CN106672923B - A kind of system of the preparation method of silicon nitride and production silicon nitride - Google Patents
A kind of system of the preparation method of silicon nitride and production silicon nitride Download PDFInfo
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- CN106672923B CN106672923B CN201510770205.2A CN201510770205A CN106672923B CN 106672923 B CN106672923 B CN 106672923B CN 201510770205 A CN201510770205 A CN 201510770205A CN 106672923 B CN106672923 B CN 106672923B
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Abstract
The invention discloses the system of a kind of preparation method of silicon nitride and production silicon nitride, preparation method the following steps are included: (1) under vacuum conditions, silicon tetrachloride gas and ammonia reaction generate nitrogenous silane compound；(2) it is heat-treated, obtains silicon nitride.The preparation method of silicon nitride in the present invention substitutes liquid-liquid interface in the prior art using the method that vacuum gas-phase reacts and reacts; reduce the reaction speed between raw material; and it does not need using organic solvent; avoid subsequent complex separations process; simple process, it is easier to which the large-scale production for realizing nitrogenous silane compound also achieves the large-scale production of silicon nitride; production capacity is high, and the manufacturing cost of silicon nitride is reduced under the premise of guaranteeing the quality of production silicon nitride.
Description
Technical field
The invention belongs to silicon nitride production technical fields, and in particular to a kind of preparation method of silicon nitride and production silicon nitride
System.
Background technique
Silicon nitride has that high mechanical strength, thermal stability be good, good chemical stability, in modern technologies often
High temperature, high speed, strong corrosive medium and the high working environment worn encountered, has special purposes.Silicon nitride is industrially
Have many uses general, can be applied to metallurgy, machinery, chemical industry, semiconductor, aerospace and auto industry field, as turbo blade,
High-temperature bearing, high-speed cutting tool, heat-resistant part, abrasion-proof corrosion-proof component etc..With silicon nitride application range it is continuous expansion and
The preparation of continuous improvement to silicon nitride quality requirements, beta-silicon nitride powder is increasingly taken seriously.
There are four types of the silicon nitride technologies of preparing of commercial applications: (1) silicon powder direct nitridation method, including low-voltage high-temperature nitrogen
Change and high pressure self- propagating nitrogenizes；(2) redox reaction generation is occurred in nitrogen by silica and carbon dust for carbothermic method
Silicon nitride；(3) low temperature silane thermal decomposition process generates the nitrogenous silane compound Si (NH) of intermediate product by silicon tetrachloride and ammonia2, then again
Pyrolysis is silicon nitride；(4) high temperature silane thermal decomposition process is directly reacted with ammonia at high temperature by silicon tetrachloride or monosilane and generates nitrogen
SiClx.In the above-mentioned methods, low temperature silane thermal decomposition process and the purification easy to accomplish to raw material of high temperature silane thermal decomposition process, are suitable for high purity silicon nitride
The preparation of silicon powder.But in high temperature silane thermal decomposition process, monosilane is inflammable and explosive, and risk is high, and when using silicon tetrachloride as raw material, need
The technologies such as using plasma, laser are wanted to carry out reaction reinforcing, investment is big, and low yield is at high cost.
Silicon nitride prepared by low temperature silane thermal decomposition process is generally received with its high quality by people, but nitrogenated silicon in low temperature silane thermal decomposition process
Hydride compounds synthesize strongly exothermic fast reaction, and entrainment chlorine element is easy in nitrogenous silane compound, therefore its life at present
It produces and is generally reacted using the liquid-liquid interface of silicon tetrachloride and ammonia to control reaction speed, then wash away ammonium chloride with a large amount of liquefied ammonia again
The method of by-product obtains pure nitrogenous silane compound, and last reheating is decomposed into silicon nitride.Liquid-liquid interface reaction rate is slow,
Complex process, production capacity is low, its cost is caused to remain high always.Develop a kind of simple low temperature silane thermal decomposition process silicon nitride preparation work
The problem of skill reduces the manufacturing cost of silicon nitride in the case where guaranteeing quality, is current urgent need to resolve.
Summary of the invention
The technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide a kind of silicon nitride
Preparation method and production silicon nitride system, this method reduce the reaction speeds between raw material, so that anti-between raw material
It answers speed can control, and does not need to avoid subsequent complex separations process, simple process using organic solvent.
The preparation method that technical solution used by present invention problem is to provide a kind of silicon nitride is solved, including following
Step:
(1) under vacuum conditions, silicon tetrachloride gas and ammonia reaction generate nitrogenous silane compound.
(2) it is heat-treated, obtains silicon nitride.
Nitrogenous silane compound of the invention is also commonly referred to as silicon diimine, is easy after absorption or releasing ammonia with Si-N-H
Based compound form exists, and nitrogenous silane compound majority can use Si (NH)2Formula expression, Si (NH)2It is not a specific object
Matter, such compound can be Si6N13H15、Si6N12H12、Si6N11H9Deng.
The preparation method reaction rate is controllable, so as to industrialized production.
Preferably, the reaction temperature of silicon tetrachloride gas described in the step (1) and the ammonia is -20~60
℃.By reacting at such a temperature and the vacuum condition, it is possible to reduce generate the folder of chlorine element in nitrogenous silane compound
Band.
Preferably, the absolute pressure of the vacuum condition in the step (1) is 10~10000Pa.
Preferably, in the step (1), contain described in the silicon tetrachloride gas and the excessive ammonia reaction generation
Nitrogen silane compound.
Preferably, the molar ratio of silicon tetrachloride gas described in the step (1) and the ammonia is 1:(6~30).
Preferably, silicon tetrachloride gas described in the step (1) and ammonia reaction generate the nitrogenous silane
By-product ammonium chloride is also generated during compound, further includes step (i) between the step (1) and the step (2)
At 500~600 DEG C, it is heat-treated 1~2h, removes the by-product ammonium chloride.
Preferably, the concrete operations condition of the heat treatment of the step (2) carries out as steps described below,
(m) under ammonia atmosphere, heating, the nitrogenous silane compound, which is decomposed, generates unbodied silicon nitride；It is logical
Crossing ammonia atmosphere can remove remaining major part chlorine element in whole system.
(n) under non-oxidizing atmosphere, heating, the unbodied silicon nitride, which is undergone phase transition, is changed into high α phase content
Silicon nitride.By step (m) and (n) two-step reaction, so that the amount of the silicon nitride of the α phase in final silicon nitride obtained can
It controls, the mass percentage content of the silicon nitride of the α phase in the silicon nitride is 90~98%.
Preferably, the heating condition of the step (m) is specially and is heat-treated 2~8 hours at 650~1200 DEG C.
Preferably, the heating condition of the step (n) is specially and is heat-treated 2~8 hours at 1250~1700 DEG C.
Preferably, the non-oxidizing atmosphere in the step (n) is inert gas atmosphere, nitrogen atmosphere, ammonia
One or more of atmosphere, Carbon monoxide reduction atmosphere.
The present invention also provides a kind of systems for producing above-mentioned silicon nitride to include:
It is solid to obtain first for making raw material silicon tetrachloride gas and raw material ammonia solid/liquid/gas reactions under vacuum condition for vacuum reactor
Body mixture, wherein first solid mixture includes that the raw material silicon tetrachloride gas and the raw material ammonia solid/liquid/gas reactions are raw
At nitrogenous silane compound and ammonium chloride；
Heating device is connect with the vacuum reactor, and the heating device is closed for being heat-treated the nitrogenous silanization
Object obtains silicon nitride.
Preferably, the heating device includes:
Primary heater is connect with the vacuum reactor, first solid mixture in the vacuum reactor
Into the primary heater, the primary heater is used under non-oxidizing atmosphere, heats first solid mixture,
The second solid matter is obtained, the ammonium chloride thermally decomposes to generate ammonia and hydrogen chloride, wherein the second solid matter packet
It includes containing the nitrogen silane compound；
Secondary heater is connect with the primary heater, second solid matter in the primary heater into
Enter in the secondary heater, the secondary heater is used under ammonia atmosphere, heats second solid matter, obtains the
Three solid matters, the third solid matter include the unbodied nitridation thermally decomposed to generate containing the nitrogen silane compound
Silicon；
Third heater is connect with the secondary heater, the third solid matter in the secondary heater into
Enter in the third heater, the third heater is used under non-oxidizing atmosphere, is heated the third solid matter, is obtained
To the 4th solid matter, the 4th solid matter includes the high α phase content that the unbodied silicon nitride is generated by heating
Silicon nitride.
The preparation method of silicon nitride in the present invention substitutes liquid liquid in the prior art using the method that vacuum gas-phase reacts
Interfacial reaction so that the reaction speed between raw material can control, and does not need to reduce the reaction speed between raw material
Using organic solvent, subsequent complex separations process, simple process are avoided, it is easier to realize the big rule of nitrogenous silane compound
Modelling production also achieves the large-scale production of silicon nitride, and production capacity is high, reduces under the premise of guaranteeing the quality of production silicon nitride
The manufacturing cost of silicon nitride, the system for producing silicon nitride substitute liquid-liquid interface reaction system in the prior art.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the system of the production silicon nitride in the embodiment of the present invention 6.
In figure: 1- vacuum reactor；The first charging aperture of 11- vacuum reactor；Second charging of 12- vacuum reactor
Mouthful；The top of 13- vacuum reactor；The bottom of 14- vacuum reactor；2- primary heater；3- secondary heater；31- second
The air inlet of heater；4- third heater.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing and specific embodiment party
Present invention is further described in detail for formula.
Embodiment 1
The present embodiment provides a kind of preparation methods of silicon nitride, comprising the following steps:
(1) under vacuum conditions, silicon tetrachloride gas and ammonia reaction generate nitrogenous silane compound；
(2) it heats, obtains silicon nitride.The preparation method reaction rate is controllable, so as to industrialized production.
The preparation method of silicon nitride in the present embodiment substitutes liquid in the prior art using the method that vacuum gas-phase reacts
Liquid interfacial reaction so that the reaction speed between raw material can control, and is not required to reduce the reaction speed between raw material
Organic solvent is used, avoids subsequent complex separations process, simple process, it is easier to realize the big of nitrogenous silane compound
Large-scale production also achieves the large-scale production of silicon nitride, and production capacity is high, drops under the premise of guaranteeing the quality of production silicon nitride
The low manufacturing cost of silicon nitride.
Embodiment 2
The present embodiment provides a kind of preparation methods of silicon nitride, comprising the following steps:
(1) under conditions of absolute pressure is 10000Pa, at 20 DEG C, the ammonia of silicon tetrachloride gas and excessive gas phase
Reaction generates nitrogenous silane compound, by reacting at such a temperature, it is possible to reduce generate chlorine element in nitrogenous silane compound
Entrainment, the silicon tetrachloride gas and ammonia reaction also generate pair during generating the nitrogenous silane compound
Product ammonium chloride；Wherein, the molar ratio of the silicon tetrachloride gas and the ammonia is 1:15.
(2) at 520 DEG C, it is heat-treated 2h, removes the by-product ammonium chloride.
(3) it under ammonia atmosphere, at 1200 DEG C, is heat-treated 4 hours, the nitrogenous silane compound, which is decomposed, generates nothing
The silicon nitride of setting；It can remove remaining major part chlorine element in whole system by ammonia atmosphere.
(4) it under non-oxidizing atmosphere, at 1400 DEG C, is heat-treated 2 hours, the unbodied silicon nitride, which is undergone phase transition, to be turned
Become the silicon nitride of α phase.By step (3) and (4) two-step reaction, so that the nitrogen of the α phase in final silicon nitride obtained
The amount of SiClx is controllable, and the mass percentage content of the silicon nitride of the α phase in the silicon nitride is 98%.
The preparation method of silicon nitride in the present embodiment substitutes liquid in the prior art using the method that vacuum gas-phase reacts
Liquid interfacial reaction so that the reaction speed between raw material can control, and is not required to reduce the reaction speed between raw material
Organic solvent is used, avoids subsequent complex separations process, simple process, it is easier to realize the big of nitrogenous silane compound
Large-scale production also achieves the large-scale production of silicon nitride, and production capacity is high, drops under the premise of guaranteeing the quality of production silicon nitride
The low manufacturing cost of beta-silicon nitride powder.
Embodiment 3
The present embodiment provides a kind of preparation methods of silicon nitride, comprising the following steps:
(1) under conditions of absolute pressure is 5000Pa, at -20 DEG C, the ammonia of silicon tetrachloride gas and excessive gas phase
Reaction generates nitrogenous silane compound, by reacting at such a temperature, it is possible to reduce generate chlorine element in nitrogenous silane compound
Entrainment, the silicon tetrachloride gas and ammonia reaction also generate pair during generating the nitrogenous silane compound
Product ammonium chloride；Wherein, the molar ratio of the silicon tetrachloride gas and the ammonia is 1:20.
(2) at 600 DEG C, it is heat-treated 1.4h, removes the by-product ammonium chloride.(3) under ammonia atmosphere, at 800 DEG C, heat
Processing 6 hours, the nitrogenous silane compound, which is decomposed, generates unbodied silicon nitride；It can remove by ammonia atmosphere whole
Remaining major part chlorine element in a system.
(4) it under non-oxidizing atmosphere, at 1600 DEG C, is heat-treated 4 hours, the unbodied silicon nitride, which is undergone phase transition, to be turned
Become the silicon nitride of α phase.By step (3) and (4) two-step reaction, so that the nitrogen of the α phase in final silicon nitride obtained
The amount of SiClx is controllable, and the mass percentage content of the silicon nitride of the α phase in the silicon nitride is 92%.
Embodiment 4
The present embodiment provides a kind of preparation methods of silicon nitride, comprising the following steps:
(1) under conditions of absolute pressure is 10Pa, at 60 DEG C, the ammonia reaction of silicon tetrachloride gas and excessive gas phase
Nitrogenous silane compound is generated, by reacting at such a temperature, it is possible to reduce generate the folder of chlorine element in nitrogenous silane compound
Band, the silicon tetrachloride gas and ammonia reaction also generate by-product during generating the nitrogenous silane compound
Ammonium chloride；Wherein, the molar ratio of the silicon tetrachloride gas and the ammonia is 1:6.
(2) at 500 DEG C, it is heat-treated 1.6h, removes the by-product ammonium chloride.(3) under ammonia atmosphere, at 1000 DEG C,
Heat treatment 2 hours, the nitrogenous silane compound, which is decomposed, generates unbodied silicon nitride；It can remove by ammonia atmosphere
Remaining major part chlorine element in whole system.
(4) in a nitrogen atmosphere, it at 1700 DEG C, is heat-treated 6 hours, the unbodied silicon nitride, which is undergone phase transition, to be changed into
The silicon nitride of α phase.By step (3) and (4) two-step reaction, so that the silicon nitride of the α phase in final silicon nitride obtained
Amount it is controllable, the mass percentage content of the silicon nitride of the α phase in the silicon nitride is 90%.
Embodiment 5
The present embodiment provides a kind of preparation methods of silicon nitride, comprising the following steps:
(1) under conditions of absolute pressure is 3000Pa, at 40 DEG C, the ammonia of silicon tetrachloride gas and excessive gas phase is anti-
Nitrogenous silane compound should be generated, by reacting at such a temperature, it is possible to reduce generate chlorine element in nitrogenous silane compound
Entrainment, the silicon tetrachloride gas and ammonia reaction also generate by-product during generating the nitrogenous silane compound
Object ammonium chloride；Wherein, the molar ratio of the silicon tetrachloride gas and the ammonia is 1:30.
(2) at 580 DEG C, it is heat-treated 1h, removes the by-product ammonium chloride.(3) under ammonia atmosphere, at 650 DEG C, at heat
Reason 8 hours, the nitrogenous silane compound, which is decomposed, generates unbodied silicon nitride；It can remove entirely by ammonia atmosphere
Remaining major part chlorine element in system.
(4) under an argon atmosphere, it at 1250 DEG C, is heat-treated 8 hours, the unbodied silicon nitride, which is undergone phase transition, to be changed into
The silicon nitride of α phase.By step (3) and (4) two-step reaction, so that the silicon nitride of the α phase in final silicon nitride obtained
Amount it is controllable, the mass percentage content of the silicon nitride of the α phase in the silicon nitride is 96%.
The resulting silicon nitride of embodiment 2~5 is content of Cl element < 60ppm high purity silicon nitride silicon powder.
Embodiment 6
As shown in Figure 1, the system of the silicon nitride in a kind of production example 1~5 of the present embodiment includes:
It is solid to obtain first for making raw material silicon tetrachloride gas and raw material ammonia solid/liquid/gas reactions under vacuum condition for vacuum reactor 1
Body mixture, wherein first solid mixture includes that the raw material silicon tetrachloride gas and the raw material ammonia solid/liquid/gas reactions are raw
At nitrogenous silane compound and ammonium chloride；Specifically, the first charging aperture of vacuum reactor is provided on vacuum reactor 1
11, it is used for raw material ammonia feed；It is additionally provided with the second charging aperture 12 of vacuum reactor on vacuum reactor 1, is used for raw material four
Silicon chloride charging.The tail gas generated after reacting in vacuum reactor 1 is discharged by the top 13 of vacuum reactor.
Heating device is connect with the vacuum reactor 1, and the heating device is closed for being heat-treated the nitrogenous silanization
Object obtains silicon nitride.
Reaction rate in vacuum reactor 1 is controllable, the entrainment of chlorine element is reduced, so as to industrialized production.
The system of production silicon nitride in the present invention substitutes liquid-liquid interface reaction system in the prior art, to reduce
Reaction speed between raw material so that the reaction speed between raw material can control, and does not need to avoid using organic solvent
Subsequent complex separations process, simple process, it is easier to which the large-scale production for realizing nitrogenous silane compound also achieves nitrogen
The large-scale production of SiClx, production capacity is high, and the manufacturing cost of silicon nitride is reduced under the premise of guaranteeing the quality of production silicon nitride.
Preferably, the heating device includes:
Primary heater 2 is connect with the vacuum reactor 1, first solid mixing in the vacuum reactor 1
Object enters the primary heater 2, and the primary heater 2 is used under non-oxidizing atmosphere, and it is mixed to heat first solid
Object is closed, obtains the second solid matter, the ammonium chloride thermally decomposes to generate ammonia and hydrogen chloride, wherein second solid
Substance includes containing the nitrogen silane compound；Heating temperature in primary heater 2 is 500~600 DEG C, is heat-treated 1~2h.Tool
Body, primary heater 2 is connect with the bottom 14 of vacuum reactor, the first solid mixture by vacuum reactor bottom 14 into
Enter in primary heater 2.Non-oxidizing atmosphere is one of inert gas atmosphere, nitrogen atmosphere, ammonia atmosphere, preferably nitrogen
Gas atmosphere.
Secondary heater 3 is connect with the primary heater 2, second solid matter in the primary heater 2
Into in the secondary heater 3, the secondary heater 3 is used under ammonia atmosphere, is heated second solid matter, is obtained
To third solid matter, the third solid matter include thermally decomposed to generate containing the nitrogen silane compound it is unbodied
Silicon nitride；Heating temperature in secondary heater 3 is 650~1200 DEG C, is heat-treated 2~8 hours.Specifically, secondary heater 3
On be provided with the air inlet 31 of secondary heater, for being passed through ammonia.
Third heater 4 is connect with the secondary heater 3, the third solid matter in the secondary heater 3
Into in the third heater 4, the third heater 4 is used under non-oxidizing atmosphere, heats the third solids
Qualitative response, obtains the 4th solid matter, and the 4th solid matter includes that the unbodied silicon nitride is generated by heating
The silicon nitride of high α phase content.The mass percentage content of the silicon nitride of α phase is 90~98% in 4th solid matter, chlorine element
Content < 60ppm.Heating temperature in third heater 4 is 1250~1700 DEG C, is heat-treated 2~8 hours.Non-oxidizing atmosphere
For one or more of inert gas atmosphere, nitrogen atmosphere, ammonia atmosphere, Carbon monoxide reduction atmosphere, preferably nitrogen gas
Atmosphere.
Secondary heater 3 in system and third heater 4 as producing silicon nitride are so that the made from final
The amount of the silicon nitride of α phase in four solid matters is controllable, and the mass percent of the silicon nitride of the α phase in the 4th solid matter contains
Amount is 90~98%.
The system of production silicon nitride in the present invention substitutes liquid-liquid interface reaction system in the prior art, to reduce
Reaction speed between raw material so that the reaction speed between raw material can control, and does not need to avoid using organic solvent
Subsequent complex separations process, simple process, it is easier to which the large-scale production for realizing nitrogenous silane compound also achieves nitrogen
The large-scale production of SiClx, production capacity is high, and the manufacturing cost of silicon nitride is reduced under the premise of guaranteeing the quality of production silicon nitride.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of silicon nitride, which comprises the following steps:
(1) under vacuum conditions, the absolute pressure of the vacuum condition is 10~10000Pa, and silicon tetrachloride gas and ammonia are anti-
Nitrogenous silane compound should be generated, the reaction temperature of the silicon tetrachloride gas and the ammonia is -20~60 DEG C；
(2) it being heat-treated, obtains silicon nitride, the concrete operations condition of the heat treatment carries out as steps described below,
(m) under ammonia atmosphere, heating, the nitrogenous silane compound, which is decomposed, generates unbodied silicon nitride；The step
Suddenly the heating condition of (m) is specially and is heat-treated 2~8 hours at 650~1200 DEG C；
(n) under non-oxidizing atmosphere, heating, the unbodied silicon nitride undergoes phase transition the nitridation for being changed into high α phase content
Silicon；The heating condition of the step (n) is specially to be heat-treated 2~8 hours at 1250~1700 DEG C.
2. the preparation method of silicon nitride according to claim 1, which is characterized in that in the step (1), four chlorination
Silicon gas and the excessive ammonia reaction generate the nitrogenous silane compound.
3. the preparation method of silicon nitride according to claim 2, which is characterized in that four chlorinations described in the step (1)
The molar ratio of silicon gas and the ammonia is 1:(6~30).
4. the preparation method of silicon nitride according to claim 1, which is characterized in that four chlorinations described in the step (1)
Silicon gas and ammonia reaction also generate by-product ammonium chloride, the step during generating the nitrogenous silane compound
Suddenly further include step (i) between (1) and the step (2) at 500~600 DEG C, be heat-treated 1~2h, remove the by-product chlorine
Change ammonium.
5. the preparation method of silicon nitride according to claim 1, which is characterized in that described non-oxygen in the step (n)
The property changed atmosphere is one or more of inert gas atmosphere, nitrogen atmosphere, ammonia atmosphere, Carbon monoxide reduction atmosphere.
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| 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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| 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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