CN1868966A - Technology of reaction sintering silicon nitride powder - Google Patents
Technology of reaction sintering silicon nitride powder Download PDFInfo
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- CN1868966A CN1868966A CN 200510070891 CN200510070891A CN1868966A CN 1868966 A CN1868966 A CN 1868966A CN 200510070891 CN200510070891 CN 200510070891 CN 200510070891 A CN200510070891 A CN 200510070891A CN 1868966 A CN1868966 A CN 1868966A
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Abstract
A process for preparing silicon nitride powder by reactive sinter method is disclosed.
Description
Technical field: new material technology field is a Technology of utilizing reaction sintering to produce silicon nitride powder.
Technical background:
The high quality alpha-silicon nitride powders that is used for the production structure pottery mainly contains reaction sintering, SiCl in the world at present
4Ammonolysis process, SiO
2Carbothermic method, from the synthetic Si of climing combustion
3N
4These several production methods of method.The powder characteristic of reaction sintering is good, and price is also more cheap, and particularly the colloidal formation ratio is easier to, so be present most widely used method.At present at home, the unique requirement that reaches practicability of the product of this method, but with more advanced is in the world compared on performance index mutually far short of what is expected as German Starck company, Japanese Danka company.
Present domestic sintering process adopts static sintering mostly, promptly feeds a certain proportion of mixed gas and control certain pressure in sintering process in stove.The drawback of this method is that the waste gas that produces in the reaction can not emptying, and the spending rate of all gases is all different again, so be the uncontrollable sintering process of a kind of atmosphere.The technology that a cover reaction sintering is made the high purity silicon nitride powder is found out in the unremitting effort in nearly ten years of high-performance ceramics company limited of Beijing Qing Hua Ziguang.
Present technique has effectively solved low, the mass defects such as oxygen level is high, contents of free si height of the ubiquitous α phase content of homemade silicon nitride powder.
Technical scheme:
1. raw material.Select the original content of high-purity raw silicon control impurity, find out suitable sintering process material fineness, especially iron level.
2. shove charge.Control the packing density parameter, the raw material silica flour is made the prefabricated component of definite shape.Simultaneously be used as gas channel, when former stock column is packed into alms bowl, note avoiding these holes at the saggar bear.
3. sintering process.Be applicable to 1000 * 700 type reaction sintering stoves of high-performance ceramics company limited of Beijing Qing Hua Ziguang.(sintering curre is seen accompanying drawing)
(1) .0-800 ℃ per hour heats up 40 ℃.
(2) 800-1150 ℃ per hour heats up 20 ℃, and insulation is 40 hours in the time of 1150 ℃.
(3) 1150-1220 ℃ per hour heats up 20 ℃, and insulation is 20 hours in the time of 1220 ℃.
(4) 1220-1300 ℃ per hour heats up 20 ℃, and insulation is 25 hours in the time of 1300 ℃.
(5) 1300-1360 ℃ per hour heats up 20 ℃, and insulation is 20 hours in the time of 1300 ℃.
4. gas control.The reaction sintering silicon nitride powder process feeds N
2, H
2, three kinds of gas H of Ar
2Be used for guaranteeing the reducing atmosphere in the Reaktionsofen, Ar is used for controls reaction speed.Different with the way of static sintering control furnace pressure, present technique is not controlled furnace pressure but the speed of response of control silicon powder nitride.Because the speed of response difference, the speed difference of gas consumption, the rate of change difference of furnace pressure is so judge speed of response from the furnace pressure velocity of variation.Gas control divides three kinds of states to ventilate, stop the supple of gas or steam, take a breath in the technology.
Concrete processing parameter is:
Vacuumize below 800 ℃-1MPa.
(1) charge into nitrogen and hydrogen .400-700 ℃ the time and applying argon gas not, inflation in average per 2 hours once.
(2) ventilation 1-2 time in vacuum 700-800 ℃ the time.
(3) 800-1150 ℃ of ventilation all the time in temperature-rise period, ratio is N
2(0.6): H
2(0.03), Ar (0.11).1150 ℃ begin insulation, and ventilation earlier is after 2 hours, and each ventilation in per 1 hour, ventilation are once.After 24 hours, each ventilation in per 2 hours, ventilation are once.
(4) 1150-1220 ℃ according to the speed of response air feed, and the Reaktionsofen internal pressure is controlled at about 1Mpa.Do not take a breath in this process.
(5) ventilate in temperature-rise period for 1220-1360 ℃, ventilation in per 3.5 hours once in 1300 ℃ and the 1360 ℃ of insulating processes.
Gordian technique wherein:
(1) select high-purity raw silicon to control the original content of impurity.
(2) the raw material silica flour is made the prefabricated component of definite shape.Simultaneously be used as gas channel, when former stock column is packed into alms bowl, note avoiding these holes at the saggar bear.
(3) the reaction sintering silicon nitride powder process feeds N
2, H
2, three kinds of gas H of Ar
2Be used for guaranteeing the reducing atmosphere in the Reaktionsofen, Ar is used for controls reaction speed.Gas control divides three kinds of states to ventilate, stop the supple of gas or steam, take a breath in technology.
(4) per hour heat up 20-40 ℃.
Beneficial effect:
It is low that present technique has effectively solved homemade silicon nitride powder α phase content of past, the defective that contents of free si is high.
The approaching German best in the world M11 powder at present of the silicon nitride powder performance index that Qing Hua Ziguang side, Beijing major company adopts present technique to produce has surpassed Japanese Denka powder, and product has exported the U.S..
Sino-German day three kinds of high quality beta-silicon nitride powder quality synopsis
| Country origin | The powder trade mark | α phase % | N％ | O％ | Fe％ | AL％ | Ca％ | D 50 | σRT(Mpa) |
| Germany | M11 | 95 | 38.5 | 1.51 | 0.003 | 0.05 | 0.004 | 0.6 | 1000-1100 |
| China | UC-P1 | 95 | 37.8 | 1.5 | 0.1 | 0.1 | 0.05 | 0.35 | 1000-1100 |
| Japan | Denka | ＞95 | 38 | 2.0 | 0.01 | 0.05 | 0.005 | 0.43 | 1200-1300 |
Claims (1)
1. the reaction sintering silicon nitride powder process feeds N
2, H
2, three kinds of gas H of Ar
2Be used for guaranteeing the reducing atmosphere in the Reaktionsofen, Ar is used for controls reaction speed.Gas control divides three kinds of states to ventilate, stop the supple of gas or steam, take a breath in technology.Concrete grammar is:
Vacuumize below 800 ℃-1MPa.
(1) charges into nitrogen and hydrogen .400-700 ℃ the time and applying argon gas not, filled once in average per 2 hours.
(2) ventilation 1-2 time in vacuum 700-800 ℃ the time.
(3) 800-1150 ℃ of ventilation all the time in temperature-rise period, ratio is N
2(0.6): H
2(0.03), Ar (0.11).1150 ℃ begin insulation, and ventilation earlier is after 2 hours, and each ventilation in per 1 hour, ventilation are once.After 24 hours, each ventilation in per 2 hours, ventilation are once.
(4) 1150-1220 ℃ according to the speed of response air feed, and the Reaktionsofen internal pressure is controlled at about 1Mpa.Do not take a breath in this process.
(5) ventilate in temperature-rise period for 1220-1360 ℃, ventilation in per 3.5 hours once in 1300 ℃ and the 1360 ℃ of insulating processes.
(6) per hour heat up 20-40 ℃, about soaking time 20-40 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510070891 CN1868966A (en) | 2005-05-23 | 2005-05-23 | Technology of reaction sintering silicon nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510070891 CN1868966A (en) | 2005-05-23 | 2005-05-23 | Technology of reaction sintering silicon nitride powder |
Publications (1)
| Publication Number | Publication Date |
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| CN1868966A true CN1868966A (en) | 2006-11-29 |
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| CN 200510070891 Pending CN1868966A (en) | 2005-05-23 | 2005-05-23 | Technology of reaction sintering silicon nitride powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468392B (en) * | 2007-12-30 | 2011-05-25 | 陈奎生 | Novel method for producing silicon nitride series alloy |
| CN106395769A (en) * | 2016-08-26 | 2017-02-15 | 河北高富氮化硅材料有限公司 | Method for preparing high purity high alpha phase silicon nitride powder |
| CN112250046A (en) * | 2020-12-11 | 2021-01-22 | 安阳亨利高科实业有限公司 | Production process of high alpha-phase silicon nitride powder |
| CN112408992A (en) * | 2020-12-11 | 2021-02-26 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
-
2005
- 2005-05-23 CN CN 200510070891 patent/CN1868966A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468392B (en) * | 2007-12-30 | 2011-05-25 | 陈奎生 | Novel method for producing silicon nitride series alloy |
| CN106395769A (en) * | 2016-08-26 | 2017-02-15 | 河北高富氮化硅材料有限公司 | Method for preparing high purity high alpha phase silicon nitride powder |
| CN112250046A (en) * | 2020-12-11 | 2021-01-22 | 安阳亨利高科实业有限公司 | Production process of high alpha-phase silicon nitride powder |
| CN112408992A (en) * | 2020-12-11 | 2021-02-26 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
| CN112408992B (en) * | 2020-12-11 | 2022-08-02 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
| CN112250046B (en) * | 2020-12-11 | 2022-11-18 | 安阳亨利高科实业有限公司 | Production process of high alpha-phase silicon nitride powder |
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