CN205133153U - System for production silicon nitride - Google Patents
System for production silicon nitride Download PDFInfo
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- CN205133153U CN205133153U CN201520900792.8U CN201520900792U CN205133153U CN 205133153 U CN205133153 U CN 205133153U CN 201520900792 U CN201520900792 U CN 201520900792U CN 205133153 U CN205133153 U CN 205133153U
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Abstract
The utility model discloses a system for production silicon nitride includes: the vacuum reactor for making raw materials silicon tetrachloride gas and the reaction of raw materials ammonia under the condition of vacuum, obtaining a solid mixture, wherein, a solid mixture includes that raw materials silicon tetrachloride gas and raw materials ammonia react nitrogenous silane compound and the ammonium chloride that generates, heating device is connected with the vacuum reactor, and heating device is used for the nitrogenous silane compound of thermal treatment to obtain the silicon nitride. The utility model provides a system for production silicon nitride replaces the liquid interface reaction system among the prior art, thereby the reaction rate between the raw materials has been reduced, make the reaction rate between the raw materials to control, and do not need with an organic solvent, subsequent complicated separation circuit has been avoided, the applied technology is simple, the extensive metaplasia of realizing nitrogenous silane compound is more easily produced, the large -scale production of silicon nitride has also been realized, and has a high capacity, the manufacturing cost of silicon nitride has been reduced under the prerequisite of the quality of guaranteeing the production silicon nitride.
Description
Technical field
The utility model belongs to silicon nitride production technical field, is specifically related to a kind of system of producing silicon nitride.
Background technology
Silicon nitride has that physical strength is high, Heat stability is good, good chemical stability, for the high temperature often run in modern technologies, at a high speed, the Working environment of strong corrosive medium and high wearing and tearing, there is special purposes.Silicon nitride having many uses industrially is general, can be applicable to metallurgy, machinery, chemical industry, semi-conductor, aerospace and auto industry field, as turbine blade, high-temperature bearing, high speed cutting instrument, heat-resistant part, abrasion-proof corrosion-proof parts etc.Along with the continuous expansion of silicon nitride range of application and improving constantly silicon nitride quality requirements, the preparation of beta-silicon nitride powder more and more comes into one's own.
The silicon nitride technology of preparing of commercial applications has four kinds: (1) silica flour direct nitridation method, comprises low-voltage high-temperature nitrogenize and the nitrogenize of high pressure self-propagating; (2), in nitrogen, there is redox reaction by silicon-dioxide and carbon dust and generate silicon nitride in carbothermic method; (3) low temperature silane thermal decomposition process, generates intermediate product nitrogenated silicon hydride compounds Si (NH) by silicon tetrachloride and ammonia
2, and then pyrolysis is silicon nitride; (4) high temperature silane thermal decomposition process, by silicon tetrachloride or silicomethane at high temperature directly and ammonia to react generation silicon nitride.In the above-mentioned methods, low temperature silane thermal decomposition process and high temperature silane thermal decomposition process easily realize, to raw-material purification, being suitable for the preparation of high purity silicon nitride silicon powder.But in high temperature silane thermal decomposition process, silicomethane is inflammable and explosive, dangerous high, and during using silicon tetrachloride as raw material, need the technology such as using plasma, laser to carry out reaction strengthening, investment is large, and productive rate is low, and cost is high.
Silicon nitride prepared by low temperature silane thermal decomposition process is generally accepted by people with its high quality, but the rapid reaction synthesizing strong heat release of nitrogenated silicon hydride compounds in low temperature silane thermal decomposition process, chlorine element is easily carried secretly in nitrogenated silicon hydride compounds, therefore its liquid-liquid interface reaction of producing general employing silicon tetrachloride and ammonia controls speed of response at present, and then obtaining pure nitrogenated silicon hydride compounds by the method that a large amount of liquefied ammonia washes away ammonium chloride by-product, last reheating is decomposed into silicon nitride.Liquid-liquid interface speed of reaction is slow, and complex process, production capacity is low, causes its cost can not to be in any more always.A kind of simple low temperature silane thermal decomposition process silicon nitride preparation technology of exploitation, in the manufacturing cost of the situation decline lower silicon nitride of ensuring the quality of products, is the problem needing solution at present badly.
Utility model content
Technical problem to be solved in the utility model is for above shortcomings in prior art, a kind of system of producing silicon nitride is provided, by which system reduces the speed of response between raw material, speed of response between raw material can be controlled, and do not need with an organic solvent, avoid follow-up complex separations operation, technique is simple.
The technical scheme that solution the utility model technical problem adopts is to provide a kind of system of producing silicon nitride and comprises:
Vacuum reactor, for making raw material silicon tetrachloride gas and raw material ammonia solid/liquid/gas reactions under vacuum condition, obtain the first solid mixture, wherein, described first solid mixture comprises the nitrogenated silicon hydride compounds and ammonium chloride that described raw material silicon tetrachloride gas and described raw material ammonia solid/liquid/gas reactions generate;
Heating unit, is connected with described vacuum reactor, and described heating unit is used for nitrogenated silicon hydride compounds described in thermal treatment and obtains silicon nitride.
Nitrogenated silicon hydride compounds of the present utility model, generally also referred to as silicon diimine, easily absorbs or exists with Si-N-H based compound form after releasing ammonia, the most available Si (NH) of nitrogenated silicon hydride compounds
2formula represents, Si (NH)
2be not a concrete material, this compounds can be Si
6n
13h
15, Si
6n
12h
12, Si
6n
11h
9deng.
Preferably, described heating unit comprises:
Primary heater, be connected with described vacuum reactor, described first solid mixture in described vacuum reactor enters described primary heater, described primary heater is used under non-oxidizing atmosphere, heat described first solid mixture, obtain the second solid matter, described ammonium chloride generation thermolysis generates ammonia and hydrogenchloride, wherein, described second solid matter comprises containing described nitrogen silane compound;
Secondary heater, be connected with described primary heater, described second solid matter in described primary heater enters in described secondary heater, described secondary heater is used under ammonia atmosphere, heat described second solid matter, obtain the 3rd solid matter, described 3rd solid matter comprises the unbodied silicon nitride generated containing described nitrogen silane compound generation thermolysis;
3rd well heater, be connected with described secondary heater, described 3rd solid matter in described secondary heater enters in described 3rd well heater, described 3rd well heater is used under non-oxidizing atmosphere, heat described 3rd solid matter, obtain the 4th solid matter, described 4th solid matter comprises the silicon nitride of described unbodied silicon nitride through the high α phase content of heating generation.
The system of the production silicon nitride in the utility model substitutes liquid-liquid interface reactive system of the prior art; thus the speed of response reduced between raw material; speed of response between raw material can be controlled; and do not need with an organic solvent; avoid follow-up complex separations operation; technique is simple; more easily realize the large-scale production of nitrogenated silicon hydride compounds; also achieve the scale operation of silicon nitride; production capacity is high, reduces the manufacturing cost of silicon nitride under the prerequisite ensureing the quality of producing silicon nitride.
Accompanying drawing explanation
Fig. 1 is the structural representation of the system of production silicon nitride in the utility model embodiment.
In figure: 1-vacuum reactor; First opening for feed of 11-vacuum reactor; Second opening for feed of 12-vacuum reactor; The top of 13-vacuum reactor; The bottom of 14-vacuum reactor; 2-primary heater; 3-secondary heater; The inlet mouth of 31-secondary heater; 4-the 3rd well heater.
Embodiment
For making those skilled in the art understand the technical solution of the utility model better, below in conjunction with the drawings and specific embodiments, the utility model is described in further detail.
Embodiment
As shown in Figure 1, a kind of system of producing silicon nitride of the present embodiment comprises:
Vacuum reactor 1, for making raw material silicon tetrachloride gas and raw material ammonia solid/liquid/gas reactions under vacuum condition, obtain the first solid mixture, wherein, described first solid mixture comprises the nitrogenated silicon hydride compounds and ammonium chloride that described raw material silicon tetrachloride gas and described raw material ammonia solid/liquid/gas reactions generate; Particularly, vacuum reactor 1 is provided with the first opening for feed 11 of vacuum reactor, for raw material ammonia feed; Vacuum reactor 1 is also provided with the second opening for feed 12 of vacuum reactor, for raw material silicon tetrachloride feeding.The tail gas produced after reacting in vacuum reactor 1 is discharged by the top 13 of vacuum reactor.
Heating unit, is connected with described vacuum reactor 1, and described heating unit is used for nitrogenated silicon hydride compounds described in thermal treatment and obtains silicon nitride.
Speed of reaction in vacuum reactor 1 is controlled, reduces carrying secretly of chlorine element, thus can suitability for industrialized production.
The system of the production silicon nitride in the utility model substitutes liquid-liquid interface reactive system of the prior art; thus the speed of response reduced between raw material; speed of response between raw material can be controlled; and do not need with an organic solvent; avoid follow-up complex separations operation; technique is simple; more easily realize the large-scale production of nitrogenated silicon hydride compounds; also achieve the scale operation of silicon nitride; production capacity is high, reduces the manufacturing cost of silicon nitride under the prerequisite ensureing the quality of producing silicon nitride.
Preferably, described heating unit comprises:
Primary heater 2, be connected with described vacuum reactor 1, described first solid mixture in described vacuum reactor 1 enters described primary heater 2, described primary heater 2 is under non-oxidizing atmosphere, heat described first solid mixture, obtain the second solid matter, described ammonium chloride generation thermolysis generates ammonia and hydrogenchloride, wherein, described second solid matter comprises containing described nitrogen silane compound; Heating temperature in primary heater 2 is 500 ~ 600 DEG C, thermal treatment 1 ~ 2h.Concrete, primary heater 2 is connected with the bottom 14 of vacuum reactor, and the first solid mixture is entered in primary heater 2 by the tower reactor 14 of vacuum reactor.Non-oxidizing atmosphere is the one in inert gas atmosphere, nitrogen atmosphere, ammonia atmosphere, is preferably nitrogen atmosphere.
Secondary heater 3, be connected with described primary heater 2, described second solid matter in described primary heater 2 enters in described secondary heater 3, described secondary heater 3 is under ammonia atmosphere, heat described second solid matter, obtain the 3rd solid matter, described 3rd solid matter comprises the unbodied silicon nitride generated containing described nitrogen silane compound generation thermolysis; Heating temperature in secondary heater 3 is 650 ~ 1200 DEG C, thermal treatment 2 ~ 8 hours.Particularly, secondary heater 3 is provided with the inlet mouth 31 of secondary heater, for passing into ammonia.
3rd well heater 4, be connected with described secondary heater 3, described 3rd solid matter in described secondary heater 3 enters in described 3rd well heater 4, described 3rd well heater 4 is under non-oxidizing atmosphere, heat described 3rd solid matter, obtain the 4th solid matter, described 4th solid matter comprises the silicon nitride of described unbodied silicon nitride through the high α phase content of heating generation.In 4th solid matter, the mass percentage content of the silicon nitride of α phase is 90 ~ 98%, content of Cl element <60ppm.Heating temperature in 3rd well heater 4 is 1250 ~ 1700 DEG C, thermal treatment 2 ~ 8 hours.Non-oxidizing atmosphere is the one in inert gas atmosphere, nitrogen atmosphere, ammonia atmosphere, is preferably nitrogen atmosphere.
By producing secondary heater 3 in the system of silicon nitride and the 3rd well heater 4 thus making the amount of the silicon nitride of the α phase in the 4th final obtained solid matter controlled, the mass percentage content of the silicon nitride of the α phase in the 4th solid matter is 90 ~ 98%.
The system of the production silicon nitride in the utility model substitutes liquid-liquid interface reactive system of the prior art; thus the speed of response reduced between raw material; speed of response between raw material can be controlled; and do not need with an organic solvent; avoid follow-up complex separations operation; technique is simple; more easily realize the large-scale production of nitrogenated silicon hydride compounds; also achieve the scale operation of silicon nitride; production capacity is high, reduces the manufacturing cost of silicon nitride under the prerequisite ensureing the quality of producing silicon nitride.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present utility model is described and adopts, but the utility model is not limited thereto.For those skilled in the art, when not departing from spirit of the present utility model and essence, can make various modification and improvement, these modification and improvement are also considered as protection domain of the present utility model.
Claims (2)
1. produce a system for silicon nitride, it is characterized in that, comprising:
Vacuum reactor, for making raw material silicon tetrachloride gas and raw material ammonia solid/liquid/gas reactions under vacuum condition, obtain the first solid mixture, wherein, described first solid mixture comprises the nitrogenated silicon hydride compounds and ammonium chloride that described raw material silicon tetrachloride gas and described raw material ammonia solid/liquid/gas reactions generate;
Heating unit, is connected with described vacuum reactor, and described heating unit is used for nitrogenated silicon hydride compounds described in thermal treatment and obtains silicon nitride.
2. the system of production silicon nitride according to claim 1, is characterized in that, described heating unit comprises:
Primary heater, be connected with described vacuum reactor, described first solid mixture in described vacuum reactor enters described primary heater, described primary heater is used under non-oxidizing atmosphere, heat described first solid mixture, obtain the second solid matter, described ammonium chloride generation thermolysis generates ammonia and hydrogenchloride, wherein, described second solid matter comprises containing described nitrogen silane compound;
Secondary heater, be connected with described primary heater, described second solid matter in described primary heater enters in described secondary heater, described secondary heater is used under ammonia atmosphere, heat described second solid matter, obtain the 3rd solid matter, described 3rd solid matter comprises the unbodied silicon nitride generated containing described nitrogen silane compound generation thermolysis;
3rd well heater, be connected with described secondary heater, described 3rd solid matter in described secondary heater enters in described 3rd well heater, described 3rd well heater is used under non-oxidizing atmosphere, heat described 3rd solid matter reaction, obtain the 4th solid matter, described 4th solid matter comprises the silicon nitride containing α phase content that described unbodied silicon nitride generates through heating.
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| CN201520900792.8U CN205133153U (en) | 2015-11-11 | 2015-11-11 | System for production silicon nitride |
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| CN201520900792.8U CN205133153U (en) | 2015-11-11 | 2015-11-11 | System for production silicon nitride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394876A (en) * | 2017-02-07 | 2018-08-14 | 新疆晶硕新材料有限公司 | Nitrogen silane and its production method, silicon nitride and its production method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394876A (en) * | 2017-02-07 | 2018-08-14 | 新疆晶硕新材料有限公司 | Nitrogen silane and its production method, silicon nitride and its production method |
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Effective date of registration: 20180404 Address after: 831500, the Xinjiang Uygur Autonomous Region Urumqi hi tech Development Zone (new urban area) Ganquan Fort economic and Technological Development Zone (Industrial Park), seven East Rd 2499 Rd building. Patentee after: Xinjiang Jing Shuo New Material Co., Ltd. Address before: The 830011 the Xinjiang Uygur Autonomous Region Urumqi national hi tech Industrial Development Zone (new town) Fort oasis high tech Industrial Park Patentee before: Xinte Energy Co.,Ltd. |