CN111548163B - Method for preparing silicon nitride ceramic ball for large-size wind power generation - Google Patents
Method for preparing silicon nitride ceramic ball for large-size wind power generation Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 56
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000000919 ceramic Substances 0.000 title claims abstract description 29
- 238000010248 power generation Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 66
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 29
- 235000015895 biscuits Nutrition 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 claims description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 9
- 238000009694 cold isostatic pressing Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000006104 solid solution Substances 0.000 abstract description 3
- 239000012298 atmosphere Substances 0.000 description 9
- 230000004927 fusion Effects 0.000 description 6
- 238000009966 trimming Methods 0.000 description 6
- 239000007921 spray Substances 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000012798 spherical particle Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention discloses a method for preparing silicon nitride ceramic balls for large-size wind power generation, which is characterized in that high-toughness silicon nitride materials are subjected to system selection through technologies such as nano modification, multi-term solid solution, particle gradation and the like; preparing large-size silicon nitride ceramic balls by adopting a cold isostatic pressing near-net-size forming technology; an optimal process route is determined by combining the air pressure sintering and the hot isostatic pressing sintering post-treatment process, so that the defects of the large-size bearing ball at present are overcome. The high-toughness silicon nitride material is subjected to system selection by technologies such as nano modification, multi-term solid solution, particle grading and the like; preparing large-size silicon nitride ceramic balls by adopting a cold isostatic pressing near-net-size forming technology; an optimal process route is determined by combining a gas pressure sintering and hot isostatic pressing sintering post-treatment process, so that the defects of large size, difficult sintering, uneven density gradient, low yield, poor batch stability and the like of the conventional large-size bearing ball are overcome.
Description
Technical Field
The invention relates to the technical field of ceramic preparation, and particularly provides a method for preparing a silicon nitride ceramic ball for large-size wind power generation.
Background
In recent years, world advanced wind power bearings including yaw bearings and pitch bearings are particularly suitableThe main shaft bearing mainly comprises a hybrid bearing, and rolling bodies used in the hybrid bearing are silicon nitride ceramic balls (C)
The material has the characteristics of high strength, high hardness, high temperature resistance, corrosion resistance, oxidation resistance, thermal shock resistance, creep resistance and good wear resistance, can still maintain the excellent performance at high temperature, and is widely applied to the high-temperature gas turbine, aerospace, nuclear industry, high-efficiency engine parts and other high-technology fields.
The silicon nitride ceramic ball mixed ceramic bearing has the working temperature range of 800 ℃, has excellent self-lubricating property, corrosion resistance and wear resistance, and has the working strength and the service life 4-5 times of those of a common all-steel bearing.
However, the production of large-size silicon nitride balls mainly has the main problems of large size, difficult sintering, uneven density gradient, low yield, poor batch stability and the like, so that the current industrialized silicon nitride bearing balls are basically in the size
The following.
Disclosure of Invention
The technical task of the invention is to provide a method for preparing silicon nitride ceramic balls for large-size wind power generation aiming at the problems existing in the prior art and aiming at overcoming the problems of non-uniform density and poor batch stability of large-size ceramic bearing balls.
In order to realize the purpose, the invention provides the following technical scheme:
a method for preparing silicon nitride ceramic balls for large-size wind power generation is provided, the method modifies silicon nitride powder by adding nano TiC, effectively improves powder sintering activity, and enhances mechanical properties of materials, and the method comprises the following steps:
the nanometer TiC and the sintering aid are premixed to be uniformly mixed, and then are dispersed and mixed with the silicon nitride powder through the high-efficiency circulating stirring mill, so that self-agglomeration of nanometer particles and superfine silicon nitride particles is reduced, and uniform mixing of the silicon nitride particles and the sintering aid is realized.
The nano TiC and the sintering aid are fully mixed in advance, so that agglomeration of fine nano particles and fine silicon nitride particles can be avoided when the nano TiC and the sintering aid are mixed with the silicon nitride later.
The silicon nitride ceramic ball is prepared from the following raw materials in parts by weight: the content of silicon nitride is 90-95%, the content of nano titanium carbide is 1-2%, and the content of sintering aid is 4-8%.
The sintering aid is one or more of yttrium oxide, magnesium oxide, aluminum oxide and tungsten carbide.
The method specifically comprises the following steps:
(1) premixing the nano TiC and the sintering aid to uniformly mix the nano TiC and the sintering aid;
(2) and then uniformly mixing the silicon nitride powder with the high-efficiency circulating stirring mill, reducing self-agglomeration of nano particles and superfine silicon nitride particles, and realizing uniform mixing of the silicon nitride particles and the sintering aid.
(3) Granulating the mixed powder in a centrifugal spray granulator to form powder for later use;
(4) pressing and molding the powder to be used formed in the step (3) to form a ball blank;
(5) shaping the pressed ball blank to prepare a bearing ball biscuit meeting the requirements;
(6) putting the bearing ball biscuit obtained in the step (5) into an atmosphere pressure sintering furnace for air pressure sintering to prepare an air pressure sintering blank ball;
(7) and (4) putting the air pressure sintering blank ball obtained in the step (6) into a hot isostatic pressing sintering furnace for hot isostatic pressing treatment after sintering.
The phase content of the silicon nitride powder is more than 92 percent.
In the step (6), the sintering temperature is 1740-1900 ℃, the temperature is kept for 4 hours, the total sintering time is 15-20 hours, and the maximum pressure of the nitrogen atmosphere is 8-20 Mpa.
The sintering temperature is preferably 1780-1850 ℃.
In the step (7), the hot isostatic pressing treatment temperature is 1600-1700 ℃, the heat preservation time is 2-4 hours, and the pressure is 160-200 Mpa.
The premixing time of the nano TiC and the sintering aid in the step (1) is 4-6h, and the mixing time of uniformly mixing the nano TiC and the sintering aid with the silicon nitride powder in the step (2) is 4-6 h.
And (5) filling the powder to be used in the step (4) into a special ball-making grinding tool, and putting the special ball-making grinding tool into a cold isostatic press for pressing and molding, wherein the pressure is set to be between 180 and 260 MPa.
Compared with the prior art, the method for preparing the silicon nitride ceramic ball for large-size wind power generation has the following outstanding beneficial effects:
the method selects a high-toughness silicon nitride material system through technologies such as nano modification, multi-term solid solution, particle grading and the like; preparing large-size silicon nitride ceramic balls by adopting a cold isostatic pressing near-net-size forming technology; an optimal process route is determined by combining a post-treatment process of air pressure sintering and hot isostatic pressing sintering, so that the defects of large size, difficult sintering, uneven density gradient, low yield, poor batch stability and the like of the conventional large-size bearing ball are overcome, and the sampling density change of different parts of the obtained ceramic ball density gradient is less than 0.4%; the hardness gradient is less than 1 percent; the bending strength is more than 800 MPa.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A method for preparing silicon nitride ceramic balls for large-size wind power generation comprises the following implementation steps:
(1) placing TiC with the content of 2%, yttrium oxide with the content of 2% and magnesium oxide with the content of 2% into a ball mill for ball milling for 4 hours;
(2) putting 95% of silicon nitride powder and the auxiliary agent obtained in the step (1) into a circulating stirring mill for full fusion for 4 hours;
(3) atomizing the slurry obtained in the step (2) through closed spray granulation to obtain spherical particles with the particle size of 100-200 microns;
(4) putting the powder obtained in the step (3) into a customized ball making grinding tool, and putting the powder into cold isostatic pressing for ball making and pressing, wherein the pressure is 160Mpa, and the pressure maintaining time is 100S;
(5) trimming the biscuit balls pressed in the step (4), and trimming redundant excess materials;
(6) sintering the biscuit balls obtained in the step (5) in an atmosphere pressure sintering furnace at 1780 ℃ and 16 MPa;
(7) putting the silicon nitride blank balls obtained in the step (6) into a hot isostatic pressing sintering furnace for post-sintering treatment, wherein the sintering temperature is 1680 ℃, the heat is preserved for 3 hours, and the atmosphere pressure is 1890 MPa;
samples were taken at radius 1/2 from the center of the sphere and tested for densities of 3.23, 2.23, and 3.24, respectively. The density gradient is 0.3 percent, the Vickers hardness is 1462, 1465 and 1468, and the hardness gradient is 0.4 percent; bending strength 910 MPa.
Example 2
A method for preparing silicon nitride ceramic balls for large-size wind power generation comprises the following implementation steps:
(1) placing 1.5% of TiC, 3% of yttrium oxide and 3% of magnesium oxide into a ball mill for ball milling for 6 hours;
(2) putting 92.5% of silicon nitride powder and the auxiliary agent obtained in the step (1) into a circulating stirring mill for full fusion, wherein the fusion time is 6 hours;
(3) atomizing the slurry obtained in the step (2) through closed spray granulation to obtain spherical particles with the particle size of 100-200 microns;
(4) putting the powder obtained in the step (3) into a customized ball making grinding tool, and putting the powder into cold isostatic pressing for ball making and pressing, wherein the pressure is 180Mpa, and the pressure maintaining time is 120S;
(5) trimming the biscuit balls pressed in the step (4) to remove redundant excess materials;
(6) placing the biscuit balls obtained in the step (5) into an atmosphere pressure sintering furnace for sintering, wherein the sintering temperature is 1760 ℃ and the pressure is 14 MPa;
(7) putting the silicon nitride blank ball obtained in the step (6) into a hot isostatic pressing sintering furnace for post-sintering treatment, wherein the sintering temperature is 1650 ℃, the temperature is kept for 3 hours, and the atmosphere pressure is 190 Mpa;
samples were taken at radius 1/2 from the center of the sphere and tested for densities of 3.24, 2.24, and 3.25, respectively. The hardness is 1465, 1470 and 1470, and the bending strength is 880 Mpa.
Example 3
A method for preparing silicon nitride ceramic balls for large-size wind power generation comprises the following implementation steps:
(1) placing 1% of TiC, 3% of yttrium oxide and 6% of alumina into a ball mill for ball milling for 6 hours;
(2) putting 90% of silicon nitride powder and the auxiliary agent obtained in the step (1) into a circulating stirring mill for full fusion for 6 hours;
(3) atomizing the slurry obtained in the step (2) through closed spray granulation to obtain spherical particles with the particle size of 100-200 microns;
(4) putting the powder obtained in the step (3) into a customized ball making grinding tool, and putting the powder into cold isostatic pressing for ball making and pressing, wherein the pressure is 180Mpa, and the pressure maintaining time is 120S;
(5) trimming the biscuit balls pressed in the step (4) to remove redundant excess materials;
(6) putting the biscuit balls obtained in the step (5) into an atmosphere pressure sintering furnace for sintering, wherein the sintering temperature is 1750 ℃ and the pressure is 10 MPa;
(7) putting the silicon nitride blank ball obtained in the step (6) into a hot isostatic pressing sintering furnace for post-sintering treatment, wherein the sintering temperature is 1630 ℃, the temperature is kept for 3 hours, and the atmosphere pressure is 180 Mpa;
samples were taken at radius 1/2 from the center of the sphere and tested at densities of 3.24, 2.25, and 3.25, respectively. Hardness 1450, 1452, 1458, bending strength 830 MPa.
Example 4
A method for preparing silicon nitride ceramic balls for large-size wind power generation comprises the following implementation steps:
(1) placing 1% of TiC, 4% of yttrium oxide, 4% of aluminum oxide and 1% of tungsten carbide into a ball mill for ball milling for 6 hours;
(2) putting 90% of silicon nitride powder and the auxiliary agent obtained in the step (1) into a circulating stirring mill for full fusion, wherein the fusion time is 6 hours;
(3) atomizing the slurry obtained in the step (2) through closed spray granulation to obtain spherical particles with the particle size of 100-200 microns;
(4) putting the powder obtained in the step (3) into a customized ball making grinding tool, and putting the powder into cold isostatic pressing for ball making and pressing, wherein the pressure is 180Mpa, and the pressure maintaining time is 120S;
(5) trimming the biscuit balls pressed in the step (4), and trimming redundant excess materials;
(6) putting the biscuit balls obtained in the step (5) into an atmosphere pressure sintering furnace for sintering, wherein the sintering temperature is 1750 ℃ and the pressure is 10 MPa;
(7) putting the silicon nitride blank balls obtained in the step (6) into a hot isostatic pressing sintering furnace for post-sintering treatment, wherein the sintering temperature is 1650 ℃, the heat preservation is carried out for 3 hours, and the atmosphere pressure is 180 Mpa;
samples were taken at radius 1/2 from the center of the sphere and tested at densities of 3.25, 2.25, and 3.26, respectively. 1460, 1462, 1468 and 840 MPa.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (8)
1. A method for preparing silicon nitride ceramic balls for large-size wind power generation is characterized in that the method modifies silicon nitride powder by adding nano TiC, and the method comprises the following steps:
premixing nano TiC and a sintering aid, and dispersing and mixing the nano TiC and the sintering aid with silicon nitride powder through a high-efficiency circulating stirring mill;
the silicon nitride ceramic ball is prepared by the following raw materials in parts by weight: the content of silicon nitride is 90-95%, the content of nano titanium carbide is 1-2%, and the content of sintering aid is 4-8%;
the sintering aid is one or more of yttrium oxide, magnesium oxide, aluminum oxide and tungsten carbide.
2. The method for preparing silicon nitride ceramic balls for large-size wind power generation according to claim 1, which specifically comprises the steps of:
(1) premixing nano TiC and a sintering aid;
(2) then evenly mixing the mixture with silicon nitride powder;
(3) granulating the mixed powder to form powder for later use;
(4) pressing and molding the powder to be used formed in the step (3) to form a ball blank;
(5) shaping the pressed ball blank to prepare a bearing ball biscuit meeting the requirements;
(6) carrying out air pressure sintering on the bearing ball biscuit obtained in the step (5) to prepare an air pressure sintering blank ball;
(7) and (5) carrying out hot isostatic pressing treatment on the air pressure sintering blank ball obtained in the step (6) after sintering.
3. The method for preparing silicon nitride ceramic balls for large-size wind power generation according to claim 2, wherein the phase content of the silicon nitride powder is greater than 92%.
4. The method for preparing silicon nitride ceramic balls for large-size wind power generation according to claim 2, wherein in the step (6), the sintering temperature is 1740-1900 ℃, the temperature is kept for 4 hours, the total sintering time is 15-20 hours, and the maximum pressure of a nitrogen atmosphere is 8-20 Mpa.
5. The method of claim 4, wherein the sintering temperature is 1780-1850 ℃.
6. The method for preparing silicon nitride ceramic balls for large-size wind power generation according to claim 2, wherein the hot isostatic pressing treatment temperature in step (7) is 1600 ℃ to 1700 ℃, the holding time is 2 to 4 hours, and the pressure is 160Mpa to 200 Mpa.
7. The method for preparing silicon nitride ceramic balls for large-size wind power generation according to claim 2, wherein the premixing time of the nano TiC and the sintering aid in step (1) is 4-6h, and the time for uniformly mixing with the silicon nitride powder in step (2) is 4-6 h.
8. The method for preparing silicon nitride ceramic balls for large-sized wind power generation according to claim 2, wherein the powder to be used in step (4) is charged into a special ball-making grinding tool and placed into a cold isostatic press for pressing and forming, and the pressure is set to be between 180Mpa and 260 Mpa.
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| CN112028637A (en) * | 2020-08-24 | 2020-12-04 | 中材高新氮化物陶瓷有限公司 | Preparation method of high-reliability long-life silicon nitride ceramic ball for aviation bearing |
| CN113135762B (en) * | 2021-05-13 | 2022-03-08 | 中材高新氮化物陶瓷有限公司 | Large-size silicon nitride ceramic ball and preparation method thereof |
| CN113185302B (en) * | 2021-06-10 | 2022-08-09 | 灵石鸿润和新材料有限公司 | Large-size silicon nitride ceramic ball for wind power generation and preparation method and application thereof |
| CN113800919B (en) * | 2021-10-26 | 2023-01-03 | 中材高新氮化物陶瓷有限公司 | High-precision silicon nitride ceramic microsphere and preparation method and application thereof |
| CN116444277A (en) * | 2022-01-07 | 2023-07-18 | 埃克诺新材料（大连）有限公司 | Preparation method of oversized silicon nitride ceramic ball for oversized bearing |
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| JP2004067432A (en) * | 2002-08-06 | 2004-03-04 | Sumitomo Electric Ind Ltd | Ceramic composite sintered body and its manufacturing process |
| CN101538162A (en) * | 2009-01-21 | 2009-09-23 | 北京中材人工晶体有限公司 | Preparation method for high reliability large-scale silicon nitride ceramic material |
| CN104119079A (en) * | 2014-08-04 | 2014-10-29 | 上海泛联科技股份有限公司 | Sintering method for improving performance consistency of silicon nitride material |
| CN107399974A (en) * | 2016-05-22 | 2017-11-28 | 河北高富氮化硅材料有限公司 | A kind of method added fluoride and prepare high heat conduction silicon nitride ceramics |
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