CN102515776A - Solidification method for gel injection molding slurry - Google Patents
Solidification method for gel injection molding slurry Download PDFInfo
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- CN102515776A CN102515776A CN2011104314451A CN201110431445A CN102515776A CN 102515776 A CN102515776 A CN 102515776A CN 2011104314451 A CN2011104314451 A CN 2011104314451A CN 201110431445 A CN201110431445 A CN 201110431445A CN 102515776 A CN102515776 A CN 102515776A
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Abstract
The invention discloses a solidification method for gel injection molding slurry. The solidification method comprises the following steps: putting a die which has been injected with ceramic slurry into a microwave heating device for low speed heating so as to allow interior temperature of the slurry to rise to 55 to 65 DEG C within 2 to 5 min; stopping heating for 1 to 5 min; carrying out low speed heating again so as to enable interior temperature of the slurry to rise to 75 to 85 DEG C within 2 to 5 min; naturally cooling the slurry to room temperature and opening the die so as to obtain a solidified ceramic biscuit. The solidification method provided in the invention has a fast solidification speed, allows solidification to be completed in 5 to 15 min, is simple and practicable, can effectively guarantee that the temperature of the slurry in the die is uniform and consistent during solidification and enables uniform high performance biscuits with a complete structure to be rapidly fabricated; furthermore, the method has the advantages of a shortened preparation period and reduced preparation cost, has important meaning and a practical value in preparation of oxide or non-oxide ceramic biscuits with a large size and a complex shape and accords with industrial application requirements.
Description
Technical field
The present invention relates to a kind of curing of gel injection slurry, belong to ceramic materials preparation technology field.
Background technology
Along with the development of modern science and technology, the advanced technology of preparing of high-performance ceramic parts becomes one of emphasis and focus of research, the particularly technology of preparing of large size, complicated shape goods.Stupalith not only is easy to generate defective in moulding process, and the defective that forms often is difficult to remedied and eliminate through subsequent technique.In addition, the high firmness of stupalith, high-wearing feature make following process relatively more difficult, and tooling cost is expensive, and for the goods of complicated shape, it is particularly thorny that processing problems seems.Therefore forming technique directly has influence on sintering, processing and the final performance of material as a key link in the preparation process.
Gel casting forming is a kind of new ceramics forming technique of U.S. Oak Ridge National Key Laboratory (Oak Ridge laboratory) in the early 1990s invention.It is a kind of near clean shape (near net-shape) forming method that polymer chemistry, colloid chemistry and ceramic technology are combined.The main raw material that gel injection molding and forming technology uses has solvent, powder, organic monomer, linking agent, initiator, catalyzer, dispersion agent and plastic agent etc.Its technology key is the stabiliser through colloidal state systems such as electrostatic stabilization or steric stabilizations, and preparation has high solids content, low viscous slurry.This technology comprises following process: at first powder is dispersed in the aqueous solution or non-aqueous solution that contains organic monomer and linking agent, adds initiator and catalyzer before the cast, after stirring and outgasing, slurry is injected mould; Under certain temperature condition, cause the organic monomer polymerization then, slurry viscosity is increased suddenly, thereby cause the slurry original position to be solidified, form wet base; After the wet base demoulding, dry at a certain temperature and humidity conditions, obtain the HS base substrate, with dry body binder removal and sintering, obtain compact components at last.
Gel injection molding and forming technology is compared with other moulding process has significant advantage: used additive can all use organism, and it is residual not have impurity behind the sintering; The green strength of moulding is very high, can directly carry out mechanical workout, is a kind of comparatively novel near net-shape in-situ solidifying forming technique, can make high quality, complex-shaped parts; With a processing difficult problem effective means and approach are provided for solving forming materials, thereby have obtained paying close attention to widely and having obtained significant progress.
Though gel casting forming successfully has been applied in oxide compound and non-oxide ceramics system; But in the preparation process, still there is a series of problem: when for example solidifying; Normally mould is placed in the thermostatic equipment in (like water-bath); Conduct heat through mould, the temperature of slurry is increased in 40～80 ℃ of scopes; After reaching design temperature, under this temperature, be incubated certain hour again, gelation reaction takes place in Gel Precursor (like acrylic amide) under the initiator effect, forms three-dimensional net structure, thereby realizes the moulding of slurry in-situ solidifying.This curing depends on the rate of heat transfer of mould and slurry; Influence because of factors such as mould size, shape, slurry quantity, rate of heat transfer, temperature controlling instrumentss; The slurry temperature of different sites is difficult to be consistent in the mould; This even, synchronous solidification process to slurry is unfavorable, thereby makes technology controlling and process become comparatively difficult; And, also can cause in the biscuit after the curing to have density gradient and structure non-uniform phenomenon because set time is long, and the ceramic particle in the slurry is because of the higher easy generation sedimentation of density; In addition, long-time curing causes the evaporation of moisture in the slurry easily and produces defective, influences the quality of product, and the probability that produces waste product increases.
Because in colloidal formations such as gel injection; The slurry solid content is often very high; The homogeneity of slurry is poor slightly will to cause defective in the base substrate after moulding, in the subsequent drying process, easily because the difference of local moisture vaporator rate; Cause the difference of the inner each several part shrinking percentage of base substrate, and then cause the appearance of body drying shrinkage anisotropy and internal stress; When internal stress during greater than the YV of plasticity base substrate, base substrate deforms; When internal stress surpassed the breakdown point of plasticity base substrate or surpasses the intensity of elasticity base substrate, base substrate ftractureed; For the sample of large size, complicated shape, this influence is particularly outstanding.Therefore, shorten set time, the temperature homogeneity of different sites when keeping solidifying guarantees to solidify synchronously, and is very crucial, also most important to subsequent drying and sintering process for preparation even structure, complete, high-quality gel injection biscuit.
At present, aspect slurry curing, still continue to use traditional curing modes such as fixed temperature and humidity curing oven, water bath with thermostatic control curing, baking oven isothermal curing both at home and abroad.Wherein the fixed temperature and humidity curing oven be under high humidity environment, realize and the water bath with thermostatic control curing seemingly.The temperature homogeneity of different sites in slurry when above curing mode can't guarantee to solidify cause the structure of biscuit inhomogeneous even introduce defective easily, and set time is long, and poor controllability is unfavorable for suitability for industrialized production.
Summary of the invention
To the problems referred to above and the deficiency that prior art exists, the purpose of this invention is to provide a kind of simple, fast, the method for efficient curing gel injection molding slurry, for preparation even structure, complete, high-quality gel injection biscuit provide a kind of convenient way.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is following:
A kind of curing of gel injection slurry comprises the steps:
The mould that a) will pour into ceramic size is put into microwave heating equipment, and heating makes the slurry internal temperature in 2～5 minutes, be raised to 55～65 ℃ at a slow speed;
B) stop to heat 1～5 minute;
C) heating at a slow speed once more makes the slurry internal temperature in 2～5 minutes, be raised to 75～85 ℃;
D) naturally cool to room temperature, open mould, promptly get the solidified biscuit of ceramics.
Described ceramic size can be oxide ceramics slurry (as: ceramic sizes such as aluminum oxide, zirconium white) or non-oxide ceramics slurry (as: ceramic sizes such as norbide, titanium carbide, silit).
The solid content of said ceramic size is preferably 40～60vol%.
The viscosity of said ceramic size is preferably 300～600mPa.s.
Described microwave heating equipment can be selected the microwave equipment that microwave oven, microwave dryer etc. can controlled heating for use.
Compared with prior art; Curing of the present invention has curing speed fast (only needing accomplish in 5～15 minutes), simple for process; The advantages such as uniformity consistency of slurry temperature in the mould in the time of effectively guaranteeing to solidify can make structural integrity, the shortening of high-performance biscuit, and preparation cycle uniformly, preparation cost reduction fast; The significant and practical value of preparation for the oxide compound or the non-oxide ceramics biscuit of large size and complicated shape meets requirement on industrial application.
Description of drawings
Fig. 1 is the cross-section morphology photo of the silicon carbide ceramics sample of biscuit of ceramics after sintering processes that made by embodiment 1.
Embodiment
Below in conjunction with embodiment and accompanying drawing to the present invention do further in detail, intactly explanation.
Embodiment 1
A) by prior art for preparing silicon carbide ceramics slurry: earlier the monomer acrylic amide is dissolved in the solution of processing 15wt% in the deionized water; Add linking agent N more successively; N '-methylene-bisacrylamide (MBAM) and dispersion agent TMAH (TMAH) are prepared premixed liquid; Add silicon carbide powder again, ball milling obtains the silicon carbide ceramics slurry about solid content 50vol%, and the viscosity of slurry is about 300～600mPa.s;
B) add initiator azo [2-(2-tetrahydroglyoxaline-2-yl)] propane hydrochloride salt (AZIP2HCl), add back violent stirring and deaeration, pour in the mould then;
The mould that c) will pour into ceramic size is put into microwave heating equipment, and heating makes the slurry internal temperature in 2 minutes, be raised to 55～65 ℃ at a slow speed; Stopped then heating 1 minute; Heating at a slow speed makes the slurry internal temperature in 2 minutes, be raised to 75～85 ℃ once more;
D) naturally cool to room temperature, open mould, promptly get the solidified ceramics biscuits of carbonized bricks.
The ceramics biscuits of carbonized bricks that makes is dry in the fixed temperature and humidity baking oven earlier, dry in a conventional oven then, to remove the moisture in the biscuit, concrete drying process can be referring to described in the Chinese patent 200910047502.9.With dried biscuit of ceramics unsticking in vacuum oven, place carbon tube furnace more then, in Ar atmosphere, carry out sintering (being warmed up to 2200 ℃ of insulation 1h), promptly obtain the silicon carbide ceramics sample.
Fig. 1 is the cross-section morphology photo of the silicon carbide ceramics sample that makes, and visible by Fig. 1: the sample microstructure is even, complete, does not have obvious crackle and defective.In addition, through observation, the sample surfaces after the polishing is a minute surface, and surface tissue is complete, does not have defective appearance such as obvious crackle.Thereby can further specify, can handle obtaining structural integrity, even, flawless high-performance ceramic biscuit by curing of the present invention.
Embodiment 2
A) by prior art for preparing titanium carbide ceramic size: earlier the monomer USAF RH-1 is dissolved in the solution of processing 15wt% in the deionized water; Add linking agent N more successively; N '-methylene-bisacrylamide (MBAM) and polyethylene of dispersing agent imines (PEI) are prepared premixed liquid; Add the titanium carbide powder again, ball milling obtains the titanium carbide ceramic size about solid content 50vol%, and the viscosity of slurry is about 300～600mPa.s;
B) add initiator ammonium persulfate (APS), add back violent stirring and deaeration, pour in the mould then;
The mould that c) will pour into ceramic size is put into microwave heating equipment, and heating makes the slurry internal temperature in 3 minutes, be raised to 55～65 ℃ at a slow speed; Stopped then heating 2 minutes; Heating at a slow speed makes the slurry internal temperature in 3 minutes, be raised to 75～85 ℃ once more;
D) naturally cool to room temperature, open mould, promptly get solidified titanium carbide biscuit of ceramics.
Through experiment showed, biscuit of ceramics structural integrity that present embodiment makes, evenly, zero defect.
Embodiment 3
A) by prior art for preparing boron carbide ceramics slurry: earlier with monomer N; The N-DMAA is dissolved in the solution of processing 15wt% in the deionized water; Add linking agent N more successively, N '-methylene-bisacrylamide (MBAM) and dispersion agent TMAH are prepared premixed liquid; Add boron carbide powder again, ball milling obtains the boron carbide ceramics slurry about solid content 57vol%, and the viscosity of slurry is about 400～600mPa.s;
B) add initiator azo (2-miaow base propane) hydrochloride (AZAP2HCl), add back violent stirring and deaeration, pour in the mould then;
The mould that c) will pour into ceramic size is put into microwave heating equipment, and heating makes the slurry internal temperature in 4 minutes, be raised to 55～65 ℃ at a slow speed; Stopped then heating 3 minutes; Heating at a slow speed makes the slurry internal temperature in 4 minutes, be raised to 75～85 ℃ once more;
D) naturally cool to room temperature, open mould, promptly get solidified boron carbide ceramics biscuit.
Through experiment showed, biscuit of ceramics structural integrity that present embodiment makes, evenly, zero defect.
Embodiment 4
A) in prior art for preparing alumina-ceramic slurry: earlier monomer acrylic amide and polyethylene glycol acrylate are dissolved in the solution of processing 15wt% in the deionized water according to 6: 1 ratio of mass ratio; Add linking agent more successively and gather (terepthaloyl moietie) dimethacrylate and dispersion agent ammonium polyacrylate, prepare premixed liquid; Add alumina powder jointedly again, ball milling obtains the alumina-ceramic slurry about solid content 50vol%, and the viscosity of slurry is about 300～600mPa.s;
B) add initiator azo [2-(2-tetrahydroglyoxaline-2-yl)] propane hydrochloride salt (AZIP2HCl), add back violent stirring and deaeration, pour in the mould then;
The mould that c) will pour into ceramic size is put into microwave heating equipment, and heating makes the slurry internal temperature in 5 minutes, be raised to 55～65 ℃ at a slow speed; Stopped then heating 4 minutes; Heating at a slow speed makes the slurry internal temperature in 5 minutes, be raised to 75～85 ℃ once more;
D) naturally cool to room temperature, open mould, promptly get solidified alumina-ceramic biscuit.
Through experiment showed, biscuit of ceramics structural integrity that present embodiment makes, evenly, zero defect.
Embodiment 5
A) by prior art for preparing zirconia ceramics slurry: earlier with monomer N; The N-DMAA is dissolved in the solution of processing 15wt% in the deionized water; Add linking agent more successively and gather (terepthaloyl moietie) dimethacrylate and dispersion agent ammonium polyacrylate, prepare premixed liquid; Add Zirconium powder again, ball milling obtains the zirconia ceramics slurry about solid content 50vol%, and the viscosity of slurry is about 300～600mPa.s;
B) add initiator azo (2-miaow base propane) hydrochloride (AZAP2HCl), add back violent stirring and deaeration, pour in the mould then;
The mould that c) will pour into ceramic size is put into microwave heating equipment, and heating makes the slurry internal temperature in 5 minutes, be raised to 55～65 ℃ at a slow speed; Stopped then heating 5 minutes; Heating at a slow speed makes the slurry internal temperature in 2 minutes, be raised to 75～85 ℃ once more;
D) naturally cool to room temperature, open mould, promptly get solidified zirconia ceramics biscuit.
Through experiment showed, biscuit of ceramics structural integrity that present embodiment makes, evenly, zero defect.
Microwave heating equipment described in the foregoing description can be selected the microwave equipment that microwave oven, microwave dryer etc. can controlled heating for use.
Be necessary at last to be pointed out that at this: above embodiment only is used for the present invention is explained further details; Can not be interpreted as restriction to protection domain of the present invention; For example: the kind of ceramic size of the present invention is not limited to described in the foregoing description, all can adopt curing of the present invention to handle so long as be applicable to the ceramic size of gel casting forming.And; Ceramic size of the present invention can adopt following prescription to make: with deionized water, ceramic powder, monomer, linking agent, initiator and dispersion agent is essentially consist; Wherein monomer can be vinylformic acid, dimethylaminoethyl methacrylate; The dimethylamino-propyl USAF RH-1; Hydroxy ethyl methacrylate, Rocryl 400, Propylene glycol monoacrylate, Rocryl 410, methoxy poly (ethylene glycol) monomethacrylates, methylacryoyloxyethyl trimethyl ammonium chloride, methacryloyl amido oxypropyl trimethyl ammonium chloride, methylacrylic acid, SSS, acrylic amide, USAF RH-1, N, any one in N-DMAA (DMAA), the vinyl pyrrolidone or the combination more than two kinds; The ratio of monomer and deionized water is between 30: 100～10: 100; Linking agent can be N, N '-methylene-bisacrylamide (MBAM) or gather (vinyl alcohol) dimethacrylate; Linking agent and monomeric mass ratio are 1: 15～1: 1; Initiator comprises ammonium persulphate/tetramethyl-ethylene base diamines (APS-TEMED), azo (2-miaow base propane) hydrochloride (AZAP2HCl) and azo [2-(2-tetrahydroglyoxaline-2-yl)] propane hydrochloride salt (AZIP2HCl); Wherein the addition of initiator is the 1/10-1/15 of monomer mass; Can select different dispersion agents for use to different powders; Also can adopt other prescription to make.
In a word, flesh and blood of the present invention is the curing to the gel injection slurry, and some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (5)
1. the curing of a gel injection slurry is characterized in that, comprises the steps:
The mould that a) will pour into ceramic size is put into microwave heating equipment, and heating makes the slurry internal temperature in 2～5 minutes, be raised to 55～65 ℃ at a slow speed;
B) stop to heat 1～5 minute;
C) heating at a slow speed once more makes the slurry internal temperature in 2～5 minutes, be raised to 75～85 ℃;
D) naturally cool to room temperature, open mould, promptly get the solidified biscuit of ceramics.
2. the curing of gel injection slurry according to claim 1 is characterized in that: described ceramic size is oxide ceramics slurry or non-oxide ceramics slurry.
3. the curing of gel injection slurry according to claim 1 is characterized in that: the solid content of said ceramic size is 40～60vol%.
4. the curing of gel injection slurry according to claim 1 is characterized in that: the viscosity of said ceramic size is 300～600mPa.s.
5. the curing of gel injection slurry according to claim 1 is characterized in that: described microwave heating equipment select for use can controlled heating microwave equipment.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242046A (en) * | 2013-05-21 | 2013-08-14 | 中国科学院上海硅酸盐研究所 | Radical system gel-casting method |
| CN105819868A (en) * | 2013-05-21 | 2016-08-03 | 中国科学院上海硅酸盐研究所 | Gel casting method for free radical system |
| CN107932706A (en) * | 2017-10-27 | 2018-04-20 | 中国科学院长春光学精密机械与物理研究所 | Gel casting forming meter level ceramics biscuits of carbonized bricks non-resistance drying device and method |
| CN108329031A (en) * | 2018-03-06 | 2018-07-27 | 济南大学 | A kind of preparation method of gel casting forming titanium carbide ceramic biscuit |
| CN109574649A (en) * | 2018-12-14 | 2019-04-05 | 镭米光学科技（宁波）有限公司 | A kind of preparation method of yttrium aluminum garnet transparent ceramic |
| CN110713387A (en) * | 2019-10-12 | 2020-01-21 | 华中科技大学 | Direct solidification injection molding method for microwave heating rapid curing ceramic slurry |
| CN115448704A (en) * | 2022-09-16 | 2022-12-09 | 中国科学院上海硅酸盐研究所 | Method for forming ceramic body |
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| CN101665360A (en) * | 2009-10-19 | 2010-03-10 | 中国海洋大学 | Microwave curing process for ceramic material gel casting |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242046A (en) * | 2013-05-21 | 2013-08-14 | 中国科学院上海硅酸盐研究所 | Radical system gel-casting method |
| CN105819868A (en) * | 2013-05-21 | 2016-08-03 | 中国科学院上海硅酸盐研究所 | Gel casting method for free radical system |
| CN105819868B (en) * | 2013-05-21 | 2018-09-28 | 中国科学院上海硅酸盐研究所 | A kind of method of free radical system gel casting forming |
| CN107932706A (en) * | 2017-10-27 | 2018-04-20 | 中国科学院长春光学精密机械与物理研究所 | Gel casting forming meter level ceramics biscuits of carbonized bricks non-resistance drying device and method |
| CN107932706B (en) * | 2017-10-27 | 2018-12-04 | 中国科学院长春光学精密机械与物理研究所 | Gel casting forming meter level ceramics biscuits of carbonized bricks non-resistance drying device and method |
| CN108329031A (en) * | 2018-03-06 | 2018-07-27 | 济南大学 | A kind of preparation method of gel casting forming titanium carbide ceramic biscuit |
| CN109574649A (en) * | 2018-12-14 | 2019-04-05 | 镭米光学科技（宁波）有限公司 | A kind of preparation method of yttrium aluminum garnet transparent ceramic |
| CN110713387A (en) * | 2019-10-12 | 2020-01-21 | 华中科技大学 | Direct solidification injection molding method for microwave heating rapid curing ceramic slurry |
| CN115448704A (en) * | 2022-09-16 | 2022-12-09 | 中国科学院上海硅酸盐研究所 | Method for forming ceramic body |
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Application publication date: 20120627 |