CN106698436A - Preparation method of high-purity silicon carbide powder - Google Patents
Preparation method of high-purity silicon carbide powder Download PDFInfo
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- CN106698436A CN106698436A CN201710019523.4A CN201710019523A CN106698436A CN 106698436 A CN106698436 A CN 106698436A CN 201710019523 A CN201710019523 A CN 201710019523A CN 106698436 A CN106698436 A CN 106698436A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention belongs to the technical field of new material processing, and provides a brand-new preparation method of high-purity silicon carbide powder. According to the method, high-purity silane and high-purity carbon powder are used as raw materials and matched with a corresponding porous graphite crucible and a graphite tray set to prepare the high-purity silicon carbide powder under the protective atmosphere of inert gas. The method avoids impurities from other substances, and uses the device prepared from pure graphite to perform the reaction, thereby achieving the required conditions for silicon carbide powder production on the premise of ensuring the purity, providing a brand-new way for production of high-purity silicon carbide, and filling up the blank in the prior art.
Description
Technical field
The invention belongs to new material field of crystal processing, and in particular to a kind of preparation method of high-purity silicon carbide powder.
Background technology
Single-crystal silicon carbide is one of most important third generation semi-conducting material, and because it has, energy gap is big, saturated electrons
The excellent properties such as mobility is high, breakdown field is powerful, thermal conductivity is high, and it is widely used in power electronics, radio-frequency devices, photoelectron
The fields such as device.High-purity silicon carbide monocrystalline is to prepare high frequency, the preferred material of HIGH-POWERED MICROWAVES device, but due to high-purity semi-insulating
Single-crystal silicon carbide is high to crystal purity requirement, so single crystal preparation technical difficulty is big, current its technology of preparing is only a small number of states
Family is grasped.The technical difficult points of high-purity semi-insulating silicon carbide monocrystalline purity are the preparations of high-purity silicon carbide raw material.Due to closing
The impurity containing higher concentration into the silica flour and carbon dust in sic raw material, so that making in the sic powder for synthesizing and subsequently
Certain density impurity is inevitably introduced in single-crystal silicon carbide with powder growth, so as to have influence on grown monocrystalline
Purity, as one of technology barriers maximum during high-purity semi-insulating silicon carbide single crystal preparation.
Prepared by current sic powder is mainly realized using self-propagating high-temperature synthetic method.This method is given instead using high temperature
Answer thing initially to generate heat, make it start to produce chemical reaction；As reaction is carried out, unreacted material is under conditions of exothermic heat of reaction
Continue to complete chemical reaction.But the impurity element of high level is usually contained in the silica flour that is used of this kind of method, it is rear
Can be participated in continuous building-up process in reaction, impurity concentration is higher in causing powder；Also, the low melting point of silica flour limits synthesis
High temperature purification treatment before reaction, causes the impurity in growing environment to remove；Additionally, self- propagating method need to generally add volume
Outer assisted reaction agent could maintain to carry out, and inevitably cause the pollution of exogenous impurity.Factors above can cause synthesis
The impurity element with higher concentration is present in sic powder, so as to have influence on the system of follow-up high-purity semi-insulating silicon carbide monocrystalline
It is standby.
The content of the invention
According to deficiency and blank that prior art is present, the present inventor provides a kind of brand-new high-purity silicon carbide
The preparation method of powder, with high purity silane and high-purity carbon dust as raw material, collocation uses corresponding porous graphite earthenware to the method
Crucible and graphite pallet, can obtain the sic powder of high-purity under the protection of inert gas；In this way, it is to avoid
The impurity that other materials are brought into, the utensil prepared by pure graphite is reacted, and before the reaction the phase can carry out environment removal of impurities,
Condition needed for sic powder production has been reached while purity is ensured, for the production of high-purity carborundum powder is provided
A kind of brand-new path, has filled up the blank of prior art.
Concrete technical scheme of the invention is as follows：
A kind of preparation method of high-purity silicon carbide powder, mainly using a kind of brand-new high-purity silicon carbide powder processing unit (plant)
Realize, the processing unit (plant) structure is as follows：
Including porous graphite crucible and built-in graphite tray set, if the graphite tray set is by dried layer graphite support disk
Composition, is carried between the graphite pallet by graphite support；Through hole is evenly arranged with the graphite crucible outer wall；
After above-mentioned special equipment is obtained, it is as follows that inventor further provides preparation method：
1. every layer of graphite pallet high-purity carbon dust layering of purity 99.9999% and the above being placed in porous graphite crucible
On, every layer of thickness of carbon dust is 5-15mm, seals burner hearth；
2. burner hearth vacuum is evacuated to 10-6Mbar, while temperature in burner hearth is risen into 1800-2300 DEG C, keeps 5-15h；
3. fire box temperature is delayed and be down to 1500-1800 DEG C, while being passed through inert protective gas, and furnace pressure is risen to
500-900mbar；
4. after boosting terminates, terminate until reacting to high purity silane is continually fed into furnace chamber；
5. in course of reaction, keep the pressure in burner hearth constant, while temperature is slowly increased into 1800-2300 DEG C, make silicon
Alkane is decomposed and fully reacted with high-purity carbon dust, and the reaction time is 100-150h；
6. after reaction terminates, temperature is delayed and is down to room temperature, you can obtain high-purity silicon carbide powder.
Protective gas wherein in step 3 is selected from argon gas or helium, and gas flow is 100-500sccm；
Silane in step 4 is selected from monosilane SiH4Or disilane Si2H6, purity is 99.9999%-99.9999999%；
Using the apparatus and method of above-mentioned offer of the invention, high-purity carbon dust is placed directly within graphite pallet during preparation, often
Carbon dust can be taken up on layer pallet, the utilization rate that improve raw material increased yield, and after selecting high purity silane as raw material,
It enters crucible in a gaseous form, is placed because high-purity carbon dust is layered, and thus considerably increases contact of the silane with carbon dust
Area, is uniformly heated advantageously in the carrying out of reaction, and after layering placement, and it is more thorough that reaction is carried out；
Because crucible employs porous design, through hole, or even crucible body bottom are also provided with its crucible cover and crucible body
Portion can similarly set through hole, so that protective gas and silane can be completely filled with whole reaction crucible, be conducive to anti-
The transmission of the carrying out answered and heat, make that whole reaction carries out is more uniform, and in order to ensure the efficiency of reaction, inventor is by every layer
The thickness control of carbon dust is 5-15mm, and space can be left when being piled up using carbon dust after this thickness, and the silane of gas phase can be allowed to soak
Enter internal layer carbon dust fully to react；And outer layer carbon dust reacts after forming silicon-carbide particle also enter with the silicon components that silane is decomposed to form
One step increases intergranular accumulation hole, so as to ensure the abundant reaction of internal layer carbon dust and silane catabolite；It is simultaneously of the invention
Using in crucible multiple layer tray set also for allow carbon dust pile up be unlikely to blocked up, so as to increase the contact with silicon components
Response area, raising reaction efficiency, while being easy to the separation and acquisition of silicon carbide powder after reaction；
In addition, the present invention replaces silica flour using high purity silane, and high purity silane is with purity higher, and building-up process
Middle flow is controllable, with more preferable operability, can preferably control the carrying out of reaction；
And compared with prior art, another difference of the invention is exactly after using above-mentioned silane, in HIGH-PURITY SILICON
Before alkane is passed through burner hearth, the carbon dust of interior only one of the placing response thing of burner hearth, this is different from silica flour and carbon in traditional synthesis
Powder is put into burner hearth simultaneously.Because the fusing point of silicon only has 1400 DEG C, to prevent silicon components from melting volatilization, can not enter in traditional handicraft
Row early stage high-temperature process (1600 DEG C of ＞) is purified, and is caused a large amount of impurity to remain in burner hearth and is incorporated into synthesis during the course of the reaction
In powder.And in the present invention, the silane that silicon components pass through subsequently to be passed through decomposes offer, carbon dust is only placed before the reaction, therefore
The melting volatilization of silicon need not be considered, fire box temperature can be promoted into more than 1800 DEG C is carried out thoroughly with by high temperature to burner hearth
Purification, so as to reduce influence of the impurity to silicon carbide powder, improves purity；
For the foregoing reasons, before whole reaction is carried out, inventor utilizes high vacuum to whole burner hearth and crucible and pallet
Removal of impurities is carried out with high temperature, the impurity in reactor can so have been removed substantially；
In addition to the above, the other guide in carborundum powder preparation process involved in the present invention, such as heating side
Formula, heat time, growth atmosphere, heating rate and cooldown rate etc., can refer to prior art completion, and inventor is herein no longer
Repeat；
In sum, a kind of preparation method of brand-new high-purity silicon carbide powder is inventor provided, the method is with high-purity
Degree silane and high-purity carbon dust are raw material, and collocation uses corresponding porous graphite crucible and graphite pallet, in the guarantor of inert gas
The lower sic powder that can obtain high-purity of shield；In this way, it is to avoid the impurity that other materials are brought into, by pure stone
Utensil prepared by ink is reacted, and the condition needed for sic powder production has been reached while purity is ensured, is high-purity
The production of sic powder provides a kind of brand-new path, has filled up the blank of prior art.
Brief description of the drawings
Fig. 1 is the structural representation of porous crucible of the present invention；
Fig. 2 is the structural representation of graphite pallet of the present invention；
Structural representation when Fig. 3 is porous crucible of the present invention and pallet is used；
1 is crucible cover in figure, and 2 is crucible body, and 3 is through hole, and 4 is graphite support, and 5 is graphite pallet, and 6 is carbon dust.
Specific embodiment
The present invention is further illustrated below by specific embodiment, it should be understood that, these embodiments are only
It is used for specifically describing in more detail, and is not to be construed as limiting the present invention in any form.
Embodiment 1
A kind of high-purity silicon carbide powder processing unit (plant), the processing unit (plant) structure is as follows：
Including porous graphite crucible and built-in graphite tray set, the porous graphite crucible includes crucible cover 1
With crucible body 2, through hole 3 is provided with the crucible cover 1 and crucible body 2；
If the graphite tray set is made up of dried layer graphite support disk 5, carried by graphite support 4 between the graphite pallet 5；
The layering of high-purity carbon dust 6 is placed on every layer of graphite pallet 5 when using, then every layer of pallet is passed through into graphite support 4 sequentially
It is stacked, and be integrally placed in crucible body 2, cover crucible cover 1.
Embodiment 2
A kind of preparation method of high-purity silicon carbide powder, realizes that specific steps are such as using the process equipment in embodiment 1
Under：
By high-purity carbon dust uniform fold that purity is 99.9999% on the multiple layer tray in crucible, carbon dust thickness is
10mm, pallet then be placed in burner hearth and sealed.Burner hearth is evacuated to 10-6Mbar, while fire box temperature is promoted to
2000 DEG C and keep 5 hours with by high temperature impurity elimination.Then, fire box temperature is down to 1800 DEG C, while with the flow of 100sccm
To high-purity Ar gas is passed through in burner hearth, furnace pressure is set to rise to 800mbar.It it is 79 to purity is passed through in burner hearth after boosting terminates
(99.99999%) high purity silane, keeping temperature and pressure it is constant and make reaction continue 100h.After reaction terminates, by burner hearth certainly
So it is cooled to room temperature, you can obtain the high-purity silicon carbide powder that impurity concentration is less than 1.5ppm, and the carbon synthesized under prior art
In SiClx powder impurity concentration generally 10ppm and more than, it is seen that the silicon carbide powder purity that is obtained of the present invention is than existing
Technology is greatly improved.
Embodiment 3
A kind of preparation method of high-purity silicon carbide powder, realizes that specific steps are such as using the process equipment in embodiment 1
Under：
By high-purity carbon dust uniform fold that purity is 99.9999% on the multiple layer tray in crucible, carbon dust thickness is
12mm, pallet then be placed in burner hearth and sealed.Burner hearth is evacuated to 10-6Mbar, while fire box temperature is promoted to
2200 DEG C and keep 10 hours with by high temperature remove burner hearth in impurity element.Then, fire box temperature is down to 1900 DEG C, together
When with the flow of 300sccm to high-purity Ar gas is passed through in burner hearth, furnace pressure is risen to 850mbar.After boosting terminates, to burner hearth
It is the high purity silane of 99 (99.9999999%) to be inside passed through purity, and keeping temperature and pressure are constant and reaction is continued 120h.
After reaction terminates, burner hearth is naturally cooled into room temperature, you can obtain high-purity silicon carbide powder of the impurity concentration less than 1ppm, and show
Have in the sic powder synthesized under technology impurity concentration generally 10ppm and more than, it is seen that the carborundum that the present invention is obtained
Powder purity is greatly improved than prior art.
Claims (4)
1. a kind of preparation method of high-purity silicon carbide powder, it is characterised in that：Comprise the following steps that：
(1) every layer of graphite pallet that be placed in porous graphite crucible for high-purity carbon dust layering of purity 99.9999% and the above by
On, every layer of thickness of carbon dust is 5-15mm, seals burner hearth；
(2) burner hearth vacuum is evacuated to 10 by-6Mbar, while temperature in burner hearth is risen into 1800-2300 DEG C, keeps 5-15h；
(3) is down to 1500-1800 DEG C by fire box temperature is slow, while being passed through inert protective gas, and furnace pressure is risen into 500-
900mbar；
(4) after boostings terminate, terminate until reacting to high purity silane is continually fed into furnace chamber；
(5) in courses of reaction, keep the pressure in burner hearth constant, while temperature is slowly increased into 1800-2300 DEG C, make silane
Decompose and fully reacted with high-purity carbon dust, the reaction time is 100-150h；
(6) after reactions terminate, temperature is delayed and is down to room temperature, you can obtain high-purity silicon carbide powder；
The process equipment concrete structure that it is used is as follows：
Including porous graphite crucible and built-in graphite tray set, the porous graphite crucible include crucible cover (1) and
Crucible body (2), through hole (3) is provided with the crucible cover (1) and crucible body (2)；
If the graphite tray set is made up of dried layer graphite support disk (5), held by graphite support (4) between the graphite pallet (5)
Carry；
High-purity carbon dust (6) layering is placed on every layer of graphite pallet (5) when using, then every layer of pallet is suitable by graphite support (4)
It is secondary stacked, and be integrally placed in crucible body (2), cover crucible cover (1).
2. the preparation method of high-purity silicon carbide powder according to claim 1, it is characterised in that：Protection in step (3)
Gas is selected from argon gas or helium, and gas flow is 100-500sccm.
3. the preparation method of high-purity silicon carbide powder according to claim 1, it is characterised in that：Silane in step (4)
Selected from monosilane SiH4Or disilane Si2H6, purity is 99.9999%-99.9999999%.
4. a kind of process equipment of high-purity silicon carbide powder, it is characterised in that：Concrete structure is as follows：
Including porous graphite crucible and built-in graphite tray set, the porous graphite crucible include crucible cover (1) and
Crucible body (2), through hole (3) is provided with the crucible cover (1) and crucible body (2)；
If the graphite tray set is made up of dried layer graphite support disk (5), held by graphite support (4) between the graphite pallet (5)
Carry.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205625A (en) * | 2017-07-03 | 2019-01-15 | 比亚迪股份有限公司 | A method of preparing silicon carbide powder |
| CN109336114A (en) * | 2018-11-02 | 2019-02-15 | 山东天岳先进材料科技有限公司 | A method of promoting high-purity silicon carbide powder combined coefficient |
| CN109502589A (en) * | 2018-11-12 | 2019-03-22 | 山东天岳先进材料科技有限公司 | A method of preparing high-purity silicon carbide powder |
| CN110950341A (en) * | 2019-12-24 | 2020-04-03 | 山东天岳先进材料科技有限公司 | Silicon carbide powder and preparation method and device thereof |
| CN111056554A (en) * | 2019-12-26 | 2020-04-24 | 山东天岳先进材料科技有限公司 | High-purity silicon carbide powder and preparation method and reactor thereof |
| WO2020087719A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | High purity carbon material prepared using residue from silicon carbide crystal growth, preparation method therefor, and use thereof |
| CN113479889A (en) * | 2021-08-20 | 2021-10-08 | 中电化合物半导体有限公司 | Synthesis method of silicon carbide powder |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205625A (en) * | 2017-07-03 | 2019-01-15 | 比亚迪股份有限公司 | A method of preparing silicon carbide powder |
| CN109205625B (en) * | 2017-07-03 | 2020-12-25 | 比亚迪股份有限公司 | Method for preparing silicon carbide powder |
| CN109336114A (en) * | 2018-11-02 | 2019-02-15 | 山东天岳先进材料科技有限公司 | A method of promoting high-purity silicon carbide powder combined coefficient |
| WO2020087719A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | High purity carbon material prepared using residue from silicon carbide crystal growth, preparation method therefor, and use thereof |
| CN109502589A (en) * | 2018-11-12 | 2019-03-22 | 山东天岳先进材料科技有限公司 | A method of preparing high-purity silicon carbide powder |
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| CN110950341A (en) * | 2019-12-24 | 2020-04-03 | 山东天岳先进材料科技有限公司 | Silicon carbide powder and preparation method and device thereof |
| CN111056554A (en) * | 2019-12-26 | 2020-04-24 | 山东天岳先进材料科技有限公司 | High-purity silicon carbide powder and preparation method and reactor thereof |
| CN111056554B (en) * | 2019-12-26 | 2021-09-14 | 山东天岳先进科技股份有限公司 | High-purity silicon carbide powder and preparation method and reactor thereof |
| CN113479889A (en) * | 2021-08-20 | 2021-10-08 | 中电化合物半导体有限公司 | Synthesis method of silicon carbide powder |
| CN113479889B (en) * | 2021-08-20 | 2022-12-09 | 中电化合物半导体有限公司 | Synthesis method of silicon carbide powder |
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