CN104030691B - A kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material - Google Patents
A kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material Download PDFInfo
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Abstract
The present invention relates to field of ceramic preparation technology, specifically disclosing a kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material, it comprises the step of batch mixing, compacting, isostatic cool pressing, sintering and aft-loaded airfoil, and ceramic raw material by weight percentage, comprises following component: Si
3n
4: 80-90%, Y
2o
3: 6-14%, α phase Al
2o
3: 1-5%, WC:1-5%, TiC:1-5%.This preparation method's step is simple, convenient and easy, stable preparation process, production efficiency is high, the hardness of the structural member pottery utilizing the method to prepare is large, intensity is high, and there is higher resistance to elevated temperatures, high voltage withstanding impact property and resist bending performance, the field that material requirements is high can be widely used in, be particularly useful for refractory ceramics bearing and ceramics turbo blade.
Description
Technical field
The present invention relates to field of ceramic preparation technology, specifically disclosing a kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material.
Background technology
Along with the continuous progress of science and technology, also more and more higher to the performance requirement of material.Silicon nitride and composite ceramic material thereof are the most promising a kind of engineering ceramic materials in structural ceramics, there is the characteristic of good high strength, high rigidity, high voltage withstanding, corrosion-resistant, anti-thermal shock and the multiple excellence such as anti-oxidant, therefore all have wide practical use in fields such as metallurgy, chemical industry, petroleum machineries.Also list clearly in " 12 " planning material component that country promulgates, silicon nitride and composite ceramic material thereof become to attach most importance to support industry, as photovoltaic industry needs resistance to 20,000 volts of voltge surges, resistance to about 500 DEG C high temperature simultaneously, steel production industry ore deposit is husky, the conveying equipments such as powder, the anti-shock plate of transfer tape and two side shields etc. need high hardness wear-resisting material, machinery, high strength plunger in pump industry replaces carbide alloy, requirement that the thermal coefficient of expansion needed in the requirement of acid-fast alkali-proof and high-speed bearing in bearing industry is little etc., silicon nitride ceramics all can be applied to these fields.
Summary of the invention
The object of the invention is to: providing a kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material, high, the high temperature resistant and high voltage withstanding impact of the intensity of the structural member pottery utilizing the method to prepare, the field that material requirements is high can be widely used in, be particularly useful for refractory ceramics bearing and ceramics turbo blade.
For achieving the above object, technical scheme of the present invention is as follows:
Take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material, it comprises the step of batch mixing, compacting, isostatic cool pressing, sintering and aft-loaded airfoil, and ceramic raw material by weight percentage, comprises following component:
Mixing method is ball mill mixing, and during batch mixing, material is 1:3 with the mass ratio of ball;
The solvent that described ball mill mixing adopts is alcohol;
The material of ball is Si
3n
4.；
The time of ball milling is 6-8 days, and the speed of ball milling is 60-80r/min;
Compacting is with mould molding on hydraulic press;
During isostatic cool pressing, institute applied pressure 200MPa;
Described sintering step, is undertaken by following technique:
(1) ceramic batch after isostatic cool pressing is loaded in graphite crucible, in air pressure stove, be warming up to 300 DEG C with the speed of 1-2 DEG C/min, and be incubated 1 hour;
(2) continue to be warming up to 400 DEG C with the speed of 5 DEG C/min in air pressure stove, employing vacuum pump evacuation, opens intake valve simultaneously and air outlet valve is filled with N
2;
(3) continue to be warming up to 1300 DEG C with the speed of 10 DEG C/min in air pressure stove, and be incubated 1 hour, then be warming up to 1700 DEG C with the speed of 1 DEG C/min, be constantly filled with N
2, make waste gas in air pressure stove along with N
2be filled with and discharge, when temperature reaches 1700 DEG C, close air outlet valve;
(4) N is strengthened
2flow makes its pressure be increased to 4-6MPa, is warming up to 1850 DEG C simultaneously, and is incubated 20-40 minute with the speed of 8-10 DEG C/min, is cooled to room temperature after stopping heating with air pressure stove.
In order to obtain better product, described aft-loaded airfoil is that cutting technique obtains structural member pottery by the ceramic block that sinters through grinding.
Preferably, described α phase Al
2o
3β phase Al
2o
3powder is obtained through 1400 DEG C of calcinings.
By technique scheme, the invention provides a kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material, and this preparation method's step is simple, convenient and easy, stable preparation process, and production efficiency is high, and the performance of the structural member pottery obtained is good.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Below the specific embodiment of the present invention is described in further detail.
Embodiment 1
Take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material, it comprises the step of batch mixing, compacting, isostatic cool pressing, sintering and aft-loaded airfoil.Take Si
3n
4powder 85kg, Y
2o
39kg, α phase Al
2o
32kg, WC2kg, TiC2kg, Si
3n
4ball 240kg, is placed in ball milling bucket and adopts alcohol as solvent, carry out ball milling 7 days with the speed of 80r/min; And then with mould just one-step forming on hydraulic press; Utilize cold isostatic press to pressurize with 200MPa pressure, make the even density of all directions of batch mixing; Again the ceramic batch after isostatic cool pressing is loaded in graphite crucible, in air pressure stove, be warming up to 300 DEG C with the speed of 2 DEG C/min, and be incubated 1 hour, continue to be warming up to 400 DEG C with the speed of 5 DEG C/min, adopt vacuum pump evacuation simultaneously, and open intake valve and air outlet valve is filled with N
2, then continue to be warming up to 1300 DEG C with the speed of 10 DEG C/min, and be incubated 1 hour, then be warming up to 1700 DEG C with the speed of 1 DEG C/min, be constantly filled with N
2, make waste gas in air pressure stove along with N
2be filled with and discharge, close air outlet valve when temperature reaches 1700 DEG C, strengthen N
2flow makes its pressure be increased to 6MPa, is warming up to 1850 DEG C simultaneously, and is incubated 40 minutes with the speed of 10 DEG C/min, is cooled to room temperature after stopping heating with air pressure stove; Again by the ceramic block that sinters through grinding, cutting technique obtains structural member pottery.
Y is added in batch mixing
2o
3with α phase Al
2o
3the generation temperature of glassy phase can be reduced, can soak and dissolve Si
3n
4powder, thus the heat-resisting quantity improving product.
During ball milling, using alcohol as solvent, play the effect of dispersant on the one hand, the reunion between batch mixing particle can be prevented, play cooling effect on the other hand, reduce surface energy.
Embodiment 2
Take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material, it comprises the step of batch mixing, compacting, isostatic cool pressing, sintering and aft-loaded airfoil.Take Si
3n
4powder 90kg, Y
2o
37kg, α phase Al
2o
31kg, WC1kg, TiC1kg, Si
3n
4ball 270kg, is placed in ball milling bucket and adopts alcohol as solvent, carry out ball milling 7 days with the speed of 70r/min; And then with mould just one-step forming on hydraulic press; Utilize cold isostatic press to pressurize with 200MPa pressure, make the even density of all directions of batch mixing; Again the ceramic batch after isostatic cool pressing is loaded in graphite crucible, in air pressure stove, be warming up to 300 DEG C with the speed of 2 DEG C/min, and be incubated 1 hour, continue to be warming up to 400 DEG C with the speed of 5 DEG C/min, adopt vacuum pump evacuation simultaneously, and open intake valve and air outlet valve is filled with N
2, then continue to be warming up to 1300 DEG C with the speed of 10 DEG C/min, and be incubated 1 hour, then be warming up to 1700 DEG C with the speed of 1 DEG C/min, be constantly filled with N
2, make waste gas in air pressure stove along with N
2be filled with and discharge, when temperature reaches 1700 DEG C, close air outlet valve, strengthen N
2flow makes its pressure be increased to 6MPa, is warming up to 1850 DEG C simultaneously, and is incubated 40 minutes with the speed of 9 DEG C/min, is cooled to room temperature after stopping heating with air pressure stove; Again by the ceramic block that sinters through grinding, cutting technique obtains structural member pottery.
Be exactly more than a kind of take silicon nitride as the method that gas pressure sintering structural member pottery prepared by raw material, its advantage is: simple to operate, stable preparation process, production efficiency is high, and the hardness of the structural member pottery obtained is large, intensity is high, there is good resistance to elevated temperatures, high voltage withstanding impact property and resist bending performance.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (3)
1. be the method that gas pressure sintering structural member pottery prepared by raw material with silicon nitride, it is characterized in that, it comprises the step of batch mixing, compacting, isostatic cool pressing, sintering and aft-loaded airfoil, and ceramic raw material by weight percentage, comprises following component:
Mixing method is ball mill mixing, and during batch mixing, material is 1:3 with the mass ratio of ball;
The solvent that described ball mill mixing adopts is alcohol;
The material of ball is Si
3n
4;
The time of ball milling is 6-8 days, and the speed of ball milling is 60-80r/min;
Compacting is with mould molding on hydraulic press;
During isostatic cool pressing, institute applied pressure 200MPa;
Described sintering step, is undertaken by following technique:
(1) ceramic batch after isostatic cool pressing is loaded in graphite crucible, in air pressure stove, be warming up to 300 DEG C with the speed of 1-2 DEG C/min, and be incubated 1 hour;
(2) continue to be warming up to 400 DEG C with the speed of 5 DEG C/min in air pressure stove, employing vacuum pump evacuation, opens intake valve simultaneously and air outlet valve is filled with N
2;
(3) continue to be warming up to 1300 DEG C with the speed of 10 DEG C/min in air pressure stove, and be incubated 1 hour, then be warming up to 1700 DEG C with the speed of 1 DEG C/min, be constantly filled with N
2, make waste gas in air pressure stove along with N
2be filled with and discharge, when temperature reaches 1700 DEG C, close air outlet valve;
(4) N is strengthened
2flow makes it pressure and is increased to 4-6MPa, is warming up to 1850 DEG C simultaneously, and is incubated 20-40 minute with the speed of 8-10 DEG C/min, is cooled to room temperature after stopping heating with air pressure stove.
2. according to claim 1 a kind of be the method that gas pressure sintering structural member pottery prepared by raw material with silicon nitride, it is characterized in that, described aft-loaded airfoil is that cutting technique obtains structural member pottery by the ceramic block that sinters through grinding.
3. according to claim 1 a kind of be the method that gas pressure sintering structural member pottery prepared by raw material with silicon nitride, it is characterized in that, described α phase Al
2o
3β phase Al
2o
3powder is obtained through 1400 DEG C of calcinings.
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| CN106808559A (en) * | 2015-11-27 | 2017-06-09 | 衡阳凯新特种材料科技有限公司 | A kind of preparation method of silicon nitride crucible |
| CN105541342A (en) * | 2016-01-08 | 2016-05-04 | 梁小利 | High-strength silicon nitride composite ceramic material and preparation method thereof |
| CN106518089B (en) * | 2016-11-25 | 2019-05-14 | 中国工程物理研究院材料研究所 | A kind of preparation method of high performance and big size silicon nitride ceramic material |
| CN108863397A (en) * | 2018-07-13 | 2018-11-23 | 威海圆环先进陶瓷股份有限公司 | A kind of technique preparing SiN ceramic with high heat conductivity crucible |
| CN110328739A (en) * | 2019-08-16 | 2019-10-15 | 刘得顺 | A kind of production method of ceramics turbo |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508574A (en) * | 2009-03-25 | 2009-08-19 | 王铀 | Ceramic material with amorphous/nanocrystalline structure and method of producing the same |
| CN102595665A (en) * | 2012-02-28 | 2012-07-18 | 威海兴泰金属制造有限公司 | Silicon nitride heating sheet and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508574A (en) * | 2009-03-25 | 2009-08-19 | 王铀 | Ceramic material with amorphous/nanocrystalline structure and method of producing the same |
| CN102595665A (en) * | 2012-02-28 | 2012-07-18 | 威海兴泰金属制造有限公司 | Silicon nitride heating sheet and manufacturing method thereof |
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