CN106698436B - A kind of preparation method of high-purity silicon carbide powder - Google Patents
A kind of preparation method of high-purity silicon carbide powder Download PDFInfo
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- CN106698436B CN106698436B CN201710019523.4A CN201710019523A CN106698436B CN 106698436 B CN106698436 B CN 106698436B CN 201710019523 A CN201710019523 A CN 201710019523A CN 106698436 B CN106698436 B CN 106698436B
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to new material processing technique fields; inventor provide a kind of preparation method of completely new high-purity silicon carbide powder; this method is using high purity silane and high-purity carbon dust as raw material; collocation uses corresponding porous graphite crucible and graphite tray set, and the sic powder of high-purity can be obtained under the protection of inert gas；In this way, the impurity that other substances are brought into is avoided, the utensil prepared by pure graphite is reacted, and the condition needed for sic powder production has been reached while ensureing purity, a kind of completely new path is provided for the production of high-purity carborundum powder, has filled up the blank of 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, because its with energy gap 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 the preferred material of high frequency, 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, its technology of preparing is only a small number of states at present
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
At the impurity containing higher concentration in the silica flour and carbon dust in sic raw material, thus synthesis sic powder and subsequently make
Certain density impurity is inevitably introduced in the single-crystal silicon carbide grown with powder, to influence grown monocrystalline
Purity becomes one of maximum technical barrier during high-purity semi-insulating silicon carbide single crystal preparation.
Sic powder preparation at present is mainly realized using self-propagating high-temperature synthetic method.This method is given instead using high temperature
It answers object initially to generate heat, it is made to start to generate chemical reaction；As reaction carries out, unreacted substance is under conditions of exothermic heat of reaction
Continue to complete chemical reaction.However the impurity element of high level is usually contained in silica flour used in such method, rear
It can be participated in reaction in continuous building-up process, cause impurity concentration in powder higher；Also, the low melting point of silica flour limits synthesis
High temperature purification processing before reaction, causes the impurity in growing environment that can not remove；In addition, self- propagating method need to usually add volume
Outer assisted reaction agent could maintain to carry out, and inevitably cause the pollution of exogenous impurity.Factors above can lead to synthesis
The impurity element with higher concentration exists in sic powder, to influence the system of follow-up high-purity semi-insulating silicon carbide monocrystalline
It is standby.
Invention content
According to the shortcomings of the prior art and blank, the present inventor provides a kind of completely new high-purity silicon carbide
The preparation method of powder, for this method using high purity silane and high-purity carbon dust as raw material, collocation uses corresponding porous graphite earthenware
Crucible and graphite pallet, can obtain the sic powder of high-purity under the protection of inert gas；In this way, it avoids
The impurity that other substances are brought into, the utensil prepared by pure graphite are reacted, and before the reaction the phase can carry out environment removal of impurities,
The condition needed for sic powder production is reached while ensureing purity, the production for high-purity carborundum powder provides
A kind of completely new path, has filled up the blank of the prior art.
The specific technical solution of the present invention is as follows：
A kind of preparation method of high-purity silicon carbide powder mainly uses a kind of completely new high-purity silicon carbide powder processing unit (plant)
It realizes, 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
It forms, is carried by graphite support between the graphite pallet；It is evenly arranged with through-hole on the graphite crucible outer wall；
After obtaining above-mentioned special equipment, it is as follows that inventor further provides preparation method：
1. high-purity carbon dust layering of 99.9999% or more purity is placed in every layer of graphite pallet in porous graphite crucible
On, the thickness of every layer 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 to 1800-2300 DEG C, keep 5-15h；
3. fire box temperature is delayed and is down to 1500-1800 DEG C, while it being passed through inert protective gas, and furnace pressure is risen to
500-900mbar；
4. after boosting, high purity silane is continually fed into furnace chamber until reaction terminates；
5. in reaction process, keeping the pressure in burner hearth constant, while temperature is slowly increased to 1800-2300 DEG C, making silicon
Alkane is decomposed and is fully reacted with high-purity carbon dust, reaction time 100-150h；
6. after reaction, 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, gas flow 100-500sccm；
Silane in step 4 is selected from monosilane SiH4Or disilane Si2H6, purity 99.9999%-99.9999999%；
Using the device and method of the above-mentioned offer of the present invention, high-purity carbon dust is placed directly on graphite pallet by when preparation, often
Layer pallet on can install carbon dust, the utilization rate for improving raw material increases yield, and select high purity silane as raw material after,
It enters crucible in a gaseous form, is placed since high-purity carbon dust is layered, thus considerably increases contact of the silane with carbon dust
Area is more conducive to the progress of reaction, and is uniformly heated after being layered placement, reacts the more thorough of progress；
Since crucible uses porous design, through-hole or even crucible body bottom are also both provided on crucible cover and crucible body
Through-hole can be similarly arranged in portion, so that protective gas and silane can be completely filled with entire reaction crucible, be conducive to anti-
The transmission of the progress and heat answered makes entirely to react the more uniform of progress, and in order to ensure the efficiency of reaction, inventor is by every layer
The thickness control of carbon dust is 5-15mm, the silane of gas phase can be allowed to soak there are gap when being accumulated using carbon dust after this thickness
Enter internal layer carbon dust fully to react；And reacted with the silicon components that silane is decomposed to form after forming silicon-carbide particle also can be into for outer layer carbon dust
One step increases intergranular accumulation hole, to ensure fully reacting for internal layer carbon dust and silane decomposition product；The present invention simultaneously
Multiple layer tray setting in used crucible is also for allowing carbon dust accumulation to be unlikely to blocked up, to increase the contact with silicon components
Response area improves reaction efficiency, while convenient for the separation and acquisition of silicon carbide powder after reaction；
In addition to this, the present invention replaces silica flour, high purity silane to have higher purity, and building-up process using high purity silane
Middle flow is controllable, has preferably operability, can preferably control the progress of reaction；
And compared with prior art, another difference of the invention is exactly after using above-mentioned silane, in HIGH-PURITY SILICON
Alkane is passed through before burner hearth, and the only carbon dust of one of placing response object in burner hearth, this is different from silica flour and carbon in traditional synthesis
Powder is put into burner hearth simultaneously.It, cannot be into prevent silicon components melting volatilization, in traditional handicraft because the fusing point of silicon only has 1400 DEG C
Row high-temperature process early period (1600 DEG C of ＞) purifies, and causes a large amount of impurity to remain in burner hearth and is introduced into synthesis during the reaction
In powder.And in the present invention, silicon components are decomposed by the silane being subsequently passed through and are provided, and only place carbon dust before the reaction, therefore
Without considering that the melting of silicon is volatilized, fire box temperature can be promoted to 1800 DEG C or more to be carried out thoroughly to burner hearth by high temperature
Purification improves purity to reduce influence of the impurity to silicon carbide powder；
Based on the above reasons, before entire reaction carries out, inventor utilizes high vacuum to entire burner hearth and crucible and pallet
It is cleaned with high temperature, the impurity in reactor can be removed substantially in this way；
In addition to the above, the other content in carborundum powder preparation process according to the present invention, such as heating side
Formula, heating time, growth atmosphere, heating rate and cooling rate etc. can refer to prior art completion, and inventor is herein no longer
It repeats；
In conclusion inventor providing a kind of preparation method of completely new high-purity silicon carbide powder, this method is with high-purity
It is raw material to spend silane and high-purity carbon dust, 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, the impurity that other substances are brought into is avoided, pure stone is passed through
Utensil prepared by ink is reacted, and the condition needed for sic powder production has been reached while ensureing purity, is high-purity
The production of sic powder provides a kind of completely new path, has filled up the blank of the prior art.
Description of the drawings
Fig. 1 is the structural schematic diagram of porous crucible of the present invention；
Fig. 2 is the structural schematic diagram of graphite pallet of the present invention；
Structural schematic diagram when Fig. 3 is porous crucible of the present invention and pallet use；
1 is crucible cover in figure, and 2 be crucible body, and 3 be through-hole, and 4 be graphite support, and 5 be graphite pallet, and 6 be carbon dust.
Specific implementation mode
It is further illustrated the present invention 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 are 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 both provided on the crucible cover 1 and crucible body 2；
If the graphite tray set is made of dried layer graphite support disk 5, carried by graphite support 4 between the graphite pallet 5；
When use by high-purity carbon dust 6 layering be placed on every layer of graphite pallet 5, then by every layer of pallet by 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 purity be 99.9999% high-purity carbon dust uniform fold on the multiple layer tray in crucible, carbon dust thickness is
Then pallet is placed in burner hearth and is sealed by 10mm.Burner hearth is evacuated to 10-6Mbar, while fire box temperature being promoted to
2000 DEG C and keep 5 hours to pass through high temperature impurity elimination.Then, fire box temperature is down to 1800 DEG C, while with the flow of 100sccm
It is passed through high-purity Ar gas into burner hearth, furnace pressure is made to rise to 800mbar.After boosting, it is 79 that purity is passed through into burner hearth
(99.99999%) high purity silane keeps temperature and pressure constant and reaction is made to continue 100h.After reaction, certainly by burner hearth
It is so 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 the prior art
Impurity concentration is usually in 10ppm or more in SiClx powder, it is seen that the silicon carbide powder purity that the present invention is obtained is compared with 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 purity be 99.9999% high-purity carbon dust uniform fold on the multiple layer tray in crucible, carbon dust thickness is
Then pallet is placed in burner hearth and is sealed by 12mm.Burner hearth is evacuated to 10-6Mbar, while fire box temperature being promoted to
2200 DEG C and keep 10 hours with pass through high temperature remove burner hearth in impurity element.Then, fire box temperature is down to 1900 DEG C, together
When high-purity Ar gas is passed through into burner hearth with the flow of 300sccm, so that furnace pressure is risen to 850mbar.After boosting, to burner hearth
It is inside passed through the high purity silane that purity is 99 (99.9999999%), keep temperature and pressure constant and reaction is made to continue 120h.
After reaction, by burner hearth cooled to room temperature, you can obtain impurity concentration and be less than the high-purity silicon carbide powder of 1ppm, and show
There is in the sic powder synthesized under technology impurity concentration usually in 10ppm or more, it is seen that the silicon carbide that the present invention is obtained
Powder purity is greatly improved compared with the prior art.
Claims (3)
1. a kind of preparation method of high-purity silicon carbide powder, it is characterised in that：It is as follows：
(1) high-purity carbon dust layering of 99.9999% or more purity is placed in every layer of graphite pallet in porous graphite crucible by
On, the thickness of every layer 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 to 1800-2300 DEG C, keep 5-15h；
(3), which delays fire box temperature, is down to 1500-1800 DEG C, while being passed through inert protective gas, and furnace pressure is risen to 500-
900mbar；
(4) after boostings, high purity silane is continually fed into furnace chamber until reaction terminates；
(5) it in reaction process, keeps the pressure in burner hearth constant, while temperature is slowly increased to 1800-2300 DEG C, makes silane
It decomposes and is fully reacted with high-purity carbon dust, reaction time 100-150h；
(6) after reaction, temperature is delayed and is down to room temperature, you can obtains high-purity silicon carbide powder；
Its used process equipment 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) is both provided with through-hole (3) on the crucible cover (1) and crucible body (2)；
If the graphite tray set is made of dried layer graphite support disk (5), held by graphite support (4) between the graphite pallet (5)
It carries；
High-purity carbon dust (6) layering is placed on every layer of graphite pallet (5) when use, 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, gas flow 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 99.9999%-99.9999999%.
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| CN109205625B (en) * | 2017-07-03 | 2020-12-25 | 比亚迪股份有限公司 | Method for preparing silicon carbide powder |
| 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 |
| CN109336114B (en) * | 2018-11-02 | 2020-11-20 | 山东天岳先进材料科技有限公司 | Method for improving synthesis efficiency of high-purity silicon carbide powder |
| 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 |
| CN110950341B (en) * | 2019-12-24 | 2021-11-02 | 山东天岳先进科技股份有限公司 | Silicon carbide powder and preparation method and device 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 |
| 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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| CN1038124C (en) * | 1994-07-19 | 1998-04-22 | 中国科学院金属研究所 | Organic silane laser gas phase synthesis of silica-base micro powder |
| WO2011043425A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Process for production of silicon carbide molded article |
| CN204162831U (en) * | 2014-11-03 | 2015-02-18 | 重庆市亚核保温材料股份有限公司 | The inflatable thermal field of single crystal furnace of a kind of ventilation and heat formula |
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Effective date of registration: 20171204 Address after: 250100 Shandong city of Ji'nan province high tech Zone Xinyu Road West Century wealth center block AB room 1106-6-01 Applicant after: Shandong Tianyue Advanced Material Technology Co., Ltd. Address before: 250118 Shandong province Huaiyin District of Ji'nan city in the middle Mile Lake Applicant before: Shandong Tianyue Crystal Material Co., Ltd. |
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Address after: No.99, Tianyue South Road, Huaiyin District, Jinan City, Shandong Province Patentee after: Shandong Tianyue advanced technology Co., Ltd Address before: Room 1106-6-01, AB Block, Century Fortune Center, West Side of Xinyu Road, Jinan High-tech Zone, Shandong Province Patentee before: Shandong Tianyue Advanced Materials Technology Co.,Ltd. |
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