CN106810264A - A kind of preparation method of silicon nitride ceramics - Google Patents
A kind of preparation method of silicon nitride ceramics Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of silicon nitride ceramics, comprise the following steps：From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material；Mixed with ball mill；It is put into drying in drying box；Granulation；Hydrostatic profile, depanning after shaping；Molding blank is put into sintering furnace, microwave sintering is carried out in microwave sintering device under protective atmosphere, taken out after being incubated a period of time after sintering, natural cooling finished product silicon nitride ceramics.Compared with prior art, the Ti in the present invention3C2Pore structure with two dimension, can be by Si3N4、Ce2O3And Al2O3Being absorbed to it has in the hole of two dimension, heating using microwave is recycled to be sintered material, sinter each molecular material, obtained silicon nitride ceramics hole is small, and the hole of two dimension can sponge external force and it be done work produced energy, become the storage energy of material internal, without being broken, therefore make obtained silicon nitride ceramics big compared to common silicon nitride ceramics bending strength, service life also increases by 30% or so.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic material, particularly a kind of preparation method of silicon nitride ceramics.
Background technology
Nitride ceramics are class purposes new ceramic materials widely, it is including aluminium nitride ceramics, silicon nitride ceramics, boron nitride ceramics etc., its composite is even more innumerable, just because of its critical role in Material Field, so being increasingly subject to the extensive attention of investigation of materials person and application person.
But due to the nitride ceramics problem of material and manufacture craft problem in itself, the intensity of obtained silicon nitride ceramic material does not reach the qualification used in some special dimensions also.
It would therefore be highly desirable to develop a kind of preparation method of silicon nitride ceramics, make that obtained silicon nitride ceramics intensity is stronger, service life is longer.
The content of the invention
A kind of deficiency the invention aims to solve prior art problem, there is provided preparation method of silicon nitride ceramics, makes obtained silicon nitride ceramics big compared to common silicon nitride ceramics bending strength, and service life also increases by 30% or so.
To reach above-mentioned purpose, the present invention is implemented according to following technical scheme：
A kind of preparation method of silicon nitride ceramics, comprises the following steps：
1）From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4；
2）Above-mentioned raw materials are mixed with ball mill；
3）Slurry is put into drying box and is dried；
4）Dry feed powder granulation will be mixed；
5）Sieving powder is put into mould, isostatic pressing, depanning after shaping；
6）Molding blank is put into sintering furnace; microwave sintering is carried out in microwave sintering device under protective atmosphere; the frequency span of microwave is 2.45GHz; the temperature of microwave sintering is 500 DEG C~3000 DEG C; pressure is 2-4MPa; taken out after being incubated a period of time after sintering, natural cooling finished product silicon nitride ceramics.
Further, the step 1）Middle Si3N4Granularity for d50 be less than 0.2 micron, Ti3C2Granularity d50 be less than 0.5 micron, Ce2O3Granularity d50 be less than 0.3 micron, Al2O3Granularity for d50 be less than 0.5 micron.
As preferred scheme of the invention, the step 5）In briquetting pressure be 190-200MPa.
As preferred scheme of the invention, the Si3N4Granularity for d50 be 0.1 micron, Ti3C2Granularity d50 be 0.4 micron, Ce2O3Granularity d50 be 0.2 micron, Al2O3Granularity for d50 be 0.4 micron.
As preferred scheme of the invention, the step 6）Protective atmosphere is nitrogen or argon gas.
As preferred scheme of the invention, the step 6）Soaking time is 3-24 hours.
Compared with prior art, the Ti in the present invention3C2Pore structure with two dimension, can be by Si3N4、Ce2O3And Al2O3Being absorbed to it has in the hole of two dimension, heating using microwave is recycled to be sintered material, sinter each molecular material, obtained silicon nitride ceramics hole is small, and the hole of two dimension can sponge external force and it be done work produced energy, become the storage energy of material internal, without being broken, therefore make obtained silicon nitride ceramics big compared to common silicon nitride ceramics bending strength, service life also increases by 30% or so.
Brief description of the drawings
Fig. 1 is the electromicroscopic photograph of silicon nitride obtained in the present invention.
Specific embodiment
With reference to specific embodiment, the invention will be further described, and the illustrative examples and explanation invented herein are for explaining the present invention but not as a limitation of the invention.
Embodiment 1
A kind of preparation method of silicon nitride ceramics as shown in Figure 1, comprises the following steps：
1）From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, Si3N4Granularity for d50 be equal to 0.1 micron, Ti3C2Granularity d50 be equal to 0.4 micron, Ce2O3Granularity d50 be equal in 0.2 micron, Al2O3Granularity for d50 be equal to 0.4 micron, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4,；
2）Above-mentioned raw materials are mixed with ball mill；
3）Slurry is put into drying box and is dried；
4）Dry feed powder granulation will be mixed；
5）Sieving powder is put into mould, isostatic pressing, briquetting pressure is 190MPa, depanning after shaping；
6）Molding blank is put into sintering furnace, microwave sintering is carried out in microwave sintering device under nitrogen or argon gas atmosphere, the frequency span of microwave is 2.45GHz, the temperature of microwave sintering is 500 DEG C, pressure is 2MPa, taken out after being incubated 3 hours after sintering, natural cooling finished product silicon nitride ceramics finished product silicon nitride ceramics.
After measured, finished product silicon nitride ceramics density is 3.44g/cm3, bending strength 320MPa.
Embodiment 2
A kind of preparation method of silicon nitride ceramics as shown in Figure 1, comprises the following steps：
1）From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, Si3N4Granularity for d50 be equal to 0.1 micron, Ti3C2Granularity d50 be equal to 0.3 micron, Ce2O3Granularity d50 be equal to 0.2 micron, Al2O3Granularity for d50 be equal to 0.3 micron, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4,；
2）Above-mentioned raw materials are mixed with ball mill；
3）Slurry is put into drying box and is dried；
4）Dry feed powder granulation will be mixed；
5）Sieving powder is put into mould, isostatic pressing, briquetting pressure is 200MPa, depanning after shaping；
6）Molding blank is put into sintering furnace, microwave sintering is carried out in microwave sintering device under nitrogen or argon gas atmosphere, the frequency span of microwave is 2.45GHz, the temperature of microwave sintering is 3000 DEG C, pressure is 4MPa, taken out after being incubated 24 hours after sintering, natural cooling finished product silicon nitride ceramics.
After measured, finished product silicon nitride ceramics density is 3.21g/cm3, bending strength 351MPa.
Embodiment 3
A kind of preparation method of silicon nitride ceramics as shown in Figure 1, comprises the following steps：
1）From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, Si3N4Granularity for d50 be equal to 0.15 micron, Ti3C2Granularity d50 be equal to 0.4 micron, Ce2O3Granularity d50 be equal to 0.1 micron, Al2O3Granularity for d50 be equal to 0.1 micron, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4,；
2）Above-mentioned raw materials are mixed with ball mill；
3）Slurry is put into drying box and is dried；
4）Dry feed powder granulation will be mixed；
5）Sieving powder is put into mould, isostatic pressing, briquetting pressure is 195MPa, depanning after shaping；
6）Molding blank is put into sintering furnace, microwave sintering is carried out in microwave sintering device under nitrogen or argon gas atmosphere, the frequency span of microwave is 2.45GHz, the temperature of microwave sintering is 1000 DEG C, pressure is 3MPa, taken out after being incubated 8 hours after sintering, natural cooling finished product silicon nitride ceramics.
After measured, finished product silicon nitride ceramics density is 3.35g/cm3, bending strength 332MPa.
Embodiment 4
A kind of preparation method of silicon nitride ceramics as shown in Figure 1, comprises the following steps：
7）From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, Si3N4Granularity for d50 be equal to 0.1 micron, Ti3C2Granularity d50 be equal to 0.2 micron, Ce2O3Granularity d50 be equal to 0.1 micron, Al2O3Granularity for d50 be equal to 0.1 micron, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4,；
8）Above-mentioned raw materials are mixed with ball mill；
9）Slurry is put into drying box and is dried；
10）Dry feed powder granulation will be mixed；
11）Sieving powder is put into mould, isostatic pressing, briquetting pressure is 200MPa, depanning after shaping；
12）Molding blank is put into sintering furnace, microwave sintering is carried out in microwave sintering device under nitrogen or argon gas atmosphere, the frequency span of microwave is 2.45GHz, the temperature of microwave sintering is 3000 DEG C, pressure is 4MPa, taken out after being incubated 24 hours after sintering, natural cooling finished product silicon nitride ceramics.
After measured, finished product silicon nitride ceramics density is 3.01g/cm3, bending strength 318MPa.
Embodiment 5
A kind of preparation method of silicon nitride ceramics as shown in Figure 1, comprises the following steps：
13）From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, Si3N4Granularity for d50 be equal to 0.18 micron, Ti3C2Granularity d50 be equal to 0.35 micron, Ce2O3Granularity d50 be equal to 0.15 micron, Al2O3Granularity for d50 be equal to 0.45 micron, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4,；
14）Above-mentioned raw materials are mixed with ball mill；
15）Slurry is put into drying box and is dried；
16）Dry feed powder granulation will be mixed；
17）Sieving powder is put into mould, isostatic pressing, briquetting pressure is 190-200MPa, depanning after shaping；
18）Molding blank is put into sintering furnace, microwave sintering is carried out in microwave sintering device under nitrogen or argon gas atmosphere, the frequency span of microwave is 2.45GHz, the temperature of microwave sintering is 2000 DEG C, pressure is 3MPa, taken out after being incubated 13 hours after sintering, natural cooling finished product silicon nitride ceramics.
After measured, finished product silicon nitride ceramics density is 3.31g/cm3, bending strength 335MPa.
Embodiment 6
A kind of preparation method of silicon nitride ceramics as shown in Figure 1, comprises the following steps：
19）From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, Si3N4Granularity for d50 be equal to 0.1 micron, Ti3C2Granularity d50 be equal to 0.4 micron, Ce2O3Granularity d50 be equal to 0.15 micron, Al2O3Granularity for d50 be equal to 0.35 micron, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4,；
20）Above-mentioned raw materials are mixed with ball mill；
21）Slurry is put into drying box and is dried；
22）Dry feed powder granulation will be mixed；
23）Sieving powder is put into mould, isostatic pressing, briquetting pressure is 200MPa, depanning after shaping；
24）Molding blank is put into sintering furnace, microwave sintering is carried out in microwave sintering device under nitrogen or argon gas atmosphere, the frequency span of microwave is 2.45GHz, the temperature of microwave sintering is 1500 DEG C, pressure is 3MPa, taken out after being incubated 18 hours after sintering, natural cooling finished product silicon nitride ceramics.
After measured, finished product silicon nitride ceramics density is 3.37g/cm3, bending strength 329MPa.
Technical scheme is not limited to the limitation of above-mentioned specific embodiment, and the technology deformation that every technology according to the present invention scheme is made is each fallen within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of silicon nitride ceramics, it is characterised in that comprise the following steps：
From Si3N4、Ti3C2、Ce2O3And Al2O3It is raw material, the Si3N4、Ti3C2、Ce2O3And Al2O3Mass ratio be:50：40：6：4；
Above-mentioned raw materials are mixed with ball mill；
Slurry is put into drying box and is dried；
Dry feed powder granulation will be mixed；
Sieving powder is put into mould, isostatic pressing, depanning after shaping；
Molding blank is put into sintering furnace; microwave sintering is carried out in microwave sintering device under protective atmosphere; the frequency span of microwave is 2.45GHz; the temperature of microwave sintering is 500 DEG C~3000 DEG C; pressure is 2-4MPa; taken out after being incubated a period of time after sintering, natural cooling finished product silicon nitride ceramics.
2. the preparation method of silicon nitride ceramics according to claim 1, it is characterised in that：The step 1）Middle Si3N4Granularity for d50 be less than 0.2 micron, Ti3C2Granularity d50 be less than 0.5 micron, Ce2O3Granularity d50 be less than 0.3 micron, Al2O3Granularity for d50 be less than 0.5 micron.
3. the preparation method of silicon nitride ceramics according to claim 1, it is characterised in that：The step 5）In briquetting pressure be 190-200MPa.
4. the preparation method of silicon nitride ceramics according to claim 2, it is characterised in that：The Si3N4Granularity for d50 be 0.1 micron, Ti3C2Granularity d50 be 0.4 micron, Ce2O3Granularity d50 be 0.2 micron, Al2O3Granularity for d50 be 0.4 micron.
5. the preparation method of silicon nitride ceramics according to claim 1, it is characterised in that：The step 6）Protective atmosphere is nitrogen or argon gas.
6. the preparation method of silicon nitride ceramics according to claim 1, it is characterised in that：The step 6）Soaking time is 3-24 hours.
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| CN107382287A (en) * | 2017-08-09 | 2017-11-24 | 赣州艺佳兴陶瓷有限公司 | A kind of preparation method of high-absorbility solar energy ceramic material |
| CN107382288A (en) * | 2017-08-09 | 2017-11-24 | 赣州艺佳兴陶瓷有限公司 | A kind of preparation technology of novel fire resistant ceramic material |
| CN107445589A (en) * | 2017-08-01 | 2017-12-08 | 赣州艺佳兴陶瓷有限公司 | A kind of super hydrophilic easily cleaning function ceramic material and its preparation technology |
| CN107555966A (en) * | 2017-08-01 | 2018-01-09 | 赣州艺佳兴陶瓷有限公司 | A kind of preparation method of electron ceramic material |
| CN107555960A (en) * | 2017-08-01 | 2018-01-09 | 赣州艺佳兴陶瓷有限公司 | A kind of functional ceramic powder material and preparation method and application |
| WO2022166598A1 (en) * | 2021-02-02 | 2022-08-11 | 中材高新氮化物陶瓷有限公司 | Preparation method for silicon nitride-based multiphase conductive ceramic |
| CN116553937A (en) * | 2023-03-20 | 2023-08-08 | 衡阳凯新特种材料科技有限公司 | Silicon nitride composite ceramic material for sealing ring and preparation method thereof |
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| CN107445589A (en) * | 2017-08-01 | 2017-12-08 | 赣州艺佳兴陶瓷有限公司 | A kind of super hydrophilic easily cleaning function ceramic material and its preparation technology |
| CN107555966A (en) * | 2017-08-01 | 2018-01-09 | 赣州艺佳兴陶瓷有限公司 | A kind of preparation method of electron ceramic material |
| CN107555960A (en) * | 2017-08-01 | 2018-01-09 | 赣州艺佳兴陶瓷有限公司 | A kind of functional ceramic powder material and preparation method and application |
| CN107445589B (en) * | 2017-08-01 | 2020-07-21 | 赣州艺佳兴陶瓷有限公司 | Super-hydrophilic easy-to-clean functional ceramic material and preparation process thereof |
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| CN107382287A (en) * | 2017-08-09 | 2017-11-24 | 赣州艺佳兴陶瓷有限公司 | A kind of preparation method of high-absorbility solar energy ceramic material |
| CN107382288A (en) * | 2017-08-09 | 2017-11-24 | 赣州艺佳兴陶瓷有限公司 | A kind of preparation technology of novel fire resistant ceramic material |
| WO2022166598A1 (en) * | 2021-02-02 | 2022-08-11 | 中材高新氮化物陶瓷有限公司 | Preparation method for silicon nitride-based multiphase conductive ceramic |
| CN116553937A (en) * | 2023-03-20 | 2023-08-08 | 衡阳凯新特种材料科技有限公司 | Silicon nitride composite ceramic material for sealing ring and preparation method thereof |
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