CN106380207A - Preparation method for aluminum nitride substrate - Google Patents
Preparation method for aluminum nitride substrate Download PDFInfo
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- CN106380207A CN106380207A CN201510897186.XA CN201510897186A CN106380207A CN 106380207 A CN106380207 A CN 106380207A CN 201510897186 A CN201510897186 A CN 201510897186A CN 106380207 A CN106380207 A CN 106380207A
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- aluminium nitride
- nitride substrate
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Abstract
The invention discloses a preparation method for an aluminum nitride substrate. The preparation method comprises the following steps: (1) preparation of slurry: adding aluminum nitride powder, a sintering aid, an organic solvent and a dispersant into a ball milling tank in proportion, carrying out ball milling for 15 to 30 h, then adding a binder and a plasticizer in proportion and carrying out ball milling for 10 to 20 h so as to obtain tape casting slurry with a viscosity of 2000 to 3000 mPa.s; (2) deaeration: subjecting the treated slurry in the step (1) to vacuum negative-pressure deaeration and then carrying out filtering; (3) tape casting and molding; (4) binder discharging; and (5) sintering. According to the invention, through selection of the appropriate dispersant, binder and plasticizer, the tape casting slurry with an appropriate viscosity, uniform dispersion and good stability is obtained; binder discharging and sintering processes are further optimized, so sintering time is shortened, and energy consumption is lowered; and the obtained green body has a uniform structure, high density and good heat conductivity.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium nitride substrate.
Background technology
AlN ceramic substrate is a kind of new substrate material, has excellent combination property, quilt
It is considered most rising highly thermally conductive ceramic substrate.With Al2O3 ceramic phase ratio, AlN
There is higher thermal conductivity, generally Al2O3Pottery more than 5 times, be suitable for high power and
Large size chip；The thermal coefficient of expansion of AlN and Si match materials；Dielectric constant is relatively low,
It is about 8～10 under 1MHz；AlN tree material is hard, remains to work as usual under harsh environmental conditions
Make, therefore AlN can make very thin substrate, to meet the application of different enclosed chips.
Flow casting molding, (Tape Casting), also known as belt cast, doctor blade method.It is eighties of last century
A kind of forming method of ceramic that the seventies grow up, first the powder crushing
Be mixed and made into the slip with certain viscosity by suitable proportioning with organic plasticizer solution, slip from
Container with flowing down, is scraped with certain thickness by scraper and is coated in special base band, drying, solid
Peeling from above after change becomes the thin film of green tape, then right according to the size and dimension needs of finished product
The processed such as green tape is punched, lamination, make blank finished product to be sintered.
It is particularly suitable for the flaky pottery product of molding 0.2mm-3mm thickness, produce such product
Have that speed is fast, high degree of automation, efficiency high, uniform texture, good product quality etc.
Many advantages.
Content of the invention
It is an object of the invention to provide a kind of preparation method of aluminium nitride substrate, obtain
Aluminium nitride substrate density is high, and thermal conductivity is good.
The solution that the present invention solves its technical problem is：A kind of system of aluminium nitride substrate
Preparation Method, comprises the following steps：
(1) prepare slurry：By aluminium nitride powder, sintering aid, organic solvent and point
Powder is proportionally added in ball grinder, ball milling 15～30h, then is proportionally added into binding agent
With plastic agent ball milling 10～20h, finally obtaining viscosity is 2000～3000mPa.s curtain coating slurry
Material；Generally aluminium nitride powder particle diameter is 1.0-1.5 micron, with spherical aluminum nitride is preferably
Good；Sintering aid can be yittrium oxide, calcium oxide etc..
(2) deaeration：The casting slurry handled well in step (1) is taken off in negative pressure of vacuum
Bubble, then filters；Condition of negative pressure is generally -9.5MPa, 30～50min of inclined heated plate.
(3) flow casting molding：With casting machine, the slurry handled well in step (2) is carried out
Flow casting molding, obtains aluminium nitride substrate biscuit.Control scraper height is 0.6～0.9mm,
Curtain coating belt speed is 0.1～0.2m/min, and hothouse one area's temperature of casting machine is 70～90 DEG C,
Hothouse two area's temperature is 120～150 DEG C, is cut, obtain aluminum-nitride-based after being dried
Laminin base；
(4) dumping：The biscuit obtaining in step (3) is arranged at 500～800 DEG C
Glue；
(5) sinter：Base substrate after dumping is sintered under nitrogen atmosphere, sintering
Temperature is 1700～1800 DEG C.
Preferably, in step (1), described sintering aid is yittrium oxide, and particle diameter is general
For 1.0-1.5 micron, addition is the 0.1～2% of aluminum nitride powder body weight.
Preferably, in step (1), described organic solvent is ethanol and acetone mixing is molten
Agent, wherein ethanol are 67 with the volume ratio of acetone:33；Organic solvent weight and aluminium nitride
The weight of powder body is than for 1～2：1.Not only can be provided good molten using azeotropic solvent
Solution characteristic, and solvent can evaporate simultaneously, base substrate is affected little.
Preferably, in step (1), described dispersant is glycerol trioleate, Oleic acid
With any one in Oleum Ricini；The amount adding is the 1～3% of aluminum nitride powder body weight；
Utilization space steric hindrance makes powder body disperse.
Binding agent can improve biscuit intensity, is easy to the demoulding and movement, binding agent in slurry
Bridging can be formed and between powder granule, after solvent volatilization, strong bonding will be led to.Simultaneously
The viscosity of slurry can be adjusted, control its stability.Preferably, in step (1),
Described binding agent is polyvinyl alcohol or polyvinyl butyral resin, and the amount of addition is aluminum nitride powder
The 3～7% of body weight.
The pliability of plastic agent principal security biscuit and ductility, are allowed to divide with backing material
From when do not rupture, and be easily worked and place.Preferably, in step (1), described
Plastic agent is glycerol, in Polyethylene Glycol and dibutyl phthalate any one or many
Kind, addition is the 5～15% of aluminum nitride powder body weight.
It is further preferred that described plastic agent is Polyethylene Glycol and phthalic acid two fourth
Ester.
Preferably, in step (3), during flow casting molding, control scraper height is
0.6～0.9mm, curtain coating belt speed is 0.1～0.2m/min, hothouse one area's temperature of casting machine
Spend for 70～90 DEG C, hothouse two area's temperature is 120～150 DEG C, cut after being dried.
Step (4) dumping primarily to exclusion base substrate in organic principle it is preferable that
Described dumping, is under air atmosphere, is first warmed up to temperature in 8～12h
500～600 DEG C, it is incubated 1～2h, in 2～3h, is then warming up to 700～800 DEG C, insulation
2～3h.
Preferably, in step (5), described sintering is in nitrogen atmosphere, and microwave burns
Knot, sintering power is 40-50kw, to reduce sintering time, and improves sintered density.
The invention has the beneficial effects as follows：The present invention passes through from suitable dispersant, binding agent
Obtain viscosity properly with plasticiser configuration, be uniformly dispersed, the casting slurry of good stability, enters one
Step, by optimizing dumping and sintering process, shortens sintering time, reducing energy consumption, and the base obtaining
Body even tissue, density is high, and thermal conductivity is good.
Specific embodiment
Technique effect below with reference to design, concrete structure and generation to the present invention for the embodiment
Carry out clear, complete description, to be completely understood by the purpose of the present invention, feature and effect.
Obviously, described embodiment is a part of embodiment of the present invention, rather than whole enforcement
Example, based on embodiments of the invention, those skilled in the art is not paying creative work
Under the premise of the other embodiment that obtained, belong to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of aluminium nitride substrate, comprises the following steps：
(1) prepare slurry：By the spherical aluminum nitride powder of 1000g 1.0-1.5 micron,
The yttrium oxide powder of 1g1.0-1.5 micron, the ethanol of 1000g and acetone mixture are (wherein
Ethanol is 67 with the volume ratio of acetone:33) and in 15g Oleum Ricini addition ball grinder, ball
Mill 20h, adds 30g polyvinyl alcohol and 50g glycerol ball milling 12h, finally obtains viscous
Spend for 2500mPa.s casting slurry.
(2) deaeration：By the described casting slurry handled well in step (2) in -9.5MPa
Subnormal ambient under carry out vacuum defoamation 50min, then filter.
(3) flow casting molding：With casting machine to the casting slurry handled well in step (3)
Carry out flow casting molding；Control scraper height is 0.7mm, and curtain coating belt speed is 0.1m/min,
Hothouse one area's temperature of casting machine is 80 DEG C, and hothouse two area's temperature is 140 DEG C, does
Cut after dry, obtained aluminium nitride substrate biscuit.
(4) dumping：It is under air atmosphere, first temperature is warmed up in 10h
500 DEG C, it is incubated 1h, in 2h, is then warming up to 800 DEG C, be incubated 2h.
(5) sinter：Sintering is in nitrogen atmosphere, 40kw microwave sintering, is warming up to
1700 DEG C, it is incubated 12h.
Base substrate after sintering is polished, polishing, obtain the nitrogen that thickness is 0.49mm
Change aluminium base sample.
Embodiment 2
A kind of preparation method of aluminium nitride substrate, comprises the following steps：
(1) prepare slurry：By the aluminium nitride powder of 1000g 1.0-1.5 micron, 10g
Yittrium oxide, the ethanol of the 1200g and acetone mixture (volume ratio of wherein ethanol and acetone
For 67:33) and in 25g glycerol trioleate addition ball grinder, ball milling 12～20h, then
Add 50g polyvinyl butyral resin and 150g Polyethylene Glycol and dibutyl phthalate
Mixing plastic agent, the wherein volume ratio of Polyethylene Glycol and dibutyl phthalate are 1:2,
Ball milling 18h, finally obtaining viscosity is 3000mPa.s casting slurry；
(2) deaeration：By the described casting slurry handled well in step (2) in -9.5MPa
Subnormal ambient under carry out vacuum defoamation 40min, then filter；
(3) flow casting molding：With casting machine to the casting slurry handled well in step (3)
Carry out flow casting molding；Control scraper height is 0.6mm, and curtain coating belt speed is 0.2m/min,
Hothouse one area's temperature of casting machine is 70 DEG C, and hothouse two area's temperature is 120 DEG C, does
Cut after dry, obtained aluminium nitride substrate biscuit；
(4) dumping：It is under air atmosphere, first temperature is warmed up in 8h 600 DEG C,
Insulation 2h, is then warming up to 800 DEG C in 2.5h, is incubated 2h.
(5) sinter：Sintering is in nitrogen atmosphere, microwave power 50kw, is heated to
1750 DEG C, then it is incubated 8h.
Base substrate after sintering is polished, polishing, obtain the nitrogen that thickness is 0.46mm
Change aluminium base sample.
Embodiment 3
A kind of preparation method of aluminium nitride substrate, comprises the following steps：
(1) prepare slurry：By the aluminium nitride powder of 1000g 1.0-1.5 micron,
The yttrium oxide powder of 20g1.0-1.5 micron, the ethanol of 2000g and acetone mixture (its
Middle ethanol is 67 with the volume ratio of acetone:33) and in 10g Oleic acid addition ball grinder, ball
Mill 12h, adds 70g polyvinyl alcohol and 120g Polyethylene Glycol, phthalic acid two
Butyl ester and glycerol mixing plastic agent, wherein Polyethylene Glycol：Dibutyl phthalate：Sweet
Oil=2：1：2 (volume ratios), ball milling 24h, finally obtaining viscosity is 2000mPa.s
Casting slurry.
(2) deaeration：By the described casting slurry handled well in step (2) in -9.5MPa
Subnormal ambient under carry out vacuum defoamation 30min, then filter.
(3) flow casting molding：With casting machine to the casting slurry handled well in step (3)
Carry out flow casting molding；Control scraper height is 0.9mm, and curtain coating belt speed is 0.15m/min,
Hothouse one area's temperature of casting machine is 90 DEG C, and hothouse two area's temperature is 150 DEG C, does
Cut after dry, obtained aluminium nitride substrate biscuit.
(4) dumping：It is under air atmosphere, first temperature is warmed up in 12h
550 DEG C, it is incubated 2h, in 2h, is then warming up to 700 DEG C, be incubated 3h.
(5) sinter：Sintering is in nitrogen atmosphere, and microwave power 45kw is warming up to
1700 DEG C, then it is incubated 10h.
Base substrate after sintering is polished, polishing, obtain the nitrogen that thickness is 0.48mm
Change aluminium base sample.
The aluminium nitride substrate obtaining in embodiment 1～3 is entered line density and thermal conductivity test, its
In in each embodiment sample take three, average after test, test result is as shown in table 1：
Table 1 aluminium nitride substrate sample tests
| Test event | Method of testing | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Density (g/m3) | Drainage | 2.94 | 2.97 | 2.96 |
| Thermal conductivity (W/m.K) | GJB1201-1-91 laser pulse method | 49.45 | 46.25 | 47.74 |
It can be seen from the results above that the preparation technology of the present invention, sintering time is short, and obtains
Aluminium nitride substrate density high, pore is few, good heat conduction effect.
Above the better embodiment of the present invention is illustrated, but the invention is simultaneously
It is not limited to described embodiment, those of ordinary skill in the art are without prejudice to before spirit of the present invention
Put and also can make a variety of equivalent modifications or replacement, these equivalent modifications or replacement all comprise
In the application claim limited range.
Claims (10)
1. a kind of preparation method of aluminium nitride substrate is it is characterised in that comprise the following steps：
（1）Prepare slurry：Aluminium nitride powder, sintering aid, organic solvent and dispersant are proportionally added in ball grinder, ball milling 15 ~ 30h, then are proportionally added into binding agent and plastic agent ball milling 10 ~ 20h, finally obtaining viscosity is 2000 ~ 3000mPa. s casting slurry；
（2）Deaeration：By step（1）In the casting slurry handled well in negative pressure of vacuum deaeration, then filter；
（3）Flow casting molding：With casting machine to step（2）In the slurry handled well carry out flow casting molding, obtain aluminium nitride substrate biscuit；
（4）Dumping：By step（3）In the biscuit that obtains carry out dumping at 500 ~ 800 DEG C；
（5）Sintering：Base substrate after dumping is sintered under nitrogen atmosphere, sintering temperature is 1700 ~ 1800 DEG C.
2. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（1）In, described sintering aid is yittrium oxide, and addition is the 0.1 ~ 2% of aluminum nitride powder body weight.
3. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（1）In, described organic solvent is ethanol and acetone mixed solvent, and wherein ethanol and the volume ratio of acetone are 67:33；The weight of organic solvent weight and aluminium nitride powder is than for 1 ~ 2：1.
4. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（1）In, described dispersant is any one in glycerol trioleate, Oleic acid and Oleum Ricini；The amount adding is the 0.5 ~ 2% of aluminum nitride powder body weight.
5. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（1）In, described binding agent is polyvinyl alcohol or polyvinyl butyral resin, and the amount of addition is the 3 ~ 7% of aluminum nitride powder body weight.
6. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（1）In, described plastic agent is any one or more in glycerol, Polyethylene Glycol and dibutyl phthalate, and addition is the 5 ~ 15% of aluminum nitride powder body weight.
7. aluminium nitride substrate according to claim 6 tape casting preparation it is characterised in that：Step（1）In, described plastic agent is Polyethylene Glycol and dibutyl phthalate.
8. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（3）In, control scraper height is 0.6 ~ 0.9mm, and curtain coating belt speed is 0.1 ~ 0.2m/min, and hothouse one area's temperature of casting machine is 70 ~ 90 DEG C, and hothouse two area's temperature is 120 ~ 150 DEG C, is cut after being dried.
9. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（4）In, described dumping, is under air atmosphere, first temperature is warmed up in 8 ~ 12h 500 ~ 600 DEG C, is incubated 1 ~ 2h, is then warming up to 700 ~ 800 DEG C in 2 ~ 3h, is incubated 2 ~ 3h.
10. aluminium nitride substrate according to claim 1 preparation method it is characterised in that：Step（5）In, described sintering is microwave sintering, and sintering power is 40-50kw.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107324812A (en) * | 2017-07-14 | 2017-11-07 | 上海大学 | Behavior of Slurry for Aluminum Nitride Ceramics and preparation method thereof |
| CN107365155A (en) * | 2017-06-27 | 2017-11-21 | 中国科学院上海硅酸盐研究所 | A kind of low-temperature sintering adjuvant system of aluminium nitride ceramics |
| CN108258081A (en) * | 2017-12-07 | 2018-07-06 | 上海大学 | CdZnTe films and AlN/CdZnTe base ultraviolet light detector preparation method and applications |
| CN111704469A (en) * | 2020-06-28 | 2020-09-25 | 北京工业大学 | Aluminum nitride ceramic substrate 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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| CN103755351A (en) * | 2013-12-30 | 2014-04-30 | 莱鼎电子材料科技有限公司 | Method for producing LED (light-emitting diode) by low-cost aluminum nitride ceramic substrate |
| 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107365155A (en) * | 2017-06-27 | 2017-11-21 | 中国科学院上海硅酸盐研究所 | A kind of low-temperature sintering adjuvant system of aluminium nitride ceramics |
| CN107365155B (en) * | 2017-06-27 | 2020-09-18 | 中国科学院上海硅酸盐研究所 | Low-temperature sintering aid system of aluminum nitride ceramic |
| 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 |
| CN107324812A (en) * | 2017-07-14 | 2017-11-07 | 上海大学 | Behavior of Slurry for Aluminum Nitride Ceramics and preparation method thereof |
| CN108258081A (en) * | 2017-12-07 | 2018-07-06 | 上海大学 | CdZnTe films and AlN/CdZnTe base ultraviolet light detector preparation method and applications |
| CN111704469A (en) * | 2020-06-28 | 2020-09-25 | 北京工业大学 | Aluminum nitride ceramic substrate 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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Application publication date: 20170208 |