CN1686945A - Silica sol solidification method for forming ceramic component - Google Patents
Silica sol solidification method for forming ceramic component Download PDFInfo
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- CN1686945A CN1686945A CN 200510011516 CN200510011516A CN1686945A CN 1686945 A CN1686945 A CN 1686945A CN 200510011516 CN200510011516 CN 200510011516 CN 200510011516 A CN200510011516 A CN 200510011516A CN 1686945 A CN1686945 A CN 1686945A
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- ceramic
- silicon sol
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- silicon
- coagulation forming
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- 239000000919 ceramic Substances 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 24
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title abstract 4
- 238000007711 solidification Methods 0.000 title 1
- 230000008023 solidification Effects 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 18
- 230000015271 coagulation Effects 0.000 claims abstract description 15
- 238000005345 coagulation Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 41
- 229910052710 silicon Inorganic materials 0.000 claims description 38
- 239000010703 silicon Substances 0.000 claims description 38
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 35
- 239000002002 slurry Substances 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 9
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 9
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- BWKOZPVPARTQIV-UHFFFAOYSA-N azanium;hydron;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [NH4+].OC(=O)CC(O)(C(O)=O)CC([O-])=O BWKOZPVPARTQIV-UHFFFAOYSA-N 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 150000003376 silicon Chemical class 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract 2
- 230000001112 coagulating effect Effects 0.000 abstract 1
- 238000000465 moulding Methods 0.000 description 10
- 238000010907 mechanical stirring Methods 0.000 description 6
- 230000002950 deficient Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000005266 casting Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a method for producing ceramic component by utilizing silica sol coagulation forming process. Said method includes the following steps: mixing ethyl orthosilicate and sodium hydroxide solution, mechanically-stirring to make the ethyl orthosilicate be hydrolyzed to obtain silica sol, then adding the engineering ceramic powder into said silica sol solution, stirring and mixing then to obtain ceramic pulp material, injuecting said ceramic pulp material into a hole-free mould, coagulating at 25-10 deg.C and forming so as to obtain the ceramic blank body with required shape.
Description
Technical field
The present invention relates to a kind of novel method of forming ceramic parts.Adopt this technology can make inviscid poor project ceramic size direct coagulation casting desired shape, obtain ceramic body with certain intensity.Belong to technical field of material.
Background technology
Engineering ceramic material, as aluminum oxide, zirconium white, silicon nitride, silicon carbide etc., because of having high strength, high rigidity, a series of excellent mechanical property and chemical stability such as high temperature resistant, wear-resistant and anticorrosive, therefore more and more many in modern science and technology and industrial circle (as aspects such as space flight, chemical industry, machinery, information, electronics, life sciences) application.These materials are many to be used as a kind of structure unit, has various different shapeies, and requires size accurate, reaches near-net-shape.Traditional forming manufacture technique such as ceramic component dry-pressing formed and the very difficult preparation of cold isostatic compaction complicated shape, and common injection forming is only limited to the thin-walled ceramic component, there is density gradient for heavy wall ceramic molding inside, and is easy to generate defective and cracking during sintering.
In recent years, some new ceramic size direct coagulation casting technologies have been developed in the world, as U.S.'s Oak Ridge National Laboratory a kind of method that is referred to as gel casting forming is proposed, this technology is the three dimensional gel network that utilizes the organic monomer polyreaction to form, thereby in-situ solidifying becomes ceramic body after making ceramic suspension body inject mould, this method can moulding different sorts and difform engineering ceramics parts, but because organic monomer has certain toxicity mostly; In addition, during monomer polymerization and the dry rear surface of air contact part such as cracks at defective.Therefore, this process application is restricted.
Summary of the invention
The present invention proposes the novel method that a kind of new ceramic size consolidation in-situ forming goes out ceramic component.Its principle is at room temperature, tetraethoxy and sodium hydroxide solution are mixed, make teos hydrolysis generate silicon sol by the mechanical force stirring, again the engineering ceramics powder is added in this silicon sol solution, mix and obtain ceramic size, this ceramic size is injected in the non-punch die, under 25～10 ℃ of temperature, just can comparatively fast solidifies, mold the ceramic body of desired shape.Adopt the plastic various complicated shape ceramic components of this method, can not produce defectives such as any crackle.
The method of the silicon sol coagulation forming ceramic component that the present invention proposes, it is characterized in that: described method is that tetraethoxy and sodium hydroxide solution are mixed, make teos hydrolysis generate silicon sol by the mechanical force stirring, again the engineering ceramics powder is added in this silicon sol solution, mix and obtain ceramic size, this ceramic size is injected in the non-punch die, under 25～10 ℃ of temperature, solidify, mold the ceramic body of desired shape, this method comprises following steps successively:
(1) at first prepare silicon sol liquid, tetraethoxy is mixed with sodium hydroxide solution, the volume ratio of the two is 6: 4～8: 2, stirs under the room temperature, places then, obtains silicon sol;
(2) with ceramic powder, add in the above-mentioned silicon sol solution as aluminum oxide, zirconium white, silicon nitride, silicon carbide, fully stir and obtain homodisperse ceramic size, the volume ratio of ceramic powder and silicon sol liquid is 40～60: 60～40;
(3) above-mentioned homodisperse ceramic size is poured into a mould, the non-punch die that adopts metal, plastics or glass material to make is placed under 10～25 ℃ of conditions behind the slurry injection mould and is solidified the demoulding.
In the method for above-mentioned silicon sol coagulation forming ceramic component, the dispersion agent of described step (2) is a polyacrylate solution, tetramethyl ammonium hydroxide solution, polyacrylic acid solution, citric acid ammonia, add any in the sodium polyacrylate solution, described dispersion agent add-on is in the 2wt% of ceramics powder weight.
In the method for above-mentioned silicon sol coagulation forming ceramic component, the sodium hydroxide solution pH value of described step (1) is 10.0～13.0.
In the method for above-mentioned silicon sol coagulation forming ceramic component, described step (3) is carried out drying in 60～100 ℃ then to the ceramic body demoulding behind the coagulation forming.
The present invention has following advantage:
1) is fit to different sorts, the moulding preparation of difform ceramic product;
2) the ceramic body any surface finish of moulding does not have any defective;
3) the molding blank dry tenacity is higher, and ceramic body is not fragile;
4) moulding process is simple, and silicon sol solution is easy to prepare, is convenient to produce.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
1) at first prepare silicon sol liquid, tetraethoxy is mixed with sodium hydroxide solution, the volume ratio of the two is 6: 4～8: 2.At room temperature stirred 1～4 hour, placed then 3～6 days, can obtain silicon sol.
2) with the engineering ceramics powder, add in the above-mentioned silicon sol solution as aluminum oxide, zirconium white, silicon nitride, silicon carbide etc., fully stir, the volume ratio of ceramic powder and silicon sol liquid is 40～60: 60～40.
3) above-mentioned homodisperse ceramic size is poured into a mould, the non-punch die that adopts metal, plastics or glass material to make, slurry was placed 20～60 minutes under 10～25 ℃ of conditions after injecting mould.The silicon sol molecule produces gel reaction gradually, forms network structure, thereby makes ceramic size be frozen into the ceramic body of desired shape.
4) ceramic body behind the coagulation forming has certain intensity, but direct demold carries out drying in 60～100 ℃ then, and dry back ceramic body bending strength can reach 5MPa.Blank strength than traditional injection forming is much bigger.
Embodiment 1: the moulding of alumina-ceramic ring
With the pH value is that 11.9 sodium hydroxide mixes under room temperature for 60 milliliters with tetraethoxy for broad 140 milliliters, and mechanical stirring 2 hours was placed 5 days then, obtained silicon sol solution.Again 700 gram ceramic powders are added this solution, add 7 milliliters of dispersion agent polyacrylate solution simultaneously.Adopt agitator to stir 1 hour, make its complete homodisperse, obtain stable ceramic size.Then above-mentioned ceramic size is injected metal die, is positioned over 15 ℃ and is cured, about 30 minutes slurries solidify and form the ceramic ring base substrate with certain intensity, get final product the demoulding.
Embodiment 2: the silicon carbide ceramic moulding
With the pH value is that 100 milliliters of 12.3 sodium hydroxide solutions mix under room temperature with 35 milliliters of tetraethoxys, and mechanical stirring 1.5 hours is placed and obtained silicon sol solution in 4 days; 480 gram silicon carbide ceramics powder are added in the above-mentioned silicon sol solution again, add 2 milliliters of tetramethyl ammonium hydroxide solutions simultaneously, mechanical stirring 1 hour reaches the stable silicon carbide ceramics slurry of complete dispersion suspension.In the mould that is about to the silicon carbide slurry injected plastic, place following 25 minutes disposed slurries of 10 ℃ of conditions to solidify, obtain the base substrate of silicon carbide ceramic.Shape is intact after the demoulding, nothing ftractures, do not have distortion.
Embodiment 3: the silicon nitride ceramics blank forming
With the pH value is that 120 milliliters of 12.8 sodium hydroxide solutions mix under room temperature with 43 milliliters of tetraethoxys, stirs about 1 hour, places and obtains silicon sol solution in 3 days.Again 570 gram silicon nitride ceramics are added and disperse in the silicon sol solution to stir, the polyacrylic acid solution that adds 1.5 milliliters simultaneously is as dispersion agent, mechanical stirring 1.5 hours, obtain finely dispersed silicon nitride slurry, slurry is injected in the glass mold, gel reaction solidifies under 15 ℃ of environment again, and disposed slurry solidify to form base substrate in about 40 minutes, then can direct demold, do not have and damage.
Embodiment 4: the zirconia ceramics moulding
Adopting the pH value is that 100 milliliters of 12.5 sodium hydroxide solutions at room temperature mix with 36 milliliters of tetraethoxys.Stirred 1.5 hours, place under the room temperature and obtained stable silicon sol solution in 4 days, again 510 gram zirconia ceramics powder are added in the above-mentioned solution, add citric acid ammonia simultaneously as dispersion agent, consumption is 5 grams, mechanical stirring 2 hours makes it to dissolve fully and disperses to obtain stable ceramic size, injects in the metal die then, carrying out gel reaction under 18 ℃ of conditions solidifies, after about 0.5 hour, slurry curing forms harder zirconia ceramics base substrate, gets final product the demoulding.At 60～100 ℃ of loft drier inner dryings, dry back ceramic body intensity further improves after the demoulding.
Embodiment 5: the moulding of quartz-ceramics rod
Quartzy powder is as the fused quartz ceramic powder, diameter of particle is about 2 microns, at first prepare silicon sol, adopting the pH value is that 150 milliliters of 12.5 sodium hydroxide solutions at room temperature mix with 55 milliliters of tetraethoxys, mechanical stirring 1 hour is placed and is obtained uniform silicon sol solution after 3 days, 700 gram quartz-ceramics powder is joined in the silicon sol solution again, adding sodium polyacrylate solution simultaneously is dispersion agent, consumption is 6 milliliters, and restir 1 hour obtains the good ceramic size of suspension, be injected in the metal die then, placed 16 ℃ of conditions following about 30 minutes, slurry solidifies, and obtains the quartz-ceramics rod, demoulding aftershaping base substrate is intact, does not have distortion and defective.
Claims (4)
1, the method for silicon sol coagulation forming ceramic component, it is characterized in that: described method is that tetraethoxy and sodium hydroxide solution are mixed, make teos hydrolysis generate silicon sol by the mechanical force stirring, again the engineering ceramics powder is added in this silicon sol solution, mix and obtain ceramic size, this ceramic size is injected in the non-punch die, under 25～10 ℃ of temperature, solidify, mold the ceramic body of desired shape, this method comprises following steps successively:
(1) at first prepare silicon sol liquid, tetraethoxy is mixed with sodium hydroxide solution, the volume ratio of the two is 6: 4～8: 2, stirs under the room temperature, places then, obtains silicon sol;
(2) with ceramic powder, add in the above-mentioned silicon sol solution as aluminum oxide, zirconium white, silicon nitride, silicon carbide, add dispersion agent again, fully stir and obtain homodisperse ceramic size, the volume ratio of ceramic powder and silicon sol liquid is 40～60: 60～40;
(3) above-mentioned homodisperse ceramic size is poured into a mould, the non-punch die that adopts metal, plastics or glass material to make is placed behind the slurry injection mould and is solidified the demoulding.
2, the method for silicon sol coagulation forming ceramic component according to claim 1 is characterized in that: the sodium hydroxide solution pH value of described step (1) is 10.0～13.0.
3, the method for silicon sol coagulation forming ceramic component according to claim 1, it is characterized in that: the dispersion agent of described step (2) is a polyacrylate solution, tetramethyl ammonium hydroxide solution, polyacrylic acid solution, citric acid ammonia, add any in the sodium polyacrylate solution, described dispersion agent add-on is in the 2wt% of ceramics powder weight.
4, the method for silicon sol coagulation forming ceramic component according to claim 1 is characterized in that: described step (3) is carried out drying in 60～100 ℃ then to the ceramic body demoulding behind the coagulation forming.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510011516 CN1686945A (en) | 2005-04-01 | 2005-04-01 | Silica sol solidification method for forming ceramic component |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510011516 CN1686945A (en) | 2005-04-01 | 2005-04-01 | Silica sol solidification method for forming ceramic component |
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Cited By (10)
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| CN102173744A (en) * | 2011-02-28 | 2011-09-07 | 吴龙华 | Ceramic dry-pressed product and preparation method thereof |
| CN101555166B (en) * | 2009-05-12 | 2012-07-04 | 东北大学 | Method for preparing ferric oxide ceramic thin film on the surface of three-dimensional network silicon carbide |
| CN102599829A (en) * | 2012-03-16 | 2012-07-25 | 王国栋 | Pollution-free durable crushing knife |
| CN103341343A (en) * | 2013-06-06 | 2013-10-09 | 华南理工大学 | Dedicated heating container for microwave synthesis of nanomaterials and preparation method thereof |
| CN105967692A (en) * | 2016-05-18 | 2016-09-28 | 顾向欣 | Manufacturing method of silicon-nitride-combined silicon carbide ceramic crucible |
| CN107188545A (en) * | 2017-06-20 | 2017-09-22 | 安徽省含山瓷业股份有限公司 | A kind of method that utilization Ludox compound suspension slip casting prepares aluminum oxide domestic ceramics base |
| CN107352557A (en) * | 2017-08-11 | 2017-11-17 | 中国天辰工程有限公司 | A kind of material for being used in rotary kiln crush block sial phosphorus molecular sieve |
| CN110328037A (en) * | 2019-07-16 | 2019-10-15 | 苏州电瓷厂股份有限公司 | A kind of porcelain insulator pretreatment of raw material ball-milling technology method and its application |
| CN111108077A (en) * | 2017-09-26 | 2020-05-05 | 德尔塔阀门公司 | Hydrogel injection molding formulations for ceramic products |
| CN112279670A (en) * | 2020-11-10 | 2021-01-29 | 衡阳凯新特种材料科技有限公司 | Low-shrinkage porous silicon nitride ceramic and preparation method thereof |
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2005
- 2005-04-01 CN CN 200510011516 patent/CN1686945A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101555166B (en) * | 2009-05-12 | 2012-07-04 | 东北大学 | Method for preparing ferric oxide ceramic thin film on the surface of three-dimensional network silicon carbide |
| CN102173744A (en) * | 2011-02-28 | 2011-09-07 | 吴龙华 | Ceramic dry-pressed product and preparation method thereof |
| CN102599829A (en) * | 2012-03-16 | 2012-07-25 | 王国栋 | Pollution-free durable crushing knife |
| CN103341343A (en) * | 2013-06-06 | 2013-10-09 | 华南理工大学 | Dedicated heating container for microwave synthesis of nanomaterials and preparation method thereof |
| CN103341343B (en) * | 2013-06-06 | 2015-09-16 | 华南理工大学 | A kind of preparation method of microwave synthetizing nano material heating container special |
| CN105967692A (en) * | 2016-05-18 | 2016-09-28 | 顾向欣 | Manufacturing method of silicon-nitride-combined silicon carbide ceramic crucible |
| CN105967692B (en) * | 2016-05-18 | 2017-05-03 | 顾向欣 | Manufacturing method of silicon-nitride-combined silicon carbide ceramic crucible |
| CN107188545A (en) * | 2017-06-20 | 2017-09-22 | 安徽省含山瓷业股份有限公司 | A kind of method that utilization Ludox compound suspension slip casting prepares aluminum oxide domestic ceramics base |
| CN107352557A (en) * | 2017-08-11 | 2017-11-17 | 中国天辰工程有限公司 | A kind of material for being used in rotary kiln crush block sial phosphorus molecular sieve |
| CN107352557B (en) * | 2017-08-11 | 2020-12-15 | 中国天辰工程有限公司 | Material for crushing massive silicon-aluminum-phosphorus molecular sieve in rotary kiln |
| CN111108077A (en) * | 2017-09-26 | 2020-05-05 | 德尔塔阀门公司 | Hydrogel injection molding formulations for ceramic products |
| US11384023B2 (en) | 2017-09-26 | 2022-07-12 | Delta Faucet Company | Aqueous gelcasting formulation for ceramic products |
| US11851376B2 (en) | 2017-09-26 | 2023-12-26 | Delta Faucet Company | Aqueous gelcasting method for ceramic products |
| CN110328037A (en) * | 2019-07-16 | 2019-10-15 | 苏州电瓷厂股份有限公司 | A kind of porcelain insulator pretreatment of raw material ball-milling technology method and its application |
| CN110328037B (en) * | 2019-07-16 | 2021-05-28 | 苏州电瓷厂股份有限公司 | Ball milling process method for pretreating porcelain insulator raw material and application thereof |
| CN112279670A (en) * | 2020-11-10 | 2021-01-29 | 衡阳凯新特种材料科技有限公司 | Low-shrinkage porous silicon nitride ceramic and preparation method thereof |
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