CN106079032A - A kind of based on agarose, the gel-casting method of ceramic size mixed solution - Google Patents
A kind of based on agarose, the gel-casting method of ceramic size mixed solution Download PDFInfo
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- CN106079032A CN106079032A CN201610424877.2A CN201610424877A CN106079032A CN 106079032 A CN106079032 A CN 106079032A CN 201610424877 A CN201610424877 A CN 201610424877A CN 106079032 A CN106079032 A CN 106079032A
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- ceramic
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- casting method
- agarose
- mixed slurry
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Classifications
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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
-
- 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
-
- 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
-
- 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
-
- 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 based on agarose, the gel-casting method of ceramic size mixed solution, the method is configured to, particularly as follows: first ceramic powder and dispersant are added to the water, the ceramic size that solid volume fraction is 53 59%, then the agarose solution that concentration is 3 4.5wt% is joined in ceramic size, after regulating its pH to 8 11, ball milling is uniform, it is injected in non-porous mold after mixed slurry is carried out froth in vacuum and fully heats, by cooling down, be dried, sintering and get final product.Owing to agarose solution and ceramic size first mix and ball milling froth in vacuum, casting the most again, bubble will not be brought in the process to make ceramic body produce defect.Use the method can prepare the mixed slurry that solid concentration is high, viscosity is low, the ceramic component of different sizes closely knit, complex-shaped after green sintering, can be obtained.In addition agarose is natural macromolecular, and in base substrate, content of organics need not binder removal less, and ceramic green has certain intensity, can carry out a certain degree of processing before sintering.
Description
Technical field
The invention belongs to technical field of ceramic material, be specifically related to a kind of based on agarose, ceramic size mixed solution
Gel-casting method.
Background technology
Gel casting forming is a kind of pottery net scale that U.S.'s Oak Ridge National Laboratory was invented the beginning of the nineties in last century
Very little forming technique, ceramic molding is combined by this technology with polymer chemistry, by the polymer monomer of polymer chemistry
It is incorporated in ceramic molding.Gel injection molding and forming technology is suitable for preparing the ceramic part of complicated shape, and consolidating of its slurry contains
Amount is high, base substrate has certain intensity, can carry out machining before ceramic post sintering.AM-MBAM system is used to industrialization
The gel rubber system produced, this system reaction controllability and strong adaptability, the gel strength of generation is the highest, cheap, source
Extensively.But AM and MBAM has neurotoxin, is easily absorbed by the skin after contact；And this more sintering of system content of organics
Before need binder removal, the industrialization of technique, automaticity are the highest.
Agarose is a kind of natural polysaccharide macro-molecular, and being heated to more than 90 DEG C in water can dissolve, at a temperature of drop to
Forming the gel of good semi-solid when 35-40 DEG C, the highest then intensity of gel strength is the highest.Introduce agarose to note as gel
Gel media in mold forming has lot of advantages: environmental protection, nontoxic, and idiosome has certain intensity, and content of organics is less, burns
Binder removal etc. is need not before knot.Use ceramic dense, power that high solid volume fraction, low viscous ceramic size prepare
Learn performance relatively good.
General agarose Ceramic gel injection molding and forming technology is suitable for preparing the ceramic part of complicated shape, owing to agarose coagulates
Glue has certain intensity, can carry out machining after blank forming before ceramic post sintering.But this method there is also shortcoming: pottery
The bubble that the froth in vacuum of porcelain slurry removes to a certain extent, but the ceramic size after the de-bubble of injection molding initial vacuum needs to rise
Temperature, is subsequently adding the most lysed agarose solution, mix and blend cooling molding.Agarose solution is in preparation process
Being heated condition, the moisture in system also can run off, and easily causes in moisture evaporation and whipping process and can produce in technological operation
Bubble, the compactness of impact pottery, so bringing inconvenience to technique.Additionally, general ceramic size solid content is difficult to into one
Step promotes.The agarose solution of this present invention offer and the gel-casting method of ceramic size mixed solution are in certain journey
Above-mentioned technologic difficulty is solved on degree.
Summary of the invention
It is an object of the invention to the deficiency overcoming prior art to exist, it is provided that one is mixed based on agarose, ceramic size
Closing the gel-casting method of solution, the method comprises the following steps: ceramic powder and dispersant are added to the water and join by (a)
Make ceramic size；B agarose powder is added to the water and is configured to agarose solution by ()；C agarose solution is joined by ()
Obtaining mixed slurry in ceramic size, regulation mixed slurry pH is ball milling after alkalescence；D the uniform mixed slurry of () ball milling carries out vacuum
De-bubble processes；E mixed slurry that step (d) is obtained by () injects in non-porous mold and fully heats；(f) non-porous mold natural cooling
It is dried to obtain ceramic green by multistep, finally sinters.
Ceramic powder and dispersant being disposably added to the water in step (a) and being configured to solid volume fraction is 53-
The ceramic size of 59%, described dispersant is ammonium citrate or ammonium polyacrylate, and its addition is ceramic powder quality
0.8%.
The agar powder concentration that is configured to soluble in water that will be equivalent to ceramic powder quality 0.7% in step (b) is 3.0-
The agarose solution of 4.5wt%.
In step (c), the pH value of regulation mixed slurry is to 8-11, and Ball-milling Time is 24h.
In step (d), vacuum shakes de-bubble 1h at ambient temperature.
Need not stir after mixed slurry at room temperature injects non-porous mold in step (e), directly be placed on 90 DEG C of environment
Lower fully heating.
By such scheme, described ceramic powder one in zirconium oxide, aluminium oxide, carborundum and silicon nitride.
By such scheme, the pH adjusting agent that regulation mixed slurry pH is used is in PH buffer, ammonia and carbamide
One.
By such scheme, non-porous mold mode of heating is the one in baking oven for heating, oil bath heating and heating in water bath.
By such scheme, described non-porous mold material is the one in metal, plastics, rubber and glass.
Compared with tradition agarose Ceramic gel injection molding and forming technology, the inventive method has the advantages that (1) point
Not Pei Zhi ceramic size and agarose solution, directly by uniform for both mixing and ball milling, to a certain extent can in the case of low viscosity
To improve solid concentration；(2) mixed slurry directly heats and need not stirring, does not affect the compactness of pottery；(3) vacuum concussion removes
Bubble excellent effect；(4) in ceramic green, content of organics is few, it is not necessary to binder removal, and drying and moulding process will not ftracture；(5) system
Standby ceramic green out has certain intensity, can be processed before sintering；(6) can make various complicated shape and
The ceramic component of size.
Detailed description of the invention
For making those of ordinary skill in the art fully understand technical scheme and beneficial effect, below in conjunction with specifically
Embodiment is described in detail.
Embodiment 1
Measuring 10ml distilled water and join in ball grinder, by the Zirconium powder of 68.78g altogether, (solid density is 6.1g/
cm3, particle diameter is 1um) and ammonium citrate (about 0.55g) that mass fraction is 0.8% disposably join stirring system in ball grinder
The zirconia ceramics slurry becoming solid volume fraction to be 53%.0.481g agarose powder is joined in 10.2ml distilled water and make
Becoming mass fraction is the agarose solution of 4.5%, and it all joins mixing and stirring in zirconia ceramics slurry.Use ammonia
Water by the pH regulator of gained mixed slurry to 8, ball milling 24 hours, the most at ambient temperature froth in vacuum 60 minutes.Vacuum is removed
After finishing into, mixed slurry is injected in nonporous glass mould under room temperature, then mould is put into 90 DEG C of baking ovens and fully heats,
During Gai, mixed slurry be without stirring.After it is cooled to room temperature and complete molding, it is dried acquisition intensity through multistep higher
Zirconium oxide green compact, finally sinter.
Embodiment 2
Measuring 10ml distilled water and join in ball grinder, by the Zirconium powder of 87.8g altogether, (solid density is 6.1g/
cm3, particle diameter is 1um) and ammonium citrate (about 0.7g) that mass fraction is 0.8% disposably join stirring in ball grinder and make
Solid volume fraction is the zirconia ceramics slurry of 59%.0.615g agarose powder is joined in 19.9ml distilled water and makes
Mass fraction is the agarose solution of 3.0%, and it all joins mixing and stirring in zirconia ceramics slurry.Use carbamide
By the pH regulator of gained mixed slurry to 9, ball milling 24 hours, the most at ambient temperature froth in vacuum 60 minutes.Froth in vacuum
After completing, mixed slurry is injected in non-porous metal mould under room temperature, then mould is put into 90 DEG C of water-baths and fully heats,
During Gai, mixed slurry be without stirring.After it is cooled to room temperature and complete molding, it is dried acquisition intensity through multistep higher
Zirconium oxide green compact, finally sinter.
Embodiment 3
Measuring 10ml distilled water and join in ball grinder, by the Zirconium powder of 77.7g altogether, (solid density is 6.1g/
cm3, particle diameter is 1um) and ammonium citrate (about 0.622g) that mass fraction is 0.8% disposably join stirring system in ball grinder
The zirconia ceramics slurry becoming solid volume fraction to be 56%.0.544g agarose powder is joined in 11.54ml distilled water
Make the agarose solution that mass fraction is 4.5%, it is all joined mixing and stirring in zirconia ceramics slurry.With
Carbamide by the pH regulator of gained mixed slurry to 10, ball milling 24 hours, the most at ambient temperature froth in vacuum 60 minutes.Vacuum
After de-bubble completes, mixed slurry is injected in atresia rubber mold under room temperature, then mould is put into 90 DEG C of water-baths abundant
Heating, during being somebody's turn to do, mixed slurry is without stirring.After it is cooled to room temperature and complete molding, it is dried acquisition intensity through multistep
Higher zirconium oxide green compact, finally sinter.
Embodiment 4
Measuring 8.88ml distilled water and join in ball grinder, by 39.7g altogether alumina powder jointed, (solid density is
3.97g/cm3) and ammonium citrate (about 0.318g) that mass fraction is 0.8% disposably join stirring in ball grinder and make solid
Phase volume fraction is the aluminium oxide ceramics slurry of 53%.0.2779g agarose powder is joined in 5.90ml distilled water and makes
Mass fraction is the agarose solution of 4.5%, and it all joins mixing and stirring in aluminium oxide ceramics slurry.Use carbamide
By the pH regulator of gained mixed slurry to 10, ball milling 24 hours, the most at ambient temperature froth in vacuum 60 minutes.Froth in vacuum
After completing, mixed slurry is injected in nonporous glass mould under room temperature, then mould is put into 90 DEG C of oil bath pans and fully heats,
During Gai, mixed slurry be without stirring.After it is cooled to room temperature and complete molding, it is dried acquisition intensity through multistep higher
Aluminium oxide green compact, finally sinter.
Embodiment 5
Measuring 8.88ml distilled water and join in ball grinder, by the silicon carbide powder of 32g altogether, (solid density is 3.2g/
cm3) and ammonium polyacrylate (about 0.256g) that mass fraction is 0.8% disposably join stirring in ball grinder and make solid phase body
Fraction is the silicon carbide ceramics slurry of 53%.0.224g agarose powder is joined and quality made by 4.99ml distilled water divides
Number is the agarose solution of 4.3%, and it all joins mixing and stirring in silicon carbide ceramics slurry.Will with pH buffer
The pH regulator of gained mixed slurry to 11, ball milling 24 hours, the most at ambient temperature froth in vacuum 60 minutes.Froth in vacuum is complete
Cheng Hou, injects mixed slurry in nonporous glass mould under room temperature, mould is then put into 90 DEG C of oil bath pans and fully heats, should
During mixed slurry without stirring.After it is cooled to room temperature and complete molding, it is dried acquisition intensity through multistep higher
Carborundum green compact, finally sinter.
Claims (10)
1. one kind based on agarose, the gel-casting method of ceramic size mixed solution, it is characterised in that include following step
Rapid: ceramic powder and dispersant are added to the water and are configured to ceramic size by (a)；B agarose powder is added to the water and joins by ()
Make agarose solution；C agarose solution is joined and obtains mixed slurry in ceramic size by (), regulation mixed slurry pH is alkalescence
Rear ball milling；D the uniform mixed slurry of () ball milling carries out froth in vacuum process；E mixed slurry that step (d) is obtained by () injects nothing
Punch die fully heats；It is dried to obtain ceramic green through multistep after (f) non-porous mold natural cooling, finally sinters.
2. gel-casting method as claimed in claim 1, it is characterised in that: by ceramic powder and dispersion in step (a)
Agent is disposably added to the water and is configured to the ceramic size that solid volume fraction is 53-59%, and described dispersant is ammonium citrate
Or ammonium polyacrylate, its addition is the 0.8% of ceramic powder quality.
3. gel-casting method as claimed in claim 1, it is characterised in that: step (b) will be equivalent to ceramic powder
The agar powder of quality 0.7% is soluble in water is configured to the agarose solution that concentration is 3.0-4.5wt%.
4. gel-casting method as claimed in claim 1, it is characterised in that: the pH of regulation mixed slurry in step (c)
Value is to 8-11, and Ball-milling Time is 24h.
5. gel-casting method as claimed in claim 1, it is characterised in that: vacuum at ambient temperature in step (d)
Concussion de-bubble 1h.
6. gel-casting method as claimed in claim 1, it is characterised in that: in step (e), mixed slurry is at room temperature
Need not stir after injecting non-porous mold, directly be placed under 90 DEG C of environment and fully heat.
7. the gel-casting method as described in any one of claim 1-6, it is characterised in that: described ceramic powder is selected from oxygen
Change the one in zirconium, aluminium oxide, carborundum and silicon nitride.
8. the gel-casting method as described in any one of claim 1-6, it is characterised in that: regulation mixed slurry pH is made
PH adjusting agent one in PH buffer, ammonia and carbamide.
9. the gel-casting method as described in any one of claim 1-6, it is characterised in that: non-porous mold mode of heating is
One in baking oven for heating, oil bath heating and heating in water bath.
10. the gel-casting method as described in any one of claim 1-6, it is characterised in that: described non-porous mold material
For the one in metal, plastics, rubber and glass.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106699138A (en) * | 2017-01-24 | 2017-05-24 | 山东倍辰新材料有限公司 | Ceramic slag separator and gel injection molding manufacturing process thereof |
| CN107571373A (en) * | 2017-08-16 | 2018-01-12 | 武汉工程大学 | A kind of efficient ceramic slurry bubble removing method |
| CN107745433A (en) * | 2017-09-30 | 2018-03-02 | 华中科技大学 | A kind of method of agar powder curing ceramic slurry |
| CN108276004A (en) * | 2018-03-06 | 2018-07-13 | 济南大学 | A kind of preparation method based on guar gum gel casting forming boron nitride biscuit |
| 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 |
| CN108358644A (en) * | 2018-03-06 | 2018-08-03 | 济南大学 | Based on xanthans gel casting forming TiB2The preparation method of composite ceramics biscuit |
| CN108503360A (en) * | 2018-04-23 | 2018-09-07 | 中国科学院上海应用物理研究所 | The preparation method of LSM block materials |
| CN109269869A (en) * | 2018-10-16 | 2019-01-25 | 重庆大学 | Three-dimensional determines the artificial porous stone preparation method of hole |
| CN110156472A (en) * | 2019-05-09 | 2019-08-23 | 中国兵器工业第五二研究所烟台分所有限责任公司 | A kind of ceramic low toxicityization preparation method of large scale AlON |
| 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 |
| CN111592341A (en) * | 2019-09-16 | 2020-08-28 | 哈尔滨理工大学 | Preparation method of porous alumina ceramic |
| CN112408989A (en) * | 2019-08-20 | 2021-02-26 | 山东工业陶瓷研究设计院有限公司 | Silicon nitride powder pretreatment and low-defect blank injection molding method |
| CN113372101A (en) * | 2021-06-29 | 2021-09-10 | 西安理工大学 | Preparation method of alumina ceramic |
| CN115122486A (en) * | 2022-08-01 | 2022-09-30 | 衡阳凯新特种材料科技有限公司 | Ceramic gel injection molding device and injection molding method |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106699138A (en) * | 2017-01-24 | 2017-05-24 | 山东倍辰新材料有限公司 | Ceramic slag separator and gel injection molding manufacturing process thereof |
| CN107571373A (en) * | 2017-08-16 | 2018-01-12 | 武汉工程大学 | A kind of efficient ceramic slurry bubble removing method |
| CN107745433A (en) * | 2017-09-30 | 2018-03-02 | 华中科技大学 | A kind of method of agar powder curing ceramic slurry |
| CN108276004A (en) * | 2018-03-06 | 2018-07-13 | 济南大学 | A kind of preparation method based on guar gum gel casting forming boron nitride biscuit |
| 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 |
| CN108358644A (en) * | 2018-03-06 | 2018-08-03 | 济南大学 | Based on xanthans gel casting forming TiB2The preparation method of composite ceramics biscuit |
| CN108503360B (en) * | 2018-04-23 | 2020-10-23 | 中国科学院上海应用物理研究所 | Preparation method of LSM bulk material |
| CN108503360A (en) * | 2018-04-23 | 2018-09-07 | 中国科学院上海应用物理研究所 | The preparation method of LSM block materials |
| CN109269869A (en) * | 2018-10-16 | 2019-01-25 | 重庆大学 | Three-dimensional determines the artificial porous stone preparation method of hole |
| CN109269869B (en) * | 2018-10-16 | 2021-08-13 | 重庆大学 | Method for preparing three-dimensional fixed-pore artificial porous stone |
| CN110156472A (en) * | 2019-05-09 | 2019-08-23 | 中国兵器工业第五二研究所烟台分所有限责任公司 | A kind of ceramic low toxicityization preparation method of large scale AlON |
| CN112408989A (en) * | 2019-08-20 | 2021-02-26 | 山东工业陶瓷研究设计院有限公司 | Silicon nitride powder pretreatment and low-defect blank injection molding method |
| CN112408989B (en) * | 2019-08-20 | 2022-11-15 | 山东工业陶瓷研究设计院有限公司 | Silicon nitride powder pretreatment and low-defect blank injection molding method |
| CN111592341A (en) * | 2019-09-16 | 2020-08-28 | 哈尔滨理工大学 | Preparation method of porous alumina ceramic |
| 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 |
| CN115122486A (en) * | 2022-08-01 | 2022-09-30 | 衡阳凯新特种材料科技有限公司 | Ceramic gel injection molding device and injection molding method |
| CN115122486B (en) * | 2022-08-01 | 2024-03-29 | 衡阳凯新特种材料科技有限公司 | Ceramic gel injection molding device and injection molding method |
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