CN105253864A - Silicon nitride powder preparation method - Google Patents
Silicon nitride powder preparation method Download PDFInfo
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- CN105253864A CN105253864A CN201510780188.0A CN201510780188A CN105253864A CN 105253864 A CN105253864 A CN 105253864A CN 201510780188 A CN201510780188 A CN 201510780188A CN 105253864 A CN105253864 A CN 105253864A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 32
- 239000000843 powder Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims abstract description 19
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 239000012265 solid product Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 20
- 238000013019 agitation Methods 0.000 claims description 16
- 238000009833 condensation Methods 0.000 claims description 16
- 230000005494 condensation Effects 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- 238000003795 desorption Methods 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 5
- -1 chloro silicoethane Chemical compound 0.000 claims description 5
- 238000012423 maintenance Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- 239000000047 product Substances 0.000 abstract description 5
- 238000007710 freezing Methods 0.000 abstract description 3
- 230000008014 freezing Effects 0.000 abstract description 3
- 239000007806 chemical reaction intermediate Substances 0.000 abstract description 2
- 230000002829 reductive effect Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- FXMNVBZEWMANSQ-UHFFFAOYSA-N chloro(silyl)silane Chemical compound [SiH3][SiH2]Cl FXMNVBZEWMANSQ-UHFFFAOYSA-N 0.000 abstract 1
- 230000005611 electricity Effects 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PMXLLFCEIKHJCZ-UHFFFAOYSA-N iminosilicon Chemical compound [Si]=N PMXLLFCEIKHJCZ-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- DSWDPPJBJCXDCZ-UHFFFAOYSA-N ctk0h9754 Chemical class N[SiH2][SiH3] DSWDPPJBJCXDCZ-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention provides a silicon nitride powder preparation method which includes the following steps that firstly, 1000 parts of liquid ammonia is added into a high-pressure reactor, and the temperature is raised; secondly, 50-200 parts of chloro-disilane is added into the high-pressure reactor under the stirring condition; thirdly, a closed filter is used for filtering reaction products; fourthly, solid products are washed through liquid ammonia to obtain (NH2)6Si2 solid; fifthly, the (NH2)6Si2 solid is desorbed in a vacuum closed furnace; sixthly, the desorbed (NH2)6Si2 solid is placed in a tubular furnace for high-temperature thermal decomposition, and silicon nitride powder is obtained after cooling along with the furnace. The silicon nitride powder preparation method has the following advantages that electricity consumption for freezing required by low-temperature reactions is greatly reduced; the reaction speed and washing efficiency are high; the reaction intermediate product (NH2)6Si2 solid is low in calcination temperature.
Description
Technical field
The invention belongs to Materials Science and Engineering technical field, relate to a kind of preparation method of inorganic powder, be specifically related to a kind of preparation method of beta-silicon nitride powder.
Background technology
Silicon nitride is atomic crystal, is a kind of important structural ceramic material.Silicon nitride has that hardness is high, oilness good, anti-oxidant good, cold-and-heat resistent impacts the excellent physical and chemical performance such as strong (be heated to more than 1000 DEG C in atmosphere, quick refrigeration sharply heats again, also can not be cracked).The intensity of silicon nitride is very high, is one of the hardest in the world material.It is extremely high temperature resistant, intensity can be maintained to the high temperature of 1200 DEG C always and not decline, melt body can not be melt into after being heated, until 1900 DEG C just can be decomposed, and have extremely strong resistance to chemical corrosion, the mineral acid that ability is nearly all and less than 30% caustic soda soln, also ability a lot of organic acid corrosion; Again a kind of high-performance electric insulating material simultaneously.
Have so excellent characteristic based on silicon nitride, people are usually that raw material manufactures the components such as high temperature resistant bearing, blade of gas turbine, rocket motor injector with silicon nitride.Traditional method preparing silicon nitride has following several: method 1---1300 ~ 1400 DEG C time, granulated metal silicon and nitrogen are reacted; Method 2---by Pure Silicon Metal and ammonia effect about 1500 DEG C time; Method 3---the mixture of ignited silicon dioxide and carbon in the nitrogen containing a small amount of hydrogen; Method 4---by SiCl
4react with liquefied ammonia, reaction product Si (NH
2)
4thermolysis obtains silicon nitride.Method 1 and method 4 have all achieved industrialized production.But method 1 has the following disadvantages: 1, the speed of reaction of Pure Silicon Metal and nitrogen is extremely slow; 2, reaction product particle is thick, and must use ball milling to obtain fine granular powder material, ball milling causes product contaminated, and the finished product pattern is inconsistent, and size-grade distribution is wide.Having the decomposition temperature of ammonia under catalyst action to be approximately 800 DEG C, in catalyst-free situation, ammonia can decompose completely at 1200 DEG C, and therefore, method A2 is identical with method 1 in essence, i.e. the reaction of nitrogen and Pure Silicon Metal, because this method 2 exists the identical shortcoming of method 1.The principle of method 3 is synchronously carried out at the reduction reaction of silicon-dioxide and nitrogenizing reaction, owing to using carbon as reductive agent, must have the residual of carbon and have a strong impact on quality product in product.The weak point of method 4 is: the process relative complex when adopting organic solvent, and when not adopting organic solvent, temperature of reaction controls lower, needs to consume a large amount of freezing energy consumptions; In addition, the intermediates that silicon tetrachloride and liquefied ammonia are obtained by reacting are imino-silicon, and the roasting of imino-silicon is that the temperature of silicon nitride is relatively high.
Summary of the invention
Goal of the invention: the present invention is directed to above-mentioned prior art Problems existing and make improvement, namely the invention discloses a kind of preparation method of beta-silicon nitride powder.
Technical scheme: a kind of preparation method of beta-silicon nitride powder, comprises the following steps:
(1), in high-pressure reactor, add 1000 parts of liquefied ammonia, then be warming up to 50 ~ 90 DEG C, wherein: high-pressure reactor is provided with high shear agitation device and condensation reflux unit;
(2), open high shear agitation device and condensation reflux unit, then in high-pressure reactor, add 50 ~ 200 parts of chloro silicoethanes by feed-pipe;
(3), fed in raw material after, stir after 1 ~ 50h at 50 ~ 90 DEG C and obtain reaction product;
(4), the reaction product that uses closed filtering device filtration step (3) to obtain under normal temperature and ammonia saturation steam pressure pressure, obtain solid product;
(5), at room temperature ~ 90 DEG C, solid product liquefied ammonia washing step (4) obtained obtains (NH
2)
6si
2solid, in washings, ammonium chloride mass content is less than till 0.1%;
(6), by (NH that step (5) obtains
2)
6si
2solid desorption 2 ~ 10 hours at 60 ~ 180 DEG C in vacuum seal stove,
(7), by (the NH through desorption in step (6)
2)
6si
2solid is placed in tube furnace, and at nitrogen atmosphere, 800 ~ 1000 DEG C of high temperature thermal decomposition 1 ~ 20 hour, namely obtain beta-silicon nitride powder after furnace cooling.
A kind of preferred version as a kind of in the present invention preparation method of beta-silicon nitride powder: the chloro silicoethane described in step (2) be disilicone hexachloride, pentachloro-silicoethane, one or more in four silicon hexachlorides.
A kind of preferred version as a kind of in the present invention preparation method of beta-silicon nitride powder: in step (3), to feed in raw material rear maintenance high shear agitation device and condensation reflux unit work, and then obtained reaction product after stirring reaction 50h at 50 ~ 90 DEG C.
Keep high shear agitation device and condensation reflux unit work in the process of stirring reaction always.
A kind of preferred version as a kind of in the present invention preparation method of beta-silicon nitride powder: step (2) is at the uniform velocity reinforced, completes reinforced in 30 ~ 180 minutes.
Beneficial effect: the preparation method that the invention discloses a kind of beta-silicon nitride powder has following beneficial effect:
1, above-mentioned technique can carry out aminating reaction and washing at a higher temperature, greatly reduces the necessary freezing power consumption of low-temp reaction, uses common cooling circulating water can reach cooling object;
2, simultaneously due to the rising of temperature of reaction and wash temperature, speed of reaction and detersive efficiency are all improved, and production efficiency improves;
3, reaction intermediate is (NH
2)
6si
2but not existing take silicon tetrachloride as the imino-silicon (Si (NH) of the technique of raw material
2), intermediates maturing temperature reduces.
Embodiment:
Below the specific embodiment of the present invention is described in detail.
Part herein all refers to mass parts.
Specific embodiment 1
A preparation method for beta-silicon nitride powder, comprises the following steps:
(1), in high-pressure reactor, add 1000 parts of liquefied ammonia, then be warming up to 50 DEG C, wherein: high-pressure reactor is provided with high shear agitation device and condensation reflux unit;
(2), open high shear agitation device and condensation reflux unit, then in high-pressure reactor, add 50 parts of chloro silicoethanes by feed-pipe;
(3), fed in raw material after, at 50 DEG C, obtain reaction product after stirring reaction 50h;
(4), the reaction product that uses closed filtering device filtration step (3) to obtain under normal temperature and ammonia saturation steam pressure pressure, obtain solid product;
(5) the solid product liquefied ammonia washing, at room temperature, step (4) obtained obtains (NH
2)
6si
2(six aminodisilanes) solid, in washings, ammonium chloride mass content is less than till 0.1%;
(6), by (NH that step (5) obtains
2)
6si
2solid desorption 10 hours at 60 DEG C in vacuum seal stove,
(7), by (the NH through desorption in step (6)
2)
6si
2solid is placed in tube furnace, and at nitrogen atmosphere, 800 DEG C of high temperature thermal decomposition 20 hours, namely obtain beta-silicon nitride powder after furnace cooling.
Further, the chloro silicoethane of step (2) is disilicone hexachloride.
Preferred as one, in step (3), fed in raw material rear maintenance high shear agitation device and condensation reflux unit work, then obtain reaction product after stirring reaction 50h at 50 DEG C.
Further, step (2) is at the uniform velocity reinforced, within 30 minutes, completes reinforced.
Specific embodiment 2
A preparation method for beta-silicon nitride powder, comprises the following steps:
(1), in high-pressure reactor, add 1000 parts of liquefied ammonia, then be warming up to 90 DEG C, wherein: high-pressure reactor is provided with high shear agitation device and condensation reflux unit;
(2), open high shear agitation device and condensation reflux unit, then in high-pressure reactor, add 200 parts of chloro silicoethanes by feed-pipe;
(3), fed in raw material after, at 90 DEG C, obtain reaction product after stirring reaction 1h;
(4), the reaction product that uses closed filtering device filtration step (3) to obtain under normal temperature and ammonia saturation steam pressure pressure, obtain solid product;
(5), at 90 DEG C, solid product liquefied ammonia washing step (4) obtained obtains (NH
2)
6si
2solid, in washings, ammonium chloride mass content is less than till 0.1%;
(6), by (NH that step (5) obtains
2)
6si
2solid desorption 2 hours at 180 DEG C in vacuum seal stove,
(7), by (the NH through desorption in step (6)
2)
6si
2solid is placed in tube furnace, and at nitrogen atmosphere, 1000 DEG C of high temperature thermal decomposition 1 hour, namely obtain beta-silicon nitride powder after furnace cooling.
Further, the chloro silicoethane of step (2) is disilicone hexachloride and pentachloro-silicoethane mixture, disilicone hexachloride and pentachloro-silicoethane mass ratio be 1:1.
Preferred as one, in step (3), fed in raw material rear maintenance high shear agitation device and condensation reflux unit work, then obtain reaction product after stirring reaction 1h at 90 DEG C.
Further, step (2) is at the uniform velocity reinforced, within 180 minutes, completes reinforced.
Specific embodiment 3
A preparation method for beta-silicon nitride powder, comprises the following steps:
(1), in high-pressure reactor, add 1000 parts of liquefied ammonia, then be warming up to 70 DEG C, wherein: high-pressure reactor is provided with high shear agitation device and condensation reflux unit;
(2), open high shear agitation device and condensation reflux unit, then in high-pressure reactor, add 100 parts of chloro silicoethanes by feed-pipe;
(3), fed in raw material after, continue to obtain reaction product after stirring reaction 5h at 70 DEG C;
(4), the reaction product that uses closed filtering device filtration step (3) to obtain under normal temperature and ammonia saturation steam pressure pressure, obtain solid product;
(5), at 40 DEG C, solid product liquefied ammonia washing step (4) obtained obtains (NH
2)
6si
2solid, in washings, ammonium chloride mass content is less than till 0.1%;
(6), by (NH that step (5) obtains
2)
6si
2solid desorption 5 hours at 100 DEG C in vacuum seal stove,
(7), by (the NH through desorption in step (6)
2)
6si
2solid is placed in tube furnace, and at nitrogen atmosphere, 900 DEG C of high temperature thermal decomposition 5 hours, namely obtain beta-silicon nitride powder after furnace cooling.
Further, the chloro silicoethane of step (2) be disilicone hexachloride, pentachloro-silicoethane, the mixture of four silicon hexachlorides.Disilicone hexachloride, pentachloro-silicoethane, the mass ratio of four silicon hexachlorides is 1:1:1.
Preferred as one, in step (3), fed in raw material rear maintenance high shear agitation device and condensation reflux unit work, then obtain reaction product after stirring reaction 5h at 70 DEG C.
Further, step (2) is at the uniform velocity reinforced, within 60 minutes, completes reinforced.
Above embodiments of the present invention are elaborated.But the present invention is not limited to above-mentioned embodiment, in the ken that art those of ordinary skill possesses, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (4)
1. a preparation method for beta-silicon nitride powder, is characterized in that, comprises the following steps:
(1), in high-pressure reactor, add 1000 parts of liquefied ammonia, then be warming up to 50 ~ 90 DEG C, wherein: high-pressure reactor is provided with high shear agitation device and condensation reflux unit;
(2), open high shear agitation device and condensation reflux unit, then in high-pressure reactor, add 50 ~ 200 parts of chloro silicoethanes by feed-pipe;
(3), fed in raw material after, continue at 50 ~ 90 DEG C stir 1 ~ 50h obtain reaction product;
(4), the reaction product that uses closed filtering device filtration step (3) to obtain under normal temperature and ammonia saturation steam pressure pressure, obtain solid product;
(5), at room temperature ~ 90 DEG C, solid product liquefied ammonia washing step (4) obtained obtains (NH
2)
6si
2solid, in washings, ammonium chloride mass content is less than till 0.1%;
(6), by (NH that step (5) obtains
2)
6si
2solid desorption 2 ~ 10 hours at 60 ~ 180 DEG C in vacuum seal stove;
(7), by (the NH through desorption in step (6)
2)
6si
2solid is placed in tube furnace, and at nitrogen atmosphere, 800 ~ 1000 DEG C of high temperature thermal decomposition 1 ~ 20 hour, namely obtain beta-silicon nitride powder after furnace cooling.
2. the preparation method of a kind of beta-silicon nitride powder according to claim 1, is characterized in that, the chloro silicoethane described in step (2) be disilicone hexachloride, pentachloro-silicoethane, one or more in four silicon hexachlorides.
3. the preparation method of a kind of beta-silicon nitride powder according to claim 1, it is characterized in that, in step (3), fed in raw material rear maintenance high shear agitation device and condensation reflux unit work, then continue at 50 ~ 90 DEG C, stir 1 ~ 50h and obtain reaction product.
4. the preparation method of a kind of beta-silicon nitride powder according to claim 1, is characterized in that, step (2) is at the uniform velocity reinforced, completes reinforced in 30 ~ 180 minutes.
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|---|---|---|---|
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|---|---|
| CN105253864A true CN105253864A (en) | 2016-01-20 |
| CN105253864B CN105253864B (en) | 2017-07-11 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107557866A (en) * | 2017-08-28 | 2018-01-09 | 青岛桥海陶瓷新材料科技有限公司 | The preparation method of silicon nitride crystal whisker |
| CN113173563A (en) * | 2021-04-27 | 2021-07-27 | 安徽工业大学 | Dehalogenation liquid and dehalogenation method for nitride precursor |
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|---|---|---|---|---|
| CN1562735A (en) * | 2004-03-19 | 2005-01-12 | 山东大学 | Method for preparing powder material of silicon nitride under low temperature |
| CN101734632A (en) * | 2009-12-10 | 2010-06-16 | 四川德诚金谷硅材料有限公司 | Production method of nano silicon nitride powders |
| CN101830495A (en) * | 2010-04-29 | 2010-09-15 | 宁夏胜蓝化工环保科技有限公司 | Comprehensive utilization method of chlorosilane |
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2015
- 2015-11-13 CN CN201510780188.0A patent/CN105253864B/en active Active
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| CN1562735A (en) * | 2004-03-19 | 2005-01-12 | 山东大学 | Method for preparing powder material of silicon nitride under low temperature |
| CN101734632A (en) * | 2009-12-10 | 2010-06-16 | 四川德诚金谷硅材料有限公司 | Production method of nano silicon nitride powders |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107557866A (en) * | 2017-08-28 | 2018-01-09 | 青岛桥海陶瓷新材料科技有限公司 | The preparation method of silicon nitride crystal whisker |
| CN113173563A (en) * | 2021-04-27 | 2021-07-27 | 安徽工业大学 | Dehalogenation liquid and dehalogenation method for nitride precursor |
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| Publication number | Publication date |
|---|---|
| CN105253864B (en) | 2017-07-11 |
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Denomination of invention: A Preparation Method of Silicon Nitride Powder Effective date of registration: 20230330 Granted publication date: 20170711 Pledgee: Industrial Bank Co.,Ltd. Yinchuan Branch Pledgor: NINGXIA SHENGLAN CHEMICAL ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Registration number: Y2023980036999 |
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Denomination of invention: A preparation method of silicon nitride powder Granted publication date: 20170711 Pledgee: Industrial Bank Co.,Ltd. Yinchuan Branch Pledgor: NINGXIA SHENGLAN CHEMICAL ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Registration number: Y2024980010536 |
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