CN104987050A - Preparation method for non-water-based high-purity nanoscale aluminum oxide ceramics - Google Patents
Preparation method for non-water-based high-purity nanoscale aluminum oxide ceramics Download PDFInfo
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Abstract
The invention relates to a preparation method for aluminum oxide ceramics, in particular to a preparation method for non-water-based high-purity nanoscale aluminum oxide ceramics. Aluminum oxide powder is added into a premixed solution to form a sizing agent, then, a binding agent is added for ball milling, a plasticizer is added for ball milling to obtain a mixture, defoaming is performed for 1-3 h under the pressure being 0.95-0.1 Mpa, the mixture is made to flow into a trough of a casting machine to obtain a green-pressing sheet, glue discharging is performed on the green-pressing sheet in advance within the oxygen atmosphere at 1000-1300 DEG C, and then the ceramics are obtained through sintering within the hydrogen atmosphere at 1700-1900 DEG C. According to the preparation method for the non-water-based high-purity nanoscale aluminum oxide ceramics, in the high-purity nanoscale aluminum oxide ceramic membrane manufacturing process, the poor phenomena of cracking, wrinkling, peeling and the like of membranes can be effectively avoided, and the rejection rate is lowered.
Description
Technical field
The present invention relates to a kind of alumina-ceramic preparation method, be specially non-water based high-purity nanoaluminium oxide ceramic preparation.
Background technology
A special dimension of high purity aluminium oxide prepares crystalline ceramics.In ceramic field, transparent alumina ceramics can found crucible, infrared detection window material, the integrated circuit substrate, high-frequency insulation material, high temperature corrosion-resisting material etc. manufactured in high-pressure sodium fluorescent tube, electronic industry of special glass.The molding mode of the inefficiency such as hot pressing, slip casting that what current high-purity nano grade aluminum oxide preparation method still adopted is.And casting method because of its production efficiency high, good product consistency, steady performance prepares the shaping a kind of effective ways of crystalline ceramics.
Due to characteristics such as the size of ultrafine inorganic powder particle are little, and specific surface area is large, superfine powder is reunited and is easy to occur, the viscosity of slurry is also very large, and in casting processes, easily occurs that diaphragm ftractures, wrinkling, the phenomenons such as peeling.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of processing method, the phenomenon such as diaphragm cracking, wrinkling, peeling that high-purity nanoaluminium oxide pottery is made can be reduced.Concrete technical scheme is:
Non-water based high-purity nanoaluminium oxide ceramic preparation, comprises the following steps:
(1) aluminum oxide powder is the submicron order aluminum oxide powder of 50 nanometers to 0.1 micron, according to parts by weight, with alumina powder jointed 100 parts for radix, solvent 50-80 part, dispersion agent 1-4 part; Aluminum oxide powder dries 8-16 hour at 100-120 DEG C of temperature, and solvent and dispersion agent pre-mixing 10-30 minute, add aluminum oxide powder in the solution of pre-mixing and form slurry, slurry ball milling 20-28 hour, and the viscosity of slurry is in the scope of 200-600mPa.s;
(2) slurry adds binding agent again, and binding agent is divided into three equal parts, and every equal portions are separated by and are added for four hours, ball milling 8-10 hour, according to parts by weight, with alumina powder jointed 100 parts for radix, binding agent 7-13 part;
(3) slurry adds softening agent again, again within ball milling 16-20 hour, obtains compound, according to parts by weight, with alumina powder jointed 100 parts for radix, softening agent 3-8 part;
(4) compound is under the pressure of negative 0.95-0.1Mpa, deaeration 1-3 hour, make viscosity within the scope of 10000-20000mPa.s, flow in casting machine hopper through filter tank again and make green sheet, the desciccator diaphragm speed of casting machine hopper is 40-100mm/min, temperature is 55-85 DEG C, and the difference of intake velocity and air-out speed is within 1-15%;
(5) green sheet of flow casting molding pre-binder removal in the oxygen atmosphere of 1000-1300 DEG C, then sinters porcelain in the atmosphere of hydrogen of 1700-1900 DEG C.
Described solvent is made up of A group solvent and B group solvent, and the volume ratio of A group solvent and B group solvent is 80-50:20-50; A group solvent is the one in pimelinketone, glycol propyl ether, butyl glycol ether, butyl glycol ether acetic ester, diethylene glycol monobutyl ether, and B solvent is the one in butanone, dehydrated alcohol, propyl alcohol, propylene glycol, Virahol.
Described dispersion agent is one or more mixing in BYK-110, the emulsifier span S80 of the BYK-180 of German Bi Ke company, German Bi Ke company.
Binding agent is one or more mixing in B72, B74, B76, B79, B90, the B98 in U.S. Shou Nuo company PVB series.
Softening agent is DBP(butyl benzyl phthalate), DDP(dibutyl phthalate), PEG(polyoxyethylene glycol) in one or more mixing.
For micron-sized high-purity nanoaluminium oxide powder, general organic solvent, as butanone, ethanol just can meet the effect of dissolving dispersion.And for nanometer grade powder, conventional solvent can not play and well dissolve and dissemination.Further, easy volatile solvent as this kind of in ethanol, for nanometer grade powder, cracking can be abnormal serious.So, select the good organic solvent for nanometer grade powder and dispersion agent most important.
Consider that the specific surface area of nano-powder is large, solvent such as more easily to volatilize at the characteristic, present invention employs organism compared with high boiling range as solvent.And the selection of dispersion agent, because of carbon-carbon skeletal chain length, branched structure, the textural factor such as C=C double bond and hydroxyl of its molecule, certain dissemination can be played, secondary solvent stops the flocculation of powder, has good homogeneity, suitable viscosity and higher solid load to make casting slurry.Find through research, the dispersion of nano pulp, depends on good solvent to a great extent, and suitable dispersion agent generally plays booster action.The present invention, from choosing excellent and being suitable for the solvent system of nano-powder curtain coating, obtain being applicable to particle size range at 50 nanometers and the alumina powder jointed ratio range of above submicron order, and solid content is greater than 50wt%.
Non-water based high-purity nanoaluminium oxide ceramic preparation provided by the invention, in making high-purity nanoaluminium oxide ceramic diaphragm process, effectively can prevent diaphragm from ftractureing, the bad phenomenon such as wrinkling, peeling occurs.Reduce fraction defective.
Embodiment
Specific embodiments of the invention are described in conjunction with the embodiments.
embodiment 1
Non-water based high-purity nanoaluminium oxide ceramic preparation, comprises the following steps:
(1) aluminum oxide powder is the submicron order aluminum oxide powder of 50 nanometers to 0.1 micron, according to parts by weight, with alumina powder jointed 100 parts for radix, solvent 80 parts, dispersion agent 3 parts; Aluminum oxide powder is dried 8 hours at 100 DEG C of temperature, and solvent and dispersion agent pre-mixing 10-30 minute, add aluminum oxide powder in the solution of pre-mixing and form slurry, slurry ball milling 20 hours, and the viscosity of slurry is in the scope of 200-600mPa.s;
Wherein, described solvent is made up of A group solvent and B group solvent, and the volume ratio of A group solvent and B group solvent is 50:50; A group solvent is pimelinketone, and B solvent is butanone.
Described dispersion agent is the BYK-180 of German Bi Ke company.
Binding agent is the weight mixing such as B72, B74, B76 in U.S. Shou Nuo company PVB series.
Softening agent is DBP, DDP two kinds mixing, mixes etc. weight.
(2) slurry adds binding agent again, and binding agent is divided into three equal parts, and every equal portions are separated by and are added for four hours, ball milling 8 hours, according to parts by weight, with alumina powder jointed 100 parts for radix, binding agent 13 parts;
(3) slurry adds softening agent again, and ball milling obtains compound in 20 hours again, according to parts by weight, with alumina powder jointed 100 parts for radix, 6 parts, softening agent;
(4) compound is under the pressure of negative 0.95-0.1Mpa, deaeration 1-3 hour, make viscosity within the scope of 10000-20000mPa.s, flow in casting machine hopper through filter tank again and make green sheet, the desciccator diaphragm speed of casting machine hopper is 40-100mm/min, temperature is 55-85 DEG C, and the difference of intake velocity and air-out speed is within 1-15%;
(5) green sheet of flow casting molding pre-binder removal in the oxygen atmosphere of 1000-1300 DEG C, then sinters porcelain in the atmosphere of hydrogen of 1700-1900 DEG C.
embodiment 2
Non-water based high-purity nanoaluminium oxide ceramic preparation, comprises the following steps:
(1) aluminum oxide powder is the submicron order aluminum oxide powder of 50 nanometers to 0.1 micron, according to parts by weight, with alumina powder jointed 100 parts for radix, solvent 50 parts, dispersion agent 1 part; Aluminum oxide powder is dried 8 hours at 120 DEG C of temperature, and solvent and dispersion agent pre-mixing 10-30 minute, add aluminum oxide powder in the solution of pre-mixing and form slurry, slurry ball milling 24 hours, and the viscosity of slurry is in the scope of 200-600mPa.s;
Wherein, described solvent is made up of A group solvent and B group solvent, and the volume ratio of A group solvent and B group solvent is 80:20; A group solvent is diethylene glycol monobutyl ether, and B solvent is propyl alcohol.
Described dispersion agent is the BYK-110 of German Bi Ke company.
Binding agent is the weight mixing such as B79, B90, B98 in U.S. Shou Nuo company PVB series.
Softening agent is PEG.
(2) slurry adds binding agent again, and binding agent is divided into three equal parts, and every equal portions are separated by and are added for four hours, ball milling 8-10 hour, according to parts by weight, with alumina powder jointed 100 parts for radix, binding agent 10 parts;
(3) slurry adds softening agent again, and ball milling obtains compound in 16 hours again, according to parts by weight, with alumina powder jointed 100 parts for radix, 3 parts, softening agent;
(4) compound is under the pressure of negative 0.95-0.1Mpa, deaeration 1-3 hour, make viscosity within the scope of 10000-20000mPa.s, flow in casting machine hopper through filter tank again and make green sheet, the desciccator diaphragm speed of casting machine hopper is 40-100mm/min, temperature is 55-85 DEG C, and the difference of intake velocity and air-out speed is within 1-15%;
(5) green sheet of flow casting molding pre-binder removal in the oxygen atmosphere of 1000-1300 DEG C, then sinters porcelain in the atmosphere of hydrogen of 1700-1900 DEG C.
embodiment 3
Non-water based high-purity nanoaluminium oxide ceramic preparation, comprises the following steps:
(1) aluminum oxide powder is the submicron order aluminum oxide powder of 50 nanometers to 0.1 micron, according to parts by weight, with alumina powder jointed 100 parts for radix, solvent 60 parts, dispersion agent 4 parts; Aluminum oxide powder is dried 16 hours at 100 DEG C of temperature, and solvent and dispersion agent pre-mixing 10-30 minute, add aluminum oxide powder in the solution of pre-mixing and form slurry, slurry ball milling 28 hours, and the viscosity of slurry is in the scope of 200-600mPa.s;
Wherein, described solvent is made up of A group solvent and B group solvent, and the volume ratio of A group solvent and B group solvent is 50:20; A group solvent is butyl glycol ether, and B solvent is dehydrated alcohol.
Described dispersion agent is emulsifier span S80.
Binding agent is the weight mixing such as B76, the B79 two kinds in U.S. Shou Nuo company PVB series.
Softening agent is DDP.
(2) slurry adds binding agent again, and binding agent is divided into three equal parts, and every equal portions are separated by and are added for four hours, ball milling 8-10 hour, according to parts by weight, with alumina powder jointed 100 parts for radix, binding agent 7 parts;
(3) slurry adds softening agent again, again within ball milling 16-20 hour, obtains compound, according to parts by weight, with alumina powder jointed 100 parts for radix, 8 parts, softening agent;
(4) compound is under the pressure of negative 0.95-0.1Mpa, deaeration 1-3 hour, make viscosity within the scope of 10000-20000mPa.s, flow in casting machine hopper through filter tank again and make green sheet, the desciccator diaphragm speed of casting machine hopper is 40-100mm/min, temperature is 55-85 DEG C, and the difference of intake velocity and air-out speed is within 1-15%;
(5) green sheet of flow casting molding pre-binder removal in the oxygen atmosphere of 1000-1300 DEG C, then sinters porcelain in the atmosphere of hydrogen of 1700-1900 DEG C.
Claims (5)
1. non-water based high-purity nanoaluminium oxide ceramic preparation, is characterized in that: comprise the following steps:
(1) aluminum oxide powder is the submicron order aluminum oxide powder of 50 nanometers to 0.1 micron, according to parts by weight, with alumina powder jointed 100 parts for radix, solvent 50-80 part, dispersion agent 1-4 part; Aluminum oxide powder dries 8-16 hour at 100-120 DEG C of temperature, and solvent and dispersion agent pre-mixing 10-30 minute, add aluminum oxide powder in the solution of pre-mixing and form slurry, slurry ball milling 20-28 hour, and the viscosity of slurry is in the scope of 200-600mPa.s;
(2) slurry adds binding agent again, and binding agent is divided into three equal parts, and every equal portions are separated by and are added for four hours, ball milling 8-10 hour, according to parts by weight, with alumina powder jointed 100 parts for radix, binding agent 7-13 part;
(3) slurry adds softening agent again, again within ball milling 16-20 hour, obtains compound, according to parts by weight, with alumina powder jointed 100 parts for radix, softening agent 3-8 part;
(4) compound is under the pressure of negative 0.95-0.1Mpa, deaeration 1-3 hour, make viscosity within the scope of 10000-20000mPa.s, flow in casting machine hopper through filter tank again and make green sheet, the desciccator diaphragm speed of casting machine hopper is 40-100mm/min, temperature is 55-85 DEG C, and the difference of intake velocity and air-out speed is within 1-15%;
(5) green sheet of flow casting molding pre-binder removal in the oxygen atmosphere of 1000-1300 DEG C, then sinters porcelain in the atmosphere of hydrogen of 1700-1900 DEG C.
2. non-water based high-purity nanoaluminium oxide ceramic preparation according to claim 1, is characterized in that: described solvent is made up of A group solvent and B group solvent, and the volume ratio of A group solvent and B group solvent is 80-50:20-50; A group solvent is the one in pimelinketone, glycol propyl ether, butyl glycol ether, butyl glycol ether acetic ester, diethylene glycol monobutyl ether, and B solvent is the one in butanone, dehydrated alcohol, propyl alcohol, propylene glycol, Virahol.
3. non-water based high-purity nanoaluminium oxide ceramic preparation according to claim 1, is characterized in that: described dispersion agent is one or more mixing in BYK-110, the emulsifier span S80 of the BYK-180 of German Bi Ke company, German Bi Ke company.
4. non-water based high-purity nanoaluminium oxide ceramic preparation according to claim 1, is characterized in that: described binding agent is one or more mixing in B72, B74, B76, B79, B90, the B98 in U.S. Shou Nuo company PVB series.
5. non-water based high-purity nanoaluminium oxide ceramic preparation according to claim 1, is characterized in that: described softening agent is one or more mixing in butyl benzyl phthalate, dibutyl phthalate, polyoxyethylene glycol.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693221A (en) * | 2016-01-15 | 2016-06-22 | 汕头大学 | Ultrathin high-purity ceramic wafer and preparation process thereof |
| CN105777079A (en) * | 2016-01-28 | 2016-07-20 | 深圳市商德先进陶瓷有限公司 | Plasma etching resistant ceramic body and manufacturing method thereof, and plasma etching device |
| CN106587268A (en) * | 2016-11-02 | 2017-04-26 | 深圳市康源环境纳米科技有限公司 | Ceramic membrane, component of ceramic membrane, contact chamber, processing system and method for heavy metal wastewater |
| CN112250469A (en) * | 2020-09-30 | 2021-01-22 | 浙江锋锂新能源科技有限公司 | Kiln material for preparing oxide solid electrolyte membrane and preparation process of thin plate type kiln |
| CN116768609A (en) * | 2022-07-29 | 2023-09-19 | 苏州瑞瓷新材料科技有限公司 | Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics |
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| CN103408294A (en) * | 2013-08-29 | 2013-11-27 | 湖南新华源科技有限公司 | Method for processing electronic ceramic casting slurry |
| CN103435358A (en) * | 2013-08-29 | 2013-12-11 | 中国人民解放军国防科学技术大学 | Organic composition added in preparation of tape-casting slurry and application of organic composition |
| CN103819196A (en) * | 2013-12-30 | 2014-05-28 | 莱鼎电子材料科技有限公司 | Modified aluminum nitride ceramic substrate and production method thereof |
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Patent Citations (4)
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| US5376606A (en) * | 1993-12-30 | 1994-12-27 | Korea Institute Of Science And Technology | Light-transmissive polycrystalline alumina ceramics |
| CN103408294A (en) * | 2013-08-29 | 2013-11-27 | 湖南新华源科技有限公司 | Method for processing electronic ceramic casting slurry |
| CN103435358A (en) * | 2013-08-29 | 2013-12-11 | 中国人民解放军国防科学技术大学 | Organic composition added in preparation of tape-casting slurry and application of organic composition |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693221A (en) * | 2016-01-15 | 2016-06-22 | 汕头大学 | Ultrathin high-purity ceramic wafer and preparation process thereof |
| CN105693221B (en) * | 2016-01-15 | 2018-12-18 | 汕头大学 | A kind of ultra-thin high-purity ceramic piece and its preparation process |
| CN105777079A (en) * | 2016-01-28 | 2016-07-20 | 深圳市商德先进陶瓷有限公司 | Plasma etching resistant ceramic body and manufacturing method thereof, and plasma etching device |
| CN106587268A (en) * | 2016-11-02 | 2017-04-26 | 深圳市康源环境纳米科技有限公司 | Ceramic membrane, component of ceramic membrane, contact chamber, processing system and method for heavy metal wastewater |
| CN106587268B (en) * | 2016-11-02 | 2019-12-20 | 深圳市康源环境纳米科技有限公司 | Ceramic membrane and component thereof, contact tank, heavy metal wastewater treatment system and method |
| CN112250469A (en) * | 2020-09-30 | 2021-01-22 | 浙江锋锂新能源科技有限公司 | Kiln material for preparing oxide solid electrolyte membrane and preparation process of thin plate type kiln |
| CN116768609A (en) * | 2022-07-29 | 2023-09-19 | 苏州瑞瓷新材料科技有限公司 | Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics |
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Application publication date: 20151021 |