CN106079032B - A kind of gel-casting method based on agarose, ceramic slurry mixed solution - Google Patents
A kind of gel-casting method based on agarose, ceramic slurry mixed solution Download PDFInfo
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- CN106079032B CN106079032B CN201610424877.2A CN201610424877A CN106079032B CN 106079032 B CN106079032 B CN 106079032B CN 201610424877 A CN201610424877 A CN 201610424877A CN 106079032 B CN106079032 B CN 106079032B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
- B28B1/261—Moulds therefor
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
Abstract
The invention discloses a kind of gel-casting method based on agarose, ceramic slurry mixed solution, this method specifically: be first added to the water ceramic powder and dispersing agent the ceramic slurry for being configured to that solid volume fraction is 53-59%, then the agarose solution that concentration is 3-4.5wt% is added in ceramic slurry, adjust ball milling after its pH to 8-11, it sufficiently heats to being injected into non-porous mold after mixed slurry progress froth in vacuum, by cooling, drying, is sintered to obtain the final product.Since agarose solution and ceramic slurry first mix and ball milling froth in vacuum, casting again, it will not bring bubble that ceramic body is made to generate defect in the process.The mixed slurry that solid concentration is high, viscosity is low can be prepared using this method, the ceramic component of closely knit, complex-shaped different sizes can be obtained after green sintering.Furthermore agarose is natural macromolecular, and content of organics does not need dumping less in green body, and ceramic green has certain intensity, and a degree of processing can be carried out before sintering.
Description
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of based on agarose, ceramic slurry mixed solution
Gel-casting method.
Background technique
Gel casting forming is a kind of ceramic net scale that U.S.'s Oak Ridge National Laboratory is invented in the beginning of the nineties in last century
Very little forming technique, the technology combine ceramic molding with polymer chemistry, by the polymer monomer of polymer chemistry
It is introduced into ceramic molding.Gel injection molding and forming technology is suitble to prepare the ceramic part of complicated shape, and consolidating for slurry contains
Amount is high, green body has certain intensity, can be machined before ceramic post sintering.AM-MBAM system is used to industrialize
The gel rubber system of production, the system react controllability and adaptable, and the gel strength of generation is very high, cheap, source
Extensively.But AM and MBAM has neurotoxin, is easily absorbed by the skin after contact；And the more sintering of system content of organics
Before need dumping, the industrialization of technique, the degree of automation be not high.
Agarose is a kind of natural polysaccharide macro-molecular, and being heated to 90 DEG C or more in water can dissolve, and temperature drops to
The gel of good semi-solid is formed at 35-40 DEG C, the more high then intensity of gel strength is higher.Agarose is introduced to infuse as gel
Gel media in mold forming has lot of advantages: environmental protection, nontoxic, idiosome has certain intensity, and content of organics is less, burns
Dumping etc. is not needed before knot.Ceramic dense, the power prepared using the ceramic slurry of high solid volume fraction, low viscosity
It is all relatively good to learn performance.
General agarose Ceramic gel injection molding and forming technology is suitble to prepare the ceramic part of complicated shape, since agarose is solidifying
Glue has certain intensity, can be machined before ceramic post sintering after blank forming.But there is also disadvantages for this method: pottery
The bubble that the froth in vacuum of porcelain slurry removes to a certain extent, but the ceramic slurry after the de-bubble of injection molding initial vacuum needs to rise
Then lysed agarose solution at high temperature is added in temperature, be mixed and be cooled and shaped.Agarose solution is during the preparation process
It is heated condition, the moisture in system can be also lost, and moisture is be easy to cause to evaporate and can generate in whipping process in technological operation
Bubble influences the compactness of ceramics, so bringing inconvenience to technique.In addition, general ceramic slurry solid content is difficult into one
Step is promoted.The gel-casting method of this agarose solution and ceramic slurry mixed solution provided by the invention is in certain journey
Solves above-mentioned technologic difficulty on degree.
Summary of the invention
It is an object of the invention to overcome the shortcomings of the prior art, provide a kind of mixed based on agarose, ceramic slurry
The gel-casting method for closing solution, matches method includes the following steps: ceramic powder and dispersing agent are added to the water by (a)
Ceramic slurry is made；(b) agarose powder is added to the water and is configured to agarose solution；(c) agarose solution is added to
Mixed slurry is obtained in ceramic slurry, adjusting mixed slurry pH is ball milling after alkalinity；(d) mixed slurry of ball milling carries out vacuum
De-bubble processing；(e) mixed slurry that step (d) obtains is injected in non-porous mold and is sufficiently heated；(f) non-porous mold natural cooling
By multistep it is dry ceramic green, be finally sintered.
Ceramic powder and dispersing agent are added at one time in water in step (a) and are configured to solid volume fraction as 53-
59% ceramic slurry, the dispersing agent are ammonium citrate or ammonium polyacrylate, and additional amount is ceramic powder quality
0.8%.
The agar powder concentration soluble in water that is configured to that will be equivalent to ceramic powder quality 0.7% in step (b) is 3.0-
The agarose solution of 4.5wt%.
The pH value of mixed slurry is adjusted in step (c) to 8-11, Ball-milling Time is for 24 hours.
Vacuum shakes de-bubble 1h at room temperature in step (d).
Mixed slurry does not have to stirring after injecting non-porous mold at room temperature in step (e), directly places it in 90 DEG C of environment
Lower sufficiently heating.
According to the above scheme, the ceramic powder is selected from one of zirconium oxide, aluminium oxide, silicon carbide and silicon nitride.
According to the above scheme, pH adjusting agent used in mixed slurry pH is adjusted in PH buffer, ammonium hydroxide and urea
One kind.
According to the above scheme, non-porous mold heating method is one of baking oven heating, oil bath heating and heating water bath.
According to the above scheme, the non-porous mold material is one of metal, plastics, rubber and glass.
Compared with traditional agarose Ceramic gel injection molding and forming technology, the method for the present invention has the advantages that (1) point
Not Pei Zhi ceramic slurry and agarose solution, it is directly that the two mixing and ball milling is uniform, to a certain extent can in low viscosity
To improve solid concentration；(2) mixed slurry, which directly heats, does not need to stir, and does not influence the compactness of ceramics；(3) vacuum concussion removes
Steep excellent effect；(4) content of organics is few in ceramic green, does not need dumping, and drying and moulding process will not cracking；(5) it makes
The standby ceramic green come out has certain intensity, can be processed before sintering；(6) can be made various complicated shapes and
The ceramic component of size.
Specific embodiment
To make those of ordinary skill in the art fully understand technical solution of the present invention and beneficial effect, below with reference to specific
Embodiment is described in detail.
Embodiment 1
It measures 10ml distilled water to be added in ball grinder, by Zirconium powder (the theoretical density 6.1g/ of total 68.78g
cm3, partial size 1um) and mass fraction be 0.8% ammonium citrate (about 0.55g) be added at one time in ball grinder stir system
The zirconia ceramics slurry for being 53% at solid volume fraction.0.481g agarose powder is added in 10.2ml distilled water and is made
The agarose solution for being 4.5% at mass fraction, its whole is added in zirconia ceramics slurry and is mixed evenly.Use ammonia
The pH of gained mixed slurry is adjusted to 8 by water, and ball milling 24 hours, froth in vacuum 60 minutes at room temperature later.Vacuum is removed
After the completion of bubble, mixed slurry is injected in nonporous glass mold at room temperature, then mold is put into 90 DEG C of baking ovens and is sufficiently heated,
Mixed slurry is without stirring during being somebody's turn to do.It is higher by the dry acquisition intensity of multistep after it is cooled to room temperature and completely molding
Zirconium oxide green compact, be finally sintered.
Embodiment 2
It measures 10ml distilled water to be added in ball grinder, by Zirconium powder (the theoretical density 6.1g/ of total 87.8g
cm3, partial size 1um) and mass fraction be 0.8% ammonium citrate (about 0.7g) be added at one time in ball grinder stirring and be made
The zirconia ceramics slurry that solid volume fraction is 59%.0.615g agarose powder is added in 19.9ml distilled water and is made
The agarose solution that mass fraction is 3.0%, its whole is added in zirconia ceramics slurry and is mixed evenly.Use urea
The pH of gained mixed slurry is adjusted to 9, ball milling 24 hours, froth in vacuum 60 minutes at room temperature later.Froth in vacuum
After the completion, mixed slurry is injected in non-porous metal mold at room temperature, then mold is put into 90 DEG C of water-baths and is sufficiently heated,
Mixed slurry is without stirring during being somebody's turn to do.It is higher by the dry acquisition intensity of multistep after it is cooled to room temperature and completely molding
Zirconium oxide green compact, be finally sintered.
Embodiment 3
It measures 10ml distilled water to be added in ball grinder, by Zirconium powder (the theoretical density 6.1g/ of total 77.7g
cm3, partial size 1um) and mass fraction be 0.8% ammonium citrate (about 0.622g) be added at one time in ball grinder stir system
The zirconia ceramics slurry for being 56% at solid volume fraction.0.544g agarose powder is added in 11.54ml distilled water
The agarose solution that mass fraction is 4.5% is made, its whole is added in zirconia ceramics slurry and is mixed evenly.With
The pH of gained mixed slurry is adjusted to 10 by urea, and ball milling 24 hours, froth in vacuum 60 minutes at room temperature later.Vacuum
After the completion of de-bubble, mixed slurry is injected in non-porous rubber mold at room temperature, is then put into mold in 90 DEG C of water-baths sufficiently
Heating, mixed slurry is without stirring during being somebody's turn to do.After it is cooled to room temperature and completely molding, intensity is obtained by multistep is dry
Higher zirconium oxide green compact, are finally sintered.
Embodiment 4
It measures 8.88ml distilled water to be added in ball grinder, by the alumina powder of total 39.7g, (theoretical density is
3.97g/cm3) and mass fraction be 0.8% ammonium citrate (about 0.318g) be added at one time in ball grinder stirring be made it is solid
The aluminium oxide ceramics slurry that phase volume fraction is 53%.0.2779g agarose powder is added in 5.90ml distilled water and is made
The agarose solution that mass fraction is 4.5%, its whole is added in aluminium oxide ceramics slurry and is mixed evenly.Use urea
The pH of gained mixed slurry is adjusted to 10, ball milling 24 hours, froth in vacuum 60 minutes at room temperature later.Froth in vacuum
After the completion, mixed slurry is injected in nonporous glass mold at room temperature, then mold is put into 90 DEG C of oil bath pans and is sufficiently heated,
Mixed slurry is without stirring during being somebody's turn to do.It is higher by the dry acquisition intensity of multistep after it is cooled to room temperature and completely molding
Aluminium oxide green compact, be finally sintered.
Embodiment 5
It measures 8.88ml distilled water to be added in ball grinder, by silicon carbide powder (the theoretical density 3.2g/ of total 32g
cm3) and mass fraction be 0.8% ammonium polyacrylate (about 0.256g) be added at one time in ball grinder stirring solid phase body be made
The silicon carbide ceramics slurry that fraction is 53%.0.224g agarose powder is added in 4.99ml distilled water, quality point is made
The agarose solution that number is 4.3%, its whole is added in silicon carbide ceramics slurry and is mixed evenly.It will with pH buffer
The pH of gained mixed slurry is adjusted to 11, and ball milling 24 hours, froth in vacuum 60 minutes at room temperature later.Froth in vacuum is complete
Mixed slurry is injected in nonporous glass mold at room temperature, then mold is put into 90 DEG C of oil bath pans and is sufficiently heated by Cheng Hou, should
Mixed slurry is without stirring in the process.It is higher by the dry acquisition intensity of multistep after it is cooled to room temperature and completely molding
Silicon carbide green compact, are finally sintered.
Claims (5)
1. a kind of gel-casting method based on agarose, ceramic slurry mixed solution, it is characterised in that including following step
It is rapid:
(a) ceramic powder and dispersing agent are added to the water and are configured to ceramic slurry；
(b) agarose powder is added to the water and is configured to agarose solution；
(c) agarose solution is added in ceramic slurry and obtains mixed slurry, adjusting mixed slurry pH is ball milling after alkalinity；
(d) mixed slurry of ball milling carries out froth in vacuum processing；
(e) mixed slurry that step (d) obtains is injected in non-porous mold and is sufficiently heated；
(f) after non-porous mold natural cooling through multistep it is dry ceramic green, be finally sintered；
Ceramic powder and dispersing agent are added at one time in water in step (a) and are configured to solid volume fraction as 53%-59%
Ceramic slurry, the dispersing agent be ammonium citrate or ammonium polyacrylate, additional amount be ceramic powder quality 0.8%；
The agar powder concentration soluble in water that is configured to that will be equivalent to ceramic powder quality 0.7% in step (b) is 3.0%-
The agarose solution of 4.5wt%；
The pH value of mixed slurry is adjusted in step (c) to 8-11, Ball-milling Time is for 24 hours；
Vacuum shakes de-bubble 1h at room temperature in step (d)；
Mixed slurry does not have to stirring after injecting non-porous mold at room temperature in step (e), directly places it under 90 DEG C of environment and fills
Divide heating.
2. gel-casting method as described in claim 1, it is characterised in that: the ceramic powder is selected from zirconium oxide, oxygen
Change one of aluminium, silicon carbide and silicon nitride.
3. gel-casting method as described in claim 1, it is characterised in that: adjust pH tune used in mixed slurry pH
It saves agent and is selected from one of PH buffer, ammonium hydroxide and urea.
4. gel-casting method as described in claim 1, it is characterised in that: non-porous mold heating method adds for baking oven
One of heat, oil bath heating and heating water bath.
5. gel-casting method as described in claim 1, it is characterised in that: the non-porous mold material is metal, modeling
One of material, rubber and glass.
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| CN106588026A (en) * | 2016-12-16 | 2017-04-26 | 哈尔滨理工大学 | Method of forming dense or multihole AlN ceramic through injection mould based on agarose gel |
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| CN111592341B (en) * | 2019-09-16 | 2022-06-10 | 哈尔滨理工大学 | Preparation method of porous alumina ceramic |
| CN111270347A (en) * | 2020-01-22 | 2020-06-12 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for preparing transparent ceramic optical fiber by gel injection molding |
| CN113372101A (en) * | 2021-06-29 | 2021-09-10 | 西安理工大学 | Preparation method of alumina ceramic |
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| CN103072182B (en) * | 2013-01-08 | 2014-09-24 | 清华大学 | Gellan gum gel-based ceramic gel injection molding method |
| CN103922757B (en) * | 2014-04-02 | 2015-04-15 | 清华大学 | Direct-coagulation injection molding method for non-oxide ceramics |
| KR20170013387A (en) * | 2014-06-04 | 2017-02-06 | 이메리스 세라믹스 프랑스 | Ceramic compositions |
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