CN109320215A - A kind of core-shell structure carbon alclad Nano capsule Al2O3Composite substrate and preparation method - Google Patents

A kind of core-shell structure carbon alclad Nano capsule Al2O3Composite substrate and preparation method Download PDF

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CN109320215A
CN109320215A CN201811301403.4A CN201811301403A CN109320215A CN 109320215 A CN109320215 A CN 109320215A CN 201811301403 A CN201811301403 A CN 201811301403A CN 109320215 A CN109320215 A CN 109320215A
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陈艳
杨旭东
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Anhui University of Technology AHUT
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Abstract

The invention discloses a kind of core-shell structure carbon alclad Nano capsule Al2O3Composite substrate and preparation method include the following steps: that core-shell structure carbon alclad Nano capsule is added to Al by (1)2O3In powder, 10~50min of ultrasonic agitation dispersion obtains mixed-powder;(2) bonding agent etc. is added in solvent, 10~60min of ultrasonic agitation dispersion obtains fluid-mixing;(3) mixed-powder is added in fluid-mixing, 2~30h is mixed on ball mill and obtains casting slurry, it is spare after degasification;(4) casting slurry is formed on casting machine and obtains green compact, be sintered and cooled after carrying out lamination, heat seal, dumping to green compact to room temperature, obtain a nanometer Al/Al2O3Composite substrate.This method avoid the volatilization of Al and oxidation, shell carbon and Al2O3Reaction in-situ Al occurs for matrix2O3+C→Al+CO2, the composite substrate consistency of preparation is high, and thermal conductivity is high, and thermal expansion coefficient is low and performance uniformity is good.

Description

A kind of core-shell structure carbon alclad Nano capsule Al2O3Composite substrate and preparation method
Technical field
The invention belongs to composite substrate preparation technical field more particularly to a kind of core-shell structure carbon alclad Nano capsule Al2O3 Composite substrate and preparation method.
Background technique
The heat generated in light emitting diode (LED) use process distributes the service life can be caused to decline not in time.Further, since Temperature raising causes generation thermal stress between chip and substrate to may cause wafer damage, chip and substrate separation.Therefore it solves Light-emitting LED heat dissipation is particularly important.Solve LED sinking path first is that improve printed circuit board (PCB) substrate thermal conductivity, will Heat quickly passes out.
Currently used PCB substrate is Al base and Cu based composites.Although its thermal conductivity is high, thermal expansion coefficient Greatly, and electrical insulation properties are poor, need that insulating layer is prepared on its surface, and are unfavorable for thermally conductive.Another common substrate is Al2O3 Ceramic substrate.Although it makes its high-power applications with good electrical insulation capability, lower thermal expansion coefficient, lower thermal conductivity It is subject to certain restrictions.So the composite substrate for obtaining a kind of good electrical insulation properties, low thermal coefficient of expansion and high heat conductance is this Field urgent problem.
In Al2O3Al is introduced in ceramic substrate, for obtaining the ceramics of great power LED high heat conductance, low thermal coefficient of expansion Substrate has important directive significance and application value.But directly in Al2O3Al powder sintering is added in ceramic base and prepares Al/Al2O3 There are the problems such as volatilization, oxidation, and then the performances such as thermal conductivity for influencing composite substrate in composite substrate, Al.
Summary of the invention
Technical problem to be solved by the present invention lies in: existing Al/Al2O3In composite substrate preparation process aluminium it is volatile, The problems such as oxidation, keeps composite substrate consistency low, and thermal conductivity is low, and thermal expansion coefficient is high, provide a kind of core-shell structure carbon alclad Nano capsule Al2O3The preparation method of composite substrate.
The present invention is to solve above-mentioned technical problem by the following technical programs, and the present invention includes a kind of core-shell structure carbon packet Aluminium Nano capsule Al2O3The preparation method of composite substrate, includes the following steps:
(1) core-shell structure carbon alclad Nano capsule is added to Al2O3In powder, ultrasonic agitation dispersion obtains mixed-powder;
(2) bonding agent, dispersing agent, plasticizer are added in solvent, ultrasonic agitation dispersion obtains fluid-mixing;
(3) mixed-powder of step (1) is added in the fluid-mixing of step (2), grinding obtains casting slurry, degasification It is spare afterwards;
(4) casting slurry of step (3) forms to obtain green compact, is sintered after carrying out lamination, heat seal, dumping to green compact, It is cooled to room temperature, obtains a nanometer Al/Al2O3Composite substrate.
Ultrasonic agitation jitter time is 10~50min in the step (1), the ultrasonic agitation in the step (2) Jitter time is 10~60min.
Grinding in the step (3) carries out on ball mill, and milling time is 2~30h, what the ball mill used Medium is stainless steel ball, and revolving speed is 150~600 revs/min, and ratio of grinding media to material is 5~20:1.
The core-shell structure carbon alclad Nano capsule and the Al2O3The volume ratio of powder is 1:7~25.
The bonding agent is polyvinyl butyral, and dispersing agent is the castor oil and polyethylene glycol of volume ratio 6~9:4~1, Plasticizer is dibutyl carboxylic acid, and solvent is dehydrated alcohol, the bonding agent: dispersing agent: plasticizer: solvent quality ratio is 7 ~9:0.4~0.6:5~7:80~86.
The mass ratio of the mixed-powder and the fluid-mixing is 1~2:1~2.
The carbon alclad Nano capsule purity is 85% or more.
Green sintering described in step (4) carries out under inert gas conditions, and the inert gas is Ar, and pressure is 10~90MPa, the sintering temperature are 1500~4000 DEG C, and sintering time is 0.5~2.0h.
A kind of core-shell structure carbon alclad Nano capsule Al2O3Composite substrate made from the preparation method of composite substrate.
The composite substrate consistency is high, and thermal conductivity is high, and thermal expansion coefficient is low, performance uniformity is high.
Core-shell structure is to be coated another nano material by chemical bond or other active forces by a kind of nano material Come the nanoscale ordered fabrication structure formed.Carbon covered metal Nano capsule is several layers of graphite flake layer closely around nano metal Grain ordered arrangement, forms class onion structure, and nano metal particles are in the core of onion.Since carbon shell can be in the space of very little Confine metallic particles, can avoid influence of the environment to nano material.
Carbon alclad Nano capsule substitution aluminium powder hot pressed sintering with core-shell structure prepares Al/Al2O3Composite substrate will be led Expect Nano capsule and Al2O3Powder first carries out ultrasonic disperse, facilitates major ingredient homogeneity of ingredients, so that it is uniform to be conducive to performance;Sintering The shell carbon of core-shell structure can not only protect Al not oxidized and volatilize in the process, guarantee the consistency of composite substrate, improve base The thermal conductivity of plate, can also be with Al2O3Reaction in-situ Al occurs for ceramic base2O3+C→Al+CO2, the Al of generation is in dispersed and tiny distribution, The thermal expansion coefficient of composite substrate is advantageously reduced, performance uniformity is improved.
Core-shell structure carbon alclad Nano capsule is first added to Al by the present invention2O3Ultrasonic disperse obtains mixed-powder again in powder It is added in fluid-mixing, core-shell structure carbon alclad Nano capsule can be made in Al2O3It is spreaded more evenly across in powder, is conducive to improve The heating conduction of the composite substrate of preparation reduces thermal expansion coefficient.
So the carbon alclad Nano capsule for having core-shell structure is applied to sintering preparation Al/Al2O3Composite substrate avoids The volatilization and oxidation of Al can be improved the comprehensive performances such as substrate consistency, thermal conductivity, while be suitble to large-scale industrial production.
The present invention has the advantage that compared with prior art
(1) present invention replaces aluminium powder using the carbon alclad Nano capsule of core-shell structure, avoids the volatilization and oxidation of Al, protects The consistency for demonstrate,proving composite substrate, guarantees the thermal conductivity of substrate;
(2) during hot pressed sintering of the present invention core-shell structure shell carbon and Al2O3Reaction in-situ Al occurs for matrix2O3+C →Al+CO2Al is generated, the Al of generation is in dispersed and tiny distribution, advantageously reduces the thermal expansion coefficient of composite substrate, improves performance Uniformity.
(3) Nano capsule is in Al2O3In powder dispersedly more evenly, the heating conduction of the composite substrate of preparation is high, thermally expands system Number is low.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation Example.
Embodiment 1
The present embodiment includes core-shell structure carbon alclad Nano capsule Al2O3The preparation method of composite substrate, steps are as follows:
(1) the carbon alclad Nano capsule for having core-shell structure is added to Al according to volume ratio 1:7.52O3In powder, ultrasonic agitation Dispersion 10min obtains mixed-powder;
(2) according to mass ratio 8.79:0.51:6.71:83.99 weigh polyvinyl butyral, volume ratio 3:2 castor oil and Polyethylene glycol, dibutyl carboxylic acid, dehydrated alcohol, and by polyvinyl butyral, castor oil, polyethylene glycol, dibutyl carboxylic acid It is added in dehydrated alcohol, ultrasonic agitation dispersion 10min obtains fluid-mixing;
(3) mixed-powder of step (1) is added in the fluid-mixing of step (2) according to mass ratio 1:1, in ball mill Upper implementation ball-milling treatment, ratio of grinding media to material 5:1, rotational speed of ball-mill 150r/min, Ball-milling Time 2h obtain casting slurry, degasification standby With;
(4) casting slurry of step (3) is formed on casting machine and obtains green compact, selecting scraper distance is 0.5mm, to life Base carries out lamination, heat seal, dumping.Then inert gas Ar sintering, pressure 10MPa are filled in hot pressing furnace, sintering temperature is 1500 DEG C, 0.5h is kept the temperature, room temperature is cooled to the furnace after sintering, obtains a nanometer Al/Al2O3Composite substrate.
This nanometer of Al/Al2O3Composite substrate consistency is high, and thermal conductivity is high, and thermal expansion coefficient is low, and performance uniformity is high.
Embodiment 2
The present embodiment includes core-shell structure carbon alclad Nano capsule Al2O3The preparation method of composite substrate, steps are as follows:
(1) the carbon alclad Nano capsule for having core-shell structure is added to Al according to volume ratio 1:202O3In powder, ultrasonic agitation Dispersion 30min obtains mixed-powder;
(2) according to mass ratio 8.79:0.51:6.71:83.99 weigh polyvinyl butyral, volume ratio 9:1 castor oil and Polyethylene glycol, dibutyl carboxylic acid, dehydrated alcohol, and by polyvinyl butyral, castor oil, polyethylene glycol, dibutyl carboxylic acid It is added in dehydrated alcohol, ultrasonic agitation dispersion 40min obtains fluid-mixing;
(3) mixed-powder of step (1) is added in the fluid-mixing of step (2) according to mass ratio 1:1, in ball mill Upper implementation ball-milling treatment, ratio of grinding media to material 10:1, rotational speed of ball-mill 400r/min, Ball-milling Time 10h obtain casting slurry, after degasification It is spare;
(4) casting slurry of step (3) is formed on casting machine and obtains green compact, selecting scraper distance is 1.0mm, to life Base carries out lamination, heat seal, dumping.Then inert gas Ar sintering, pressure 50MPa are filled in hot pressing furnace, sintering temperature is 3000 DEG C, 1h is kept the temperature, room temperature is cooled to the furnace after sintering, obtains a nanometer Al/Al2O3Composite substrate.
This nanometer of Al/Al2O3Composite substrate consistency is high, and thermal conductivity is high, and thermal expansion coefficient is low, and performance uniformity is high.
Embodiment 3
The present embodiment includes core-shell structure carbon alclad Nano capsule Al2O3The preparation method of composite substrate, steps are as follows:
(1) the carbon alclad Nano capsule for having core-shell structure is added to Al according to volume ratio 1:252O3In powder, ultrasonic agitation Dispersion 50min obtains mixed-powder;
(2) according to mass ratio 8.79:0.51:6.71:83.99 weigh polyvinyl butyral, volume ratio 7:3 castor oil and Polyethylene glycol, dibutyl carboxylic acid, dehydrated alcohol, and by polyvinyl butyral, castor oil, polyethylene glycol, dibutyl carboxylic acid It is added in dehydrated alcohol, ultrasonic agitation dispersion 60min obtains fluid-mixing;
(3) mixed-powder of step (1) is added in the fluid-mixing of step (2) according to mass ratio 1:1, in ball mill Upper implementation ball-milling treatment, ratio of grinding media to material 20:1, rotational speed of ball-mill 600r/min, Ball-milling Time 30h obtain casting slurry, after degasification It is spare;
(4) casting slurry of step (3) is formed on casting machine and obtains green compact, selecting scraper distance is 2.0mm, to life Base carries out lamination, heat seal, dumping.Then inert gas Ar sintering, pressure 90MPa are filled in hot pressing furnace, sintering temperature is 4000 DEG C, 2h is kept the temperature, room temperature is cooled to the furnace after sintering, obtains a nanometer Al/Al2O3Composite substrate.
Al powder is directly added in measurement of comparison embodiment 2 and adds the Al/Al that carbon alclad Nano capsule is prepared2O3It is multiple The consistency for closing substrate is respectively 86.2% and 91.5%, improves 6.15%;Thermal coefficient is respectively 18.6W.m-1.K-1With 22.5W.m-1.K-1, improve 20.97%.It can be seen that this nanometer of Al/Al2O3Composite substrate consistency is high, and thermal conductivity is high, heat The coefficient of expansion is low, and performance uniformity is high.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (9)

1. a kind of core-shell structure carbon alclad Nano capsule Al2O3The preparation method of composite substrate, which is characterized in that including walking as follows It is rapid:
(1) core-shell structure carbon alclad Nano capsule is added to Al2O3In powder, ultrasonic agitation dispersion obtains mixed-powder;
(2) bonding agent, dispersing agent, plasticizer are added in solvent, ultrasonic agitation dispersion obtains fluid-mixing;
(3) mixed-powder of step (1) is added in the fluid-mixing of step (2), grinding obtains casting slurry, degasification standby With;
(4) casting slurry of step (3) forms to obtain green compact, is sintered and cooled after carrying out lamination, heat seal, dumping to green compact To room temperature, a nanometer Al/Al is obtained2O3Composite substrate.
2. a kind of core-shell structure carbon alclad Nano capsule Al according to claim 12O3The preparation method of composite substrate, It is characterized in that, ultrasonic agitation jitter time is 10~50min in the step (1), the ultrasonic agitation in the step (2) Jitter time is 10~60min.
3. a kind of core-shell structure carbon alclad Nano capsule Al according to claim 12O3The preparation method of composite substrate, It is characterized in that, the grinding in the step (3) carries out on ball mill, and milling time is 2~30h, and the ball mill uses Medium be stainless steel ball, revolving speed be 150~600 revs/min, ratio of grinding media to material be 5~20:1.
4. a kind of core-shell structure carbon alclad Nano capsule Al according to claim 12O3The preparation method of composite substrate, It is characterized in that, the core-shell structure carbon alclad Nano capsule and the Al2O3The volume ratio of powder is 1:15~25.
5. a kind of core-shell structure carbon alclad Nano capsule Al according to claim 12O3The preparation method of composite substrate, It is characterized in that, the bonding agent is polyvinyl butyral, and dispersing agent is the castor oil and poly- second two of volume ratio 6~9:4~1 Alcohol, plasticizer are dibutyl carboxylic acid, and solvent is dehydrated alcohol, the bonding agent: dispersing agent: plasticizer: solvent quality ratio For 7~9:0.4~0.6:5~7:80~86.
6. a kind of core-shell structure carbon alclad Nano capsule Al according to claim 12O3The preparation method of composite substrate, It is characterized in that, the mass ratio of the mixed-powder and the fluid-mixing is 1~2:1~2.
7. a kind of core-shell structure carbon alclad Nano capsule Al according to claim 12O3The preparation method of composite substrate, It is characterized in that, the purity of the carbon alclad Nano capsule is 85% or more.
8. a kind of core-shell structure carbon alclad Nano capsule Al according to claim 12O3The preparation method of composite substrate, It is characterized in that, green sintering described in step (4) carries out under inert gas conditions, and the inert gas is Ar, pressure For 10~90MPa, the sintering temperature is 1500~4000 DEG C, and sintering time is 0.5~2.0h.
9. a kind of core-shell structure carbon alclad Nano capsule Al as described in any one of claims 1 to 82O3The preparation of composite substrate Composite substrate made from method.
CN201811301403.4A 2018-11-02 2018-11-02 A kind of core-shell structure carbon alclad Nano capsule Al2O3Composite substrate and preparation method Pending CN109320215A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111205099A (en) * 2020-01-20 2020-05-29 武汉科技大学 Batch-type operation high-temperature kiln near-zero heat loss refractory material lining body and preparation method thereof
CN113548877A (en) * 2021-08-11 2021-10-26 江苏师范大学 Efficient heat dissipation composite ceramic substrate and preparation method thereof

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CN102718498A (en) * 2012-07-04 2012-10-10 珠海微晶新材料科技有限公司 Coating preparation method for flakey aluminum oxide ceramic
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