CN102795860A - Method for preparing silicon nitride ceramic balls - Google Patents
Method for preparing silicon nitride ceramic balls Download PDFInfo
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- CN102795860A CN102795860A CN2012102411080A CN201210241108A CN102795860A CN 102795860 A CN102795860 A CN 102795860A CN 2012102411080 A CN2012102411080 A CN 2012102411080A CN 201210241108 A CN201210241108 A CN 201210241108A CN 102795860 A CN102795860 A CN 102795860A
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- silicon nitride
- biscuit
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- ceramic ball
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Abstract
The invention provides a method for preparing a silicon nitride ceramic ball, comprising the following steps of: (1) mixing silicon nitride with sintering auxiliaries, and then performing pelleting and cold isostatic pressing treatment, thereby obtaining the silicon nitride biscuit of the ceramic ball; (2) coating the biscuit obtained in the step (1) with an isolation layer, drying the biscuit and then putting the biscuit in a glass container, after thermal treatment, performing oxyhydrogen flame soldering seal in vacuum, and adding the same material as the glass container to the soldering pint, thereby obtaining the glass container packaged biscuit; and (3) under the state of no pressure, putting the glass container packaged biscuit obtained in the step (2) in a crucible, firstly, increasing the temperature so that the glass container is softened and then performing hot isostatic pressing sintering under the protection of nitrogen or argon, thereby obtaining the silicon nitride ceramic ball. The silicon nitride ceramic ball prepared by the method provided by the invention has the advantages of being high in compactness, even in crystalline grain, excellent in performance, simple in process operation and capable of realizing industrialization, and the like.
Description
Technical field
The invention belongs to the engineering ceramics preparation field, be specifically related to a kind of preparation method of silicon nitride ceramic ball, particularly a kind of Glass Containers encapsulating heat and other static pressuring processes prepares the method for high-performance, large-scale silicon nitride Ceramic Balls.
Background technology
Silicon nitride ceramics has low density, HS, high rigidity, high firmness, low-expansion coefficient, excellent performance such as corrosion-resistant, widespread use in the engineering ceramics field.Silicon nitride ceramics itself has self-lubricating property and spalling failure characteristic; Make it can significantly improve bearing rotating speed, bearing grade, bearing life as bearing roller; Therefore, adopt silicon nitride ceramics to be with a wide range of applications in fields such as space flight, the energy, machineries as the combined bearing of rolling body.
Silicon nitride is the strong covalent bond compound, and spread coefficient is little, and sinterability is poor.In order to obtain the silicon nitride sinter of density height, homogeneous microstructure, generally add suitable additive (like MgO, Al
2O
3, Y
2O
3, La
2O
3, Yb
2O
3, CeO
2Deng) promote densification sintering as sintering aid.The densification sintering technology that generally adopts at present has hot pressing (HP) and atmosphere pressures (GPS) sintering process.Adopt hot pressing (HP) silicon nitride sintered material, there is anisotropy in its performance, unit cost is high simultaneously, and material use efficiency is low, is difficult to carry out mass production; Adopt gas pressure sintering (GPS) silicon nitride material, exist microstructure inhomogeneous, there are defectives such as pore, crackle in intercrystalline, has reduced mechanical property, fatigue resistance and the reliability of material of material.
Hot isostatic pressing (HIP) technology has overcome hot-pressing sintering technique and the existing defective of gas pressure sintering technology.The less sintering aid of hot isostatic pressing (HIP) sintered silicon nitride process using; Under HTHP, promote the material densification; Eliminate defectives such as intercrystalline pore, crackle simultaneously, and can suppress growing up unusually of crystal grain, obtain homogeneous microstructure, excellent performance, isotropic silicon nitride material.To hot isostatic pressing (HIP) sintering process of pottery, mainly be to carry out HTHP agglomerating method after employing is sealed at present.Encapsulating material has multiple materials such as refractory metal (like metal Ni, Mo etc.), glass, pottery.
One Chinese patent application 200910055161.X discloses a kind of method that adopts glass encapsulating heat and other static pressuring processes to prepare silicon nitride ceramic ball, and this method is mixed silicon nitride and auxiliary agent, handles obtaining base substrate through moulding, isostatic cool pressing; Apply one deck graphite sealing coat in billet surface with solution dipping method then, put into crucible after the drying, on every side the embedding glass cullet; Be warming up to 1100 ~ 1900 ℃; Make glass melting form complete sealing, the 100 ~ 200Mpa that pressurizes then is warming up to 1700 ~ 1900 ℃; Carry out HIP sintering behind insulation 1 ~ 3h, obtain silicon nitride ceramic ball.The silicon nitride ceramic ball size diameter is 5 ~ 60mm, and microhardness is 1510 ~ 1600 Kg/mm
2, fracture toughness property is 5.0 ~ 7.8 MPam
1/2
One Chinese patent application 200410014284.6 discloses a kind of glass and has coated the method that hot isostatic pressing prepares the high-performance silicon nitride ceramics, and this method is used silicon nitride goods biscuit and invaded crystal pulling method, at its surfaces coated matcoveredn; Prevent that the high temperature lower-glass from immersing in the silicon nitride goods, silicon nitride goods biscuit is imbedded in the glass powder, in the hot isostatic pressing stove, vacuumize, heat; Glass is fusion at high temperature; Coated silicon nitride goods biscuit, and then pressurization, silicon nitride ceramics obtained; Its compactness is good, homogeneous microstructure.
One Chinese patent application 200610030103.8 discloses a kind of preparation method of large scale ceramic ball; Comprise batch mixing, moulding and sintering; This method is a raw material with silicon nitride and additive, and the quality proportioning of silicon nitride powder and additive is 100:15 ~ 5, and described additive comprises Y
2O
3, Al
2O
3, La
2O
3, CeO
2Take by weighing raw material by above-mentioned quality proportioning, adopt the method for ball milling to mix, dry-pressing formed; Carry out isostatic cool pressing then and handle, the gained base substrate adopts glass bag technology under the protection of nitrogen or argon gas, to carry out HIP sintering, insulation for some time; Sintering finishes back control cooling, obtains product.Microhardness is 1500 ~ 1550 Kg/mm
2, fracture toughness property is 5.4 ~ 6.3 MPam
1/2
At present, in the silicon nitride ceramic ball preparation field, its product exist void content many, defectives such as crackle, compactness is poor, tissue odds is even, performance is low are arranged.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of high-performance, large-scale silicon nitride Ceramic Balls, this method have technological operation simple, can realize advantage such as industrialization.The silicon nitride ceramic ball compactness height of this method preparation, uniform crystal particles, excellent performance, safety height.
The objective of the invention is to realize through following technical scheme:
A kind of preparation method of silicon nitride ceramic ball, this preparation method comprises the steps:
(1) silicon nitride and sintering aid mixing, granulation, cold isostatic compaction are handled, obtained the silicon nitride ceramic ball biscuit;
(2) the biscuit surfaces coated sealing coat that obtains in step (1) after heat treatment, is put into Glass Containers, under vacuum, carries out the oxyhydrogen flame sealing, and weld adds and said Glass Containers identical materials, obtains the biscuit that Glass Containers is sealed;
(3) under passive state, the biscuit that the Glass Containers that step (2) is obtained is sealed is put into crucible, and it is softening to be warming up to Glass Containers earlier, under nitrogen or argon shield, carries out HIP sintering then, promptly gets.
Preferably, by mass percentage, silicon nitride is 92% ~ 98%, and sintering aid is 2% ~ 8%.
Preferably, described sintering aid adopts MgO, Al
2O
3, Y
2O
3, La
2O
3, Yb
2O
3, CeO
2, Lu
2O
3And Eu
2O
3In one or more; Be preferably Al
2O
3, Y
2O
3
Preferably, in step (1), the pressure that said cold isostatic compaction is handled is 100 ~ 250MPa; Be preferably 150 ~ 220MPa.
Preferably, in step (2), said sealing coat is SP 1 or graphite.
Preferably, in step (2), said Glass Containers is quartz container, borosilicate glass container, vagcor container or aluminosilicate glass container; Preferably, the softening temperature of said Glass Containers is 1000 ~ 1400 ℃.
Preferably, in step (2), said heat treated temperature is 900 ~ 1300 ℃, and soaking time is 0.5 ~ 3h.
Preferably, in step (2), vacuum tightness is 10
-1~ 10
-3Pa is preferably 10
-2Pa.
Preferably, in step (3), the temperature of said HIP sintering is 1700 ~ 2000 ℃, and soaking time is 0.5 ~ 5h, and the pressure of nitrogen or argon gas is 50 ~ 250MPa.
The silicon nitride ceramics spherical diameter that above-mentioned preparation method prepares according to the present invention is 25 ~ 80mm.Concrete performance index are following: density is higher than 99.8%; Microhardness is higher than 1500 Kg/mm
2Bending strength is higher than 900 Mpa; Fracture toughness property is 6 ~ 9MPam
1/2The Wei Buer modulus is higher than 15.
Compared with prior art, the present invention has following beneficial effect at least:
(1) silicon nitride ceramic ball that adopts preparation method of the present invention to prepare have compactness height, uniform crystal particles, excellent performance, technological operation simple, can realize advantage such as industrialization;
(2) the present invention adopts Glass Containers to seal, and under vacuum, carries out oxyhydrogen flame soldering and sealing simultaneously, forms imporous complete sealing, and helps reaching complete densification, and (Ф 25 ~ 80mm) thereby help preparing large-sized silicon nitride ceramic ball;
(3) silicon nitride ceramic ball that adopts preparation method of the present invention to prepare has excellent performance, and its correlated performance detects as follows: density is>=99.8%, microhardness>=1500Kg/mm
2, bending strength>=900Mpa, fracture toughness property is 6 ~ 9 MPam
1/2, Wei Buer modulus>=15.This performance helps improving the bearing shock resistance, prolongs fatigue lifetime, guarantees the safety of silicon nitride ceramics bearing ball simultaneously.
Embodiment
The concrete embodiment of following reference explains the present invention.It will be appreciated by those skilled in the art that these embodiment only are used to explain the present invention, the scope that it does not limit the present invention in any way.
Experimental technique among the following embodiment like no specified otherwise, is ordinary method.
Embodiment 1
With the prescription of silicon nitride and sintering aid, by mass percentage, Si
3N
498wt%, Y
2O
31wt%, Al
2O
31wt% carries out uniform mixing, and after the granulation, under 150MPa, the 3min that keep-ups pressure carries out cold isostatic compaction and handles the silicon nitride ceramic ball biscuit that obtains.At this Ceramic Balls biscuit surfaces coated last layer SP 1 protective membrane,, after the thermal treatment of insulation 1h, put into quartz container then, guaranteeing that vacuum tightness is 10 through being warming up to 1000 ℃
-2Under the situation of Pa, carry out the oxyhydrogen flame vacuum seal, weld adds silica glass material.The Glass Containers of sealing is put into plumbago crucible, and the hot isostatic pressing of packing into (HIP) stove, begin to charge into nitrogen after being warming up to 1400 ℃; Be warming up to 2000 ℃ then; The 200MPa that pressurizes simultaneously behind heat-insulation pressure keeping 4h HIP sintering, promptly obtains silicon nitride ceramic ball.
After adopting the silicon nitride ceramics ball warp Performance Detection of Ф 25mm of above-mentioned prepared, its compactness reaches 99.8%, uniform crystal particles, defectives such as pore-free, crackle simultaneously.Microhardness 1650Kg/mm
2, bending strength 950Mpa, fracture toughness property 6.7MPam
1/2, Wei Buer modulus 17.
Embodiment 2
With the prescription of silicon nitride and sintering aid, by mass percentage, Si
3N
495wt%, Y
2O
33wt%, Al
2O
32wt% carries out uniform mixing, after the granulation, under 250MPa, carries out cold isostatic compaction and obtains the silicon nitride ceramic ball biscuit.At this Ceramic Balls biscuit surfaces coated last layer graphite sealing coat,, after the thermal treatment of insulation 0.5h, put into the borosilicate glass container then, guaranteeing that vacuum tightness is 10 through being warming up to 900 ℃
-1Under the situation of Pa, carry out the oxyhydrogen flame vacuum seal, weld adds the borosilicate glass material.The Glass Containers of sealing is put into plumbago crucible, and the hot isostatic pressing of packing into (HIP) stove, when being warming up to 1000 ℃, begin to charge into argon gas, be warming up to 1900 ℃ then, the 120Mpa that pressurizes simultaneously, behind heat-insulation pressure keeping 2h HIP sintering, i.e. silicon nitride ceramic ball.
After adopting the silicon nitride ceramics ball warp Performance Detection of Ф 45mm of above-mentioned prepared, its compactness reaches 99.9%, uniform crystal particles, defectives such as pore-free, crackle simultaneously.Microhardness 1500Kg/mm
2, bending strength 950Mpa, fracture toughness property 7.6MPam
1/2, Wei Buer modulus 18.
Embodiment 3
With the prescription of silicon nitride and sintering aid, by mass percentage, Si
3N
497wt%, Yb
2O
3After 3wt% carries out uniform mixing, granulation, carry out the cold isostatic compaction processing at 220Mpa and obtain the silicon nitride ceramic ball biscuit.At this Ceramic Balls biscuit surfaces coated last layer SP 1 protective membrane,, after the insulation 3h thermal treatment, put into the borosilicate glass container then, guaranteeing that vacuum tightness is 10 through being warming up to 1300 ℃
-2Under the situation of Pa, carry out the oxyhydrogen flame vacuum seal, weld adds the borosilicate glass material.The Glass Containers of sealing is put into plumbago crucible, and the hot isostatic pressing of packing into (HIP) stove, when being warming up to 900 ℃; Begin to charge into argon gas, be warming up to 2000 ℃ then, 180MPa simultaneously pressurizes; Behind heat-insulation pressure keeping 3h HIP sintering, the silicon nitride ceramic ball that promptly obtains.
After adopting the silicon nitride ceramics ball warp Performance Detection of Ф 57mm of above-mentioned prepared, its compactness reaches 99.8%, uniform crystal particles, defectives such as pore-free, crackle simultaneously.Microhardness 1700Kg/mm
2, bending strength 920MPa, fracture toughness property 6.9MPam
1/2, Wei Buer modulus 19.
Embodiment 4
With the prescription of silicon nitride and sintering aid, by mass percentage, Si
3N
492wt%, MgO 4wt%, CeO
2After 4wt% carries out uniform mixing, granulation, carry out cold isostatic compaction at 150MPa and obtain the silicon nitride ceramic ball biscuit.At this Ceramic Balls biscuit surfaces coated last layer graphite sealing coat,, after the insulation 2h thermal treatment, slowly put into the borosilicate glass container then, guaranteeing that vacuum tightness is 10 through being warming up to 1100 ℃
-3Situation under, carry out the oxyhydrogen flame vacuum seal, weld adds the borosilicate glass material.The Glass Containers of sealing is put into plumbago crucible, and the hot isostatic pressing of packing into (HIP) stove, when being warming up to 900 ℃; The Glass Containers fusion is sealed, and is warming up to 1750 ℃ then, and 150MPa simultaneously pressurizes; Behind heat-insulation pressure keeping 3h HIP sintering, promptly obtain silicon nitride ceramic ball.
After adopting the Ф 80mm silicon nitride ceramics ball warp Performance Detection of above-mentioned prepared, its compactness reaches 99.8%, uniform crystal particles, defectives such as pore-free, crackle simultaneously.Microhardness 1530Kg/mm
2, bending strength 910Mpa, fracture toughness property 9.0MPam
1/2, Wei Buer modulus 17.
Embodiment 5
The silicon nitride formulation material is pressed Si
3N
496wt%, MgO 2wt%, Eu
2O
31wt%, Lu
2O
31wt% carries out uniform mixing, after the granulation, carries out the cold isostatic compaction processing at 200Mpa and obtains the silicon nitride ceramic ball biscuit.At this Ceramic Balls biscuit surfaces coated last layer graphite sealing coat,, after the insulation 1h thermal treatment, put into the vagcor container then, guaranteeing that vacuum tightness is 10 through being warming up to 1150 ℃
-1Under the situation of Pa, carry out the oxyhydrogen flame vacuum seal, weld adds the vagcor material.The Glass Containers of sealing is put into plumbago crucible, and the hot isostatic pressing of packing into (HIP) stove, when being warming up to 1100 ℃; Begin to charge into nitrogen, be warming up to 1800 ℃ then, 200Mpa simultaneously pressurizes; Behind heat-insulation pressure keeping 0.5h HIP sintering, promptly obtain silicon nitride ceramic ball.
After adopting the Ф 52mm silicon nitride ceramics ball warp Performance Detection of above-mentioned prepared, its compactness reaches 99.9%, uniform crystal particles, defectives such as pore-free, crackle simultaneously.Microhardness 1600Kg/mm
2, bending strength 930MPa, fracture toughness property 8.4MPam
1/2, Wei Buer modulus 21.
More than the description of the specific embodiment of the invention is not limited the present invention, those skilled in the art can make various changes or distortion based on the present invention, only otherwise break away from spirit of the present invention, all should belong to the scope of accompanying claims of the present invention.
Claims (9)
1. the preparation method of a silicon nitride ceramic ball, this preparation method comprises the steps:
(1) silicon nitride and sintering aid mixing, granulation, cold isostatic compaction are handled, obtained the silicon nitride ceramic ball biscuit;
(2) the biscuit surfaces coated sealing coat that obtains in step (1) is put into Glass Containers after the drying, after heat treatment, under vacuum, carry out the oxyhydrogen flame sealing, and weld adds and said Glass Containers identical materials, obtains the biscuit that Glass Containers is sealed;
(3) under passive state, the biscuit that the Glass Containers that step (2) is obtained is sealed is put into crucible, and it is softening to be warming up to Glass Containers earlier, under nitrogen or argon shield, carries out HIP sintering then, promptly gets.
2. preparation method according to claim 1 is characterized in that, by mass percentage, silicon nitride is 92% ~ 98%, and sintering aid is 2% ~ 8%.
3. preparation method according to claim 1 and 2 is characterized in that, described sintering aid adopts MgO, Al
2O
3, Y
2O
3, La
2O
3, Yb
2O
3, CeO
2, Lu
2O
3And Eu
2O
3In one or more; Be preferably Al
2O
3, Y
2O
3
4. according to each described preparation method in the claim 1 to 3, it is characterized in that in step (1), the pressure that said cold isostatic compaction is handled is 100 ~ 250MPa; Be preferably 150 ~ 220MPa.
5. according to each described preparation method in the claim 1 to 4, it is characterized in that in step (2), said sealing coat is SP 1 or graphite.
6. according to each described preparation method in the claim 1 to 5, it is characterized in that in step (2), said Glass Containers is quartz container, borosilicate glass container, vagcor container or aluminosilicate glass container; Preferably, the softening temperature of said Glass Containers is 1000 ~ 1400 ℃.
7. according to each described preparation method in the claim 1 to 6, it is characterized in that in step (2), said heat treated temperature is 900 ~ 1300 ℃, soaking time is 0.5 ~ 3h.
8. according to each described preparation method in the claim 1 to 7, it is characterized in that in step (2), said vacuum tightness is 10-1 ~ 10-3Pa, is preferably 10-1Pa.
9. according to each described preparation method in the claim 1 to 8, it is characterized in that in step (3), the temperature of said HIP sintering is 1700 ~ 2000 ℃, soaking time is 0.5 ~ 5h, and the pressure of nitrogen or argon gas is 50 ~ 250MPa.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524133A (en) * | 2013-10-30 | 2014-01-22 | 郑州骏科纳鑫特种陶瓷制品有限公司 | Preparation technology of silicon nitride ceramic balls |
| CN105819864A (en) * | 2016-03-08 | 2016-08-03 | 江苏金盛陶瓷科技有限公司 | Long-life silicon nitride material for bearing balls, and preparation method thereof |
| CN107498688A (en) * | 2017-06-19 | 2017-12-22 | 宁波百诺肯轴承有限公司 | A kind of automobile bearing manufacture device |
| CN111393170A (en) * | 2020-03-19 | 2020-07-10 | 西安澳秦新材料有限公司 | Method for preparing high-density silicon nitride ceramic through multi-factor optimization and prepared silicon nitride ceramic |
| CN112811912A (en) * | 2021-01-20 | 2021-05-18 | 中国科学院上海硅酸盐研究所 | Batch sintering method of high-performance silicon nitride ceramic substrate |
| CN113651642A (en) * | 2018-09-13 | 2021-11-16 | 中国兵器工业第五九研究所 | Preparation method of compact component |
| CN114195521A (en) * | 2021-12-27 | 2022-03-18 | 中国科学院上海硅酸盐研究所 | Method for treating silicon nitride ceramic by hot isostatic pressing |
| CN115551818A (en) * | 2020-05-07 | 2022-12-30 | Ａｇｃ株式会社 | Method for producing ceramic sintered body and ceramic sintered body |
| CN115849919A (en) * | 2022-12-12 | 2023-03-28 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524133A (en) * | 2013-10-30 | 2014-01-22 | 郑州骏科纳鑫特种陶瓷制品有限公司 | Preparation technology of silicon nitride ceramic balls |
| CN105819864A (en) * | 2016-03-08 | 2016-08-03 | 江苏金盛陶瓷科技有限公司 | Long-life silicon nitride material for bearing balls, and preparation method thereof |
| CN107498688A (en) * | 2017-06-19 | 2017-12-22 | 宁波百诺肯轴承有限公司 | A kind of automobile bearing manufacture device |
| CN113651642A (en) * | 2018-09-13 | 2021-11-16 | 中国兵器工业第五九研究所 | Preparation method of compact component |
| CN111393170A (en) * | 2020-03-19 | 2020-07-10 | 西安澳秦新材料有限公司 | Method for preparing high-density silicon nitride ceramic through multi-factor optimization and prepared silicon nitride ceramic |
| CN115551818A (en) * | 2020-05-07 | 2022-12-30 | Ａｇｃ株式会社 | Method for producing ceramic sintered body and ceramic sintered body |
| CN112811912A (en) * | 2021-01-20 | 2021-05-18 | 中国科学院上海硅酸盐研究所 | Batch sintering method of high-performance silicon nitride ceramic substrate |
| CN112811912B (en) * | 2021-01-20 | 2021-11-02 | 中国科学院上海硅酸盐研究所 | Batch sintering method of high-performance silicon nitride ceramic substrate |
| CN114195521A (en) * | 2021-12-27 | 2022-03-18 | 中国科学院上海硅酸盐研究所 | Method for treating silicon nitride ceramic by hot isostatic pressing |
| CN114195521B (en) * | 2021-12-27 | 2022-12-13 | 中国科学院上海硅酸盐研究所 | Method for treating silicon nitride ceramic by hot isostatic pressing |
| CN115849919A (en) * | 2022-12-12 | 2023-03-28 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
| CN115849919B (en) * | 2022-12-12 | 2024-04-05 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
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Application publication date: 20121128 |