CN108892511A - A method of preparing silicon carbide in submicro level powder - Google Patents
A method of preparing silicon carbide in submicro level powder Download PDFInfo
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- CN108892511A CN108892511A CN201810945556.6A CN201810945556A CN108892511A CN 108892511 A CN108892511 A CN 108892511A CN 201810945556 A CN201810945556 A CN 201810945556A CN 108892511 A CN108892511 A CN 108892511A
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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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Abstract
The invention belongs to Techniques for Preparation of SiC Powder fields, disclose a kind of method for preparing silicon carbide in submicro level powder, include the following steps:Raw material silicon carbide powder is situated between with mill and carries out dry grinding together;Material after grinding is sieved through sieve;After the material that screening obtains is mixed with dispersing agent and water, it is situated between with mill and carries out wet grinding together, obtain carbide fine powder slurry;Carbide fine powder slurry is successively delivered in alkaline purified reaction kettle, is purified in acidity purified reaction kettle with neutralization pond, then slurry after purification is delivered in transferring storage container, drying dispersing aid is added, it precipitates after mixing evenly, supernatant is discharged after precipitating, and the progress filters pressing of obtained precipitating is obtained into filter cake;Filter cake loading pallet is dried, dried material is taken out and obtains silicon carbide in submicro level powder after crushed.The application can overcome inflection point and inverse point in process, improve production efficiency.
Description
Technical field
The invention belongs to Techniques for Preparation of SiC Powder field, in particular to a kind of silicon carbide in submicro level powder for preparing
Method.
Background technique
Silicon carbide ceramics is high with hardness, elevated temperature strength is big, thermal conductivity is high, chemical stability is good, thermal expansion coefficient is small, exhausted
Edge is good and the wide lamp excellent performance of band gap, obtains in fields such as aerospace, automobile, machinery, electronics, chemical industry, the energy and environmental protection
To being widely applied.Research shows that:In the preparation process of silicon carbide ceramics, the granularity with silicon carbide powder raw material becomes smaller,
Its sintering character and mechanical property can all be significantly improved, therefore to burn out the fine ceramics product haveing excellent performance, just
There must be the silicon carbide super powder that rational size distribution, purity is high, performance are good.
There are many preparation methods of superfine silicon carbide powder, such as airflow counter-collision comminuting method, vibromill comminuting method, Ball-stirring mill
Comminuting method etc..But these methods are all more or less when preparing superfine silicon carbide powder that there are some problems, such as air-flow
Mill comminuting method advantage is dry method, high-efficient, pollution is small but poor with fine powder effectiveness of classification to 3 μm, inefficient;Vibrating mill
Comminuting method advantage be dry method, pollution it is small, the disadvantage is that superfine powder still need to classification processing, grading effect it is difficult to ensure that;Or it is grinding
Be milled it is broken during be easy to appear reunion and show, easily there is " inflection point " or inverse point.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing silicon carbide in submicro level powder.
To achieve the goals above, the technical solution that the application uses for:A kind of silicon carbide in submicro level powder of preparing
Method includes the following steps:
(1) it is raw material that selection granularity, which is the silicon carbide powder of 100 mesh~1000 mesh, SiC content not less than 70%, with first
Mill is situated between is added to progress dry grinding 8h~10h in ball mill together;Material after grinding passes through 1500 mesh~2000 mesh screens
It is sieved;
First mill Jie is the cast steel ball that diameter is 5mm~12mm, and is 0.3 with the weight ratio of silicon carbide powder raw material
~5:1;
(2) will be added in sand mill after the obtained material of screening mix with dispersing agent and water, with second grind Jie together into
Row wet grinding obtains carbide fine powder slurry, carborundum granularity D in the carbide fine powder slurry50=0.3 μm~1.0 μm,
D100≤2.0μm;
It is 1mm~12mm cast steel ball that second mill Jie, which is diameter,;And with the weight ratio of silicon carbide powder raw material be 0.3~
5:1;
The dosage of the dispersing agent is 5wt%~10wt% of silicon carbide powder raw material, and the dispersing agent is sodium pyrophosphate
Or one of sorbitan fatty acid rouge;
The weight ratio of water and silicon carbide powder raw material is 1:0.3~6;
(3) the obtained carbide fine powder slurry of step (2) is successively delivered in alkaline purified reaction kettle, acid purification
It is purified in reaction kettle with neutralization pond, then slurry after purification is delivered in transferring storage container, it is thin that silicon carbide is added
The drying dispersing aid of powder slurry weight 0.001%~0.9% precipitates 10h~30h after mixing evenly, is discharged after precipitating
Supernatant, and obtained precipitating is subjected to filters pressing, filter cake is obtained, it is spare;
(4) filter cake that step (3) obtains pallet is packed into be dried, it is dry to be no more than 0.03% to moisture content, it takes
Dried material obtains silicon carbide in submicro level powder after crushed out.
Further, the cast steel ball of the step (1) includes the major diameter cast steel ball and diameter that diameter is 10mm~12mm
For the middle diameter cast steel ball of 5mm~10mm, and the weight proportion of the major diameter cast steel ball and middle diameter cast steel ball is 1:3.
Further, the cast steel ball of the step (2) include diameter be 10mm~12mm major diameter cast steel ball, diameter be
The middle diameter cast steel ball and diameter of 5mm~10mm is the minor diameter cast steel ball of 1mm~5mm, and the major diameter cast steel ball, described
The weight proportion of middle diameter cast steel ball and the minor diameter cast steel ball is 1:3:3.
Further, the drying dispersing aid in the step (3) is inorganic dispersant.
Further, the inorganic dispersant is one of waterglass, sodium tripolyphosphate, calgon.
What step (3) was recorded is successively delivered to alkaline purified reaction kettle for the obtained carbide fine powder slurry of step (2)
In interior, acid purified reaction kettle and detailed process that neutralization pond is purified is:
Firstly, the obtained carbide fine powder slurry of step (2) is delivered in alkaline purified reaction kettle, and it is heavy that its is added
The alkaline matter of amount 1%~20% heats 2h or more, by slurry pipeline transport after heating under conditions of temperature is not less than 50 DEG C
To neutralization pond, pH≤8 of slurry are controlled, obtain alkali-treated slurry, it is spare;
Then, above-mentioned alkali-treated slurry is delivered in acid purified reaction kettle, its weight 1%~15% is added
Mixed acid purifies 2h or more under normal temperature conditions, by slurry pipeline transport to neutralization pond after purification, the pH for controlling slurry is 5~
8, the processed slurry of acid is obtained, it is spare;
Finally, the processed slurry of acid obtained above is handled with alkaline matter again, it is not less than 50 in temperature
2h or more is heated under conditions of DEG C, and slurry pipeline transport is controlled into pH≤8 of slurry to neutralization pond processing after heating;Then will
Obtained slurry pipeline transport is into transferring storage container.
Compared with prior art, the beneficial effects of the invention are as follows:Silicon carbide in submicro level can be obtained, and can be overcome super
Inflection point and inverse point in fine powder process, save and are classified process again, improve production efficiency and powder characteristic.
Specific embodiment
Technological means of the invention, creation characteristic, achieving the goal is easy to understand with effect in order to make, below in conjunction with
Technical solution of the present invention is clearly and completely described in specific embodiments of the present invention.
Embodiment 1
A method of silicon carbide in submicro level powder is prepared, is included the following steps:
(1) choose granularity be 100 mesh~1000 mesh, SiC content 70.7% silicon carbide powder be raw material, with first mill be situated between
It is added to progress dry grinding 8h in ball mill together;Material after grinding is sieved by 1500 mesh~2000 mesh screens;
First mill Jie is the cast steel ball that diameter is 5mm~12mm, and is 0.3 with the weight ratio of silicon carbide powder raw material:1;
Wherein cast steel ball includes the major diameter cast steel ball that diameter is 10mm~12mm and the middle diameter cast steel ball that diameter is 5mm~10mm,
And the weight proportion of major diameter cast steel ball and middle diameter cast steel ball is 1:3.
(2) will be added in sand mill after the obtained material of screening mix with dispersing agent and water, with second grind Jie together into
Row wet grinding obtains carbide fine powder slurry, carborundum granularity D in carbide fine powder slurry50=0.3 μm~1.0 μm, D100
It is 2.0 μm;
It is 1mm~12mm cast steel ball that second mill Jie, which is diameter,;And with the weight ratio of silicon carbide powder raw material be 0.3:1;Casting
Steel ball include diameter be 10mm~12mm major diameter cast steel ball, diameter be 5mm~10mm middle diameter cast steel ball and diameter be
The minor diameter cast steel ball of 1mm~5mm, and the weight proportion of major diameter cast steel ball, middle diameter cast steel ball and minor diameter cast steel ball is
1:3:3.
The dosage of dispersing agent is the 5wt% of silicon carbide powder raw material, and dispersing agent is sodium pyrophosphate;
The weight ratio of water and silicon carbide powder raw material is 1:0.3;
(3) the obtained carbide fine powder slurry of step (2) is successively delivered in alkaline purified reaction kettle, acid purification
It is purified in reaction kettle with neutralization pond, then slurry after purification is delivered in transferring storage container, it is thin that silicon carbide is added
The drying dispersing aid of powder slurry weight 0.001% precipitates 10h after mixing evenly, supernatant is discharged after precipitating, and incite somebody to action
The precipitating arrived carries out filters pressing, obtains filter cake, spare;Drying dispersing aid is inorganic dispersant, and inorganic dispersant is waterglass;
(4) filter cake that step (3) obtains pallet is packed into be dried, it is dry to moisture content 0.03%, take out drying
Material obtains silicon carbide in submicro level powder after crushed.
Embodiment 2
A method of silicon carbide in submicro level powder is prepared, is included the following steps:
(1) choose granularity be 100 mesh~1000 mesh, SiC content 83.7% silicon carbide powder be raw material, with first mill be situated between
It is added to progress dry grinding 10h in ball mill together;Material after grinding is sieved by 1500 mesh~2000 mesh screens;
First mill Jie is the cast steel ball that diameter is 5mm~12mm, and is 5 with the weight ratio of silicon carbide powder raw material:1;Casting
The middle diameter cast steel ball that steel ball includes the major diameter cast steel ball that diameter is 10mm~12mm and diameter is 5mm~10mm, and it is described
The weight proportion of major diameter cast steel ball and middle diameter cast steel ball is 1:3.
(2) will be added in sand mill after the obtained material of screening mix with dispersing agent and water, with second grind Jie together into
Row wet grinding obtains carbide fine powder slurry, carborundum granularity D in the carbide fine powder slurry50=0.3 μm~1.0 μm,
D100It is 1.8 μm;
It is 1mm~12mm cast steel ball that second mill Jie, which is diameter,;And with the weight ratio of silicon carbide powder raw material be 5:1;Cast steel
Ball include diameter be 10mm~12mm major diameter cast steel ball, diameter be 5mm~10mm middle diameter cast steel ball and diameter be 1mm
The minor diameter cast steel ball of~5mm, and the weight of the major diameter cast steel ball, the middle diameter cast steel ball and the minor diameter cast steel ball
Amount proportion is 1:3:3.
The dosage of dispersing agent is the 10wt% of silicon carbide powder raw material, and dispersing agent is sorbitan fatty acid rouge;
The weight ratio of water and silicon carbide powder raw material is 1:6;
(3) the obtained carbide fine powder slurry of step (2) is successively delivered in alkaline purified reaction kettle, acid purification
It is purified in reaction kettle with neutralization pond, then slurry after purification is delivered in transferring storage container, it is thin that silicon carbide is added
The drying dispersing aid of powder slurry weight 0.9% precipitates 30h after mixing evenly, supernatant is discharged after precipitating, and will obtain
Precipitating carry out filters pressing, obtain filter cake, it is spare;Drying dispersing aid is inorganic dispersant.Inorganic dispersant is sodium tripolyphosphate.
(4) filter cake that step (3) obtains pallet is packed into be dried, it is dry to be no more than 0.03% to moisture content, it takes
Dried material obtains silicon carbide in submicro level powder after crushed out.
Embodiment 3
A method of silicon carbide in submicro level powder is prepared, is included the following steps:
(1) choose granularity be 100 mesh~1000 mesh, SiC content 91.8% silicon carbide powder be raw material, with first mill be situated between
It is added to progress dry grinding 9h in ball mill together;Material after grinding is sieved by 1500 mesh~2000 mesh screens;
First mill Jie is the cast steel ball that diameter is 5mm~12mm, and is 3 with the weight ratio of silicon carbide powder raw material:1;Casting
The middle diameter cast steel ball that steel ball includes the major diameter cast steel ball that diameter is 10mm~12mm and diameter is 5mm~10mm, and it is described
The weight proportion of major diameter cast steel ball and middle diameter cast steel ball is 1:3.
(2) will be added in sand mill after the obtained material of screening mix with dispersing agent and water, with second grind Jie together into
Row wet grinding obtains carbide fine powder slurry, carborundum granularity D in the carbide fine powder slurry50=0.3 μm~1.0 μm,
D100It is 1.2 μm;
It is 1mm~12mm cast steel ball that second mill Jie, which is diameter,;And with the weight ratio of silicon carbide powder raw material be 3:1;Cast steel
Ball include diameter be 10mm~12mm major diameter cast steel ball, diameter be 5mm~10mm middle diameter cast steel ball and diameter be 1mm
The minor diameter cast steel ball of~5mm, and the weight of the major diameter cast steel ball, the middle diameter cast steel ball and the minor diameter cast steel ball
Amount proportion is 1:3:3.
The dosage of dispersing agent is the 7.5wt% of silicon carbide powder raw material, and dispersing agent is sodium pyrophosphate;
The weight ratio of water and silicon carbide powder raw material is 1:4;
(3) the obtained carbide fine powder slurry of step (2) is successively delivered in alkaline purified reaction kettle, acid purification
It is purified in reaction kettle with neutralization pond, then slurry after purification is delivered in transferring storage container, it is thin that silicon carbide is added
The drying dispersing aid of powder slurry weight 0.45% precipitates 20h after mixing evenly, supernatant is discharged after precipitating, and incite somebody to action
The precipitating arrived carries out filters pressing, obtains filter cake, spare;Drying dispersing aid is inorganic dispersant.Inorganic dispersant is hexa metaphosphoric acid
Sodium.
(4) filter cake that step (3) obtains pallet is packed into be dried, it is dry to be no more than 0.03% to moisture content, it takes
Dried material obtains silicon carbide in submicro level powder after crushed out.
The application respectively carries out the size distribution of the preparation-obtained silicon carbide powder of embodiment 1-3 using laser method
Detection, as a result such as table 1.
The size distribution of silicon carbide powder prepared by each embodiment of table 1
The partial size for the silicon carbide powder that each embodiment is prepared in the application as can be known from Table 1 is all satisfied submicron order,
Average grain diameter is 0.37 μm.
Examination sintering is carried out as raw material using silicon carbide in submicro level powder prepared by the application, the sintered density of manufactured goods is reachable
To 3.29g/cm2~3.31g/cm2, it is the 97.6%~99.2% of theoretical density.
In conclusion silicon carbide in submicro level can be obtained, and can overcome inflection point in superfine powder process and
Inverse point, saves and is classified process again, improves production efficiency and powder characteristic.
Disclosed above is only presently preferred embodiments of the present invention, and still, the embodiment of the present invention is not limited to this, Ren Heben
What the technical staff in field can think variation should all fall into protection scope of the present invention.
Claims (5)
1. a kind of method for preparing silicon carbide in submicro level powder, which is characterized in that include the following steps:
(1) it is raw material that selection granularity, which is the silicon carbide powder of 100 mesh~1000 mesh, SiC content not less than 70%, is situated between with the first mill
It is added to progress dry grinding 8h~10h in ball mill together;Material after grinding is carried out by 1500 mesh~2000 mesh screens
Screening;
First mill Jie is the cast steel ball that diameter is 5mm~12mm, and is 0.3~5 with the weight ratio of silicon carbide powder raw material:
1;
(2) it after mixing the material that screening obtains with dispersing agent and water, is added in sand mill, being situated between with the second mill, it is wet to carry out together
Method grinding, obtains carbide fine powder slurry, carborundum granularity D in the carbide fine powder slurry50=0.3 μm~1.0 μm, D100
≤2.0μm;
It is 1mm~12mm cast steel ball that second mill Jie, which is diameter,;And with the weight ratio of silicon carbide powder raw material be 0.3~5:1;
The dosage of the dispersing agent is 5wt%~10wt% of silicon carbide powder raw material, and the dispersing agent is sodium pyrophosphate or mountain
One of pears polyol fatty acid rouge;
The weight ratio of water and silicon carbide powder raw material is 1:0.3~6;
(3) the obtained carbide fine powder slurry of step (2) is successively delivered in alkaline purified reaction kettle, acid purified reaction
It is purified in kettle with neutralization pond, then slurry after purification is delivered in transferring storage container, carbide fine powder slurry is added
Expect the drying dispersing aid of weight 0.001%~0.9%, precipitates 10h~30h after mixing evenly, supernatant is discharged after precipitating
Liquid, and obtained precipitating is subjected to filters pressing, filter cake is obtained, it is spare;
(4) filter cake that step (3) obtains pallet is packed into be dried, it is dry to be no more than 0.03% to moisture content, it takes out dry
Dry material obtains silicon carbide in submicro level powder after crushed.
2. the method for preparing silicon carbide in submicro level powder as described in claim 1, which is characterized in that the step (1)
The middle diameter cast steel ball that cast steel ball includes the major diameter cast steel ball that diameter is 10mm~12mm and diameter is 5mm~10mm, and institute
The weight proportion for stating major diameter cast steel ball and middle diameter cast steel ball is 1:3.
3. the method for preparing silicon carbide in submicro level powder as described in claim 1, which is characterized in that the step (2)
Cast steel ball include diameter be 10mm~12mm major diameter cast steel ball, diameter be 5mm~10mm middle diameter cast steel ball and diameter
For the minor diameter cast steel ball of 1mm~5mm, and the major diameter cast steel ball, the middle diameter cast steel ball and the minor diameter cast steel
The weight proportion of ball is 1:3:3.
4. the method for preparing silicon carbide in submicro level powder as described in claim 1, which is characterized in that in the step (3)
Drying dispersing aid be inorganic dispersant.
5. the method for preparing silicon carbide in submicro level powder as claimed in claim 4, which is characterized in that the inorganic dispersant
For one of waterglass, sodium tripolyphosphate, calgon.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113174147A (en) * | 2021-04-12 | 2021-07-27 | 华南理工大学 | Submicron spherical zinc oxide particle and preparation method thereof |
CN113582699A (en) * | 2021-07-22 | 2021-11-02 | 武汉工程大学 | Low-viscosity high-solid-content ceramic slurry and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113174147A (en) * | 2021-04-12 | 2021-07-27 | 华南理工大学 | Submicron spherical zinc oxide particle and preparation method thereof |
CN113582699A (en) * | 2021-07-22 | 2021-11-02 | 武汉工程大学 | Low-viscosity high-solid-content ceramic slurry and preparation method thereof |
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