CN106915966A - A kind of preparation method of reaction sintering silicon carbide ceramic product - Google Patents
A kind of preparation method of reaction sintering silicon carbide ceramic product Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of reaction sintering silicon carbide ceramic product, comprise the following steps：(1) slurry is prepared, slurry is put into batch mixing pulping equipment, stirs and is prepared into slip casting slurry；(2) slurry is injected into and is molded in porous resin moulds, obtains green compact, and green compact are being obtained dry body by note (3) as in baking oven.(4) dry body is carried out into siliconising reaction-sintered in high-temperature vacuum sintering furnace, under vacuum maximum temperature be 1350~1750 DEG C at carry out siliconising, insulation 0.5~5 hour, cooling after obtain finished product.The Preparation equipment floor space of the method is small, production efficiency is high, can realize automated production, and the product of shaping has the advantages that consistency is high, uniformity is good；Advantages of nontoxic raw materials, and drying efficiency is high, it is with short production cycle；Its cost is greatly reduced, and the uniformity of product is more preferable；The product of production is more diversified, can meet the production of large size special-shaped the part with complicated structure.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, ceramic colloidal pressure molding technique technique is related generally to, it is specific next
Say it is a kind of preparation method of use high-pressure slip-casting shaping reaction sintering silicon carbide ceramic product.
Background technology
Reaction sintering silicon carbide ceramic is reacted prepare at high temperature using molten silicon with carbon containing/carborundum biscuit
Silicon/silicon carbide composite, the method sintering process does not have change in size, for prepare big-size complicated shape product have compared with
Obvious advantage.
Reaction sintering silicon carbide ceramic have excellent wearability, high intensity, preferable toughness, corrosion resistance and preferably
Inoxidizability, it is widely used in technical fields such as mechanical seal, chemical industry, the energy and military projects.
The forming method of current reaction sintering silicon carbide ceramic have gypsum mould grouting shaping, gel casting forming, dry-pressing into
Type and extrusion molding etc..Gypsum injection forming is a kind of more traditional preparation method, and its process is the slurry that will first prepare
Material carries out midge shaping in being injected into plaster mold, and the demoulding obtains green compact after base substrate has some strength；Given birth to using this technique
Product reaction sintering silicon carbide ceramic efficiency is low, product thickness is limited, need substantial amounts of gypsum mold and larger place to be produced
And product yield rate is relatively low and poor-performing.
" a kind of preparation method of silicon carbide reaction-sintered " disclosed in Application No. 2015106629369.3 is noted using gel
The slurry that mold forming method will be prepared forms gel in being injected into mould, and the demoulding obtains green compact after product has some strength.
Using the monomer of acrylamide as gel, it has stronger neurotoxin to this technique, is unfavorable for large-scale production；
And green compact moisture content after the demoulding is higher so that being easy to the phenomenons such as product craze and transfiguration occur in drying process, it usually needs
The drying device of high humility so that drying efficiency is low, the production cycle is long.
" a kind of reaction sintering silicon carbide ceramic and its production method " of Patent No. CN101289319B using dry-pressing into
By mist projection granulating powder in mould, then shaping, the demoulding obtain overall shellproof sheet material green compact to the method for type under a certain pressure.Adopt
The preferable mist projection granulating powder of mobility is generally required in this way so that production cost is greatly improved, and is used dry-pressing formed
Method be difficult to for the shaping of abnormal complex shaped products, and, product poor for large scale product uniformity
Can be difficult to reach requirement.
The method that a kind of " silicon carbide green body and its production technology " of Patent No. CN102219520B uses extrusion molding
Silicon carbide reaction-sintered square beam, club class product are molded.Extruding-out process is generally needed using vacuum pugging device system
The standby preferable pug of quality, and extrusion molding is difficult to be molded the product of complicated shape, and extrusion molding product thickness compared with
It is small.
The content of the invention
The technical problem to be solved in the present invention is to provide and a kind of is carbonized with existing conventional cast injection forming reaction-sintered
The preparation method of silicon ceramics is compared to its occupation area of equipment is small, production efficiency is high, can realize automated production, and the product being molded
Product have the advantages that consistency is high, uniformity is good；Compared with gel casting forming, advantages of nontoxic raw materials, and also drying efficiency is high, production
Cycle is short；Compared with dry-pressing formed, it need not carry out mist projection granulating, and its cost is greatly reduced, and product uniformity
More preferably；Compared with extrusion molding, the product of production is more diversified, can meet the reaction of the production of large size special-shaped the part with complicated structure
The preparation method of sintered silicon carbide ceramics product.
The technical scheme is that, there is provided a kind of a kind of reaction sintering silicon carbide ceramic product with following methods
Preparation method, comprises the following steps：(1) slurry is prepared, the slurry includes each component of following percentage by weight：Carborundum powder
Body is that 45~98wt% carbon sources are 2~50wt%, and dispersant is 0.1~8wt%, and bonding agent is 0.1~20wt%, deionized water
It is 20~50wt%, above each component weight sum is 100%；The above raw material is put into batch mixing pulping equipment, stirring is equal
It is even to be prepared into slip casting slurry；(2) first slip casting slurry is drawn into the filling of the storing of high-pressure grout injector, is then injected into slurry
It is molded in porous resin moulds, obtains green compact, it is 5~800 seconds certain pressing time that slip casting condition is, grouting pressure 1.5~
10MPa, the dwell time is 10~800s, the 0.1~10MPa of injection forming pressure of the high-pressure grout injector, the porous resin
The resin stomata meso-position radius of mould are 5~50 μm；(3) by green compact as the drying 5~24 at a temperature of 30~150 DEG C in baking oven
Dry body is obtained after hour.(4) dry body is carried out into siliconising reaction-sintered in high-temperature vacuum sintering furnace, under vacuum the highest temperature
Spend to obtain finished product after siliconising, insulation 0.5~5 hour, cooling are carried out at 1350~1750 DEG C.
The carbon source be carbon black, graphite powder, coke blacking, petroleum coke powder and organic matter pyrolysis carbon in one kind or one kind with
Upper mixing.
The dispersant is ammoniacal liquor, TMAH, ammonium polyacrylate, polyethyleneimine, calgon, trimerization
One or more mixing in sodium phosphate, polyethylene glycol, PVP.
The bonding agent is sodium carboxymethylcellulose, gum arabic, xanthans, phenolic resin, polyvinyl alcohol, propylene
One or more mixing in acid, lignosulfite, dextrin.
The dry body being eventually fabricated includes overall tabular, cylindric, ring-type and other abnormal complex shapes of sizes
Shape etc..
2~the 80mm of thickness of the dry body being eventually fabricated.
After above step, the technology of the present invention compared with prior art, with advantages below：The present invention is first by high pressure
Slip-casting shaping process is applied in the moulding process of reaction sintering silicon carbide ceramic product, is carbonized compared to the existing reaction-sintered for preparing
The technology of silicon ceramic, green compact preparation time of the present invention is short, and production efficiency is high, by slurry direct voltage injection forming, not only
The Production requirement of the Complex Different Shape product of sizes can be met, and production cost is greatly reduced, and the uniformity of product is greatly
Improve；The moisture content for preparing green compact is relatively low, and contraction distortion is small in drying process, and drying efficiency is high；In addition the technology can also be real
Existing automatic production process flow, and all big raising of product quality.(1) is anti-with existing conventional cast injection forming simultaneously
Answer that the preparation method of sintered silicon carbide ceramics is small by 1 compared to its occupation area of equipment, equipment is small；2nd, gypsum mould grouting needs substantial amounts of
Space is placed mould, the method for the present invention and is used and can complete that 3, production efficiency is high once secondary mould, and gypsum injection forming is given birth to
Base generally requires 24h, and the method for the present invention obtained green compact with regard to 10 minutes；4th, the green compact moisture content that the inventive method is obtained is low, does
Dry efficiency is improved；5th, automated production can be realized, because high-pressure slip-casting shaping sanitaryware has been carried out automation, Er Qiecheng
The product of type has consistency high, and the dependence of conventional cast injection forming is capillary force, and particle packing is not fine and close enough, and
This method is shaping under condition of high voltage, and its briquetting pressure is more much bigger than capillary force, and the accumulation of such natural particle is more
Closely；6th, uniformity is good, and gypsum mould grouting forming process relies on capillary force, is in a thickness direction to deposit in the consistency of product
In relatively large deviation, the local consistency near gypsum is high, and the local consistency away from plaster mold is low, and the method for the present invention is
Injection forming under high pressure, the difference on product thickness direction is significantly reduced, and uniformity is good.And gel casting forming (two)
Compare, advantages of nontoxic raw materials, and drying efficiency is high, it is with short production cycle.(3), compared with dry-pressing formed, it need not be sprayed
Granulation, is greatly reduced its cost, and the uniformity of product is more preferable；Compared with extrusion molding, the product of production is more various
Change, the production of large size special-shaped the part with complicated structure can be met.
Specific embodiment
The invention will be further described for specific embodiment below.
Embodiment 1：
(1) by 98wt% carborundum, 2wt% graphite powders, 1.2wt% calgons, 10wt% phenolic resin, 35wt%
Deionized water stirring mixing 24 hours, obtains slip casting slurry.
(2) good high-pressure slip-casting slurry made above is sucked into high-pressure grout injector storing by suction tube to fill, by high pressure
Slip casting machine carries out injection forming, and injection forming pressure increases to 4MPa in 50s by 0.1MPa, is then protected under the high pressure of 4MPa
Pressure 100s, release, opening mold releasability, obtain green product, and the resin stomata meso-position radius of the porous resin moulds are 25 μm.
(3) by green product as baking oven in, dried 12 hours at 50 DEG C, 90 DEG C of dryings 2 hours are then warming up to again,
Obtain dry body product.
(4) carry out burying silicon sintering after dry body product is dewaxed in dewaxing furnace, 1600 DEG C of guarantors of the highest temperature under vacuum atmosphere
Warm 1h, density ＞ 3.00g/cm after the burning of product3, bending strength is ＞ 300MPa.
Embodiment 2：
(1) by 55wt% carborundum, 20wt% graphite powders, 25wt% carbon powders, 1.2wt% calgons, 0.6wt%
Carboxymethylcellulose calcium, 50wt% deionized waters stirring mixing 24 hours, obtain slip casting slurry.
(2) good high-pressure slip-casting slurry made above is sucked into high-pressure grout injector storing by suction tube to fill, by high pressure
Slip casting machine carries out injection forming, and injection forming pressure increases to 4MPa in 50s by 0.1MPa, is then protected under the high pressure of 4MPa
Pressure 200s, release, opening mold releasability, obtain green product, and the resin stomata meso-position radius of the porous resin moulds are 25 μm.
(3) by green product as baking oven in, dried 12 hours at 50 DEG C, 90 DEG C of dryings 2 hours are then warming up to again,
Obtain dry body product.
(4) carry out burying silicon sintering after dry body product is dewaxed in dewaxing furnace, 1610 DEG C of guarantors of the highest temperature under vacuum atmosphere
Warm 1h, density ＞ 3.00g/cm after the burning of product3, bending strength is ＞ 300MPa.
Embodiment 3：
(1) by 75wt% carborundum, 25wt% graphite powders, 1.2wt% calgons, 0.6wt% carboxymethylcellulose calciums,
40wt% deionized waters stirring mixing 24 hours, obtains slip casting slurry.
(2) good high-pressure slip-casting slurry made above is sucked into high-pressure grout injector storing by suction tube to fill, by high pressure
Slip casting machine carries out injection forming, and injection forming pressure increases to 4MPa in 50s by 0.1MPa, is then protected under the high pressure of 4MPa
Pressure 100s, release, opening mold releasability, obtain green product, and the resin stomata meso-position radius of the porous resin moulds are 25 μm.
(3) by green product as baking oven in, dried 12 hours at 50 DEG C, 90 DEG C of dryings 2 hours are then warming up to again,
Obtain dry body product.
(4) carry out burying silicon sintering after dry body product is dewaxed in dewaxing furnace, 1610 DEG C of guarantors of the highest temperature under vacuum atmosphere
Warm 1h, density ＞ 3.00g/cm after the burning of product3, bending strength is ＞ 300MPa.
Embodiment 4：
(1) by 75wt% carborundum, 25wt% carbon powders, 1.2wt% calgons, 0.6wt% carboxymethylcellulose calciums,
45wt% deionized waters stirring mixing 24 hours, obtains slip casting slurry.
(2) good high-pressure slip-casting slurry made above is sucked into high-pressure grout injector storing by suction tube to fill, by high pressure
Slip casting machine carries out injection forming, and injection forming pressure increases to 4MPa in 50s by 0.1MPa, is then protected under the high pressure of 4MPa
Pressure 100s, release, opening mold releasability, obtain green product, the resin stomata meso-position radius of the porous resin moulds are 25 μm.
(3) by green product as baking oven in, dried 12 hours at 50 DEG C, 90 DEG C of dryings 2 hours are then warming up to again,
Obtain dry body product.
(4) carry out burying silicon sintering after dry body product is dewaxed in dewaxing furnace, 1610 DEG C of guarantors of the highest temperature under vacuum atmosphere
Warm 1h, density ＞ 3.00g/cm after the burning of product3, bending strength is ＞ 300MPa.
The above is only feature implementation example of the invention, the scope of the present invention is not limited in any way.It is all to use same
The technical scheme formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.
Claims (6)
1. a kind of preparation method of reaction sintering silicon carbide ceramic product, it is characterised in that：Comprise the following steps：(1) slurry is prepared
Material, the slurry includes each component of following percentage by weight：Silicon carbide powder is that 45~98wt% carbon sources are 2~50wt%,
Dispersant be 0.1~8wt%, bonding agent be 0.1~20wt%, deionized water be 20~50wt%, above each component weight it
Be 100%；The above raw material is put into batch mixing pulping equipment, is stirred and is prepared into slip casting slurry；(2) first slip casting is starched
Material is drawn into the filling of the storing of high-pressure grout injector, is then injected into slurry and is molded in porous resin moulds, obtains green compact, is noted
It is 5~800 seconds certain pressing time that slurry condition is, 1.5~10MPa of grouting pressure, the dwell time is 10~800s, the high pressure
0.1~the 10MPa of injection forming pressure of slip casting machine, the resin stomata meso-position radius of the porous resin moulds are 5~50 μm；(3)
By green compact as obtaining dry body after being dried 5~24 hours at a temperature of 30~150 DEG C in baking oven.(4) it is dry body is true in high temperature
Siliconising reaction-sintered is carried out in empty sintering furnace, under vacuum maximum temperature be 1350~1750 DEG C at carry out siliconising, insulation
0.5~5 hour, cooling after obtain finished product.
2. the preparation method of a kind of reaction sintering silicon carbide ceramic product according to claim 1, it is characterised in that：It is described
Carbon source is one or more mixing in carbon black, graphite powder, coke blacking, petroleum coke powder and organic matter pyrolysis carbon.
3. the preparation method of a kind of reaction sintering silicon carbide ceramic product according to claim 1, it is characterised in that：It is described
Dispersant is ammoniacal liquor, TMAH, ammonium polyacrylate, polyethyleneimine, calgon, sodium tripolyphosphate, poly- second
One or more mixing in glycol, PVP.
4. the preparation method of a kind of reaction sintering silicon carbide ceramic product according to claim 1, it is characterised in that：It is described
Bonding agent is sodium carboxymethylcellulose, gum arabic, xanthans, phenolic resin, polyvinyl alcohol, acrylic acid, sulfite cellulose
One or more mixing in waste liquid, dextrin.
5. the preparation method of a kind of reaction sintering silicon carbide ceramic product according to claim 1, it is characterised in that：It is described
Etc. the overall tabular of the dry body being eventually fabricated including sizes, cylindric, ring-type and other abnormal complex shapes.
6. the preparation method of a kind of reaction sintering silicon carbide ceramic product according to claim 1, it is characterised in that：It is described
2~the 80mm of thickness of the dry body being eventually fabricated.
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Cited By (9)
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| CN107673761A (en) * | 2017-10-27 | 2018-02-09 | 潍坊华美精细技术陶瓷股份有限公司 | A kind of preparation method of big specification compact silicon carbide ceramic plate |
| CN107696235A (en) * | 2017-09-20 | 2018-02-16 | 中山市华通达陶瓷科技有限公司 | A kind of molding method for preparing of zirconia ceramics cell phone rear cover |
| CN107827466A (en) * | 2017-11-27 | 2018-03-23 | 朱胜利 | The forming method and mould of reaction sintering silicon carbide ceramic are made using infiltration method |
| CN108706977A (en) * | 2018-06-04 | 2018-10-26 | 陕西固勤材料技术有限公司 | A kind of shove charge method of silicon carbide reaction-sintered |
| CN110002878A (en) * | 2019-02-25 | 2019-07-12 | 常州金艺广告传媒有限公司 | A kind of preparation method of high combination degree type silicon carbide/graphite sealing material |
| CN113134893A (en) * | 2020-01-20 | 2021-07-20 | 西部宝德科技股份有限公司 | Preparation method of ceramic fiber filter tube for high-temperature flue gas purification |
| CN114230356A (en) * | 2022-01-21 | 2022-03-25 | 辽宁科技大学 | Preparation method of silicon carbide fiber reinforced silicon carbide ceramic through catalytic conversion of glass fiber |
| CN114538950A (en) * | 2022-01-27 | 2022-05-27 | 南京航空航天大学 | Porous silicon carbide ceramic skeleton based on biomass powder as carbon source and preparation method thereof |
| CN116425550A (en) * | 2023-06-09 | 2023-07-14 | 成都超纯应用材料有限责任公司 | Reaction sintering silicon carbide and wet forming preparation method thereof |
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| CN116425550A (en) * | 2023-06-09 | 2023-07-14 | 成都超纯应用材料有限责任公司 | Reaction sintering silicon carbide and wet forming preparation method thereof |
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