CN1055279C - Method for preparing ceramic powder - Google Patents
Method for preparing ceramic powder Download PDFInfo
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- CN1055279C CN1055279C CN97111777A CN97111777A CN1055279C CN 1055279 C CN1055279 C CN 1055279C CN 97111777 A CN97111777 A CN 97111777A CN 97111777 A CN97111777 A CN 97111777A CN 1055279 C CN1055279 C CN 1055279C
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Abstract
The present invention discloses a method for preparing sialon ceramic powder, which belongs to the technical field of preparing ceramic powder. The method comprises the following steps that firstly, the raw materials are prepared according to the content requirement of designers; secondly, 10 to 30% of sialon powder is added into the reacting raw materials to be used as diluting agent, and then, the uniformly blended mixture is loaded into a high pressure reactor in which 60 to 100 atm of N2 gas is filled; thirdly, the reacting raw materials are ignited by a metal wire for reacting, the volatile matters on the surface of the products are cleaned after the reaction, the products are crushed for wet grinding, and the condition for wet grinding is that the ratio of balls to alcohol to raw materials is 3 to 1 to 1. Compared with the prior art, the method of the present invention has the advantages of simple technology and high production rate.
Description
The invention belongs to the preparation field of ceramic powder.Be specially adapted to the preparation method of a kind of SiAlON ceramic powder (Sialon).
SiAlON ceramic (Sialon) is a kind of in the silicon nitride ceramics, many structural compounds group's that it is made up of Si, Al, four kinds of elements of O, N general name, and SiAlON ceramic has the hot strength height, red hardness is good, corrosion-resistant, wear-resistant, anti-oxidant and advantages such as fracture toughness property height and good thermal shock.The existing production method of this pottery is normally with Si
3N
4, Al
2O
3, ALN, SiO
2After sintering aid mixing and coldmoulding, make with normal pressure-sintered or pressing methods again.The main drawback of this sintering method is that pottery can only react in sintering process and forms, and can not manufacture powder, this has been subjected to very big restriction in the application of pottery, therefore the prepared stupalith of this production method can not satisfy the service requirements of thermospray materials, function-graded material, powder metallurgy aspect usefulness powder.The production method that adopts kaolin synthesizing sialon ceramic powder is arranged in addition, and this method is that the selection composition is 44.6%SiO
2, 39.6%Al
2O
3And small amount of Fe
2O
3The kaolin of impurity and five times of SiO
2After the graphite of molar content mixes, at 1350 ℃ and 80%N
2+ 20%H
2Nitrogenize is 5 hours in the atmosphere, and then is heated to 700 ℃ of insulations 5 hours in air, carries out de-carbon, handles just to make after 90 minutes to match with 28% hydrochloric acid again after product is come out of the stove and swells powder.The deficiency of this method is a complex process, the production cost height, and also residual phase is many in the composition, and composition is restive etc.
The objective of the invention is to propose that a kind of production technique is simple, economy and productivity height, the SiAlON ceramic powder, preparation method thereof of composition precise control.
According to purpose of the present invention, the ultimate principle of the production SiAlON ceramic powder method that we proposed is to be put in N after the preparation of raw material
2In, light partly reactant reaction then, because the heat release of the thing that responds impels other reactant to participate in reaction again, because reactant is at high pressure N
2In mutually provocative reaction, make this reaction guarantee to be maintained to total overall reaction and finish, and in reaction process formation SiAlON ceramic body, can process again according to different service requirementss then.
According to purpose of the present invention and principle, the method that we propose to produce the SiAlON ceramic powder is that the composition scope is (weight %) Si35-74%, Al 0-23%, Al
2O
30-28%, SiO
20-24%, AlN 0-12% are mixed with raw material, and the SiAlON ceramic powder that it is characterized in that sneaking into (weight %) 10-30% in reaction raw materials is as thinner, will add the reaction material mixing of SiAlON ceramic powder thinner then and be contained in to charge into N in the high-pressure reactor
2Gas is lighted reaction material by the wire conduction heating, and question response end back cleaning reaction-ure surface volatile matter fragmentation again carries out wet-milling.Wet grinding media is an alcohol, and the ball milling ratio is ball, alcohol, and the ratio of ceramic material 3: 1: 1 gets final product the sialon ceramic powder oven dry behind the ball milling again.
The form that adopts the inventive method to produce the technical process of SiAlON ceramic is: batching-→ the reaction material combustion reactions-→ cleaning of reaction material surface volatile matter-→ wet ball mill-→ finished product.The inventive method is Si for general formula
6-
ZAl
ZO
ZN
8-Z, the β of (Z=0～4.2)---Sai Long (Sialon) can be with the forming process of following three equation expression responses:
Adopt the inventive method compared with prior art, it is simple to have production technique, the productivity height, and the characteristics such as composition precise control of the grand porcelain powder of match, more prior in addition is to have remarkable energy saving effect.
Embodiment
The requirement of method constructed in accordance, we have prepared (Sialon) SiAlON ceramic powder body material of 6 kinds of different components content altogether, and its concrete component content sees Table 1.Raw material powder is mixed in the high-pressure reactor of packing into after 2 hours, and light raw material powder, charge into N before the reaction by the energising tungsten filament
2N when pressure and reaction
2Pressure peak sees Table 2, and given in table 2 is each processing parameter of the embodiment of the invention and powder characteristic.Question response can be cleared up the product surface volatile matter after finishing, and adopts jaw crusher to carry out fragmentation then, and the wet wheeling machine of again particle being packed into carries out ball milling, and the ratio of ball, alcohol, material is 3: 1: 1, and the ball milling time is 8 hours, and its product powder the results are shown in Table 2.
Table 1 embodiment of the invention material composition contrast (weight percent)
| The composition sequence number | Si | Al | Al 2O 3 | SiO2 | ALN | Sialon | Theoretical Z value |
| 1 | 63 | 6 | / | 6 | / | 25 | 0.5 |
| 2 | 74 | / | 8 | / | 3 | 15 | 0.5 |
| 3 | 50 | 14 | / | 15 | / | 21 | 1.2 |
| 4 | 65 | 5 | 20 | / | / | 10 | 1.2 |
| 5 | 46 | / | 28 | / | 12 | 14 | 2.0 |
| 6 | 35 | 23 | / | 24 | / | 17 | 2.0 |
Processing parameter and powder characteristic in table 2 embodiment of the invention
| Sequence number | N 2Beginning presses | N 2Peak pressure | Actual measurement Z value | Purity | Particle diameter d50 | Free Si | Other phase |
| 1 | 90atm | 146atm | 0.48 | 99.0 | 2.6μm | 0.2 | Trace |
| 2 | 95atm | 154atm | 0.51 | 98.8 | 2.4μm | 0.3 | Trace |
| 3 | 85atm | 145atm | 1.10 | 98.9 | 2.0μm | 0.15 | Trace |
| 4 | 100atm | 150atm | 1.20 | 99.1 | 2.2μm | 0.2 | Trace |
| 5 | 100atm | 155atm | 1.92 | 92.4 | 1.8μm | 0.3 | Trace |
| 6 | 90atm | 160atm | 2.06 | 99.2 | 1.6μm | 0.2 | Trace |
| The kaolin method | The Z value is uncontrollable, and SiC, SiO in the powder 2、Al 2O 3Surplus deposit mutually more | ||||||
Claims (2)
1, a kind of preparation method of ceramics powder, this method are (weight %) Si 35-74%, Al 0-23%, Al with the composition scope
2O
30-28%, SiO
20-24%, AlN 0-12% are mixed with raw material, and the SiAlON ceramic powder that it is characterized in that sneaking into (weight %) 10～30% in reaction raw materials charges into N as thinner in the high-pressure reactor of again reaction material of mixing being packed into
2Gas, and light reaction material by metal tungsten wire energising, reaction finishes back cleaning reaction-ure surface volatile matter and carries out fragmentation and wet-milling again, and the wet-milling condition is that the ratio of ball, alcohol, material is 3: 1: 1.
2, according to the described method of claim 1, it is characterized in that charging into N in the reactor
2Pressure should be 60-100atm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97111777A CN1055279C (en) | 1997-05-13 | 1997-05-13 | Method for preparing ceramic powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97111777A CN1055279C (en) | 1997-05-13 | 1997-05-13 | Method for preparing ceramic powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1168872A CN1168872A (en) | 1997-12-31 |
| CN1055279C true CN1055279C (en) | 2000-08-09 |
Family
ID=5171868
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97111777A Expired - Fee Related CN1055279C (en) | 1997-05-13 | 1997-05-13 | Method for preparing ceramic powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1055279C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305808C (en) * | 2003-02-14 | 2007-03-21 | 中国科学院上海硅酸盐研究所 | Process for preparation of self-spread high-temperature synthesizing low-cost diphase alpha/beta-sialon powder |
| CN100391899C (en) * | 2003-02-14 | 2008-06-04 | 中国科学院上海硅酸盐研究所 | Process for preparation of self-spread high-temperature synthesizing low cost alpha-sialon powder |
| CN106892666A (en) * | 2017-03-17 | 2017-06-27 | 太原理工大学 | A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092053A (en) * | 1993-03-13 | 1994-09-14 | 山东工业陶瓷研究设计院 | Sialon combined silicon carbide refractory ceramic material |
| CN1142478A (en) * | 1995-08-04 | 1997-02-12 | 中国科学院上海硅酸盐研究所 | Composite ceramics and production thereof |
-
1997
- 1997-05-13 CN CN97111777A patent/CN1055279C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092053A (en) * | 1993-03-13 | 1994-09-14 | 山东工业陶瓷研究设计院 | Sialon combined silicon carbide refractory ceramic material |
| CN1142478A (en) * | 1995-08-04 | 1997-02-12 | 中国科学院上海硅酸盐研究所 | Composite ceramics and production thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1168872A (en) | 1997-12-31 |
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Inventor after: Han Huanqing Inventor after: Ge Qilu Inventor after: Chu Zhengjun Inventor after: Chen Yuping Inventor before: Han Huanqing Inventor before: Ge Qilu Inventor before: Chu Zhengjun |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: HAN HUANQING; GE QILU ZHU ZHENGJUN TO: HAN HUANQING; GE QILU; ZHU ZHENGJUN; CHEN YUPING |
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Owner name: ANTAI SCIENCE AND TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: GENERAL RESEARCH INST. OF IRON AND STEEL, MINISTRY OF METALLURGICAL INDUSTRY Effective date: 20071012 |
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Effective date of registration: 20071012 Address after: 100081 No. 76 South College Road, Beijing Patentee after: Antai Science and Technology Co., Ltd. Address before: 100081 No. 76 South College Road, Beijing Patentee before: Iron and Steel Central Research Institute of Ministry of Metallurgical Industry |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Beijing Gang Yan Diamond Products Company Assignor: Antai Science and Technology Co., Ltd. Contract fulfillment period: 2007.12.15 to 2013.12.15 contract change Contract record no.: 2008990001252 Denomination of invention: Method for preparing ceramic powder Granted publication date: 20000707 License type: Exclusive license Record date: 20081121 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.12.15 TO 2013.12.15; CHANGE OF CONTRACT Name of requester: BEIJING AETNA GANGYAN ULTRAHARD MATERIALS PRODUCTS Effective date: 20081121 |
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