CN1970667A - Preparation method of Al2O3/BN composite powder heat-conductive filler for heat-conductive adhesive - Google Patents
Preparation method of Al2O3/BN composite powder heat-conductive filler for heat-conductive adhesive Download PDFInfo
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- CN1970667A CN1970667A CN 200610118159 CN200610118159A CN1970667A CN 1970667 A CN1970667 A CN 1970667A CN 200610118159 CN200610118159 CN 200610118159 CN 200610118159 A CN200610118159 A CN 200610118159A CN 1970667 A CN1970667 A CN 1970667A
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- composite granule
- heat
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- conductive adhesive
- heat filling
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Abstract
The invention discloses a making method of Al2O3/BN composite powder conductive fill of heat conductive adhesive, which comprises the following steps: (1) making BN clad nanometer alumina powder through gel-sol method; (2) grafting to modify the powder through multi-functional compound with isocyanic acid group. The invetnio is compatible with epoxide resin to bind and pack electronic device, which possesses excellent radiation effect.
Description
Technical field
The present invention relates to a kind of Al for thermal conductive adhesive
2O
3The preparation method of/BN composite granule heat filling belongs to inorganic filler composite granule fabricating technology field.
Background technology
The Heat Conductive Insulation Adhesive that is used for encapsulation and bonding requires good heat dissipation, has higher thermal conductivity, adopts the inorganic filling material of high thermal conductivity then to be significant.Adopted many heat conductive fillers to mainly contain heat conduction inorganic powders such as aluminum oxide, aluminium nitride, boron nitride, silicon carbide in the past.Above-mentioned inorganic heat conductive filler with common micro powder grade often needs the high thermal conductivity that could improve polymer adhesive of filling, need be filled into the 50Vol1% of volume as AlN more than positive effect is arranged, but when improving the polymer adhesive thermal conductivity, the specific inductivity of filler is also increased, and mechanical mechanics property also sustains damage.In addition, the undue interpolation of inorganic filler can cause in thermal conductive adhesive viscosity rise, storage and the solidification process degradation problem under filler layering, the mechanical performance.
Al
2O
3The powder electrical insulating property is good, has certain thermal conductivity, and the source is abundant, and as the heat filling of thermal conductive adhesive aspect, its application is the most general.But aluminum oxide is compared other heat conduction inorganic fillers, and thermal conductivity is still too low; Improving thermal conductivity can not solve problem by the filling ratio that improves filler, and the filling ratio raising can cause negative impact, as causes the too high processing characteristics that influences of viscosity, and mechanical property also can be influenced.
BN thermal conductivity fortune is far above Al
2O
3But BN complicated process of preparation cost is too high.
One of desired solution that overcomes the above problems is exactly to concentrate both advantages, seeks a kind of powder surface modification method simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of with low cost, have an Al
2O
3Al with the BN premium properties
2O
3/ BN composite granule heat filling and preparation method thereof.
A kind of Al for thermal conductive adhesive of the present invention
2O
3The preparation method of/BN composite granule heat filling is characterized in that having following technical process and step:
A. it is alumina powder jointed to prepare the BN clad nano by sol-gel method:
With Al (NO
3)
39H
2O is dissolved in the ethanol, the ethanolic solution of KOH is dripped into gradually as precipitating reagent, simultaneously 0 ℃ of lower vigorous stirring 1 hour; Centrifugation is 20 minutes then, obtains boehmite sol; The ethanolic solution that adds then urea and boric acid, the content of control and regulation BN accounts for 50～90Vol%; With rotary evaporator alcohol solvent is vapored away, in baking oven, dry subsequently, the mixture of oven dry was calcined 7～8 hours under 600～900 ℃; Obtain Al
2O
3/ BN composite granule;
B. with containing the polyfunctional compound of isocyano group to Al
2O
3/ BN composite granule carries out surface graft modification:
Having under the argon shield condition, under 60～80 ℃ of temperature, using the isocyanates or derivatives thereof to Al
2O
3/ BN composite granule carries out surface graft modification; Finally obtain the Al through modification
2O
3/ BN composite granule heat filling.
In the above-mentioned preparation process, described precipitating reagent can also adopt ammoniacal liquor, urea, LiOH9H except KOH
2Among the O any; Described surface graft modification also can adopt silane coupler.
Among the above-mentioned preparation technology, select the inorganic salts aluminum nitrate to make raw material, because the inorganic salts price is lower, handling safety, and the ratio of the nitrate ion in the nitrate is easier to remove by roasting; Selecting ethanol as solvent, is because its easy dissolve inorganic salts, and nontoxic, volatile.
The Al that the inventive method makes
2O
3/ BN composite granule heat filling, its electrical insulation capability is good, and has a good thermal conductivity, higher thermal conductivity is applicable to as filler to be added in the organic polymer resin, such as epoxy resin, phenolic resins, mylar, polyurethane, cooperate and be modulated into Heat Conductive Insulation Adhesive, this adhesive can be used for bonding and the encapsulation of electronic devices and components, can disperse rapidly the heat accumulation of heating element as thermal interfacial material, prolongs the service life of electronic equipment.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
The preparation process and the step of present embodiment are as described below:
At first take by weighing a certain amount of Al (NO
3)
39H
2O is dissolved in the ethanol, gets a certain amount of KOH again and is dissolved in the ethanol colloidal sol, and the ethanolic solution of this KOH is slowly dripped in above-mentioned aluminum nitrate solution as precipitating reagent, uses simultaneously agitator 0 ℃ of lower vigorous stirring 1 hour; Use then the centrifugal separator centrifugation 20 minutes, and obtained boehmite sol; The percent by volume that the ethanol colloidal sol that adds then a certain amount of urea and boric acid, control and regulation make the consumption of the urea that forms BN and boric acid mixed solution account for complete soln is 75Vol%; Add thermal response, constantly stir, question response is complete, with rotary evaporator alcohol solvent is vapored away, and dries in baking oven then, and the mixture of oven dry was calcined 7～8 hours under 600～900 ℃, obtains Al
2O
3/ BN composite granule also namely is coated with the nano alumina powder jointed of BN.Then, the argon shield condition is being arranged, under 60～80 temperature with isocyanates to Al
2O
3/ BN composite granule carries out surface graft modification; Finally obtain the Al through modification
2O
3/ BN composite granule heat filling.
The filler that makes in the present embodiment has compatibility, high-insulativity and the high-termal conductivity good with epoxy resin, is applicable to organic polymer resin to cooperate modulation, makes Heat Conductive Insulation Adhesive.This adhesive is applicable to bonding and the encapsulation as electronic device, has great heat radiation effect.
Claims (2)
1. Al who is used for thermal conductive adhesive
2O
3The preparation method of/BN composite granule heat filling is characterized in that having following technical process and step:
A. it is alumina powder jointed to prepare the BN clad nano by sol-gel process: with Al (NO
3)
39H
2O is dissolved in the ethanol, the ethanolic solution of KOH is dripped into gradually as precipitating reagent, simultaneously 0 ℃ of lower vigorous stirring 1 hour; Centrifugation is 20 minutes then, obtains boehmite sol; The ethanolic solution that adds then urea and boric acid, the content of control and regulation BN accounts for 50～90Vol%; With rotary evaporator alcohol solvent is vapored away, in baking oven, dry subsequently, the mixture of oven dry was calcined 7～8 hours under 600～900 ℃; Obtain Al
2O
3/ BN composite granule;
B. with containing the polyfunctional compound of isocyano group to Al
2O
3/ BN composite granule carries out surface graft modification: having under the argon shield condition, using the isocyanates or derivatives thereof to Al under 60～80 ℃ of temperature
2O
3/ BN composite granule carries out surface graft modification; Finally obtain the Al through modification
2O
3/ BN composite granule heat filling.
2. a kind of Al for thermal conductive adhesive as claimed in claim 1
2O
3The preparation method of/BN composite granule heat filling is characterized in that described precipitating reagent except KOH, can also adopt ammoniacal liquor, urea, LiOH9H
2Among the O any; Described surface graft modification also can adopt silane coupler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610118159 CN1970667A (en) | 2006-11-09 | 2006-11-09 | Preparation method of Al2O3/BN composite powder heat-conductive filler for heat-conductive adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610118159 CN1970667A (en) | 2006-11-09 | 2006-11-09 | Preparation method of Al2O3/BN composite powder heat-conductive filler for heat-conductive adhesive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1970667A true CN1970667A (en) | 2007-05-30 |
Family
ID=38111700
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|---|---|---|---|
| CN 200610118159 Pending CN1970667A (en) | 2006-11-09 | 2006-11-09 | Preparation method of Al2O3/BN composite powder heat-conductive filler for heat-conductive adhesive |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102407626A (en) * | 2011-09-08 | 2012-04-11 | 鹤山东力电子科技有限公司 | Pressing technology of aluminum base copper-clad plate |
| CN102604330A (en) * | 2012-03-07 | 2012-07-25 | 天津大学 | Preparing method of epoxy resin composite material based on boron nitride nanoparticles |
| CN103073924A (en) * | 2013-01-23 | 2013-05-01 | 苏州大学 | Boron nitride comprising phosphonitrile structure and preparation method thereof |
| WO2014022963A1 (en) * | 2012-08-07 | 2014-02-13 | Feng Lin | Thermally conductive insulating material of high power led substrate and preparation method therefor |
| CN108753246A (en) * | 2018-04-04 | 2018-11-06 | 苏州达同新材料有限公司 | High heat conduction two-component casting glue |
| CN112063020A (en) * | 2020-09-04 | 2020-12-11 | 四川大学 | Core-shell spherical heat-conducting filler and preparation method and application thereof |
| CN113150484A (en) * | 2021-03-23 | 2021-07-23 | 浙江大学 | COC-based composite substrate material for high-frequency copper-clad plate and preparation method |
| KR20210136276A (en) * | 2020-05-07 | 2021-11-17 | 삼성에스디아이 주식회사 | Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated using the same |
| US11306239B2 (en) | 2018-11-30 | 2022-04-19 | Taiwan Union Technology Corporation | High thermal conductivity prepreg and uses of the same |
| CN116376321A (en) * | 2023-03-30 | 2023-07-04 | 武汉理工大学 | Preparation method and application of aluminum oxide coated hexagonal boron nitride composite powder |
-
2006
- 2006-11-09 CN CN 200610118159 patent/CN1970667A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102407626A (en) * | 2011-09-08 | 2012-04-11 | 鹤山东力电子科技有限公司 | Pressing technology of aluminum base copper-clad plate |
| CN102407626B (en) * | 2011-09-08 | 2015-07-15 | 鹤山东力电子科技有限公司 | Pressing technology of aluminum base copper-clad plate |
| CN102604330A (en) * | 2012-03-07 | 2012-07-25 | 天津大学 | Preparing method of epoxy resin composite material based on boron nitride nanoparticles |
| WO2014022963A1 (en) * | 2012-08-07 | 2014-02-13 | Feng Lin | Thermally conductive insulating material of high power led substrate and preparation method therefor |
| CN103764743A (en) * | 2012-08-07 | 2014-04-30 | 冯林 | Thermally conductive insulating material of high power LED substrate and preparation method therefor |
| CN103764743B (en) * | 2012-08-07 | 2015-08-12 | 常州通宝光电股份有限公司 | Heat-conducting insulation material of high-capacity LED substrate and preparation method thereof |
| CN103073924A (en) * | 2013-01-23 | 2013-05-01 | 苏州大学 | Boron nitride comprising phosphonitrile structure and preparation method thereof |
| CN103073924B (en) * | 2013-01-23 | 2014-09-17 | 苏州大学 | Boron nitride comprising phosphonitrile structure and preparation method thereof |
| CN108753246A (en) * | 2018-04-04 | 2018-11-06 | 苏州达同新材料有限公司 | High heat conduction two-component casting glue |
| US11306239B2 (en) | 2018-11-30 | 2022-04-19 | Taiwan Union Technology Corporation | High thermal conductivity prepreg and uses of the same |
| KR20210136276A (en) * | 2020-05-07 | 2021-11-17 | 삼성에스디아이 주식회사 | Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated using the same |
| CN112063020A (en) * | 2020-09-04 | 2020-12-11 | 四川大学 | Core-shell spherical heat-conducting filler and preparation method and application thereof |
| CN113150484A (en) * | 2021-03-23 | 2021-07-23 | 浙江大学 | COC-based composite substrate material for high-frequency copper-clad plate and preparation method |
| CN113150484B (en) * | 2021-03-23 | 2022-05-13 | 浙江大学 | COC-based composite substrate material for high-frequency copper-clad plate and preparation method |
| CN116376321A (en) * | 2023-03-30 | 2023-07-04 | 武汉理工大学 | Preparation method and application of aluminum oxide coated hexagonal boron nitride composite powder |
| CN116376321B (en) * | 2023-03-30 | 2024-06-04 | 武汉理工大学 | Preparation method and application of aluminum oxide coated hexagonal boron nitride composite powder |
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