CN103819196A - Modified aluminum nitride ceramic substrate and production method thereof - Google Patents
Modified aluminum nitride ceramic substrate and production method thereof Download PDFInfo
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- CN103819196A CN103819196A CN201310742139.9A CN201310742139A CN103819196A CN 103819196 A CN103819196 A CN 103819196A CN 201310742139 A CN201310742139 A CN 201310742139A CN 103819196 A CN103819196 A CN 103819196A
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Abstract
The invention discloses a modified aluminum nitride ceramic substrate which is characterized by being prepared from aluminum nitride, alpha-Al2O3 nano powder, a sintering aid, a non-benzene ternary solvent system, a dispersing agent, a binding agent and a plasticizer, wherein the average particle size of the alpha-Al2O3 nano powder is 15-25nm; the specific surface area of the alpha-Al2O3 nano powder is greater than or equal to 240m<2>/g; the sintering aid is mixed via any two or more of CaO, Y2O3, CaF, BN and CaC at a ratio; the non-benzene ternary solvent system is a mixed solvent of alcohol, isopropanol and butanone; and the substrate is prepared via a tape casting and low temperature sintering method. According to the substrate, the adopted alpha-Al2O3 nano powder is uniform in particle size distribution, high in purity, excellent in dispersity and large in specific surface area; the strength of the substrate is improved; a tape casting technology greatly improves the production efficiency; a ternary sintering agent is added to aluminum nitride powder, so that high heat conductivity is reached during sintering under medium and low temperature conditions, the energy consumption is saved, and the production cost is lowered; and the non-benzene ternary solvent system is good in dispersity, nontoxic and harmless.
Description
Technical field
The present invention relates to a kind of aluminium nitride ceramic substrate, be specifically related to a kind of aluminium nitride ceramic substrate that adds alumina nano powder and carry out modification, also relate to the production method of this aluminium nitride ceramic substrate.
Background technology
Along with the raising of high power module circuit level and the development of great power LED, insulated substrate material used is had higher requirement, aluminium nitride ceramics material, owing to having higher thermal conductivity, has been widely used in the insulated substrate material of various great-power electronic original papers.But, in some miniaturized application fields, except having higher thermal conductivity, also require aluminum nitride ceramic substrate to there is higher mechanical property, be especially less than in the thin plate of 0.38mm at thickness, require aluminum nitride ceramic substrate to there is higher bending strength.In the heat-radiating substrate of some (PCC) powers or the application of the bracket of semiconducter device, in order to obtain good mechanical property and thermal shock resistance, people often adopt the method for controlling grain growing to obtain thin brilliant microstructure.Obtain thin brilliant microstructure by the method for control grain growing and improve mechanical property and thermal shock resistance, defect is that the thermal conductivity of aluminium nitride ceramic substrate has reduced.
Summary of the invention
The technical problem to be solved in the present invention is to provide one and has high heat conductance, high-intensity modification aluminium nitride ceramic substrate.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of modification aluminium nitride ceramic substrate, its innovative point is: by aluminium nitride, α-Al
2o
3nanometer powder, sintering agent, prepare without benzene ternary solvent system, dispersion agent, binding agent and softening agent.
Further, described α-Al
2o
3the median size of nanometer powder is 15-25nm, specific surface area>=240m
2/ g; Described sintering agent is by CaO, Y
2o
3, two or more composition arbitrarily in CaF, BN and CaC; Described is the mixed solvent of ethanol, Virahol and butanone without benzene ternary solvent system; Described dispersion agent is the one in fish oil, glycerine or Viscotrol C; Described binding agent is polyvinyl butyral acetal; Described softening agent is dibutyl phthalate.
Further, described α-Al
2o
3the quality of nanometer powder is the 1-3% of aluminium nitride quality; The quality of described sintering agent is the 2-10% of aluminium nitride quality; The described quality without benzene ternary solvent system is the 1-8% of aluminium nitride quality; The quality of described dispersion agent is the 2-4% of aluminium nitride quality; The quality of described binding agent is the 10-13% of aluminium nitride quality; The quality of described softening agent is the 4-9% of aluminium nitride quality.
Another object of the present invention is to provide a kind of production method of modification aluminium nitride ceramic substrate, adopts the method for flow casting molding to be prepared, specific as follows: by aluminium nitride, α-Al
2o
3nanometer powder and sintering agent are mixed in proportion; Mixed powder is dissolved in without in benzene ternary solvent system, then adds dispersion agent, carry out ball milling on ball mill one time, Ball-milling Time is 24-26 hour, and then adds binding agent and softening agent to grind 24-28 hour; Froth in vacuum under subnormal ambient; The slurry of handling well is carried out to flow casting molding with casting machine, controlling scraper height is 0.5mm, and curtain coating belt speed is 0.1-0.3m/min, and drying temperature is 20-90 ℃; Curtain coating idiosome is continuous binder removal 18-20h in continous way draft glue discharging furnace, and temperature is 580 ℃; Curtain coating green compact are put into sintering oven, sintering under nitrogen protection, sintering temperature is 1550-1680 ℃.
Beneficial effect of the present invention:
1) α-Al that the present invention adopts
2o
3nanometer powder even particle size distribution, purity be high, have fabulous dispersion, and its specific surface is high, has resistant to elevated temperatures inertia, high reactivity, and porousness, hardness is high, good stability of the dimension, has improved moulding and sintering character, improves product strength.
2) casting molding processes, enhances productivity greatly, adds ternary agglutinant in aluminium nitride powder, makes sintering under middle cold condition reach high thermal conductivity, and energy efficient, reduces production costs.
3) the present invention adopts without benzene ternary solvent system, good dispersity, and nontoxic.
Embodiment
Specific embodiment elaborates to technical scheme of the present invention below.
Embodiment 1
A kind of modification aluminium nitride ceramic substrate, the α-Al that is 15nm by aluminium nitride, median size
2o
3nanometer powder, Y
2o
3mixed solvent, glycerine, polyvinyl butyral acetal and the dibutyl phthalate of-CaF sintering agent, ethanol, Virahol and butanone prepares; Specific surface area>=the 240m of aluminium oxide nano powder
2/ g.
Adopt casting method to prepare modification aluminium nitride ceramic substrate through low-temperature sintering, by aluminium nitride, α-Al
2o
3the mass ratio that nanometer powder and sintering agent are pressed 1:0.01:0.02 mixes; Mixed powder is dissolved in the mixed solvent of ethanol, Virahol and butanone (1:1:2) that quality is aluminium nitride quality 1%, adding quality is aluminium nitride quality 2% glycerine again, on ball mill, carry out ball milling one time, Ball-milling Time is 24-26 hour, is then that aluminium nitride quality 10% polyvinyl butyral acetal and quality are that aluminium nitride quality 4% dibutyl phthalate grinds 24-28 hour adding quality; Froth in vacuum under subnormal ambient; The slurry of handling well is carried out to flow casting molding with casting machine, controlling scraper height is 0.5mm, and curtain coating belt speed is 0.1m/min, and drying temperature is 30 ℃; Curtain coating idiosome is continuous binder removal 18h in continous way draft glue discharging furnace, and temperature is 580 ℃; Curtain coating green compact are put into sintering oven, sintering under nitrogen protection, sintering temperature is 1600 ℃, makes target product.
Embodiment 2
A kind of modification aluminium nitride ceramic substrate, the α-Al that is 20nm by aluminium nitride, median size
2o
3nanometer powder, Y
2o
3mixed solvent, Viscotrol C, polyvinyl butyral acetal and the dibutyl phthalate of-BN sintering agent, ethanol, Virahol and butanone prepares; Specific surface area>=the 240m of aluminium oxide nano powder
2/ g.
Adopt casting method to prepare modification aluminium nitride ceramic substrate through low-temperature sintering, by aluminium nitride, α-Al
2o
3the mass ratio that nanometer powder and sintering agent are pressed 1:0.02:0.06 mixes; Mixed powder is dissolved in the mixed solvent of ethanol, Virahol and butanone (1:1:2) that quality is aluminium nitride quality 4%, adding quality is the Viscotrol C of aluminium nitride quality 3% again, on ball mill, carry out ball milling one time, Ball-milling Time is 24-26 hour, is then that the polyvinyl butyral acetal of aluminium nitride quality 12% and quality are that the dibutyl phthalate of aluminium nitride quality 7% grinds 24-28 hour adding quality; Froth in vacuum under subnormal ambient; The slurry of handling well is carried out to flow casting molding with casting machine, control scraper height 0.5mm, curtain coating belt speed is 0.1m/min, and drying temperature is 50 ℃; Curtain coating idiosome is continuous binder removal 19h in continous way draft glue discharging furnace, and temperature is 580 ℃; Curtain coating green compact are put into sintering oven, sintering under nitrogen protection, sintering temperature is 1620 ℃, makes target product.
Embodiment 3
A kind of modification aluminium nitride ceramic substrate, the α-Al that is 15nm by aluminium nitride, median size
2o
3nanometer powder, CaO-Y
2o
3mixed solvent, fish oil, polyvinyl butyral acetal and the dibutyl phthalate of sintering agent, ethanol, Virahol and butanone prepares; Specific surface area>=the 240m of aluminium oxide nano powder
2/ g.
Adopt casting method to prepare modification aluminium nitride ceramic substrate through low-temperature sintering, by aluminium nitride, α-Al
2o
3the mass ratio that nanometer powder and sintering agent are pressed 1:0.03:0.08 mixes; Mixed powder is dissolved in the mixed solvent of ethanol, Virahol and butanone (1:1:2) that quality is aluminium nitride quality 3%, adding quality is the % fish oil of aluminium nitride quality 4 again, on ball mill, carry out ball milling one time, Ball-milling Time is 24-26 hour, is then that the polyvinyl butyral acetal of aluminium nitride quality 13% and quality are that the dibutyl phthalate of aluminium nitride quality 9% grinds 24-28 hour adding quality; Froth in vacuum under subnormal ambient; The slurry of handling well is carried out to flow casting molding with casting machine, controlling scraper height is 0.5mm, and curtain coating belt speed is 0.1m/min, and drying temperature is 90 ℃; Curtain coating idiosome is continuous binder removal 20h in continous way draft glue discharging furnace, and temperature is 580 ℃; Curtain coating green compact are put into sintering oven, sintering under nitrogen protection, sintering temperature is 1680 ℃, makes target product.
Above-described embodiment is only in order to illustrate technical scheme of the present invention; but not design of the present invention and protection domain are limited; those of ordinary skill in the art modifies or is equal to replacement technical scheme of the present invention; and not departing from aim and the scope of technical scheme, it all should be encompassed in claim scope of the present invention.
Claims (4)
1. a modification aluminium nitride ceramic substrate, is characterized in that: described ceramic substrate is by aluminium nitride, α-Al
2o
3nanometer powder, sintering agent, prepare without benzene ternary solvent system, dispersion agent, binding agent and softening agent.
2. a kind of modification aluminium nitride ceramic substrate according to claim 1, is characterized in that: described α-Al
2o
3the median size of nanometer powder is 15-25nm, specific surface area>=240m
2/ g; Described sintering agent is by CaO, Y
2o
3, two or more composition arbitrarily in CaF, BN and CaC; Described is the mixed solvent of ethanol, Virahol and butanone without benzene ternary solvent system; Described dispersion agent is the one in fish oil, glycerine or Viscotrol C; Described binding agent is polyvinyl butyral acetal; Described softening agent is dibutyl phthalate.
3. a kind of modification aluminium nitride ceramic substrate according to claim 1, is characterized in that: described α-Al
2o
3the quality of nanometer powder is the 1-3% of aluminium nitride quality; The quality of described sintering agent is the 2-10% of aluminium nitride quality; The described quality without benzene ternary solvent system is the 1-8% of aluminium nitride quality; The quality of described dispersion agent is the 2-4% of aluminium nitride quality; The quality of described binding agent is the 10-13% of aluminium nitride quality; The quality of described softening agent is the 4-9% of aluminium nitride quality.
4. a production method that realizes modification aluminium nitride ceramic substrate claimed in claim 1, is characterized in that: adopt the method for flow casting molding to be prepared, and specific as follows: by aluminium nitride, α-Al
2o
3nanometer powder and sintering agent are mixed in proportion; Mixed powder is dissolved in without in benzene ternary solvent system, then adds dispersion agent, carry out ball milling on ball mill one time, Ball-milling Time is 24-26 hour, and then adds binding agent and softening agent to grind 24-28 hour; Froth in vacuum under subnormal ambient; The slurry of handling well is carried out to flow casting molding with casting machine, controlling scraper height is 0.5mm, and curtain coating belt speed is 0.1-0.3m/min, and drying temperature is 20-90 ℃; Curtain coating idiosome is continuous binder removal 18-20h in continous way draft glue discharging furnace, and temperature is 580 ℃; Curtain coating green compact are put into sintering oven, sintering under nitrogen protection, sintering temperature is 1550-1680 ℃.
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Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104829238A (en) * | 2015-04-02 | 2015-08-12 | 朱卫 | Ternary composite burning aid for preparation of high-thermal conductivity ceramic substrate |
CN104987050A (en) * | 2015-06-18 | 2015-10-21 | 浙江长兴电子厂有限公司 | Preparation method for non-water-based high-purity nanoscale aluminum oxide ceramics |
CN106380207A (en) * | 2015-12-07 | 2017-02-08 | 蒋宏凯 | Preparation method for aluminum nitride substrate |
CN106588025A (en) * | 2016-12-08 | 2017-04-26 | 南通博泰美术图案设计有限公司 | Method for producing aluminum nitride ceramic substrate by adopting composite powder grain shape |
CN106631046A (en) * | 2016-11-30 | 2017-05-10 | 莱鼎电子材料科技有限公司 | Composite sintering aid for producing aluminum nitride ceramic substrate |
CN106673665A (en) * | 2016-12-30 | 2017-05-17 | 莱鼎电子材料科技有限公司 | Efficient ball milling slurrying process |
CN106938935A (en) * | 2017-04-26 | 2017-07-11 | 南通博泰美术图案设计有限公司 | Modified aluminium nitride ceramic substrate and its production method |
CN107188568A (en) * | 2017-07-11 | 2017-09-22 | 中国人民大学 | A kind of aluminum nitride ceramic substrate and preparation method thereof |
CN107540381A (en) * | 2016-12-30 | 2018-01-05 | 莱鼎电子材料科技有限公司 | A kind of aluminium nitride ceramic substrate slurry |
CN112266266A (en) * | 2020-11-05 | 2021-01-26 | 衡阳凯新特种材料科技有限公司 | Porous silicon nitride ceramic and preparation method thereof |
CN112573926A (en) * | 2020-12-28 | 2021-03-30 | 无锡海古德新技术有限公司 | Aluminum nitride conductor material and aluminum nitride full-ceramic heating structure device |
CN113213944A (en) * | 2021-05-24 | 2021-08-06 | 南京工程学院 | BN nanosheet toughened high-thermal-conductivity AlN ceramic substrate and preparation method thereof |
CN113582702A (en) * | 2021-08-12 | 2021-11-02 | 山东鹏程陶瓷新材料科技有限公司 | Aluminum nitride ceramic composite material for electronic packaging and preparation method thereof |
CN114014669A (en) * | 2021-12-16 | 2022-02-08 | 河北中瓷电子科技股份有限公司 | Preparation method of stretch-resistant aluminum nitride raw ceramic substrate |
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CN101386539A (en) * | 2008-10-16 | 2009-03-18 | 清华大学 | Aluminium nitride ceramics material and preparation method thereof |
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2013
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Patent Citations (1)
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CN101386539A (en) * | 2008-10-16 | 2009-03-18 | 清华大学 | Aluminium nitride ceramics material and preparation method thereof |
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CN104829238A (en) * | 2015-04-02 | 2015-08-12 | 朱卫 | Ternary composite burning aid for preparation of high-thermal conductivity ceramic substrate |
CN104987050A (en) * | 2015-06-18 | 2015-10-21 | 浙江长兴电子厂有限公司 | Preparation method for non-water-based high-purity nanoscale aluminum oxide ceramics |
CN106380207A (en) * | 2015-12-07 | 2017-02-08 | 蒋宏凯 | Preparation method for aluminum nitride substrate |
CN106631046A (en) * | 2016-11-30 | 2017-05-10 | 莱鼎电子材料科技有限公司 | Composite sintering aid for producing aluminum nitride ceramic substrate |
CN106588025A (en) * | 2016-12-08 | 2017-04-26 | 南通博泰美术图案设计有限公司 | Method for producing aluminum nitride ceramic substrate by adopting composite powder grain shape |
CN107540381A (en) * | 2016-12-30 | 2018-01-05 | 莱鼎电子材料科技有限公司 | A kind of aluminium nitride ceramic substrate slurry |
CN106673665A (en) * | 2016-12-30 | 2017-05-17 | 莱鼎电子材料科技有限公司 | Efficient ball milling slurrying process |
CN106938935A (en) * | 2017-04-26 | 2017-07-11 | 南通博泰美术图案设计有限公司 | Modified aluminium nitride ceramic substrate and its production method |
CN107188568A (en) * | 2017-07-11 | 2017-09-22 | 中国人民大学 | A kind of aluminum nitride ceramic substrate and preparation method thereof |
CN112266266A (en) * | 2020-11-05 | 2021-01-26 | 衡阳凯新特种材料科技有限公司 | Porous silicon nitride ceramic and preparation method thereof |
CN112573926A (en) * | 2020-12-28 | 2021-03-30 | 无锡海古德新技术有限公司 | Aluminum nitride conductor material and aluminum nitride full-ceramic heating structure device |
CN113213944A (en) * | 2021-05-24 | 2021-08-06 | 南京工程学院 | BN nanosheet toughened high-thermal-conductivity AlN ceramic substrate and preparation method thereof |
CN113582702A (en) * | 2021-08-12 | 2021-11-02 | 山东鹏程陶瓷新材料科技有限公司 | Aluminum nitride ceramic composite material for electronic packaging and preparation method thereof |
CN114014669A (en) * | 2021-12-16 | 2022-02-08 | 河北中瓷电子科技股份有限公司 | Preparation method of stretch-resistant aluminum nitride raw ceramic substrate |
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