CN106672923A - Preparation method of silicon nitride and system for producing silicon nitride - Google Patents
Preparation method of silicon nitride and system for producing silicon nitride Download PDFInfo
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- CN106672923A CN106672923A CN201510770205.2A CN201510770205A CN106672923A CN 106672923 A CN106672923 A CN 106672923A CN 201510770205 A CN201510770205 A CN 201510770205A CN 106672923 A CN106672923 A CN 106672923A
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Abstract
The invention discloses a preparation method of silicon nitride and a system for producing silicon nitride. The preparation method comprises the steps of (1) reacting silicon tetrachloride gas with ammonia gas to generate a nitrogen-containing silane compound in a vacuum condition; and (2) carrying out thermal treatment to obtain silicon nitride. According to the preparation of silicon nitride, liquid-liquid interfacial reaction in the prior art is replaced with a vacuum vapor reaction method, the reaction rate of the raw materials is reduced, an organic solvent does not need to be utilized, the subsequent complicated separation procedure is avoided, the process is simple, and massive production of the nitrogen-containing silane compound is easier to implement, the massive production of silicon nitride is also achieved, the productivity is high, and the manufacturing cost of silicon nitride is reduced on the premise of ensuring the quality of the produced silicon nitride.
Description
Technical field
The invention belongs to silicon nitride production technical field, and in particular to a kind of system of silicon nitride
The system of Preparation Method and production silicon nitride.
Background technology
Silicon nitride has that high mechanical strength, heat stability be good, good chemical stability,
For the high temperature, high speed, strong corrosive medium and height abrasion frequently encountered in modern technologies
Working environment, with special purposes.Silicon nitride having many uses industrially is general, can
Metallurgy, machinery, chemical industry, quasiconductor, Aero-Space and auto industry field are applied to,
As turbo blade, high-temperature bearing, high-speed cutting instrument, heat-resistant part, abrasion-proof corrosion-proof
Part etc..With the continuous expansion of silicon nitride range of application and to silicon nitride quality requirements
Improve constantly, the preparation of beta-silicon nitride powder is increasingly taken seriously.
The silicon nitride technology of preparing of commercial applications has four kinds：(1) the direct nitrogen of silica flour
Change method, including low-voltage high-temperature nitridation and the nitridation of high pressure self- propagating；(2) carbothermic method,
There is redox reaction in nitrogen by silicon dioxide and carbon dust and generate silicon nitride；(3)
Low temperature silane thermal decomposition process, generates the nitrogenous silane compound of intermediate product by Silicon chloride. and ammonia
Si(NH)2, then it is pyrolyzed again as silicon nitride；(4) high temperature silane thermal decomposition process, by Silicon chloride. or
Monosilane is directly reacted generation silicon nitride with ammonia at high temperature.In the above-mentioned methods,
Low temperature silane thermal decomposition process and high temperature silane thermal decomposition process easily realize the purification to raw material, are suitable for high-purity
The preparation of beta-silicon nitride powder.It is but in high temperature silane thermal decomposition process, monosilane is inflammable and explosive, dangerous
Height, and during using Silicon chloride. as raw material, need the technologies such as using plasma, laser
Reaction reinforcing is carried out, investment is big, low yield, high cost.
Silicon nitride prepared by low temperature silane thermal decomposition process is generally received by people with its high-quality, but
In low temperature silane thermal decomposition process, nitrogenous silane compound synthesizes strongly exothermic fast reaction, nitrogenous
Easily carry chlorine element in silane compound secretly, therefore its production typically adopts four chlorinations at present
The liquid-liquid interface of silicon and ammonia reacts to control response speed, is then washed away with a large amount of liquefied ammonia again
The method of ammonium chloride by-product obtains pure nitrogenous silane compound, finally thermally decomposes again
For silicon nitride.Liquid-liquid interface reaction rate is slow, and complex process, production capacity are low, cause its into
This can be in any more always.A kind of simple low temperature silane thermal decomposition process silicon nitride preparation technology is developed,
The manufacturing cost of silicon nitride is reduced in the case where quality is ensured, is current urgent need to resolve
Problem.
The content of the invention
The technical problem to be solved be for present in prior art it is above-mentioned not
A kind of foot, there is provided the system of preparation method of silicon nitride and production silicon nitride, the method drop
Response speed between low raw material so that the response speed between raw material can be controlled,
And need not use organic solvent, it is to avoid follow-up complex separations operation, process is simple.
The technical scheme adopted by solution present invention problem is to provide a kind of silicon nitride
Preparation method, comprises the following steps：
(1) under vacuum, Silicon chloride. gas and ammonia reaction generates nitrogenous silane
Compound.
(2) heat treatment, obtains silicon nitride.
The nitrogenous silane compound of the present invention is also commonly referred to as silicon diimine, easily absorb or
Exist with Si-N-H based compounds form after releasing ammonia, nitrogenous silane compound majority can
With Si (NH)2Formula represents, Si (NH)2It is not a specific material, such chemical combination
Thing can be Si6N13H15、Si6N12H12、Si6N11H9Deng.
The preparation method reaction rate is controllable such that it is able to industrialized production.
Preferably, Silicon chloride. gas described in the step (1) and the ammonia
Reaction temperature is -20～60 DEG C.By reaction and described vacuum condition at such a temperature,
The entrainment for generating chlorine element in nitrogenous silane compound can be reduced.
Preferably, the absolute pressure of the vacuum condition in the step (1) is
10～10000Pa.
Preferably, in the step (1), the institute of the Silicon chloride. gas and excess
State ammonia reaction and generate the nitrogenous silane compound.
Preferably, Silicon chloride. gas described in the step (1) and the ammonia
Mol ratio is 1：(6～30).
Preferably, described in the step (1), Silicon chloride. gas and the ammonia are anti-
By-product ammonium chloride, institute are generated during the nitrogenous silane compound should be generated also
State,
1～2h of heat treatment, removes the by-product ammonium chloride.
Preferably, the concrete operations condition of the heat treatment of the step (2) is according to following
Step is carried out,
M (), under ammonia atmosphere, heating, the nitrogenous silane compound are decomposed
Generate unbodied silicon nitride；Can remove what is remained in whole system by ammonia atmosphere
Most of chlorine element.
N (), under non-oxidizing atmosphere, there is phase in heating, the unbodied silicon nitride
Change is changed into the silicon nitride of high α phase contents.By step (m) and (n) two-step reaction,
So that the amount of the silicon nitride of α phases in final obtained silicon nitride is controllable, the nitridation
The mass percentage content of the silicon nitride of the α phases in silicon is 90～98%.
Preferably, the heating condition of the step (m) is specially at 650～1200 DEG C,
Heat treatment 2～8 hours.
Preferably, the heating condition of the step (n) is specially at 1250～1700 DEG C,
Heat treatment 2～8 hours.
Preferably, the non-oxidizing atmosphere in the step (n) is noble gases
One or more in atmosphere, nitrogen atmosphere, ammonia atmosphere, Carbon monoxide reduction atmosphere.
The present invention also provides a kind of system for producing above-mentioned silicon nitride to be included：
Vacuum reactor, for raw material Silicon chloride. gas and raw material ammonia are made under vacuum condition
Solid/liquid/gas reactions, obtain the first solid mixture, wherein, first solid mixture includes
The raw material Silicon chloride. gas is closed with the nitrogenous silanization that the raw material ammonia solid/liquid/gas reactions are generated
Thing and ammonium chloride；
Heater, is connected with the vacuum reactor, and the heater is used at heat
Manage the nitrogenous silane compound and obtain silicon nitride.
Preferably, the heater includes：
Primary heater, is connected with the vacuum reactor, in the vacuum reactor
First solid mixture enters the primary heater, and the primary heater is used for
Under non-oxidizing atmosphere, first solid mixture is heated, the second solidss are obtained
Matter, the ammonium chloride thermally decompose to generate ammonia and hydrogen chloride, wherein, described second
Solid matter is included containing the nitrogen silane compound；
Secondary heater, is connected with the primary heater, in the primary heater
Second solid matter is entered in the secondary heater, and the secondary heater is used for
Under ammonia atmosphere, second solid matter is heated, the 3rd solid matter, institute is obtained
Stating the 3rd solid matter includes determining containing the nothing that the nitrogen silane compound is thermally decomposed to generate
The silicon nitride of shape；
3rd heater, is connected with the secondary heater, in the secondary heater
3rd solid matter is entered in the 3rd heater, and the 3rd heater is used for
Under non-oxidizing atmosphere, the 3rd solid matter is heated, the 4th solid matter is obtained,
4th solid matter includes the high α that the unbodied silicon nitride is generated through heating
The silicon nitride of phase content.
The preparation method of the silicon nitride in the present invention is substituted using the method for vacuum gas-phase reaction
Liquid-liquid interface reaction of the prior art, so as to reduce the response speed between raw material,
Response speed between raw material is controlled, and organic solvent need not be used, kept away
Follow-up complex separations operation, process is simple are exempted from, it is easier to realize that nitrogenous silanization is closed
The large-scale production of thing, also achieves the large-scale production of silicon nitride, and production capacity is high,
The manufacturing cost of silicon nitride, production are reduced on the premise of the quality for ensureing production silicon nitride
The system of silicon nitride substitutes liquid-liquid interface response system of the prior art..
Description of the drawings
Fig. 1 is the structural representation of the system of the production silicon nitride in the embodiment of the present invention 6.
In figure：1- vacuum reactors；The first charging aperture of 11- vacuum reactors；12- vacuum
The second charging aperture of reactor；The top of 13- vacuum reactors；The bottom of 14- vacuum reactors
Portion；2- primary heaters；3- secondary heaters；The air inlet of 31- secondary heaters；4-
3rd heater.
Specific embodiment
To make those skilled in the art more fully understand technical scheme, tie below
Close the drawings and specific embodiments to be described in further detail the present invention.
Embodiment 1
The present embodiment provides a kind of preparation method of silicon nitride, comprises the following steps：
(1) under vacuum, Silicon chloride. gas and ammonia reaction generates nitrogenous silane
Compound；
(2) heat, obtain silicon nitride.The preparation method reaction rate is controllable, so as to
Enough industrialized production.
The preparation method of the silicon nitride in the present embodiment is replaced using the method that vacuum gas-phase reacts
React for liquid-liquid interface of the prior art, so as to reduce the response speed between raw material,
Response speed between raw material is controlled, and organic solvent need not be used, kept away
Follow-up complex separations operation, process is simple are exempted from, it is easier to realize that nitrogenous silanization is closed
The large-scale production of thing, also achieves the large-scale production of silicon nitride, and production capacity is high,
The manufacturing cost of silicon nitride is reduced on the premise of the quality for ensureing production silicon nitride.
Embodiment 2
The present embodiment provides a kind of preparation method of silicon nitride, comprises the following steps：
(1) under conditions of absolute pressure is 10000Pa, at 20 DEG C, Silicon chloride.
The ammonia reaction of the gas phase of gas and excess generates nitrogenous silane compound, by the temperature
Degree is lower to react, it is possible to reduce generate the entrainment of chlorine element in nitrogenous silane compound, described
During Silicon chloride. gas and ammonia reaction generate the nitrogenous silane compound
By-product ammonium chloride is generated also；Wherein, the Silicon chloride. gas and the ammonia
Mol ratio is 1：15.
(2) at 520 DEG C, heat treatment 2h removes the by-product ammonium chloride.
(3) under ammonia atmosphere, at 1200 DEG C, heat treatment 4 hours is described nitrogenous
Silane compound is decomposed and generates unbodied silicon nitride；Can be removed by ammonia atmosphere
Go the most of chlorine element remained in whole system.
(4) under non-oxidizing atmosphere, at 1400 DEG C, heat treatment 2 hours is described
Unbodied silicon nitride undergoes phase transition the silicon nitride for being changed into α phases.By step (3) and
(4) two-step reaction, so that the silicon nitride of the α phases in final obtained silicon nitride
Amount is controllable, and the mass percentage content of the silicon nitride of the α phases in the silicon nitride is 98%.
The preparation method of the silicon nitride in the present embodiment is replaced using the method that vacuum gas-phase reacts
React for liquid-liquid interface of the prior art, so as to reduce the response speed between raw material,
Response speed between raw material is controlled, and organic solvent need not be used, kept away
Follow-up complex separations operation, process is simple are exempted from, it is easier to realize that nitrogenous silanization is closed
The large-scale production of thing, also achieves the large-scale production of silicon nitride, and production capacity is high,
The manufacturing cost of beta-silicon nitride powder is reduced on the premise of the quality for ensureing production silicon nitride.
Embodiment 3
The present embodiment provides a kind of preparation method of silicon nitride, comprises the following steps：
(1) under conditions of absolute pressure is 5000Pa, at -20 DEG C, Silicon chloride. gas
The ammonia reaction of the gas phase of body and excess generates nitrogenous silane compound, by the temperature
Lower reaction, it is possible to reduce the entrainment of chlorine element in the nitrogenous silane compound of generation, described four
Silicon chloride gas and ammonia reaction are gone back during generating the nitrogenous silane compound
Generate by-product ammonium chloride；Wherein, the Silicon chloride. gas and the ammonia rub
You are than being 1：20.
(2) at 600 DEG C, heat treatment 1.4h removes the by-product ammonium chloride.(3)
Under ammonia atmosphere, at 800 DEG C, heat treatment 6 hours, the nitrogenous silane compound are sent out
Solution estranged generates unbodied silicon nitride；Can be removed in whole system by ammonia atmosphere
Most of chlorine element of residual.
(4) under non-oxidizing atmosphere, at 1600 DEG C, heat treatment 4 hours is described
Unbodied silicon nitride undergoes phase transition the silicon nitride for being changed into α phases.By step (3) and
(4) two-step reaction, so that the silicon nitride of the α phases in final obtained silicon nitride
Amount is controllable, and the mass percentage content of the silicon nitride of the α phases in the silicon nitride is 92%.
Embodiment 4
The present embodiment provides a kind of preparation method of silicon nitride, comprises the following steps：
(1) under conditions of absolute pressure is 10Pa, at 60 DEG C, Silicon chloride. gas
Nitrogenous silane compound is generated with the reaction of the ammonia of excessive gas phase, by such a temperature
Reaction, it is possible to reduce generate the entrainment of chlorine element in nitrogenous silane compound, the tetrachloro
SiClx gas and ammonia reaction are also given birth to during generating the nitrogenous silane compound
Into by-product ammonium chloride；Wherein, the Silicon chloride. gas and the ammonia mole
Than for 1：6.
(2) at 500 DEG C, heat treatment 1.6h removes the by-product ammonium chloride.(3)
Under ammonia atmosphere, at 1000 DEG C, heat treatment 2 hours, the nitrogenous silane compound
Decompose and generate unbodied silicon nitride；Whole system can be removed by ammonia atmosphere
Most of chlorine element of middle residual.
(4) in a nitrogen atmosphere, at 1700 DEG C, heat treatment 6 hours, the nothing are fixed
The silicon nitride of shape undergoes phase transition the silicon nitride for being changed into α phases.By step (3) and (4)
Two-step reaction, so that the amount of the silicon nitride of the α phases in final obtained silicon nitride can
Control, the mass percentage content of the silicon nitride of the α phases in the silicon nitride is 90%.
Embodiment 5
The present embodiment provides a kind of preparation method of silicon nitride, comprises the following steps：
(1) under conditions of absolute pressure is 3000Pa, at 40 DEG C, Silicon chloride. gas
The ammonia reaction of the gas phase of body and excess generates nitrogenous silane compound, by the temperature
Lower reaction, it is possible to reduce the entrainment of chlorine element in the nitrogenous silane compound of generation, described four
Silicon chloride gas and ammonia reaction are gone back during generating the nitrogenous silane compound
Generate by-product ammonium chloride；Wherein, the Silicon chloride. gas and the ammonia rub
You are than being 1：30.
(2) at 580 DEG C, heat treatment 1h removes the by-product ammonium chloride.(3)
Under ammonia atmosphere, at 650 DEG C, heat treatment 8 hours, the nitrogenous silane compound are sent out
Solution estranged generates unbodied silicon nitride；Can be removed in whole system by ammonia atmosphere
Most of chlorine element of residual.
(4) under an argon atmosphere, at 1250 DEG C, heat treatment 8 hours, the nothing are fixed
The silicon nitride of shape undergoes phase transition the silicon nitride for being changed into α phases.By step (3) and (4)
Two-step reaction, so that the amount of the silicon nitride of the α phases in final obtained silicon nitride can
Control, the mass percentage content of the silicon nitride of the α phases in the silicon nitride is 96%.
Silicon nitride obtained by embodiment 2～5 is content of Cl element<The high purity silicon nitride of 60ppm
Silica flour.
Embodiment 6
As shown in figure 1, silicon nitride in a kind of production example of the present embodiment 1～5 is
System includes：
Vacuum reactor 1, for raw material Silicon chloride. gas and raw material are made under vacuum condition
Ammonia reacts, and obtains the first solid mixture, wherein, the first solid mixture bag
Include the nitrogenous silanization that the raw material Silicon chloride. gas is generated with the raw material ammonia solid/liquid/gas reactions
Compound and ammonium chloride；Specifically, the of vacuum reactor is provided with vacuum reactor 1
One charging aperture 11, for raw material ammonia feed；Vacuum is additionally provided with vacuum reactor 1
The second charging aperture 12 of reactor, for raw material silicon tetrachloride feeding.Vacuum reactor 1
The tail gas produced after inside reacting is discharged by the top 13 of vacuum reactor.
Heater, is connected with the vacuum reactor 1, and the heater is used for heat
Process the nitrogenous silane compound and obtain silicon nitride.
Reaction rate in vacuum reactor 1 is controllable, reduces the entrainment of chlorine element, from
And being capable of industrialized production.
It is anti-that the system of the production silicon nitride in the present invention substitutes liquid-liquid interface of the prior art
System is answered, so as to reduce the response speed between raw material so that the reaction between raw material
Speed can be controlled, and need not use organic solvent, it is to avoid follow-up complex separations
Operation, process is simple, it is easier to realize the large-scale production of nitrogenous silane compound,
The large-scale production of silicon nitride is also achieved, production capacity is high, in the matter for ensureing production silicon nitride
The manufacturing cost of silicon nitride is reduced on the premise of amount.
Preferably, the heater includes：
Primary heater 2, is connected with the vacuum reactor 1, the vacuum reactor 1
Interior first solid mixture enters the primary heater 2, the primary heater
2, for, under non-oxidizing atmosphere, heating first solid mixture, obtain second solid
Body material, the ammonium chloride thermally decompose to generate ammonia and hydrogen chloride, wherein, it is described
Second solid matter is included containing the nitrogen silane compound；Heating in primary heater 2
Temperature is 500～600 DEG C, 1～2h of heat treatment.Specifically, primary heater 2 and vacuum
The bottom 14 of reactor connects, bottom 14 of first solid mixture by vacuum reactor
Into in primary heater 2.Non-oxidizing atmosphere be inert gas atmosphere, nitrogen atmosphere,
One kind in ammonia atmosphere, preferably nitrogen atmosphere.
Secondary heater 3, is connected with the primary heater 2, the primary heater 2
Interior second solid matter is entered in the secondary heater 3, second heating
Device 3 is for, under ammonia atmosphere, heating second solid matter obtains the 3rd solid
Material, the 3rd solid matter include that thermal decomposition life occurs containing the nitrogen silane compound
Into unbodied silicon nitride；Heating-up temperature in secondary heater 3 is 650～1200 DEG C,
Heat treatment 2～8 hours.Specifically, secondary heater is provided with secondary heater 3
Air inlet 31, for being passed through ammonia.
3rd heater 4, is connected with the secondary heater 3, the secondary heater 3
Interior the 3rd solid matter is entered in the 3rd heater 4, the 3rd heating
Device 4 is obtained under non-oxidizing atmosphere, heating the 3rd solid matter reaction
4th solid matter, the 4th solid matter include that the unbodied silicon nitride is passed through
The silicon nitride of the high α phase contents that heating is generated.The silicon nitride of α phases in 4th solid matter
Mass percentage content be 90～98%, content of Cl element<60ppm.3rd heater 4
Interior heating-up temperature is 1250～1700 DEG C, heat treatment 2～8 hours.Non-oxidizing atmosphere is
In inert gas atmosphere, nitrogen atmosphere, ammonia atmosphere, Carbon monoxide reduction atmosphere one
Plant or several, preferably nitrogen atmosphere.
By produce silicon nitride system in secondary heater 3 and the 3rd heater 4 from
And cause the amount of the silicon nitride of the α phases in final obtained 4th solid matter controllable, should
The mass percentage content of the silicon nitride of the α phases in the 4th solid matter is 90～98%.
It is anti-that the system of the production silicon nitride in the present invention substitutes liquid-liquid interface of the prior art
System is answered, so as to reduce the response speed between raw material so that the reaction between raw material
Speed can be controlled, and need not use organic solvent, it is to avoid follow-up complex separations
Operation, process is simple, it is easier to realize the large-scale production of nitrogenous silane compound,
The large-scale production of silicon nitride is also achieved, production capacity is high, in the matter for ensureing production silicon nitride
The manufacturing cost of silicon nitride is reduced on the premise of amount.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present
And the illustrative embodiments for adopting, but the invention is not limited in this.For ability
For those of ordinary skill in domain, in the situation without departing from spirit and substance of the present invention
Under, various modifications and improvement can be made, these modifications and improvement are also considered as the present invention's
Protection domain.
Claims (12)
1. a kind of preparation method of silicon nitride, it is characterised in that comprise the following steps：
(1) under vacuum, Silicon chloride. gas and ammonia reaction generates nitrogenous silane
Compound；
(2) heat treatment, obtains silicon nitride.
2. the preparation method of silicon nitride according to claim 1, it is characterised in that
Described in the step (1), the reaction temperature of Silicon chloride. gas and the ammonia is
- 20～60 DEG C.
3. the preparation method of silicon nitride according to claim 1, it is characterised in that
The absolute pressure of the vacuum condition in the step (1) is 10～10000Pa.
4. the preparation method of silicon nitride according to claim 1, it is characterised in that
In the step (1), the ammonia reaction of the Silicon chloride. gas and excess is generated
The nitrogenous silane compound.
5. the preparation method of silicon nitride according to claim 4, it is characterised in that
The mol ratio of Silicon chloride. gas and the ammonia described in the step (1) is 1：
(6～30).
6. the preparation method of silicon nitride according to claim 1, it is characterised in that
Silicon chloride. gas described in the step (1) and ammonia reaction generate described nitrogenous
By-product ammonium chloride, the step (1) and institute are generated during silane compound also
To state between step (2), 1～2h of heat treatment,
Remove the by-product ammonium chloride.
7. the preparation method of silicon nitride according to claim 1, it is characterised in that
The concrete operations condition of the heat treatment of the step (2) is carried out as steps described below,
M (), under ammonia atmosphere, heating, the nitrogenous silane compound are decomposed
Generate unbodied silicon nitride；
N (), under non-oxidizing atmosphere, there is phase in heating, the unbodied silicon nitride
Change is changed into the silicon nitride of high α phase contents.
8. the preparation method of silicon nitride according to claim 7, it is characterised in that
The heating condition of the step (m) is specially at 650～1200 DEG C, and heat treatment 2～8 is little
When.
9. the preparation method of silicon nitride according to claim 7, it is characterised in that
The heating condition of the step (n) is specially at 1250～1700 DEG C, and heat treatment 2～8 is little
When.
10. the preparation method of silicon nitride according to claim 7, it is characterised in that
The non-oxidizing atmosphere in the step (n) be inert gas atmosphere, nitrogen atmosphere,
One or more in ammonia atmosphere, Carbon monoxide reduction atmosphere.
A kind of 11. systems of the silicon nitride produced in claim 1, it is characterised in that
Including：
Vacuum reactor, for raw material Silicon chloride. gas and raw material ammonia are made under vacuum condition
Solid/liquid/gas reactions, obtain the first solid mixture, wherein, first solid mixture includes
The raw material Silicon chloride. gas is closed with the nitrogenous silanization that the raw material ammonia solid/liquid/gas reactions are generated
Thing and ammonium chloride；
Heater, is connected with the vacuum reactor, and the heater is used at heat
Manage the nitrogenous silane compound and obtain silicon nitride.
The system of 12. production silicon nitrides according to claim 11, it is characterised in that
The heater includes：
Primary heater, is connected with the vacuum reactor, in the vacuum reactor
First solid mixture enters the primary heater, and the primary heater is used for
Under non-oxidizing atmosphere, first solid mixture is heated, the second solidss are obtained
Matter, the ammonium chloride thermally decompose to generate ammonia and hydrogen chloride, wherein, described second
Solid matter is included containing the nitrogen silane compound；
Secondary heater, is connected with the primary heater, in the primary heater
Second solid matter is entered in the secondary heater, and the secondary heater is used for
Under ammonia atmosphere, second solid matter is heated, the 3rd solid matter, institute is obtained
Stating the 3rd solid matter includes determining containing the nothing that the nitrogen silane compound is thermally decomposed to generate
The silicon nitride of shape；
3rd heater, is connected with the secondary heater, in the secondary heater
3rd solid matter is entered in the 3rd heater, and the 3rd heater is used for
Under non-oxidizing atmosphere, the 3rd solid matter is heated, the 4th solid matter is obtained,
4th solid matter includes the high α that the unbodied silicon nitride is generated through heating
The silicon nitride of phase content.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272283A (en) * | 2018-03-14 | 2019-09-24 | 江苏中能硅业科技发展有限公司 | A kind of production method of silicon nitride powder |
| CN110342494A (en) * | 2019-08-15 | 2019-10-18 | 苏州第一元素纳米技术有限公司 | The preparation and application of silicon nitride enveloped carbon nanometer tube |
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| JPS59162110A (en) * | 1983-02-28 | 1984-09-13 | Nippon Denso Co Ltd | Preparation of fine powder of silicon nitride |
| CN1051153A (en) * | 1990-12-20 | 1991-05-08 | 清华大学 | The method of making ultrafine powder of silicon nitride by dual-tube pressuring |
| CN1445161A (en) * | 2002-11-29 | 2003-10-01 | 白万杰 | Technique for preparing silicon nitride powders with high alpha phase by using plasma chemical vapor phase process |
| CN101821356A (en) * | 2007-10-10 | 2010-09-01 | 宇部兴产株式会社 | [beta]-sialon phosphor powder and process for production of the same |
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2015
- 2015-11-11 CN CN201510770205.2A patent/CN106672923B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59162110A (en) * | 1983-02-28 | 1984-09-13 | Nippon Denso Co Ltd | Preparation of fine powder of silicon nitride |
| CN1051153A (en) * | 1990-12-20 | 1991-05-08 | 清华大学 | The method of making ultrafine powder of silicon nitride by dual-tube pressuring |
| CN1445161A (en) * | 2002-11-29 | 2003-10-01 | 白万杰 | Technique for preparing silicon nitride powders with high alpha phase by using plasma chemical vapor phase process |
| CN101821356A (en) * | 2007-10-10 | 2010-09-01 | 宇部兴产株式会社 | [beta]-sialon phosphor powder and process for production of the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272283A (en) * | 2018-03-14 | 2019-09-24 | 江苏中能硅业科技发展有限公司 | A kind of production method of silicon nitride powder |
| CN110342494A (en) * | 2019-08-15 | 2019-10-18 | 苏州第一元素纳米技术有限公司 | The preparation and application of silicon nitride enveloped carbon nanometer tube |
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| CN106672923B (en) | 2019-05-17 |
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