CN107285287A - The production method and beta phase silicon nitride of a kind of beta phase silicon nitride - Google Patents
The production method and beta phase silicon nitride of a kind of beta phase silicon nitride Download PDFInfo
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- CN107285287A CN107285287A CN201610205705.6A CN201610205705A CN107285287A CN 107285287 A CN107285287 A CN 107285287A CN 201610205705 A CN201610205705 A CN 201610205705A CN 107285287 A CN107285287 A CN 107285287A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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Abstract
The invention discloses a kind of production method of beta phase silicon nitride and beta phase silicon nitride, this method comprises the following steps：Raw silicon and nitrogen are passed at least fluidized bed plant of two-stage series connection and reacted, reaction temperature is 1281~1600 DEG C, obtains beta phase silicon nitride.Raw silicon and nitrogen are passed at least fluidized bed plant of two-stage series connection in the present invention and reacted at 1281~1600 DEG C, by the fluidized bed plant of plural serial stage so as to extend the residence time of raw silicon and nitrogen in it, so as to improve the time of contact of raw silicon and nitrogen, be conducive to the extension reaction time to improve reaction efficiency, further increase the yield of the beta phase silicon nitride of generation.Preparation method of the invention is simple, performance is controllable and with short production cycle, significantly reduces production cost, is adapted to large-scale industrial production.
Description
Technical field
The invention belongs to technical field of polysilicon production, and in particular to a kind of beta phase silicon nitride
Production method and beta phase silicon nitride.
Background technology
The advantage that silicon nitride is protruded includes that high mechanical strength, heat endurance be good, chemical property
It is stable, these advantages cause it be widely applied to metallurgy, machinery, the energy, chemical industry,
Semiconductor, Aero-Space, auto industry, Nuclear Power Engineering and engineering in medicine field, nitrogen
SiClx fully meets high temperature, high speed, strong corrosive medium and the height that modern technologies are frequently encountered
The working environment of abrasion, and long working life, technical performance are stable, can be closed with high temperature
Gold matches in excellence or beauty, and application effect is satisfactory.Constantly expand with the application of silicon nitride material
Greatly, high-performance, the preparation of the beta-silicon nitride powder of low cost increasingly cause the attention of people.
But want to obtain the silicon nitride ceramic material of function admirable it may first have to prepare
Go out the beta-silicon nitride powder of high-quality.The main preparation methods of current beta-silicon nitride powder have directly
Nitriding, carbon carbothermic method, ammonolysis process, plasma (orifice) gas phase synthesi PCVD, heat
There is larger difference in decomposition method, beta-silicon nitride powder product quality prepared by distinct methods.
Crystal content is also different in powder simultaneously.
Relative to the various production methods of silicon nitride, the letter of the direct nitridation method technological process of production
Single, production cost is relatively low, and the quality of production silicon nitride product disclosure satisfy that extensive engineer applied
Requirement, while Direct-Nitridation silica flour process does not have byproduct.But conventional direct nitridation method
There is big production cycle length, labor intensity, low production efficiency, intermittent life in production technology
There is pollution environment and occupational health infringement in production, product quality homogeneity is poor etc. a series of
Problem.
The content of the invention
The technical problems to be solved by the invention be for present in prior art it is above-mentioned not
Foot passes through multistage string there is provided a kind of production method of beta phase silicon nitride and beta phase silicon nitride
The fluidized bed plant of connection so as to extend the residence time of raw silicon and nitrogen in it, from
And the time of contact of raw silicon and nitrogen is improved, be conducive to the extension reaction time to improve anti-
Answer efficiency.
The technical scheme that solution present invention problem is used is to provide a kind of β phases and nitrogenized
The production method of silicon, comprises the following steps：
Raw silicon and nitrogen are passed at least fluidized bed plant of two-stage series connection and carried out instead
Should, reaction temperature is 1281~1600 DEG C, obtains beta phase silicon nitride.
Preferably, the fluidized bed plant is 2~10 grades of series connection.
Preferably, the fluidized bed plant is 3 grades of series connection.
Preferably, the pressure in the fluidized bed plant is 0~100KPag.
Preferably, the reaction time in every grade of fluidized bed plant of series connection is
60~600 seconds.
Preferably, the particle diameter of the silicon is 1~100 μm.
Preferably, being also passed through in the fluidized bed plant during reaction to separate
Or the auxiliary material of evacuation silicon solid phase.
Preferably, the auxiliary material is beta phase silicon nitride.The auxiliary material has separation or evacuated
The effect of silicon solid phase, it is to avoid the generation of accessory substance, so as to further be conducive to β phases
The raising of the yield of silicon nitride.
It is further preferred that the particle diameter of the auxiliary material is more than the particle diameter of the raw silicon.
Preferably, the mass ratio of the silicon and the auxiliary material is (10:1)~(1:10).
Preferably, the fluidized bed plant of at least two-stage series connection is independent by least two
Fluid bed be in series and/or the body of heater of the fluidized bed plant in be provided with least one
Deflector, the deflector is used to the body of heater being divided into interconnect at least
Two sub- bodies of heater.
The present invention provides a kind of beta phase silicon nitride, and it is produced by above-mentioned method.
Raw silicon and nitrogen are passed into the fluidized bed plant of at least two-stage series connection in the present invention
It is interior to be reacted at 1281~1600 DEG C, by the fluidized bed plant of plural serial stage so as to extend
The residence time of raw silicon and nitrogen in it, so as to improve connecing for raw silicon and nitrogen
The reaction rate of the time of touching, control silicon and nitrogen, is conducive to the extension reaction time to improve anti-
Efficiency is answered, shortens the production cycle, further increases the yield of the beta phase silicon nitride of generation
And homogeneity.Preparation method of the invention is simple, performance is controllable and with short production cycle,
Production cost is significantly reduced, is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is that the structure of the system of the production beta phase silicon nitride in the embodiment of the present invention 2 is shown
It is intended to；
Fig. 2 is that the structure of the system of the production beta phase silicon nitride in the embodiment of the present invention 3 is shown
It is intended to.
In figure：1- crushing and screening devices；11- roller-crushing mills；12- feed bins；13- screening machines；
14- feeders；2- processes mixing device；21- airslide disintegrating mills；22- auxiliary materials storehouse；3- is supplied
Device；31- preheaters；32- air inlet pipe；33- flow controllers；4- fluidized bed plants；
401- fluid beds；402- bodies of heater；403- deflectors；404- temperature elements；405- first
Sub- body of heater；The sub- bodies of heater of 406- second；407- first entrances；408- second entrances；409- goes out
Mouthful；410- heating plates；411- deflectors；5- cooling devices；51- cooling tubes；52- is fed
Pipe；6- separators；61- bags of filter separators；62- air-introduced machines.
Embodiment
To make those skilled in the art more fully understand technical scheme, tie below
The drawings and specific embodiments are closed to be described in further detail the present invention.
Embodiment 1
The present embodiment provides a kind of production method of beta phase silicon nitride, comprises the following steps：
Raw silicon and nitrogen are passed at least fluidized bed plant of two-stage series connection and carried out instead
Should, reaction temperature is 1281~1600 DEG C, obtains beta phase silicon nitride.
The fluid bed that raw silicon and nitrogen are passed into at least two-stage series connection in the present embodiment is filled
Reacted in putting at 1281~1600 DEG C, by the fluidized bed plant of plural serial stage so as to extend
The residence time of raw silicon and nitrogen in it, so as to improve raw silicon and nitrogen
The reaction rate of time of contact, control silicon and nitrogen, is conducive to the extension reaction time to improve
Reaction efficiency, shortens the production cycle, further increases the production of the beta phase silicon nitride of generation
Rate and homogeneity.
Embodiment 2
As shown in figure 1, the present embodiment provides a kind of production method of beta phase silicon nitride, bag
Include following steps：
By the auxiliary material silicon nitride that silica flour, nitrogen, particle diameter that particle diameter is 1 μm are 20 μm
Be passed into the fluidized bed plant 4 of two-stage tandem and reacted, wherein, the silica flour and
The mass ratio of the auxiliary material is 1：10, the pressure in fluidized bed plant 4 is 50KPag,
Reaction temperature is 1400 DEG C, and the reaction time in every grade of fluidized bed plant 4 of series connection is
600 seconds, obtain beta phase silicon nitride.The auxiliary material can separate or evacuate silicon solid phase.Institute
State auxiliary material silicon nitride have separate or evacuation silicon solid phase effect, it is to avoid accessory substance
Generation, so as to further be conducive to the raising of the yield of beta phase silicon nitride.
The fluid bed that raw silicon and nitrogen are passed into at least two-stage series connection in the present embodiment is filled
Put in 4 and reacted at 1400 DEG C, by the fluidized bed plant 4 of plural serial stage so as to extend
The residence time of raw silicon and nitrogen in it, so as to improve raw silicon and nitrogen
The reaction rate of time of contact, control silicon and nitrogen, is conducive to the extension reaction time to improve
Reaction efficiency, shortens the production cycle, further increases the production of the beta phase silicon nitride of generation
Rate and homogeneity.
Preferably, the fluidized bed plant 4 of at least two-stage series connection is only by least two
Vertical fluid bed 401 be in series and/or the body of heater 402 of the fluidized bed plant 4 in set
At least one deflector 403 is equipped with, the deflector 403 is used for the body of heater
402 are divided into the sub- body of heater of at least two interconnected.
Specifically, the system of production beta phase silicon nitride includes：
Crushing and screening device 1, for carrying out crushing and screening to silica flour；
Mixing device 2 is processed, for carrying out batch mixing, processing mixing device 2 includes being used for
Carry out the broken airslide disintegrating mill 21 of air-flow and be arranged on the airslide disintegrating mill 21
Auxiliary material storehouse 22, airslide disintegrating mill 21 is connected with the crushing and screening device 1, auxiliary material storehouse
22 are used to auxiliary material being added in airslide disintegrating mill 21 so that silica flour is mixed with auxiliary material；It is excellent
Choosing, auxiliary material storehouse 22 is disposed proximate in the exit of airslide disintegrating mill 21, and is leaned on
Nearly fluidized bed plant 4, so may be such that entrance enters airslide disintegrating mill by auxiliary material storehouse 22
Auxiliary material in 21 hardly passes through airslide disintegrating mill 21, but auxiliary material but can be very good with
Silica flour in airslide disintegrating mill 21 is mixed.The high velocity impact in airslide disintegrating mill, has
Beneficial to the uniformity of raising mixing, and then improve the uniformity of subsequent reactions.
Feeder 3, is connected with fluidized bed plant 4, and feeder 3 is used for fluidisation
Nitrogen is passed through in bed apparatus 4；
Fluidized bed plant 4, is connected with airslide disintegrating mill 21, fluidized bed plant 4 be used for into
Row reaction.Specifically, silica flour, nitrogen, auxiliary material can be passed into fluidized bed plant 4,
Silica flour is used to separating or evacuating silicon solid phase, prevented with nitrogen reaction generation silicon nitride, auxiliary material
When only silica flour reacts with nitrogen, silica flour conglomeration.
Cooling device 5, is connected with feeder 3, and cooling device 5 is used to cool down from stream
Change the mixture that bed apparatus 4 comes out；
Separator 6, is connected with cooling device 5, and the separator 6 is used to separate
Mixture, by the silicon nitride and nitrogen separation in mixture.
Device 1 crushes qualified silicon powder particle and added by auxiliary material storehouse 22 after crushing and screening
Auxiliary material is admitted to fluidized bed plant 4 after being well mixed in processing mixing device 2, with being supplied
The unstripped gas that device of air 3 is heated, is reacted in fluidized bed plant 4, reacted
Gas-solid phase mixture carries out cooling down in cooling device 5, eventually passes separator
6 separated after pack.
Silica flour used refers to polycrystalline silicon rod particle diameter produced by shattering process in the present embodiment
0.1-10mm silicon powder particle, and polysilicon are produced during vapor deposition reaction
The grade amorphous silica flour of superfine nano.
Described crushing and screening device 1 includes being used to carry out broken roller-crushing mill 11, be used for
The feed bin 12 fed into roller-crushing mill 11, the screening machine 13 being connected with roller-crushing mill 11, point
Not Lian Jie screening machine 13 and feed bin 12 feeder 14.Specifically, described broken sieve
Particle diameter 0.1-10mm silicon powder particle is delivered to roller-crushing mill 11 by separating device 1 from feed bin 12,
Roller-crushing mill 11 controls broken particle diameter extremely by adjusting the emery wheel gap of roller-crushing mill 11
Between 0.05-5mm.Silica flour after broken is separated into screening machine 13, is not broken
It is broken to 0.05-5mm silica flour and delivers to feed bin 12 by the way that the feeder 14 of vacuum is again counter,
Second-time breakage is carried out, qualified silica flour then enters processing mixing device 2.Crushing and screening device
1 includes polyurethane, resistance to nanotesla, zirconium oxide, porcelain with the material of the liner of material contact portion
One or more in corundum, silicon nitride.The feeder 14 of crushing and screening device 1 has
Automatic charging function, production process can realize continuous and automatic, whole closed, prevent powder
Dirt leaks pollution.
Processing the material of mixing device 2 and the liner of material contact portion includes polyurethane,
One or more in resistance to nanotesla, zirconium oxide, porcelain corundum, silicon nitride.The processing is mixed
Material device 2 is that the silicon powder particle that can not further refine conventional roller-crushing mill 11 passes through at a high speed
The form of collision is refined again, while carrying out silica flour and auxiliary material under stream condition
Uniform mixing.The qualified silica flour of particle diameter enters after broken described in crushing and screening device 1
The auxiliary material for entering airslide disintegrating mill 21 with entering from auxiliary material storehouse 22 is mixed.The auxiliary material
It is to add auxiliary material in proportion while silica flour enters airslide disintegrating mill 21, air-flow crushing
Machine 21 is provided with first charging aperture and second charging aperture, and first charging aperture is used to add silica flour,
Second charging aperture is used to add auxiliary material, and the outlet in auxiliary material storehouse 22 is connected with second charging aperture.
The silica flour size controlling that mutually collision is crushed again under action of high-speed airflow makes at 1 μm
Obtain powder raw material up to standard and fluidized bed plant 4 is delivered to by delivery pipe.
Described fluidized bed plant 4 includes body of heater 402, is arranged at the outer layer of body of heater 402
Insulation body, deflector 403 and temperature element 404, deflector 403 is by body of heater
402 are divided into the sub- body of heater of at least two interconnected, i.e., the first sub- body of heater 405 and second
Sub- body of heater 406.It is provided with the body of heater 402 of fluidized bed plant 4：For being passed through solids
The first entrance 407 of material；Second entrance 408 for being passed through gas；Outlet 409；Plus
Hot plate 410, the heating plate 410 is that gas phase divides equally heating plate 410, and gas phase divides equally heating plate
410 be cellular heating plate 410.Specifically, the deflector 403 in the present embodiment enters
The silica flour of fluidized bed device 4 is under the drive of nitrogen in fluidized state in body of heater 402
Motion, by the throughput size for adjusting each position so that the powder of fluidisation shape is from first
Sub- body of heater 405 is slowly moved after deflector 403 to the second sub- body of heater 406, is being moved
Silica flour grain is gradated as beta phase silicon nitride powder in dynamic process.
The material of body of heater 402 of fluidized bed plant 4 includes Cr23Ni13、Cr17Ni12Mo2、
Cr19Ni10、Cr19Mo2One or more in NbTi.
The insulation body material includes high temperature insulating carbon felt, mullite, ceramic fibre
One or more in felt, calcium silicate board with microporous.
The gas phase divides equally heating plate 410 for cellular heating plate 410, by body of heater 402
Entrance enter material through gas phase divide equally heating plate 410 divide equally hole enter body of heater 402,
Gas phase divides equally workpiece of the heating plate 410 for intensity height, high temperature resistant and good heat conductivity,
Its material includes the one or more in aluminum oxide, silicon nitride, aluminium nitride, graphite block.
Preferably, the body of heater 402 is divided into what is interconnected by deflector 403
2~10 sub- bodies of heater, silica flour can fully react during flowing, be fully converted to
Beta phase silicon nitride powder.
Preferably, the deflector 403 includes at least one deflector 411, institute
State deflector 411 to be arranged in the cylindrical sidewall of body of heater 402, the deflector 411 is handed over
Mistake is set, so that the circulation passage of forming curves so that material flows in body of heater 402
Resistance is formed, so that flowing velocity is reduced, when improving stop of the material in body of heater 402
Between.
As shown in figure 1, specifically, the system of production beta phase silicon nitride is filled including fluid bed
4 are put, the fluidized bed plant 4 includes a fluid bed 401, the body of heater 402 of fluid bed 401
A deflector 403 is inside provided with, body of heater 402 is divided into mutually by the deflector 403
Two sub- bodies of heater being connected, by the outlet 409 of first entrance 407 to fluid bed 401
Arrangement is the first sub- body of heater 405, the second sub- body of heater 406 successively, and the fluidized bed plant 4 is
The single unit system of two-stage tandem, wherein, deflector 403 includes two deflectors 411,
Deflector 411 is arranged in the cylindrical sidewall of body of heater 402, and the Vertical Square in body of heater 402
It is arranged alternately above and below, so that the circulation passage of forming curves, same deflector 403
Adjacent two deflector 411 between level interval be path length in the tubular of body of heater 402
The 1/5~1/2 of degree, one end of deflector 411 is arranged on the inwall of body of heater 402, deflector
411 other end is path length in the tubular of body of heater 402 with the hollow distance of the inwall of body of heater 402
The 1/5~1/2 of degree.Material sets up bed respectively in the two sub- bodies of heater, in the work of nitrogen
State is fluidized with lower formed, and is reacted.Tandem is realized in the effect of deflector 403
Fluidized bed plant 4, changes the flow direction of material so that material is built in different sub- bodies of heater respectively
Vertical bed, by the fluidized bed plant 4 of two-stage series connection so as to extend raw silicon and nitrogen
Residence time in it, so as to improve the time of contact of raw silicon and nitrogen, favorably
Reaction efficiency is improved in the extension reaction time, the beta phase silicon nitride of generation is further increased
Yield.Silica flour, nitrogen, additive set up bed into the first sub- body of heater 405, build
Vertical fluidisation state, silica flour and nitrogen reaction generation silicon nitride, obtain gas-solid phase fluid, pass through
Fluid velocity declines after deflector 403, reacted silicon nitride and unreacted silica flour
Mixture falls into the sub- body of heater 406 of follow-up second, and sets up bed, then the nitrogen with being passed through
Gas sets up fluidisation state, continues to react, terminates until reacting, finished product discharge.
Described feeder 3 include preheater 31, with entering that fluidized bed plant 4 is connected
Tracheae 32, and the flow controller 33 being arranged in air inlet pipe 32, preheater 31 are used
Preheated in the nitrogen to being passed through air inlet pipe 32, flow controller 33 uses single loop
Flowmeter is controlled to carry out the regulation of nitrogen flow.When in the body of heater 402 of fluidized bed plant 4
At least one deflector 403 is provided with, the deflector 403 is used for the body of heater
402 are divided into the sub- body of heater of at least two interconnected, then along close to body of heater 402
Entrance to the entrance for being gradually distance from body of heater 402 direction arrange sub- body of heater in nitrogen
Flow is gradually decreased in gradient.Specifically, the total flow of the nitrogen in body of heater 402 is
1~50Nm3/ h, the air velocity of nitrogen is 0.1~3m/min.
The air inlet pipe 32 of the feeder 3 is connected with fluid bed 401, air inlet pipe
32 quantity are 2~20, are evenly distributed on the bottom of fluid bed 401.
The preheater 31 of described feeder 3 include electric heater, microwave applicator,
One or more in plasma heater.
The feeder 3 by the gas at normal temperature from public auxiliary engineering be preheated to 200 DEG C~
600 DEG C, heated gas includes nitrogen and/or is not involved in reacting but plays stable reaction speed
The auxiliary gas of rate, auxiliary gas bag includes hydrogen, argon gas.
Described cooling device 5 includes being used to be passed through the cooling tube 51 that refrigerant is cooled down,
Feed pipe 52 for being passed through material, cooling tube 51 and the transmission of heat by contact of feed pipe 52.It is cold
But the material of device 5 and the liner of material contact portion includes polyurethane, resistance to nanotesla, oxygen
Change the one or more in zirconium, porcelain corundum, silicon nitride.Specifically, cooling device 5 makes
The reactant of vapor solid is cooled down with recirculated water, the reactant of the vapor solid after cooling
Temperature≤100 DEG C, are separated into separator 6.
Described separator 6 includes bag and filters separator 61 and connected air-introduced machine
62, preferably described air-introduced machine 62 is high-pressure suction fan, and separator 6 connects with material
The material of the liner of contact portion point includes polyurethane, resistance to nanotesla, zirconium oxide, porcelain corundum, nitrogen
One or more in SiClx.
The effect of the separator 6 is to generate the gas for having neither part nor lot in reaction with reaction
Silicon nitride, unreacted free silica carry out gas-solid phase separation.
The preparation method of the present embodiment is simple, performance is controllable, consecutive production, without powder
Leak, and it is with short production cycle, production cost is significantly reduced, is adapted to large-scale industry
Metaplasia is produced.
By producing the superfine silicon nitride powder that the systematic collection of beta phase silicon nitride is arrived, through X
X ray diffraction analysis x is：Beta phase silicon nitride accounting is up to more than 92wt%, total metal contents in soil
In below 50ppm, contents of free si is in below 0.2wt%.
Embodiment 3
As shown in Fig. 2 the present embodiment provides a kind of production method of beta phase silicon nitride, bag
Include following steps：
Particle diameter is passed into thtee-stage shiplock for 60 μm of silica flour, nitrogen, auxiliary material silicon nitride
Fluidized bed plant 4 in reacted, wherein, the quality of the silica flour and the auxiliary material
Than for 10：1, the pressure in fluidized bed plant 4 is 0KPag, and reaction temperature is 1600
DEG C, the reaction time in every grade of fluidized bed plant 4 of series connection is 300 seconds, obtains β
Phase silicon nitride.The auxiliary material can separate or evacuate silicon solid phase.The auxiliary material silicon nitride
With separate or evacuation silicon solid phase effect, it is to avoid the generation of accessory substance, so as to enter
One step is conducive to the raising of the yield of beta phase silicon nitride.
As shown in Fig. 2 the production beta phase silicon nitride used in the production method of the present embodiment
The difference of system and the system in embodiment 2 is：Fluidized bed plant 4 in the present embodiment,
The fluidized bed plant 4 includes three fluid beds 401, and three fluid beds 401 are connected, that is, flowed
Change bed apparatus 4 is thtee-stage shiplock.Material is set up successively in three fluid beds 401 respectively
Bed, forms fluidisation state and is reacted, by the fluidized bed plant 4 of thtee-stage shiplock so that
The residence time of raw silicon and nitrogen in it is extended, so as to improve raw silicon and nitrogen
The reaction rate of the time of contact of gas, control silicon and nitrogen, is conducive to extending the reaction time
Reaction efficiency is improved, shortens the production cycle, further increases the beta phase silicon nitride of generation
Yield and homogeneity.
The preparation method of the present embodiment is simple, performance is controllable, consecutive production, without powder
Leak, and it is with short production cycle, production cost is significantly reduced, is adapted to large-scale industry
Metaplasia is produced.
By producing the superfine silicon nitride powder that the systematic collection of beta phase silicon nitride is arrived, through X
X ray diffraction analysis x is：Beta phase silicon nitride accounting is up to more than 93wt%, total metal contents in soil
In below 45ppm, contents of free si is in below 0.3wt%.
Embodiment 4
The present embodiment provides a kind of production method of beta phase silicon nitride, comprises the following steps：
By the auxiliary material nitridation that silica flour, nitrogen, particle diameter that particle diameter is 100 μm are 200 μm
Silicon, which is passed into the fluidized bed plant 4 of ten grades of series connection, to be reacted, wherein, the silica flour
Mass ratio with the auxiliary material is 5：1, the pressure in fluidized bed plant 4 is 100KPag,
Reaction temperature is 1281 DEG C, and the reaction time in every grade of fluidized bed plant 4 of series connection is
60 seconds, obtain beta phase silicon nitride.The auxiliary material can separate or evacuate silicon solid phase.Institute
State auxiliary material silicon nitride have separate or evacuation silicon solid phase effect, it is to avoid accessory substance
Generation, so as to further be conducive to the raising of the yield of beta phase silicon nitride.
By producing the superfine silicon nitride powder that the systematic collection of beta phase silicon nitride is arrived, through X
X ray diffraction analysis x is：Beta phase silicon nitride accounting is up to more than 91wt%, total metal contents in soil
In below 60ppm, contents of free si is in below 0.2wt%.
Embodiment 5
The present embodiment provides a kind of production method of beta phase silicon nitride, comprises the following steps：
By particle diameter for 80 μm silica flour, nitrogen be passed into Pyatyi series connection fluidized bed plant 4
It is interior to be reacted, wherein, the pressure in fluidized bed plant 4 is 80KPag, reaction temperature
For 1400 DEG C, the reaction time in every grade of fluidized bed plant 4 of series connection is 400 seconds,
Obtain beta phase silicon nitride.The auxiliary material can separate or evacuate silicon solid phase.The auxiliary material
Silicon nitride have separate or evacuation silicon solid phase effect, it is to avoid the generation of accessory substance,
So as to further be conducive to the raising of the yield of beta phase silicon nitride.
By producing the superfine silicon nitride powder that the systematic collection of beta phase silicon nitride is arrived, through X
X ray diffraction analysis x is：Beta phase silicon nitride accounting is up to more than 92wt%, total metal contents in soil
In below 55ppm, contents of free si is in below 0.4wt%.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present
And the illustrative embodiments used, but the invention is not limited in this.For ability
For those of ordinary skill in domain, the situation of spirit and substance of the present invention is not being departed from
Under, various changes and modifications can be made therein, and these variations and modifications are also considered as the present invention's
Protection domain.
Claims (10)
1. a kind of production method of beta phase silicon nitride, it is characterised in that comprise the following steps：
Raw silicon and nitrogen are passed at least fluidized bed plant of two-stage series connection and carried out instead
Should, reaction temperature is 1281~1600 DEG C, obtains beta phase silicon nitride.
2. the production method of beta phase silicon nitride according to claim 1, its feature exists
In the fluidized bed plant is 2~10 grades of series connection.
3. the production method of beta phase silicon nitride according to claim 1, its feature exists
In the pressure in the fluidized bed plant is 0~100KPag.
4. the production method of beta phase silicon nitride according to claim 1, its feature exists
In the reaction time in every grade of fluidized bed plant of series connection is 60~600 seconds.
5. the production method of beta phase silicon nitride according to claim 1, its feature exists
In the particle diameter of the silicon is 1~100 μm.
6. the producer of the beta phase silicon nitride according to Claims 1 to 5 any one
Method, it is characterised in that being also passed through in the fluidized bed plant during reaction to divide
From or evacuation silicon solid phase auxiliary material.
7. the production method of beta phase silicon nitride according to claim 6, its feature exists
In the auxiliary material is beta phase silicon nitride.
8. the production method of beta phase silicon nitride according to claim 6, its feature exists
In the mass ratio of the silicon and the auxiliary material is (10:1)~(1:10).
9. the producer of the beta phase silicon nitride according to Claims 1 to 5 any one
Method, it is characterised in that the fluidized bed plant of at least two-stage series connection is only by least two
Vertical fluid bed be in series and/or the body of heater of the fluidized bed plant in be provided with least one
Individual deflector, the deflector be used for the body of heater is divided into interconnect to
Few two sub- bodies of heater.
10. a kind of beta phase silicon nitride, it is characterised in that it is any by claim 1~9
Method production described in one.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108501250A (en) * | 2018-04-16 | 2018-09-07 | 四川大学 | Air-flow spheroidization reactor and its method for preparing polymer matrix spherical powder material |
| CN110240131A (en) * | 2019-05-13 | 2019-09-17 | 天津炜润达新材料科技有限公司 | A kind of preparation method of silicon nitride |
| CN110743469A (en) * | 2019-11-25 | 2020-02-04 | 成都天保节能环保工程有限公司 | Device for preventing high-temperature reverse connection of fluidized bed to feeder and technological method thereof |
| CN112794295A (en) * | 2021-03-02 | 2021-05-14 | 北京科技大学 | Method and device for continuously synthesizing amorphous/microcrystalline silicon nitride powder under normal pressure |
| CN112813500A (en) * | 2021-02-02 | 2021-05-18 | 北京绿清科技有限公司 | Single-layer multi-furnace melting system |
| CN112923733A (en) * | 2021-02-02 | 2021-06-08 | 北京绿清科技有限公司 | Method for producing silicon carbide by adopting multi-furnace series connection grading melting furnace and special production system |
| CN113003549A (en) * | 2021-03-08 | 2021-06-22 | 昆明理工大学 | Fast preparation of beta-Si by gas-solid reaction3N4And method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108501250A (en) * | 2018-04-16 | 2018-09-07 | 四川大学 | Air-flow spheroidization reactor and its method for preparing polymer matrix spherical powder material |
| CN110240131A (en) * | 2019-05-13 | 2019-09-17 | 天津炜润达新材料科技有限公司 | A kind of preparation method of silicon nitride |
| CN110743469A (en) * | 2019-11-25 | 2020-02-04 | 成都天保节能环保工程有限公司 | Device for preventing high-temperature reverse connection of fluidized bed to feeder and technological method thereof |
| CN112813500A (en) * | 2021-02-02 | 2021-05-18 | 北京绿清科技有限公司 | Single-layer multi-furnace melting system |
| CN112923733A (en) * | 2021-02-02 | 2021-06-08 | 北京绿清科技有限公司 | Method for producing silicon carbide by adopting multi-furnace series connection grading melting furnace and special production system |
| CN112794295A (en) * | 2021-03-02 | 2021-05-14 | 北京科技大学 | Method and device for continuously synthesizing amorphous/microcrystalline silicon nitride powder under normal pressure |
| CN113003549A (en) * | 2021-03-08 | 2021-06-22 | 昆明理工大学 | Fast preparation of beta-Si by gas-solid reaction3N4And method thereof |
| US11602725B2 (en) | 2021-03-08 | 2023-03-14 | Kunming University Of Science And Technology | Device for rapidly preparing beta-Si3N4 by gas-solid reaction, and method thereof |
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