.
The base substrate process for calcining of this stupalith is: dried base substrate obtains to contain the fused quartz ceramic material of norbide and silicon nitride more earlier through 1100 ℃ of heating 1～2 hour after 1～3 hour high temperature of 1250～1400 ℃ of insulations burns till.
Embodiment
Embodiment 1
The fused quartz ceramic material weight percent raw materials used and raw material that contains norbide and silicon nitride is: the fused quartz fine powder 99% of particle diameter＜0.065mm, the norbide fine powder 0.5% of particle diameter＜0.074mm, the silicon nitride fine powder 0.5% of particle diameter＜0.074mm.Fused quartz fine powder, norbide fine powder, silicon nitride fine powder were done mixed 5 minutes after by the proportioning metering; Polyvinyl alcohol solution 6% (the weight percent that under continuous whipped state, progressively adds mass concentration 2% then; Add); Continue to mix and cross 40 mesh sieves after 10 minutes, the continued of sieving stirs and was placed on ageing mixture in the airtight plastics bag in 3 minutes, but obtains the blank of voltage supply power moulding behind the ageing mixture through 5 hours.Blank is adopted the hydropress moulding, and blank forming pressure is 50MPa.Base substrate after the moulding 60 ℃ of dryings 2 hours, 90 ℃ of dryings 1 hour, is obtained the dry base substrate that Gong to burn till afterwards.Dried base substrate through 1100 ℃ of insulations 2 hours, was burnt till the fused quartz ceramic material that the back obtains to contain norbide and silicon nitride in 1 hour 1350 ℃ of soaks.
The coefficient of thermal expansion of this stupalith is 0.08% (1000 ℃); The sample coefficient of thermal expansion of introducing 1% norbide separately is 0.24% (1000 ℃); The sample coefficient of thermal expansion of introducing 1% silicon nitride separately is 0.50% (1000 ℃); And the check sample coefficient of thermal expansion of not introducing norbide and silicon nitride is 1.02% (1000 ℃).It is thus clear that it is low to contain the fused quartz ceramic material coefficient of thermal expansion rate of 1% norbide and silicon nitride; The fused quartz crystallization is that the degree of cristobalite is little; The coefficient of thermal expansion of this stupalith sample is merely 7.8% of blank sample, shows that norbide and silicon nitride have tangible crystallization to fused quartz and suppress effect.
Embodiment 2
The fused quartz ceramic material weight percent raw materials used and raw material that contains norbide and silicon nitride is: the fused quartz fine powder 99% of particle diameter＜0.065mm, the norbide fine powder 0.5% of particle diameter＜0.074mm, the silicon nitride fine powder 0.5% of particle diameter＜0.074mm.Fused quartz fine powder, norbide fine powder, silicon nitride fine powder were done mixed 5 minutes after by the proportioning metering; Polyvinyl alcohol solution 6% (the weight percent that under continuous whipped state, progressively adds mass concentration 2% then; Add); Continue to mix and cross 40 mesh sieves after 10 minutes, the continued of sieving stirs and was placed on ageing mixture in the airtight plastics bag in 3 minutes, but obtains the blank of voltage supply power moulding behind the ageing mixture through 5 hours.Blank is adopted the hydropress moulding, and blank forming pressure is 50MPa.Base substrate after the moulding 60 ℃ of dryings 2 hours, 90 ℃ of dryings 1 hour, is obtained the dry base substrate that Gong to burn till afterwards.Dried base substrate through 1100 ℃ of insulations 2 hours, was burnt till the fused quartz ceramic material that the back obtains to contain norbide and silicon nitride in 1 hour 1400 ℃ of soaks.
The coefficient of thermal expansion of this stupalith is 0.12% (1000 ℃); The sample coefficient of thermal expansion of introducing 1% norbide separately is 0.27% (1000 ℃); The sample coefficient of thermal expansion of introducing 1% silicon nitride separately is 0.65% (1000 ℃); And the check sample coefficient of thermal expansion of not introducing norbide and silicon nitride is 1.61% (1100 ℃).It is thus clear that it is low to contain the fused quartz ceramic material coefficient of thermal expansion rate of 1% norbide and silicon nitride; The fused quartz crystallization is that the degree of cristobalite is little; The coefficient of thermal expansion of this stupalith sample is merely 8.5% of blank sample, shows that norbide and silicon nitride have tangible crystallization to fused quartz and suppress effect.
The embodiment summary sheet
Claims (8)
1. the present invention is the fused quartz ceramic preparation methods that contains norbide and silicon nitride, it is characterized in that this stupalith weight percent raw materials used and raw material is: fused quartz fine powder 97～99%, the mixing fine powders 1～3% of norbide and silicon nitride.This ceramic material may further comprise the steps: the blank preparation; Blank forming; Body drying; Base substrate burns till.
2. the fused quartz ceramic preparation methods that contains norbide and silicon nitride as claimed in claim 1 is characterized in that the particle diameter＜0.065mm of used fused quartz fine powder, and the weight percent of fused quartz fine powder purity is: SiO
2>=99.9%.
3. the fused quartz ceramic preparation methods that contains norbide and silicon nitride as claimed in claim 1 is characterized in that the mixing fine powders weight percent of used norbide and silicon nitride is: norbide fine powder 50%, silicon nitride fine powder 50%.
4. the fused quartz ceramic preparation methods that contains norbide and silicon nitride as claimed in claim 1 is characterized in that the particle diameter of used norbide fine powder is＜0.074mm, and the weight percent of norbide fine powder purity is: B
4C>=95.0%; The particle diameter of silicon nitride fine powder is＜0.074mm, and the weight percent of silicon nitride fine powder purity is: Si
3N
4>=90.0%.
5. the fused quartz ceramic preparation methods that contains norbide and silicon nitride as claimed in claim 1; The preparation method who it is characterized in that blank does after fused quartz fine powder, norbide fine powder, silicon nitride fine powder are measured by proportioning to mix 3～10 minutes; Polyvinyl alcohol solution bonding 6% (the weight percent that under continuous whipped state, progressively adds mass concentration 2% then; Add); Continue to mix and cross 40 mesh sieves after 10～15 minutes, the continued of sieving stirs and was placed on ageing mixture in the airtight plastics bag in 2～5 minutes, but obtains the blank of voltage supply power moulding behind the ageing mixture through 4～6 hours.
6. the fused quartz ceramic preparation methods that contains norbide and silicon nitride as claimed in claim 1; The forming method that it is characterized in that base substrate is to mix and adopt hydropress to be shaped to base substrate through the blank of ageing mixture above-mentioned, and blank forming pressure is >=50MPa.
7. the fused quartz ceramic preparation methods that contains norbide and silicon nitride as claimed in claim 1, the drying means that it is characterized in that base substrate are the dry base substrates that base substrate after the moulding Gong to be burnt till in the acquisition in 2～3 hours of 60～90 ℃ of dryings.
8. the fused quartz ceramic preparation methods that contains norbide and silicon nitride as claimed in claim 1; The process for calcining that it is characterized in that base substrate is with dried base substrate 1100 ℃ of heating of warp earlier 1～2 hour, after 1～3 hour high temperature of 1250～1400 ℃ of insulations burns till, obtains to contain the fused quartz ceramic material of norbide and silicon nitride again.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496853A (en) * | 2013-09-23 | 2014-01-08 | 河北联合大学 | Zirconium boride contained fused quartz ceramic material and preparation method thereof |
| CN106278211A (en) * | 2016-08-26 | 2017-01-04 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of preparation method of labyrinth quartz ceramic |
| CN106431422A (en) * | 2015-08-05 | 2017-02-22 | 江苏中正耐火材料有限公司 | Fused quartz repair material |
| CN106587963A (en) * | 2016-12-27 | 2017-04-26 | 郑州源冉生物技术有限公司 | High-strength ceramic with small expansion coefficient and preparation method thereof |
| CN106927801A (en) * | 2015-12-31 | 2017-07-07 | 湖南工业大学 | The preparation method and functionalization fused quartz powder of the functionalization fused quartz powder prepared for quartz-ceramics |
| CN106927800A (en) * | 2015-12-31 | 2017-07-07 | 湖南工业大学 | A kind of process for preparing note solidification forming fused quartz ceramic |
| CN108374196A (en) * | 2018-04-28 | 2018-08-07 | 烟台同立高科新材料股份有限公司 | A kind of polycrystalline silicon ingot casting fused silica crucible and preparation method thereof |
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| CN101767983A (en) * | 2009-12-25 | 2010-07-07 | 河北理工大学 | Fused silica ceramic material containing ytterbium oxide and preparation method thereof |
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2011
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| CN101767983A (en) * | 2009-12-25 | 2010-07-07 | 河北理工大学 | Fused silica ceramic material containing ytterbium oxide and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496853A (en) * | 2013-09-23 | 2014-01-08 | 河北联合大学 | Zirconium boride contained fused quartz ceramic material and preparation method thereof |
| CN106431422A (en) * | 2015-08-05 | 2017-02-22 | 江苏中正耐火材料有限公司 | Fused quartz repair material |
| CN106927801A (en) * | 2015-12-31 | 2017-07-07 | 湖南工业大学 | The preparation method and functionalization fused quartz powder of the functionalization fused quartz powder prepared for quartz-ceramics |
| CN106927800A (en) * | 2015-12-31 | 2017-07-07 | 湖南工业大学 | A kind of process for preparing note solidification forming fused quartz ceramic |
| CN106927801B (en) * | 2015-12-31 | 2020-04-14 | 湖南工业大学 | Preparation method of functionalized fused quartz powder for quartz ceramic preparation and functionalized fused quartz powder |
| CN106927800B (en) * | 2015-12-31 | 2020-05-05 | 湖南工业大学 | Process method for preparing gel-casting fused quartz ceramic |
| CN106278211A (en) * | 2016-08-26 | 2017-01-04 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of preparation method of labyrinth quartz ceramic |
| CN106587963A (en) * | 2016-12-27 | 2017-04-26 | 郑州源冉生物技术有限公司 | High-strength ceramic with small expansion coefficient and preparation method thereof |
| CN108374196A (en) * | 2018-04-28 | 2018-08-07 | 烟台同立高科新材料股份有限公司 | A kind of polycrystalline silicon ingot casting fused silica crucible and preparation method thereof |
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| CN102515725B (en) | 2014-07-23 |
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