CN108752003A - The preparation method of silicon carbide fine ceramics silicon carbide micro-powder - Google Patents
The preparation method of silicon carbide fine ceramics silicon carbide micro-powder Download PDFInfo
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- CN108752003A CN108752003A CN201810940508.8A CN201810940508A CN108752003A CN 108752003 A CN108752003 A CN 108752003A CN 201810940508 A CN201810940508 A CN 201810940508A CN 108752003 A CN108752003 A CN 108752003A
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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
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- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2006/80—Compositional purity
Abstract
The invention belongs to thyrite technical fields, and in particular to a kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder.Sic raw material is ground into the silicon carbide powder A of 25~40 microns of grain size by this method；Flotation is carried out to silicon carbide powder A as flotation agent using paraffin oil and terebinthine mixture, until no longer emersion free carbon in slurry, final to collect silicon carbide powder A, be cleaned by ultrasonic with water and dried, obtain level-one purified powder；Level-one purified powder is ground into the silicon carbide powder B of 10~15 microns of grain size, shaping then is carried out to silicon carbide powder B using ball mill, 1~2h of ball milling obtains shaping powder；Then distinguish pickling and alkali cleaning carries out two level purification, disperseed, be classified, packed.The method of the present invention can purify sic raw material, and sic raw material gradation diameter section is crushed, by shaping and the content for purifying the free carbon, free silica and silica that alternately can effectively reduce in sic raw material.
Description
Technical field
The invention belongs to thyrite technical fields, and in particular to a kind of silicon carbide fine ceramics silicon carbide is micro-
The preparation method of powder.
Background technology
Silicon carbide ceramics has that wear-resisting, thermal conductivity is high, heat-resisting, corrosion-resistant etc. excellent as a kind of high-temperature structural ceramics
Mechanics and thermal property.Nowadays, silicon carbide ceramics has been widely used in the fields such as machinery, electronics, petrochemical industry, metallurgy.
Currently, the preparation method of silicon carbide ceramics includes mainly：Reaction-sintered, the carbonization of normal pressure-sintered and hot pressed sintering etc. are several
Major class.The ceramic performance that different methods is prepared is different.Wherein reaction sintering method technical difficulty is small, easy grasp, but
It is to contain free silica in the ceramic product prepared, may be only available for requiring in less high machinery.Normal pressure-sintered and hot pressed sintering
There is ceramic product prepared by method high tenacity, high intensity, mechanical property and thermal property to be superior to the pottery of reaction-sintered preparation
Porcelain products.
The quality of silicon carbide ceramics is not only related to the preparation method of ceramics, also close with the quality of silicon carbide micro-powder raw material
It is related.The properties such as purity, granularity, the grain shape of powder material directly determine the sintering character of raw material micro mist, from source
Affect the quality of silicon carbide ceramics.
In the prior art, the production procedure of silicon carbide micro-powder mainly include smelt, crush, purification and classification and etc.,
Middle smelting and pulverising step technology are more mature, but since powder size is small, difficulty is caused to purification and classification, therefore, system
Still contain more free carbon impurity in standby silicon carbide micro-powder.
Invention content
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder provided by the invention, can to sic raw material into
Row purification, makes free carbon, free silica and dioxide-containing silica therein decline.
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder provided by the invention, includes the following steps：
Sic raw material is ground into the silicon carbide powder A of 25~40 microns of grain size by S1；
S2, level-one purification：Silicon carbide powder A is floated as flotation agent with terebinthine mixture using paraffin oil
Choosing is cleaned by ultrasonic and is dried with water, it is pure to obtain level-one until no longer emersion free carbon in slurry, final to collect silicon carbide powder A
Change powder；
S3, ball milling：Level-one purified powder is ground into the silicon carbide powder B of 10~15 microns of grain size, then utilizes ball milling
Machine carries out shaping to silicon carbide powder B, and 1~2h of ball milling obtains shaping powder；
S4, two level purification：Shaping powder is placed in 65 DEG C of 2~3h of pickling, then 70 DEG C of alkali cleaning 2.5h is being placed in, is finally using
Water is cleaned by ultrasonic, dry, obtains two level purified powder；
S5, dispersion, classification, packaging：Two level purified powder is dispersed in water, is then classified, classification is obtained
The silicon carbide powder of different-grain diameter specification is detached, is dried and packs respectively, obtains silicon carbide micro-powder.
Preferably, the preparation method of above-mentioned silicon carbide fine ceramics silicon carbide micro-powder in S1, is carbonized in sic raw material
Content >=94% of silicon.
Preferably, the preparation method of above-mentioned silicon carbide fine ceramics silicon carbide micro-powder, in S2, paraffin oil with it is terebinthine
Volume ratio is 1:1.
Preferably, the preparation method of above-mentioned silicon carbide fine ceramics silicon carbide micro-powder is cleaned by ultrasonic in S2 and in S4
Power is 1000W, time 30min.
Preferably, the preparation method of above-mentioned silicon carbide fine ceramics silicon carbide micro-powder, the washing lotion of pickling is hydrogen in S4
The washing lotion of fluoric acid, alkali cleaning is 10mol/L sodium hydroxide solutions.
Compared with prior art, the preparation method of a kind of silicon carbide fine ceramics silicon carbide micro-powder provided by the invention,
It has the advantages that：
The present invention method sic raw material can be purified, by sic raw material gradation diameter section crush, by shaping with
Purification is alternately.It is first ground into the silicon carbide powder A of 25~40 microns of grain size, carries out level-one purification, level-one purification makes flotation
The larger particle of grain size is easily separated in the process, is not easy to agglomerate, flotation efficiency can be improved；It is then comminuted into 10~15 microns of grain size
Silicon carbide powder B carries out two level purification, and two level purification is mainly pickling and caustic scrubbing step, we are directly by level-one purified powder
It is processed into the grain size and shape of needs so that the material after pickling and alkali cleaning is directly available.Two prepared using the method for the present invention
Content >=99.82% of silicon carbide, free carbon content≤0.05%, contents of free si≤0.05%, dioxy in grade purified powder
SiClx content≤0.11%.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail, but should not be construed as the limitation of the present invention.It is following
The test method of actual conditions is not specified in embodiment, operates usually according to normal condition, agents useful for same is commercially available, due to not
It is related to inventive point, therefore its step is not described in detail.
Unless otherwise defined, all technical and scientific terms and those skilled in the art of the present technique used in the present invention are usual
The meaning of understanding is identical.Except used in embodiment specific method, equipment, in addition to material, according to those skilled in the art
The record of grasp and the present invention to the prior art, can also use and the method described in the embodiment of the present invention, equipment, material
Any method, equipment and the material of the similar or equivalent prior art realizes the present invention.
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder provided by the invention, includes the following steps：
Sic raw material is ground into the silicon carbide powder A of 25~40 microns of grain size by S1；
S2, level-one purification：Silicon carbide powder A is floated as flotation agent with terebinthine mixture using paraffin oil
Choosing is cleaned by ultrasonic and is dried with water, it is pure to obtain level-one until no longer emersion free carbon in slurry, final to collect silicon carbide powder A
Change powder；
S3, ball milling：Level-one purified powder is ground into the silicon carbide powder B of 10~15 microns of grain size, then utilizes ball milling
Machine carries out shaping to silicon carbide powder B, and 1~2h of ball milling obtains shaping powder；
S4, two level purification：Shaping powder is placed in 65 DEG C of 2~3h of pickling, then 70 DEG C of alkali cleaning 2.5h is being placed in, is finally using
Water is cleaned by ultrasonic, dry, obtains two level purified powder；Content >=99.82% of silicon carbide, free carbon contain in two level purified powder
Amount≤0.05%, contents of free si≤0.05%, dioxide-containing silica≤0.11%.
S5, dispersion, classification, packaging：Two level purified powder is dispersed in water, is then classified, classification is obtained
The silicon carbide powder of different-grain diameter specification is detached, is dried and packs respectively, obtains silicon carbide micro-powder.
Preferably, a kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, specifically includes following embodiment.Under
It states in embodiment, the content of silicon carbide is 94% in the sic raw material of selection, free carbon content 1.2%, contents of free si
It is 1.1%, dioxide-containing silica 1.5%.
Embodiment 1
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, includes the following steps：
Sic raw material is ground into the silicon carbide powder A of 35~40 microns of grain size using pulverizer by S1；
S2, level-one purification：Silicon carbide powder A is floated as flotation agent with terebinthine mixture using paraffin oil
Choosing is cleaned by ultrasonic and is dried with water, it is pure to obtain level-one until no longer emersion free carbon in slurry, final to collect silicon carbide powder A
Change powder；Wherein paraffin oil and terebinthine volume ratio are 1:1；The power of ultrasonic cleaning is 1000W, time 30min；
S3, ball milling：Level-one purified powder is ground into the silicon carbide powder B of 10~15 microns of grain size, then utilizes ball milling
Machine carries out shaping to silicon carbide powder B, and ball milling 1h obtains shaping powder；
S4, two level purification：Shaping powder is placed in 65 DEG C of pickling 3h in hydrofluoric acid, is then being placed in 10mol/L hydroxides
70 DEG C of alkali cleaning 2.5h, are finally cleaned by ultrasonic with water in sodium solution, and the power of ultrasonic cleaning is 1000W, time 30min；Microwave
Drying box is dried, and two level purified powder is obtained；The content 99.82% of silicon carbide, free carbon content in two level purified powder
0.05%, contents of free si 0.05%, dioxide-containing silica 0.11%.
S5, dispersion, classification, packaging：Two level purified powder is dispersed in water, is then classified, classification is obtained
The silicon carbide powder of different-grain diameter specification is detached, is dried and packs respectively, obtains silicon carbide micro-powder.Wherein, phase is added when dispersion
When in β-sodium sulfonate formaldehyde condensation products of two level purified powder weight 0.2%, 40r/min stirs pulp 30min, obtains slurries；
Physical dispersion and classification are carried out to slurries using hydraulic classification equipment (water velocity is 400~900L/h) when classification, obtained not
With the silicon carbide micro-powder of model specification；Microwave drying box is used when drying.
Embodiment 2
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, includes the following steps：
Sic raw material is ground into the silicon carbide powder A of 35~40 microns of grain size using pulverizer by S1；
S2, level-one purification：Silicon carbide powder A is floated as flotation agent with terebinthine mixture using paraffin oil
Choosing is cleaned by ultrasonic and is dried with water, it is pure to obtain level-one until no longer emersion free carbon in slurry, final to collect silicon carbide powder A
Change powder；Wherein paraffin oil and terebinthine volume ratio are 1:1；The power of ultrasonic cleaning is 1000W, time 30min；
S3, ball milling：Level-one purified powder is ground into the silicon carbide powder B of 10~15 microns of grain size, then utilizes ball milling
Machine carries out shaping to silicon carbide powder B, and ball milling 2h obtains shaping powder；
S4, two level purification：Shaping powder is placed in 65 DEG C of pickling 2h in hydrofluoric acid, is then being placed in 10mol/L hydroxides
70 DEG C of alkali cleaning 2.5h, are finally cleaned by ultrasonic with water in sodium solution, and the power of ultrasonic cleaning is 1000W, time 30min；Microwave
Drying box is dried, and two level purified powder is obtained；The content 99.88% of silicon carbide, free carbon content in two level purified powder
0.04%, contents of free si 0.05%, dioxide-containing silica≤0.10%.
S5, dispersion, classification, packaging step are the same as embodiment 1.
Embodiment 3
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, includes the following steps：
Sic raw material is ground into the silicon carbide powder A of 25~30 microns of grain size using pulverizer by S1；
S2, level-one purification：Silicon carbide powder A is floated as flotation agent with terebinthine mixture using paraffin oil
Choosing is cleaned by ultrasonic and is dried with water, it is pure to obtain level-one until no longer emersion free carbon in slurry, final to collect silicon carbide powder A
Change powder；Wherein paraffin oil and terebinthine volume ratio are 1:1；The power of ultrasonic cleaning is 1000W, time 30min；
S3, ball milling：Level-one purified powder is ground into the silicon carbide powder B of 10~15 microns of grain size, then utilizes ball milling
Machine carries out shaping to silicon carbide powder B, and ball milling 2h obtains shaping powder；
S4, two level purification：Shaping powder is placed in 65 DEG C of pickling 3h in hydrofluoric acid, is then being placed in 10mol/L hydroxides
70 DEG C of alkali cleaning 2.5h, are finally cleaned by ultrasonic with water in sodium solution, and the power of ultrasonic cleaning is 1000W, time 30min；Microwave
Drying box is dried, and two level purified powder is obtained；The content 99.85% of silicon carbide, free carbon content in two level purified powder
0.03%, contents of free si 0.05%, dioxide-containing silica≤0.09%.
S5, dispersion, classification, packaging step are the same as embodiment 1.
Comparative example 1
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, includes the following steps：
Sic raw material is ground into the silicon carbide powder of 10~15 microns of grain size using pulverizer by S1；
S2, level-one purification：Flotation is carried out to silicon carbide powder as flotation agent using paraffin oil and terebinthine mixture,
Until no longer emersion free carbon in slurry, finally collects silicon carbide powder, is cleaned by ultrasonic with water and is dried, obtains level-one and purify powder
End；Wherein paraffin oil and terebinthine volume ratio are 1:1；The power of ultrasonic cleaning is 1000W, time 30min；
S3, ball milling：Shaping is carried out to silicon carbide powder using ball mill, ball milling 1h obtains shaping powder；
S4, two level purification：Shaping powder is placed in 65 DEG C of pickling 3h in hydrofluoric acid, is then being placed in 10mol/L hydroxides
70 DEG C of alkali cleaning 2.5h, are finally cleaned by ultrasonic with water in sodium solution, and the power of ultrasonic cleaning is 1000W, time 30min；Microwave
Drying box is dried, and two level purified powder is obtained；The content 99.5% of silicon carbide, free carbon content in two level purified powder
0.07%, contents of free si 0.07%, dioxide-containing silica 0.15%.
S5, dispersion, classification, packaging step are the same as embodiment 1.
Compared with Example 1, sic raw material is directly ground into the carborundum powder of 10~15 microns of grain size by comparative example 1
End has lacked the step of segmentation crushes, although the step of also having carried out flotation, pickling and alkali cleaning, refining effect is than real
It is poor to apply example 1.
Comparative example 2
A kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, includes the following steps：
Sic raw material is ground into the silicon carbide powder of 10~15 microns of grain size using pulverizer by S1；
S2, ball milling：Shaping is carried out to silicon carbide powder using ball mill, ball milling 1h obtains shaping powder；
S3, level-one purification：Flotation is carried out to shaping powder as flotation agent using paraffin oil and terebinthine mixture, directly
To no longer emersion free carbon in slurry, silicon carbide powder is finally collected, is cleaned by ultrasonic with water and is dried, obtains level-one purifying powder
End；Wherein paraffin oil and terebinthine volume ratio are 1:1；The power of ultrasonic cleaning is 1000W, time 30min；
S4, two level purification：Shaping powder is placed in 65 DEG C of pickling 3h in hydrofluoric acid, is then being placed in 10mol/L hydroxides
70 DEG C of alkali cleaning 2.5h, are finally cleaned by ultrasonic with water in sodium solution, and the power of ultrasonic cleaning is 1000W, time 30min；Microwave
Drying box is dried, and two level purified powder is obtained；The content 99.4% of silicon carbide, free carbon content in two level purified powder
0.06%, contents of free si 0.07%, dioxide-containing silica 0.18%.
S5, dispersion, classification, packaging step are the same as embodiment 1.
Compared with Example 1, sic raw material is directly ground into the carborundum powder of 10~15 microns of grain size by comparative example 2
End, and ball milling is at the shape of needs, has both lacked the step of segmentation crushes, also by shaping with purification alternately the step of,
Although the step of also having carried out flotation, pickling and alkali cleaning, refining effect are poorer than embodiment 1.
It should be noted that when the present invention provides numberical range, it should be appreciated that except non-present invention is otherwise noted, per number
Any one numerical value can be selected between being worth two endpoints and two endpoints of range.Although having been described that the present invention's is preferred
Embodiment, once a person skilled in the art knows basic creative concepts, then can be made in addition to these embodiments
Change and modification.So the following claims are intended to be interpreted as including preferred embodiment and falls into the institute of the scope of the invention
Have altered and changes.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (5)
1. a kind of preparation method of silicon carbide fine ceramics silicon carbide micro-powder, which is characterized in that include the following steps：
Sic raw material is ground into the silicon carbide powder A of 25~40 microns of grain size by S1；
S2, level-one purification：Flotation is carried out to silicon carbide powder A as flotation agent using paraffin oil and terebinthine mixture, directly
To no longer emersion free carbon, final collection silicon carbide powder A are cleaned by ultrasonic and are dried with water in slurry, level-one purifying powder is obtained
End；
S3, ball milling：Level-one purified powder is ground into the silicon carbide powder B of 10~15 microns of grain size, then utilizes ball mill pair
Silicon carbide powder B carries out shaping, and 1~2h of ball milling obtains shaping powder；
S4, two level purification：Shaping powder is placed in 65 DEG C of 2~3h of pickling, is then being placed in 70 DEG C of alkali cleaning 2.5h, it is finally super with water
Sound cleans, dry, obtains two level purified powder；
S5, dispersion, classification, packaging：Two level purified powder is dispersed in water, is then classified, the difference that classification is obtained
The silicon carbide powder of grain size specification is detached, is dried and packs respectively, obtains silicon carbide micro-powder.
2. the preparation method of silicon carbide fine ceramics silicon carbide micro-powder according to claim 1, which is characterized in that S1
In, content >=94% of silicon carbide in sic raw material.
3. the preparation method of silicon carbide fine ceramics silicon carbide micro-powder according to claim 2, which is characterized in that S2
In, paraffin oil is 1 with terebinthine volume ratio:1.
4. the preparation method of silicon carbide fine ceramics silicon carbide micro-powder according to claim 2, which is characterized in that in S2
It is 1000W, time 30min with the power being cleaned by ultrasonic in S4.
5. the preparation method of silicon carbide fine ceramics silicon carbide micro-powder according to claim 2, which is characterized in that in S4
The washing lotion of pickling is hydrofluoric acid, and the washing lotion of alkali cleaning is 10mol/L sodium hydroxide solutions.
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Cited By (3)
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| CN114956087A (en) * | 2022-04-20 | 2022-08-30 | 长沙宁曦新材料有限公司 | Method for preparing nano silicon carbide by alkaline solution etching |
| WO2023162721A1 (en) * | 2022-02-24 | 2023-08-31 | 株式会社トクヤマ | Silicon carbide powder, and production method thereof |
| EP4212480A3 (en) * | 2021-12-23 | 2023-11-01 | SENIC Inc. | Silicon carbide powder, method for manufacturing silicon carbide ingot using the same, and silicon carbide wafer |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4212480A3 (en) * | 2021-12-23 | 2023-11-01 | SENIC Inc. | Silicon carbide powder, method for manufacturing silicon carbide ingot using the same, and silicon carbide wafer |
| WO2023162721A1 (en) * | 2022-02-24 | 2023-08-31 | 株式会社トクヤマ | Silicon carbide powder, and production method thereof |
| CN114956087A (en) * | 2022-04-20 | 2022-08-30 | 长沙宁曦新材料有限公司 | Method for preparing nano silicon carbide by alkaline solution etching |
| CN114956087B (en) * | 2022-04-20 | 2024-01-16 | 长沙宁曦新材料有限公司 | Method for preparing nano silicon carbide by etching alkali solution |
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