CN105461310A - Gel cast molding method for preparing shaped ceramic body - Google Patents

Gel cast molding method for preparing shaped ceramic body Download PDF

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CN105461310A
CN105461310A CN201510790682.5A CN201510790682A CN105461310A CN 105461310 A CN105461310 A CN 105461310A CN 201510790682 A CN201510790682 A CN 201510790682A CN 105461310 A CN105461310 A CN 105461310A
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deionized water
ceramic
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agent
preparation
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江国健
贺常付
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Shanghai Institute of Technology
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    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6022Injection moulding

Abstract

The invention provides a gel cast molding method for preparing a shaped ceramic body. The method is as below: adding, a binder, an additive and a dispersant into a solvent of deionized water, stirring for 10-30 min to obtain a solution, wherein the weight ratio of dispersant, binder, additive and deionized water is (0.15-1.5):(1-3):(0.45-0.9):100; adding a ceramic powder into the above solution, wherein the weight ratio of ceramic powder and deionized water is (160-650):100; conducting ball milling; degassing the obtained slurry under vacuum to obtain a ceramic slurry; and injecting the obtained ceramic slurry into a mold, curing at 30-80 DEG C, stripping and drying to obtain the gel cast molding shaped ceramic body. The preparation method of the invention has the advantages of low content of total organic matters, low production cost, and easiness to control; the ceramic biscuit has high strength, smooth surface, intactness and smoothness. The method is especially for molding of ceramic parts with complex shapes.

Description

A kind of preparation method of gel casting forming special-shaped ceramics base substrate
Technical field
The invention belongs to field of ceramic preparation technology, relate to a kind of preparation method of special-shaped ceramics base substrate, specifically a kind of preparation method of gel casting forming ceramic body.
Background technology
Ceramic body is shaping is a key link in stupalith preparation technology, and the defect that moulding process causes often is difficult to be eliminated in sintering process thereafter, so it directly affects the stuctures and properties of material.Traditional moulding process (as dry-pressing formed) is difficult to the ceramic component preparing profiled shape; And common injection forming is only limited to thin wall ceramic parts, density gradient is existed for thicker-walled ceramic base substrate inside, when burning till, easily produces defect and cracking.
Since the nineties in 20th century, many scientific research institutions are devoted to the research of novel colloidal state forming technique, make some progress.Wherein the most successfully example is the gel-casting technology that U.S.'s Oak Ridge laboratory proposed in 1991.The three-dimensional network gel that this technology utilization organic monomer polyreaction is formed, makes ceramic slurry curing become to have the base substrate of suitable intensity.This technique is applicable to multiple ceramic systems, and the blank strength of acquisition is high, good uniformity, can carry out mechanical workout.(CN1705545A) adds hot preparation base substrate by mould to green compact separately " to prepare the method for ceramic green ", solvent is spun off between green surface and mould from green compact and forms solvent membrane, be easy to the demoulding, the billet surface of preparation be smooth, outward appearance not damaged; The toughener that " a kind of ceramic green body reinforcing agent and application " (CN103420680) makes with Xylo-Mucine, wilkinite and trisodium phosphate different ratio prepares ceramic body, prepared ceramic body intensity is high, be easy to shaping, improve the bonding properties of powder, improve the problems such as base substrate vibration on the conveyor line, distortion; " method of water-soluble epoxy resin in situ solidification for preparing ceramic blank " (CN1864961A) is with polymine or dipropanetriamine and water miscible epoxy resin in situ solidification for preparing ceramic blank, high and the good toughness of prepared ceramic body intensity, shaping for oxide ceramics, non-oxide ceramics or composite ceramics.But there is deficiency clearly in above method:
(1), because the oxygen in air can hinder polyreaction, therefore billet surface polyreaction is incomplete, can peel off, cannot prepare intact ceramic body after drying.In order to overcome the inhibition of surperficial oxygen, the method adopted at present is cured under inert atmosphere protection.So not only equipment requirements improves greatly, and complex process, is difficult to apply.
, organism large usage quantity used, and toxicity is comparatively large, as monomeric acrylamide, methylene-bisacrylamide, solidifying agent polymine have hormesis to eyes, skin, respiratory tract and mucous membrane, can endanger the health of operator; In sintering process, organic burning produces a large amount of waste gas simultaneously, and environmental pollution is serious, more makes this technique not easily be accepted.
(3), in this class methods preparation process organism amount ratio is comparatively large, and cost compare is high, is unsuitable for large-scale production.And some other novel colloidal state forming technique (as shaping in direct coagulation casting, temperature-induced flocculation) is because be only applicable to minority ceramic systems, and gained blank strength is low, is difficult to promote industrialization.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation method of gel casting forming ceramic body, the preparation method of described this gel casting forming ceramic body solves method complex process, cost is high, blank strength is low, environmental pollution the is serious technical problem of preparing ceramic body of the prior art.
The invention provides a kind of preparation method of gel casting forming special-shaped ceramics base substrate, comprise the following steps:
1) take deionized water as solvent, binding agent, auxiliary agent and dispersion agent are added in deionized water, stir 10-30min, obtained solution, wherein, the mass ratio of dispersion agent, binding agent, auxiliary agent and deionized water is (0.15-1.5): (0.5-3): (0.45-0.9): 100; Described dispersion agent is any one in Triammonium citrate, polyoxyethylene glycol or polyacrylic acid and multipolymer thereof, and the purity of above-mentioned substance is 98.50%-99.00%; Described auxiliary agent is any one in silicon sol or rare earth oxide, and the purity of above-mentioned substance is 30.00%-50.00%; Described binding agent is any one in carboxymethyl cellulose-methyl methacrylate graft copolymer, polyvidone or TDE-85 epoxy resin, and the purity of above-mentioned substance is 98.00%-99.00%;
2) in above-mentioned solution, ceramic powder is added, ball milling 0.5-1.5h, to the slurry obtained degasification 5 ~ 20min under vacuum; Wherein, the mass ratio of ceramic powder and deionized water is (160-650): 100; Described ceramic powder is alumina powder jointed, Zirconium powder, silicon carbide powder or SiC/SiO 2any one in composite granule;
3) ceramic size obtained is injected mould, under 30-80 DEG C of condition, solidify 2-5h, then the demoulding, dry, the ceramic body of obtained gel casting forming abnormity component.
Finally, dried biscuit is carried out pre-burning and pressureless sintering obtains special-shaped ceramics.
Further, described mould is any one in the waterproof mould be made up of metal, glass, rubber or plastics.
Further, described drying is dry under humidity is greater than the room temperature of 40%.
Preparation method of the present invention is owing to have employed lower than dispersion agent, binding agent, auxiliary agent total content in prior art, and namely the mass ratio of organic total amount and deionized water is (1.1-5.4): 100, greatly reduces organic consumption.Further, preparation method of the present invention is owing to have employed dispersion agent, binding agent, auxiliary agent unlike the prior art, thus this technology is suitable for oxide powder, non-oxide powder or that their composite granules are dissimilar and profiled shape is ceramic is shaping, gained billet surface is smooth, intensity is high, and the acrylamide system comparatively commonly used of intensity and water-soluble epoxy resin system increase 5%-25%.And owing to have employed dispersion agent, binding agent, auxiliary agent unlike the prior art, their equal safety non-toxics, to operator and environmental hazard little, therefore in safety in utilization etc., be provided with technique effect more better than prior art.
The present invention compares with prior art, and its technical progress is significant.Preparation method of the present invention is a kind of aqueous colloidal forming method, and technique is simple, does not need specific equipment; production process environmental friendliness, to operator and environmental hazard little, total amount of organic is low; production cost is low, easily controls, and biscuit of ceramics intensity is high; smooth surface; intact bright and clean, be particularly useful for the shaping of complicated shape ceramic component, applied widely; be easy to large-scale production, application prospect is large.
Accompanying drawing explanation
Fig. 1 and Fig. 2 is the photo of the embodiment of the present invention 1 gained base substrate after burning till, and the bright and clean nothing of sample surfaces is peeled off.
Embodiment
Below by specific embodiment, also the present invention is further elaborated by reference to the accompanying drawings, but be not limited to the present invention.
Embodiment 1
Take deionized water as solvent, dispersion agent, binding agent and auxiliary agent are added in deionized water, stir 10min, obtained solution; Wherein, dispersion agent: binding agent: auxiliary agent: the mass ratio of deionized water is 0.15:1:0.5:100, alumina powder jointed: the mass ratio of deionized water is 350:100, alumina-ceramic powder median size 20 μm.With planetary ball mill mixing 20min, and to the slurry obtained degasification 10min under vacuum, obtained alumina slurry, described alumina slurry is injected special metal die, 3h is solidified under 80 DEG C of conditions, the demoulding, dry be greater than the room temperature condition of 50% in humidity under, obtained size is good, the alumina sensor base for supporting ceramic body of any surface finish.
Embodiment 2
Take deionized water as solvent, dispersion agent, binding agent and auxiliary agent are added in deionized water, stir 10min, obtained solution; Wherein, dispersion agent: binding agent: auxiliary agent: the mass ratio of deionized water is 0.35:0.5:0.8:100, alumina powder jointed: the mass ratio of deionized water is 450:100, alumina-ceramic powder median size 10 μm.With planetary ball mill mixing 25min, and to the slurry obtained degasification 10min under vacuum, obtained alumina slurry, described alumina slurry is injected special metal die, 3.5h is solidified under 80 DEG C of conditions, the demoulding, dry be greater than the room temperature condition of 40% in humidity under, obtained size is intact, the alumina tube ceramic body of any surface finish.
Embodiment 3
Take deionized water as solvent, dispersion agent, binding agent and auxiliary agent are added in deionized water, stir 5min, obtained solution; Wherein, dispersion agent: binding agent: auxiliary agent: the mass ratio of deionized water is 1.5:2.5:0.45:100, Zirconium powder: the mass ratio of deionized water is 650:100, zirconia ceramics powder median size 50 μm.With planetary ball mill mixing 35min, and to the slurry obtained degasification 15min under vacuum, obtained zirconium white suspended nitride, described zirconia slurry is injected special rubber mold, 2h is solidified under 70 DEG C of conditions, then the demoulding, is greater than under the room temperature condition of 70% dry in humidity, can obtain shape, zirconium white special-shaped ceramics base substrate that size is intact.
Embodiment 4
Take deionized water as solvent, dispersion agent, binding agent and auxiliary agent are added in deionized water, stir 5min, obtained solution; Wherein, dispersion agent: binding agent: auxiliary agent: the mass ratio of deionized water is 1.25:3:0.9:100, silicon carbide powder: the mass ratio of deionized water is 380:100, silicon carbide ceramics powder median size 10 μm.With planetary ball mill mixing 40min, and to the slurry obtained degasification 10min under vacuum, obtained silicon carbide suspended nitride, injects special mould of plastics by described silicon carbide slurry, under 70 DEG C of conditions, solidifies 30min, then the demoulding, base substrate after the demoulding is put into enclosed space, avoids air flowing, place more than 10h, then dry 2h under 60 DEG C of conditions in an oven, can obtain structural integrity, ganoid carborundum porous ceramics base substrate.
Embodiment 5
Take deionized water as solvent, dispersion agent, binding agent and auxiliary agent are added in deionized water, stir 5min, obtained solution; Wherein, dispersion agent: binding agent: auxiliary agent: the mass ratio of deionized water is 0.15:3:0.15:100, SiC/SiO 2powder: the mass ratio of deionized water is 480:100, SiC/SiO 2ceramics powder median size 25 μm.Successively SiC/SiO is disperseed by ultrasonic wave 2mixed powder 20min, and to the slurry obtained degasification 12min under vacuum, obtain uniform suspension, obtained mixed slurry, by described SiC/SiO 2homogeneous phase mixing slurry injects special metal die, in-situ solidifying 2h, the then demoulding under 80 DEG C of conditions, is greater than under the room temperature condition of 80% dry in humidity, can obtain shape, SiC/SiO that size is intact 2composite ceramics base substrate.
Embodiment 6
Take deionized water as solvent, dispersion agent, binding agent and auxiliary agent are added in deionized water, stir 5min, obtained solution; Wherein, dispersion agent: binding agent: auxiliary agent: the mass ratio of deionized water is 0.80:1.5:0.75:100, the AlON powder of anti-hydration process: the mass ratio of deionized water is 300:100, AlON ceramics powder median size 20 μm.With planetary ball mill mixing 40min, and to the slurry obtained degasification 20min under vacuum, obtained AlON suspended nitride, described AlON slurry is injected special rubber mold, 2h is solidified under 40 DEG C of conditions, then the demoulding, is greater than under the room temperature condition of 50% dry in humidity, can obtain that shape is intact, the AlON crystalline ceramics base substrate of any surface finish.
In sum, the preparation method of a kind of gel casting forming special-shaped ceramics base substrate of the present invention is a kind of aqueous colloidal forming method; technique is simple, does not need specific equipment, production process environmental friendliness; to operator and environmental hazard little, total amount of organic is low, and production cost is low; easy control, biscuit of ceramics intensity is high, smooth surface; intact bright and clean, be particularly useful for the shaping of complicated shape ceramic component, applied widely; be easy to large-scale production, application prospect is large.
The content of above-described embodiment be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.

Claims (3)

1. a preparation method for gel casting forming special-shaped ceramics base substrate, is characterized in that comprising the following steps:
1) take deionized water as solvent, binding agent, auxiliary agent and dispersion agent are added in deionized water, stirs 10-30min, obtained solution, wherein, the mass ratio of dispersion agent, binding agent, auxiliary agent and deionized water is (0.15-1.5): (0.5-3): (0.45-0.9): 100; Described dispersion agent is any one in Triammonium citrate, polyoxyethylene glycol or polyacrylic acid and multipolymer thereof, and the purity of above-mentioned substance is 98.50%-99.00%; Described auxiliary agent is any one in silicon sol or rare earth oxide, and the purity of above-mentioned substance is 30.00%-50.00%; 2) described binding agent is any one in carboxymethyl cellulose-methyl methacrylate graft copolymer, polyvidone or TDE-85 epoxy resin, and the purity of above-mentioned substance is 98.00%-99.00%;
2) in above-mentioned solution, ceramic powder is added, ball milling 0.5-1.5h, to the slurry obtained degasification 5 ~ 20min under vacuum; Wherein, the mass ratio of ceramic powder and deionized water is (160-650): 100; Described ceramic powder is alumina powder jointed, Zirconium powder, silicon carbide powder or SiC/SiO 2any one in composite granule;
3) ceramic size obtained is injected mould, under 30-80 DEG C of condition, solidify 2-5h, then the demoulding, dry, the ceramic body of obtained gel casting forming abnormity component.
2. the preparation method of gel casting forming special-shaped ceramics base substrate according to claim 1, is characterized in that: described mould is any one in the waterproof mould be made up of metal, glass, rubber or plastics.
3. the preparation method of gel casting forming special-shaped ceramics base substrate according to claim 1, is characterized in that: described drying is dry under humidity is greater than the room temperature of 40%.
CN201510790682.5A 2015-11-17 2015-11-17 Gel cast molding method for preparing shaped ceramic body Pending CN105461310A (en)

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CN107935628A (en) * 2017-11-28 2018-04-20 北京航空航天大学 A kind of properties of SiC foam ceramics and preparation method thereof
CN108096928A (en) * 2017-11-25 2018-06-01 福建省德化县稀德利精密陶瓷有限公司 Compound alumina ceramic filter and preparation method thereof
CN109761614A (en) * 2019-03-11 2019-05-17 北京中材人工晶体研究院有限公司 A kind of gel-casting method of AlON ceramics
CN113511918A (en) * 2021-06-30 2021-10-19 武汉工程大学 SiC smoke particle collector and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108096928A (en) * 2017-11-25 2018-06-01 福建省德化县稀德利精密陶瓷有限公司 Compound alumina ceramic filter and preparation method thereof
CN107935628A (en) * 2017-11-28 2018-04-20 北京航空航天大学 A kind of properties of SiC foam ceramics and preparation method thereof
CN107935628B (en) * 2017-11-28 2020-07-28 北京航空航天大学 Foam silicon carbide ceramic and preparation method thereof
CN109761614A (en) * 2019-03-11 2019-05-17 北京中材人工晶体研究院有限公司 A kind of gel-casting method of AlON ceramics
CN113511918A (en) * 2021-06-30 2021-10-19 武汉工程大学 SiC smoke particle collector and preparation method thereof
CN113511918B (en) * 2021-06-30 2022-09-27 武汉工程大学 SiC smoke particle collector and preparation method thereof

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Application publication date: 20160406