CN108892513A - A method of silicon carbide powder is prepared using induction furnace - Google Patents
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract
A kind of method preparing silicon carbide powder using induction furnace of the invention, including steps are as follows：Step 1, silicon substrate is consolidated into material progress high-temperature calcination and the processing that pulverizes and sieves, silicon substrate clinker is made；Step 2, according to the ratio, silicon substrate clinker: reducing agent=100: (10~45) mix the two, and ball milling must mix material；Step 3, small size graphite crucible is placed in large scale graphite crucible by (1), and piles natural graphite powder two crucible contact positions；(2) material will be mixed to be placed in small size graphite crucible, and the natural graphite powder sufficient in the covering of small graphite crucible pot cover upper end；(3) large scale graphite crucible is placed in induction furnace coil, at a temperature of 1300~1600 DEG C, 2~5min of heating, which is made, prepares silicon carbide powder using induction furnace.The method achieve the efficient increment material utilizations that silicon substrate is expected admittedly, and operation is simple, is swift in response, and substantially increase production efficiency and product quality, and silicon carbide powder average grain diameter obtained is 0.5~1 μm.
Description
Technical field：
The invention belongs to the nonmetallic resource utilization of industry and ceramic powder material preparation technical fields, and in particular to a kind of
The method for preparing silicon carbide powder using induction furnace.
Background technique：
SiC engineering ceramics is because it is with the excellent properties such as high temperature resistant, anticorrosive, wear-resistant, in metallurgy, chemical industry, aviation boat
The fields such as it are by favor.The acquisition of its excellent performance is largely dependent upon the microstructural fining of sintered body.And it burns
Size, pattern and the distribution situation of the microstructure of knot body and feed particles etc. is closely related.How the powder of high quality is obtained
Key as preparation high-performance SiC engineering material.
Currently, traditional SiC powder preparation method is all solid phase method, and it is the main method of industrial production SiC, is produced
Amount is more than the 90% of total output.It is straight that solid phase method is broadly divided into inferior (Acheson) method of Archie, vertical oven process, high temperature converter process, carbon silicon
Connect reaction method etc..Although solid phase method is industrially widely applied, the quality of its powder is to be improved, and granularity cannot expire with purity
The demand of sufficient high-performance ceramics, and its long preparation period, efficiency are lower.Therefore, the silicon carbide of high quality how is quickly prepared
Powder is an important research direction.
Induction furnace is a kind of industrial furnace of principle heating or melting materialss using electromagnetic induction, because its have heat it is fast
The features such as speed, temperature be high, convenient operation and control, so that material is during heating from pollution, to guarantee the quality of product.
Therefore, free of contamination silicon carbide powder can be quickly prepared using induction furnace, had not only improved the quality of silicon carbide powder, but also mentioned
High production efficiency, substantially reduces the production cycle.
Summary of the invention：
The purpose of the present invention is overcoming above-mentioned the shortcomings of the prior art, provides and a kind of prepare silicon carbide using induction furnace
The method of powder.The master operation of this method is as follows：It is pre-processed firstly, silicon substrate is consolidated material, clinker is made；Then, root
Suitable reducing agent is mixed according to the component that silicon substrate is expected admittedly, mixture is uniformly mixed；Finally, production graphite crucible device, by one
The mixture for determining quality is placed in graphite crucible, and silicon carbide powder is made in sensed furnace under the conditions of burying carbon.
To achieve the above object, the present invention uses following technical scheme：
A method of silicon carbide powder being prepared using induction furnace, is carried out according to the following steps：
Step 1：Pretreatment of raw material
Silicon substrate is consolidated into material progress high-temperature calcination and the processing that pulverizes and sieves, silicon substrate clinker is made；
Step 2：Mixing
According to the ratio, silicon substrate clinker: reducing agent=100: (10~45) mix the two, and ball milling must mix material；
Step 3：High―temperature nuclei
(1) small size graphite crucible is placed in large scale graphite crucible, and piles natural stone two crucible contact positions
Ink powder；
(2) material will be mixed to be placed in small size graphite crucible, and the day sufficient in the covering of small graphite crucible pot cover upper end
Right graphite powder.
(3) large scale graphite crucible is placed in induction furnace coil, heating, which is made, prepares silicon carbide powder using induction furnace；
Wherein, 1300~1600 DEG C of the heating temperature, 2~5min of heating time.
In the step 1, the silicon substrate is expected admittedly for crystalline silicon cutting waste material, iron ore tailings, gangue, fine coal
One of ash, clay, alabaster, andalusite or sillimanite are a variety of.
In the step 1, processing is calcined and pulverized and sieved for removing the impurity in industrial silicon substrate waste residue.
In the step 1, the calcination operation carries out in calcining furnace, and calcination temperature is 900 DEG C, and calcination time is
5h, the calcining furnace are in box resistance wire furnace, silicon carbide rod furnace, Si-Mo rod furnace and the tunnel oven used under unprotect atmosphere
One kind.
In the step 1, the treatment process that pulverizes and sieves is：Using jaw crusher pulverization process, powder warp
After 200 meshes, silicon substrate clinker is made.
In the step 2, the reducing agent is carbonaceous material, be one of carbon black, fat coal or active carbon or
It is a variety of.
In the step 2, the reducing agent dosage should be higher than that silicon substrate in expecting admittedly containing SiO2, Si principal component and metallic iron
The consumption that the impurity components such as oxide are reacted with reducing agent.
In the step 2, the silicon substrate clinker and the reducing agent equipment that ball milling uses together for planetary ball mill,
With 200~400rmin-15~8h of revolving speed unidirectional operation.
In the step 3 (1), the height of the small size graphite crucible is lower than large scale graphite crucible.
In the step 3 (2), the mixing material additive amount is subject to not higher than the 1/3 of small graphite crucible volume.
In the step 3 (3), the induction coil is copper coil, guarantees that large scale graphite crucible is placed in copper coil
It is interior, and make large scale graphite crucible and 1~2cm of copper coil distance.
In the step 3 (3), silicon carbide powder average grain diameter obtained is 0.5~1 μm.
In the step 3 (3), the induction furnace is in intermediate frequency furnace, power frequency induction furnace or vaccum sensitive stove
It is a kind of.
Beneficial effects of the present invention：
1. a kind of method for preparing silicon carbide powder using induction furnace of the invention realizes the efficient synthesis that silicon substrate is expected admittedly
It utilizes, while quickly preparing high quality silicon carbide powder, can also increase substantially the utilization rate and add that silicon substrate is expected admittedly
Value, especially solution silicon substrate solid waste give environment bring pollution problem.
2. it is of the invention it is a kind of using induction furnace prepare the method for silicon carbide powder operation is simple, be swift in response, greatly
Production efficiency is improved greatly.
3. a kind of method for preparing silicon carbide powder using induction furnace of the invention, the incorporation of preparation process free from admixture, are convenient for
Prepare the silicon carbide powder of high quality.
Detailed description of the invention：
Fig. 1 is the process flow chart for the method that the embodiment of the present invention 1~3 prepares silicon carbide powder using induction furnace；
Fig. 2 is silicon carbide powder XRD diagram prepared by the embodiment of the present invention 1；
Fig. 3 is silicon carbide powder XRD diagram prepared by the embodiment of the present invention 2；
Fig. 4 is silicon carbide powder XRD diagram prepared by the embodiment of the present invention 3.
Specific embodiment：
Below with reference to embodiment, the present invention is described in further detail.
For the small size graphite crucible diameter used in following embodiment for 40mm, large scale graphite crucible diameter is 70mm.
The height of small size graphite crucible is lower than large scale graphite crucible.
In the step 3 (2), the mixing material additive amount is subject to not higher than the 1/3 of small graphite crucible volume
As shown in Figure 1, a kind of method that silicon carbide powder is prepared using induction furnace.
Embodiment 1
A method of preparing silicon carbide powder using induction furnace, process flow chart as shown in Figure 1, according to the following steps into
Row：
Step 1：Pretreatment of raw material
Crystalline silicon cutting waste material is placed in box resistance wire furnace, 5h is calcined at 900 DEG C, then through jaw crusher crushing at
Reason, powder remove polyethylene glycol and water through 200 meshes, silicon substrate clinker are made；
Step 2：Mixing
With 100：10 quality proportioning configures silicon substrate clinker and active carbon, two substances is placed in planetary ball mill and are filled
Divide mixing, ball milling speed 400rmin-1, unidirectional operation 5h obtains mixing material；
Step 3：High―temperature nuclei
(1) a small size graphite crucible is placed in large scale graphite crucible, and piles day two crucible contact positions
Right graphite powder；
(2) the 7g powder mixed is placed in small size graphite crucible, and sufficient in the covering of graphite crucible pot cover upper end
Natural graphite powder.
(3) large scale graphite crucible is placed in copper coil to and is not contacted copper coil, large scale graphite crucible and copper coil
1~2cm of distance is allowed to induction furnace rapid synthesizing silicon carbide powder in 2 minutes, and incuding furnace temperature at this time is about 1300 degree, system
It is as shown in Figure 2 to obtain silicon carbide powder XRD diagram.
Through detecting, the main object of gained silicon carbide powder is mutually 6H-SiC, C (graphite), a small amount of SiO2, and synthetic powder
Average grain diameter be 0.5 μm.
Embodiment 2
A method of preparing silicon carbide powder using induction furnace, process flow chart as shown in Figure 1, according to the following steps into
Row：
Step 1：Pretreatment of raw material
Crystalline silicon cutting waste material is placed in box resistance wire furnace, 5h is calcined at 900 DEG C, then through jaw crusher crushing at
Reason, powder remove polyethylene glycol and water through 200 meshes, silicon substrate clinker are made；
Step 2：Mixing
With 100：25 quality proportioning configures silicon substrate clinker and active carbon, two substances is placed in planetary ball mill and are filled
Divide mixing, ball milling speed 400rmin-1, unidirectional operation 5h obtains mixing material；
Step 3：High―temperature nuclei
(1) a small size graphite crucible is placed in large scale graphite crucible, and piles day two crucible contact positions
Right graphite powder；
(2) the 7g powder mixed is placed in small size graphite crucible, and sufficient in the covering of graphite crucible pot cover upper end
Natural graphite powder.
(3) large scale graphite crucible is placed in copper coil to and is not contacted copper coil, large scale graphite crucible and copper coil
1~2cm of distance is allowed to induction furnace rapid synthesizing silicon carbide powder in 2 minutes, and incuding furnace temperature at this time is about 1300 degree, system
It is as shown in Figure 3 to obtain silicon carbide powder XRD diagram.
Through detecting, the object of gained silicon carbide powder is mutually 6H-SiC, C (graphite), no SiO2, and the average grain of synthetic powder
Diameter is 0.5 μm.
Embodiment 3
A method of preparing silicon carbide powder using induction furnace, process flow chart as shown in Figure 1, according to the following steps into
Row：
Step 1：Pretreatment of raw material
Crystalline silicon cutting waste material is placed in box resistance wire furnace, 5h is calcined at 900 DEG C, then through jaw crusher crushing at
Reason, powder remove polyethylene glycol and water through 200 meshes, silicon substrate clinker are made；
Step 2：Mixing
With 100：45 quality proportioning configures silicon substrate clinker and active carbon, two substances is placed in planetary ball mill and are filled
Divide mixing, ball milling speed 400r.min-1, unidirectional operation 5h obtains mixing material；
Step 3：High―temperature nuclei
(1) a small size graphite crucible is placed in large scale graphite crucible, and piles day two crucible contact positions
Right graphite powder；
(2) the 7g powder mixed is placed in small size graphite crucible, and sufficient in the covering of graphite crucible pot cover upper end
Natural graphite powder.
(3) large scale graphite crucible is placed in copper coil to and is not contacted copper coil, large scale graphite crucible and copper coil
1~2cm of distance is allowed to induction furnace rapid synthesizing silicon carbide powder in 5 minutes, and incuding furnace temperature at this time is about 1600 degree, carbon
SiClx powder XRD diagram is as shown in Figure 4.
Through detecting, the object of gained silicon carbide powder is mutually β-SiC, and the average grain diameter of synthetic powder is 1 μm.
Claims (10)
1. a kind of method for preparing silicon carbide powder using induction furnace, which is characterized in that carry out according to the following steps：
Step 1：Pretreatment of raw material
Silicon substrate is consolidated into material progress high-temperature calcination and the processing that pulverizes and sieves, silicon substrate clinker is made；
Step 2：Mixing
According to the ratio, silicon substrate clinker: reducing agent=100: (10~45) mix the two, and ball milling must mix material；
Step 3：High―temperature nuclei
(1) small size graphite crucible is placed in large scale graphite crucible, and piles natural graphite powder two crucible contact positions；
(2) material will be mixed to be placed in small size graphite crucible, and the natural stone sufficient in the covering of small graphite crucible pot cover upper end
Ink powder；
(3) large scale graphite crucible is placed in induction furnace coil, heating, which is made, prepares silicon carbide powder using induction furnace；Its
In, 1300~1600 DEG C of the heating temperature, 2~5min of heating time.
2. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 1, the silicon substrate is expected admittedly for crystalline silicon cutting waste material, iron ore tailings, gangue, flyash, clay, alabaster, andalusite
Or one of sillimanite or a variety of.
3. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 1, processing is calcined and pulverized and sieved for removing the impurity in industrial silicon substrate waste residue.
4. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 1, the calcination operation carries out in calcining furnace, and calcination temperature is 900 DEG C, calcination time 5h, and the calcining furnace is
One of box resistance wire furnace, silicon carbide rod furnace, Si-Mo rod furnace and tunnel oven for being used under unprotect atmosphere.
5. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 1, the treatment process that pulverizes and sieves is：Using jaw crusher pulverization process, silicon substrate is made after 200 meshes in powder
Clinker.
6. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 2, the reducing agent is one of carbon black, fat coal or active carbon or a variety of.
7. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 2, the silicon substrate clinker and the reducing agent equipment that ball milling uses together is planetary ball mills, with 200~400rmin-1
5~8h of revolving speed unidirectional operation.
8. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 3 (2), the mixing material additive amount is subject to not higher than the 1/3 of small graphite crucible volume.
9. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In 3 (3), the induction coil is copper coil, guarantees that large scale graphite crucible is placed in copper coil, and make large scale graphite earthenware
Crucible and 1~2cm of copper coil distance.
10. the method according to claim 1 for preparing silicon carbide powder using induction furnace, which is characterized in that the step
In rapid 3 (3), silicon carbide powder average grain diameter obtained is 0.5~1 μm.
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| PCT/CN2019/080545 WO2020057095A1 (en) | 2018-09-20 | 2019-03-29 | Method for preparing silicon carbide powder by using induction furnace |
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| WO2020057095A1 (en) * | 2018-09-20 | 2020-03-26 | 东北大学 | Method for preparing silicon carbide powder by using induction furnace |
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| CN101423235A (en) * | 2008-11-26 | 2009-05-06 | 东北大学 | Method for preparing alumina-silicon carbide composite powder |
| CN103508454A (en) * | 2012-06-19 | 2014-01-15 | 上海硅酸盐研究所中试基地 | Preparation method of highly pure silicon carbide raw material |
| CN105503194A (en) * | 2015-12-10 | 2016-04-20 | 中国地质大学（北京） | Method for preparing SiC-Al2O3 complex phase powder through transformation and phase inversion of kyanite mill tailings |
| CN107651691A (en) * | 2017-11-01 | 2018-02-02 | 东北大学 | A kind of method that crystalline silicon cutting waste material prepares high-quality silicon carbide |
| CN107686369A (en) * | 2017-08-22 | 2018-02-13 | 东北大学 | A kind of method for preparing carborundum porous ceramics with the carborundum cutting waste material of crystalline silicon |
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| US20060051281A1 (en) * | 2004-09-09 | 2006-03-09 | Bhabendra Pradhan | Metal carbides and process for producing same |
| CN108892513A (en) * | 2018-09-20 | 2018-11-27 | 东北大学 | A method of silicon carbide powder is prepared using induction furnace |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423235A (en) * | 2008-11-26 | 2009-05-06 | 东北大学 | Method for preparing alumina-silicon carbide composite powder |
| CN103508454A (en) * | 2012-06-19 | 2014-01-15 | 上海硅酸盐研究所中试基地 | Preparation method of highly pure silicon carbide raw material |
| CN105503194A (en) * | 2015-12-10 | 2016-04-20 | 中国地质大学（北京） | Method for preparing SiC-Al2O3 complex phase powder through transformation and phase inversion of kyanite mill tailings |
| CN107686369A (en) * | 2017-08-22 | 2018-02-13 | 东北大学 | A kind of method for preparing carborundum porous ceramics with the carborundum cutting waste material of crystalline silicon |
| CN107651691A (en) * | 2017-11-01 | 2018-02-02 | 东北大学 | A kind of method that crystalline silicon cutting waste material prepares high-quality silicon carbide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020057095A1 (en) * | 2018-09-20 | 2020-03-26 | 东北大学 | Method for preparing silicon carbide powder by using induction furnace |
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Application publication date: 20181127 |