CN109369189A - A kind of moulding process of silicon carbide ceramics ball - Google Patents
A kind of moulding process of silicon carbide ceramics ball Download PDFInfo
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- CN109369189A CN109369189A CN201811351229.4A CN201811351229A CN109369189A CN 109369189 A CN109369189 A CN 109369189A CN 201811351229 A CN201811351229 A CN 201811351229A CN 109369189 A CN109369189 A CN 109369189A
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- silicon carbide
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Abstract
The present invention provides a kind of silicon carbide ceramics balls, be made of the following raw material of parts by weight through mixing, granulation, the production of hybrid seeds, molding, sintering and grinding: major ingredient: carbide fine powder 87%~96%, high carbon residue phenolic resin 5%~11%, sintering aid 1.2%~5%, the sintering aid are B, C, B4C、Al2O3And Y2O3At least one of;Auxiliary material: binder, dispersing agent, dosage are followed successively by the 0.9%~11% of major ingredient weight, 0.5%~3.5%, and binder is at least one of polyvinyl alcohol, dextrin and carboxymethyl cellulose;Dispersing agent is at least one of polyethylene glycol, tetramethylammonium hydroxide, aluminophosphates, polyacrylic acid.Silicon carbide ceramics ball density of the present invention is big, and chemical property is stablized;It can satisfy the preparation of the silicon carbide ceramics ball of more specification partial sizes, range is wide, can produce from 1mm-50mm;One-time investment is few, and it is easy to expand production.
Description
Technical field
The present invention relates to Ceramic Balls and preparation method fields, more particularly to a kind of moulding process of silicon carbide ceramics ball
Background technique
Silicon carbide ceramics has high intensity, low creep properties, rub resistance abrasion, corrosion resistance and good inoxidizability, and
And its excellent mechanical performance, lower thermal expansion coefficient and the higher coefficient of heat conduction determine the anti-thermal shock of silicon carbide ceramics
Performance is very good.Based on above-mentioned advantage, silicon carbide ceramics ball as mill ball and ceramic bearing, ball valve key components and parts in height
It has a wide range of applications in the harshness operating condition such as temperature, strong acid, highly basic, shock resistance.
Silicon carbide ceramics ball pelletizing method in the prior art mainly include the following types:
(1) extrusion: powder is sintered after ball milling, filters pressing, pugging, extruding, cutting, molding and obtains Ceramic Balls, this method
Forming process process is more, and spherical control is poor, and the later period is needed to grind to obtain desired size.
(2) wet bag method isostatic cool pressing: it is that isostatic cool pressing is put into after sealing in spherical rubber pattern that powder, which is filled into inner cavity,
In working chamber, is pressurizeed by superhigh pressure liquid medium to rubber pattern surrounding equalization, demoulded outside cylinder after release.The molding pottery of this method
Porcelain ball density is high and uniform, but entire pressurization and stress-relief process are slow, generally will be at 10 minutes or more, and the degree of automation is low, needs
Very important person's tooling moulding/demoulding, shape is affected by human factors larger.
(3) dry bag method isostatic cool pressing: being current state-of-the-art forming method, high degree of automation, by artifical influence factor
It is small.Powder processability is required high, it is necessary to be the powder by mist projection granulating.Production chains are poor, produce different size
Product, it is necessary to replace whole set of die, or even also to be replaced together with isostatic pressure chamber.Compare and compacting diameter is suitble to be greater than 15
Product.
(4) hot pressing sintering method: uniformly mixed powder (containing sintering aid and binder) is packed into mold, in high temperature sintering
Hot pressed sintering is carried out in furnace.The disadvantage is that the product quantity of every furnace sintering is few, and mold cannot be used for multiple times.
(5) HIP sintering method: it is spherical good although the Ceramic Balls density of HIP sintering is high, compared to other
Preparation method, cost is excessively high, low efficiency, is not suitable for large-scale production.
Therefore, it is necessary to find a kind of preparation method of high-density silicon carbide ceramics ball, production cost is reduced, it can high-volume
Production, in favor of the popularization and use of silicon carbide ceramics ball.
Summary of the invention
Based on this, it is necessary to a kind of moulding process of silicon carbide ceramics ball is provided, to solve the above problems.
A kind of silicon carbide ceramics ball, by the following raw material of parts by weight through mixing, granulation, the production of hybrid seeds, molding, sintering and grinding and
It is made:
Major ingredient: carbide fine powder 87%~96%, high carbon residue phenolic resin 5%~11%, sintering aid 1.2%~5%,
The sintering aid is B, C, B4C、Al2O3And Y2O3At least one of;
Auxiliary material: binder, dispersing agent, dosage are followed successively by the 0.9%~11% of major ingredient weight, 0.5%~3.5%, institute
Stating binder is at least one of polyvinyl alcohol, dextrin and carboxymethyl cellulose;The dispersing agent is polyethylene glycol, tetramethyl
At least one of ammonium hydroxide, aluminophosphates, polyacrylic acid.
Further, the carbide fine powder is a phase, and median particle diameter 0.5um, purity is greater than 98.5%.
Further, silicon carbide ceramics ball moulding process the following steps are included:
(1) powder is made: with 87%~96% carbide fine powder, 5%~11% high carbon residue phenolic resin and 1.2%
~5% sintering aid is main constitutive material, and deionized water is added, sequentially adds binder and dispersing agent, mixed with ball milling
After closing 12~24 hours, distributed slurry is obtained after 80~200 mesh net filtrations, and its solid content is made to reach 50%~70%,
Above-mentioned binder, dispersing agent weight be respectively the 0.9%~11% of main material, 0.5%~3.5%;
(2) mist projection granulating: being dried gained slurry with spray dryer, sets hot wind inlet temperature as 160~300
DEG C, outlet temperature be 60~200 DEG C, slurry flow be 10~100 ㎏/h, atomizer adjust the speed 10~30Hz, to above-mentioned slurry into
Row drying crosses 100~200 meshes, obtains the compound powder of silicon carbide;
(3) production of hybrid seeds: taking the compound powder to be pressed into ceramics biscuits of carbonized bricks, crosses 40~100 meshes after being crushed to it
Up to the seed of balling-up;
(4) balling-up: seed is put into nodulizer, opens nodulizer, adjusts nodulizer revolving speed and angle, turns nodulizer
Speed and angle are directly proportional to the size of ball, 20~50r/min of revolving speed, and 10~80 ° of angle, continuously spraying water and be added into machine is granulated
Powder, circulating rolling repeat this operating process, until Ceramic Balls grow to required size;
(5) it is sintered: silicon carbide ceramics ball base is put into vacuum sintering furnace, heat up sintering after vacuumizing, and argon gas protection rises
Warm rate is 3~30 DEG C/min, is warming up to 1820~2280 DEG C, then keep the temperature 120~240 minutes, is caused after Temperature fall up to high
Close silicon carbide ceramics ball.
The beneficial effects of the present invention are:
(1) silicon carbide ceramics ball density of the present invention is big, and chemical property is stablized;
(2) preparation process of the present invention can satisfy the preparation of the silicon carbide ceramics ball of more specification partial sizes, and range is wide, from 1mm-
50mm can be produced;
(3) present invention process is simple, and one-time investment is few, and it is easy to expand production.
Specific embodiment
The preferred embodiments of the present invention will be described in detail below so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that so as to make a clearer definition of the protection scope of the present invention.
Embodiment 1
A kind of preparation method of high-density silicon carbide ceramics ball, by carbide fine powder (a phase, median particle diameter 0.5um, purity
Greater than 98.5%), high carbon residue phenolic resin and sintering aid (Al2O3And Y2O3It half-and-half) is configured to main material, each ingredient in proportion
Mass percent is successively are as follows: 87% carbide fine powder, 5% resin, 1.2% sintering aid successively follow the steps below:
1) mixing: main material is put into deionized water, sequentially adds binder (polyvinyl alcohol) and dispersing agent (tetramethyl
Ammonium hydroxide), after ball milling mixing 12 hours, distributed slurry is obtained after 100 mesh net filtrations.Above-mentioned binder, dispersing agent
Weight is respectively the 1% of main material, 0.5%.
2) mist projection granulating: above-mentioned slurry is dried using spray dryer, obtains compound powder.Spray dryer
Hot wind inlet temperature is set as 160 DEG C, outlet temperature is 60 DEG C, and slurry flow is 10 ㎏/h, and atomizer adjusts the speed 10Hz.Pelletizing
It sieves with 100 mesh sieve.
3) production of hybrid seeds: ceramics biscuits of carbonized bricks of the above-mentioned pelletizing through 200T four-column press compacting F50mm × 15mm is broken to it
80 meshes are crossed after broken obtains balling-up seed.
4) balling-up: seed is put into nodulizer, unlatching nodulizer, setting speed 25r/min, and 30 ° of angle, continuously to machine
Interior to spray water and add pelletizing, circulating rolling repeats this operating process, obtains the Ceramic Balls base of diameter 3mm.
5) it is sintered: silicon carbide ceramics ball base is put into vacuum sintering furnace, heat up sintering after vacuumizing, and argon gas protection rises
Warm rate is 5 DEG C/min, is warming up to 1850 DEG C, keeps the temperature 120 minutes, obtains silicon carbide ceramics ball, density after natural cooling cooling
For 3.18g/cm 3.
Embodiment 2: a kind of preparation method of high-density silicon carbide ceramics ball, by carbide fine powder, high carbon residue phenolic resin
It is configured to main material in proportion with sintering aid, each ingredient percent is respectively as follows: carbide fine powder 90%, high carbon residue phenolic aldehyde
Resin 7%, sintering aid (B4C) 3%, successively follow the steps below:
1) mixing: main material is put into deionized water, sequentially adds binder (carboxymethyl cellulose) and dispersing agent is (poly-
Propenyl), after ball milling mixing 18 hours, distributed slurry is obtained after 140 mesh net filtrations.The weight of above-mentioned binder, dispersing agent
Amount is respectively 5%, the 1.5% of main material.
2) mist projection granulating: above-mentioned slurry is dried using spray dryer, obtains compound powder.Spray dryer
Hot wind inlet temperature is set as 210 DEG C, outlet temperature is 100 DEG C, and slurry flow is 40 ㎏/h, and atomizer adjusts the speed 20Hz.It is granulated
Powder crosses 140 meshes.
3) production of hybrid seeds: ceramics biscuits of carbonized bricks of the seed of balling-up through 200T four-column press compacting F50mm × 15mm, to it
It is crossed obtained by 60 meshes after broken.
4) balling-up: seed is put into nodulizer, unlatching nodulizer, setting speed 40r/min, and 50 ° of angle, continuously to machine
Interior water spray and plus pelletizing.Circulating rolling repeats this operating process, obtains the Ceramic Balls base of diameter 10mm.
5) it is sintered: silicon carbide ceramics ball base is put into vacuum sintering furnace, heat up sintering after vacuumizing, and argon gas protection rises
Warm rate is 10 DEG C/min, is warming up to 2000 DEG C, keeps the temperature 180 minutes, silicon carbide ceramics ball is obtained after Temperature fall, density is
3.15g/cm 3。
Embodiment 3: a kind of preparation method of high-density silicon carbide ceramics ball, by carbide fine powder, high carbon residue phenolic resin
It is configured to main material in proportion with sintering aid, each ingredient percent is respectively as follows: 95% carbide fine powder, and 4% resin is burnt
Auxiliary agent B 1% is tied, is successively followed the steps below:
1) mixing: main material is put into deionized water, sequentially adds binder (dextrin) and dispersing agent (aluminophosphates),
After ball milling mixing 24 hours, distributed slurry is obtained after 180 mesh net filtrations.Above-mentioned binder, dispersing agent weight be respectively
10%, the 3% of main material.
2) mist projection granulating: above-mentioned slurry is dried using spray dryer, obtains compound powder.Spray dryer
Hot wind inlet temperature is set as 260 DEG C, outlet temperature is 110 DEG C, and slurry flow is 80 ㎏/h, and atomizer adjusts the speed 30Hz.It is granulated
Powder crosses 200 meshes.
3) production of hybrid seeds: ceramics biscuits of carbonized bricks of the seed of balling-up through 200T four-column press compacting F50mm × 15mm, to it
Gained is sieved with 100 mesh sieve after broken.
4) balling-up: seed is put into nodulizer, unlatching nodulizer, setting speed 50r/min, and 70 ° of angle, continuously to machine
Interior water spray and plus pelletizing.Circulating rolling repeats this operating process, obtains the Ceramic Balls base of diameter 30mm.
5) it is sintered: silicon carbide ceramics ball base is put into vacuum sintering furnace, heat up sintering after vacuumizing, and argon gas protection rises
Warm rate is 20 DEG C/min, is warming up to 2200 DEG C, keeps the temperature 240 minutes, silicon carbide ceramics ball is obtained after Temperature fall, density is
3.13g/cm 3。
Change each specific technological parameter or equivalent replacement in above-described embodiment, multiple specific realities can be formed
Example is applied, is common variation range of the invention, is no longer described in detail one by one herein.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (3)
1. a kind of silicon carbide ceramics ball, which is characterized in that by the following raw material of parts by weight through mixing, granulation, the production of hybrid seeds, molding, burning
It ties and grinds and be made:
Major ingredient: carbide fine powder 87%~96%, high carbon residue phenolic resin 5%~11%, sintering aid 1.2%~5%, it is described
Sintering aid is B, C, B4C、Al2O3And Y2O3At least one of;
Auxiliary material: binder, dispersing agent, dosage is followed successively by the 0.9%~11% of major ingredient weight, 0.5%~3.5%, described viscous
Knot agent is at least one of polyvinyl alcohol, dextrin and carboxymethyl cellulose;The dispersing agent is polyethylene glycol, tetramethyl hydrogen-oxygen
Change at least one of ammonium, aluminophosphates, polyacrylic acid.
2. silicon carbide ceramics ball according to claim 1, which is characterized in that the carbide fine powder is a phase, median particle diameter
For 0.5um, purity is greater than 98.5%.
3. the moulding process of silicon carbide ceramics ball according to claim 1, which comprises the following steps:
(1) powder is made: with 87%~96% carbide fine powder, 5%~11% high carbon residue phenolic resin and 1.2%~
5% sintering aid is main constitutive material, and deionized water is added, binder and dispersing agent are sequentially added, with ball milling mixing
After 12~24 hours, distributed slurry is obtained after 80~200 mesh net filtrations, and its solid content is made to reach 50%~70%, on
State binder, the weight of dispersing agent is respectively the 0.9%~11% of main material, 0.5%~3.5%;
(2) mist projection granulating: being dried gained slurry with spray dryer, sets hot wind inlet temperature as 160~300 DEG C,
Outlet temperature is 60~200 DEG C, and slurry flow is 10~100 ㎏/h, and atomizer adjusts the speed 10~30Hz, does to above-mentioned slurry
It is dry, 100~200 meshes are crossed, the compound powder of silicon carbide is obtained;
(3) production of hybrid seeds: taking the compound powder to be pressed into ceramics biscuits of carbonized bricks, crosses 40~100 meshes after being crushed to it to obtain the final product
The seed of balling-up;
(4) balling-up: seed is put into nodulizer, opens nodulizer, adjusts nodulizer revolving speed and angle, make nodulizer revolving speed and
Angle is directly proportional to the size of ball, 20~50r/min of revolving speed, 10~80 ° of angle, continuously sprays water and be added pelletizing into machine,
Circulating rolling repeats this operating process, until Ceramic Balls grow to required size;
(5) it is sintered: silicon carbide ceramics ball base is put into vacuum sintering furnace, heat up sintering after vacuumizing, argon gas protection, heating speed
Rate is 3~30 DEG C/min, is warming up to 1820~2280 DEG C, then keep the temperature 120~240 minutes, up to high-densit carbon after Temperature fall
SiClx Ceramic Balls.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111848174A (en) * | 2020-07-30 | 2020-10-30 | 山东中鹏特种陶瓷有限公司 | Method for producing wear-resistant silicon carbide ceramic block based on press machine |
CN112479716A (en) * | 2020-12-14 | 2021-03-12 | 山田研磨材料有限公司 | Extrusion molding process for pressureless sintering silicon carbide |
CN114538896A (en) * | 2022-01-28 | 2022-05-27 | 中国科学院近代物理研究所 | Method for producing beryllium oxide ceramic balls in large scale by adopting roll forming process |
CN115925425A (en) * | 2022-12-02 | 2023-04-07 | 江苏高越高新科技有限公司 | Silicon carbide ball manufacturing process |
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JPS56145000A (en) * | 1980-04-15 | 1981-11-11 | Kyoto Ceramic | Ball for ball pen in nonoxide group ceramic |
JP2004189524A (en) * | 2002-12-10 | 2004-07-08 | Nippon Steel Corp | Method of manufacturing silicon carbide fine particles-dispersed ceramic sintered compact |
CN102311268A (en) * | 2011-08-30 | 2012-01-11 | 河南新大新材料股份有限公司 | Highly compact ceramic ball of silicon carbide and preparation process thereof |
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JPS56145000A (en) * | 1980-04-15 | 1981-11-11 | Kyoto Ceramic | Ball for ball pen in nonoxide group ceramic |
JP2004189524A (en) * | 2002-12-10 | 2004-07-08 | Nippon Steel Corp | Method of manufacturing silicon carbide fine particles-dispersed ceramic sintered compact |
CN102311268A (en) * | 2011-08-30 | 2012-01-11 | 河南新大新材料股份有限公司 | Highly compact ceramic ball of silicon carbide and preparation process thereof |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111848174A (en) * | 2020-07-30 | 2020-10-30 | 山东中鹏特种陶瓷有限公司 | Method for producing wear-resistant silicon carbide ceramic block based on press machine |
CN112479716A (en) * | 2020-12-14 | 2021-03-12 | 山田研磨材料有限公司 | Extrusion molding process for pressureless sintering silicon carbide |
CN114538896A (en) * | 2022-01-28 | 2022-05-27 | 中国科学院近代物理研究所 | Method for producing beryllium oxide ceramic balls in large scale by adopting roll forming process |
CN115925425A (en) * | 2022-12-02 | 2023-04-07 | 江苏高越高新科技有限公司 | Silicon carbide ball manufacturing process |
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