CN109355543A - A kind of core-shell structure carbon covered metal Nano capsule Al2O3Composite substrate and preparation method - Google Patents
A kind of core-shell structure carbon covered metal Nano capsule Al2O3Composite substrate and preparation method Download PDFInfo
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- CN109355543A CN109355543A CN201811302238.4A CN201811302238A CN109355543A CN 109355543 A CN109355543 A CN 109355543A CN 201811302238 A CN201811302238 A CN 201811302238A CN 109355543 A CN109355543 A CN 109355543A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
Abstract
The invention discloses a kind of core-shell structure carbon covered metal Nano capsule Al2O3Composite substrate and preparation method include the following steps: that carbon alclad, carbon nickel coat, carbon copper-clad Nano capsule are 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/Ni/Cu/Al2O3Composite substrate.This method avoid the volatilization of metal Al, Ni, Cu 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
Technical field
The invention belongs to composite substrate preparation technical field more particularly to a kind of core-shell structure carbon covered metal Nano capsules
Al2O3Composite 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, Ni, Cu are introduced in ceramic substrate, for obtaining great power LED high heat conductance, low thermal coefficient of expansion
Ceramic substrate have important directive significance and application value.But directly in Al2O3Al powder, Ni powder, Cu powder are added in ceramic base
Sintering preparation Al/Ni/Cu/Al2O3Composite substrate, there is the problems such as volatilization, oxidation in metal Al, Ni, Cu, and then influence composite base
The performances such as the thermal conductivity of plate.
Summary of the invention
Technical problem to be solved by the present invention lies in: existing metal/Al2O3Metal is easy in composite substrate preparation process
The problems such as volatilization, oxidation, keep composite substrate consistency low, and thermal conductivity is low, and thermal expansion coefficient is high, provide a kind of core-shell structure carbon
Gold filled belongs to 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
Metal nano capsules A l2O3The preparation method of composite substrate, includes the following steps:
(1) carbon alclad, carbon nickel coat, carbon copper-clad Nano capsule are added to Al2O3In powder, ultrasonic agitation dispersion is 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 and cooled after carrying out lamination, heat seal, dumping to green compact
To room temperature, the Al/Ni/Cu/Al of nanostructure is obtained2O3Composite 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 carbon alclad Nano capsule, carbon nickel coat Nano capsule, carbon copper-clad Nano capsule, Al2O3The volume ratio of powder is 1
~3:1~3:1~3:20~60.
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 is 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.
In the step (3), the mass ratio of mixed-powder and fluid-mixing is 1~2:1~2.
Casting slurry in the step (4), which is molded on casting machine, to carry out, and scraper height is 0.5~2.0mm when molding.
Green sintering carries out under inert gas conditions in the step (4), 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 covered metal Nano capsule Al2O3Composite substrate made from the preparation method of composite substrate.
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, carbon nickel coat, carbon copper-clad Nano capsule substitution aluminium, nickel, the preparation of copper powder hot pressed sintering with core-shell structure
Al/Ni/Cu/Al2O3Composite substrate, by major ingredient Nano capsule and Al2O3Powder first carries out ultrasonic disperse, and it is equal to facilitate major ingredient ingredient
Even property, so that it is uniform to be conducive to performance；The shell carbon of core-shell structure not only can protect Al, Ni, Cu not oxidized in sintering process
And volatilization, guarantee the consistency of composite substrate, it can also be with Al2O3Reaction in-situ Al occurs for ceramic base2O3+C→Al+CO2, generation
Al forms stratum nucleare nano metal and Al2O3The transition zone that ceramic base combines, makes stratum nucleare metal and Al2O3It is well combined between ceramic base,
Substrate consistency is improved, the thermal conductivity of the higher substrate of consistency is better.In addition the Al of generation is reacted in dispersed and tiny distribution, favorably
In the thermal expansion coefficient for reducing composite substrate, improve performance uniformity.Cu has excellent heat transfer property, and the low temperature of Ni is anti-oxidant
Property is good, high-temperature volatile is low.Compared to Al/Al made of independent addition carbon alclad Nano capsule2O3Composite substrate, compound addition
Carbon alclad, carbon nickel coat, Al/Ni/Cu/Al made of carbon copper-clad Nano capsule2O3Composite substrate has better processing performance and biography
Hot property.
Carbon alclad, carbon nickel coat, carbon copper-clad Nano capsule are first added to Al by the present invention2O3Ultrasonic disperse is mixed in powder
Powder is then added in fluid-mixing, and carbon alclad, carbon nickel coat, carbon copper-clad Nano capsule can be made in Al2O3More uniformly divide in powder
It dissipates, is conducive to improve the heating conduction of the composite substrate of preparation, reduces thermal expansion coefficient.
So the carbon alclad for having core-shell structure, carbon nickel coat, carbon copper-clad Nano capsule are applied to hot pressed sintering Al/Ni/
Cu/Al2O3In composite substrate preparation process, the volatilization and oxidation of metal Al, Ni, Cu are not only avoided, and can be improved nanometer
Metal and Al2O3The comprehensive performances such as associativity, substrate consistency, thermal conductivity between ceramic base, while being suitble to large-scale industry metaplasia
It produces.
The present invention has the advantage that compared with prior art
(1) present invention replaces aluminium, nickel, copper powder using the carbon alclad, carbon nickel coat, carbon copper-clad Nano capsule of core-shell structure, keeps away
The volatilization and oxidation for having exempted from metal Al, Ni, Cu, guarantee the consistency of composite substrate, guarantee 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 forms stratum nucleare nano metal and Al2O3Ceramic base combine transition zone, make stratum nucleare metal and
Al2O3It is well combined between ceramic base, improves substrate consistency, improve the thermal conductivity of substrate；
(3) Al that reaction in-situ of the present invention generates is in dispersed and tiny distribution, advantageously reduces the thermal expansion system of composite substrate
Number improves performance uniformity.
(4) 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 covered metal Nano capsule Al/Ni/Cu/Al2O3The preparation method of composite substrate,
Steps are as follows:
(1) the carbon alclad for having core-shell structure, carbon nickel coat, carbon copper-clad Nano capsule are added to according to volume ratio 1:1:1:15
Al2O3In 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/Ni/Cu/Al2O3Composite substrate.
This nanometer of Al/Ni/Cu/Al2O3Composite substrate nano metal and Al2O3It being well combined between ceramic base, consistency is high,
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 covered metal Nano capsule Al/Ni/Cu/Al2O3The preparation method of composite substrate,
Steps are as follows:
(1) the carbon alclad for having core-shell structure, carbon nickel coat, carbon copper-clad Nano capsule are added to according to volume ratio 1:1:1:20
Al2O3In 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 300r/min, Ball-milling Time 15h 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 0.9mm, to life
Base carries out lamination, heat seal, dumping.Then inert gas Ar sintering, pressure 30MPa are filled in hot pressing furnace, sintering temperature is
2800 DEG C, 1h is kept the temperature, room temperature is cooled to the furnace after sintering, obtains a nanometer Al/Ni/Cu/Al2O3Composite substrate.
This nanometer of Al/Ni/Cu/Al2O3Composite substrate nano metal and Al2O3It being well combined between ceramic base, consistency is high,
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 covered metal Nano capsule Al/Ni/Cu/Al2O3The preparation method of composite substrate,
Steps are as follows:
(1) the carbon alclad for having core-shell structure, carbon nickel coat, carbon copper-clad Nano capsule are added to according to volume ratio 1:1:1:25
Al2O3In 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, 2.0h is kept the temperature, room temperature is cooled to the furnace after sintering, obtains a nanometer Al/Ni/Cu/Al2O3Composite substrate.
Measurement of comparison individually adds carbon alclad Nano capsule and compound addition carbon alclad, carbon nickel coat and carbon copper-clad Nano capsule
The Al/Al being prepared2O3And Al/Ni/Cu/Al2O3The consistency of composite substrate is respectively 91.5% and 92.7%, is improved
1.31%；Thermal coefficient is respectively 22.5W.m-1.K-1And 28.3W.m-1.K-1, improve 25.8%.It can be seen that this nanometer of Al/
Ni/Cu/Al2O3Composite substrate nano metal and Al2O3It is well combined between ceramic base, consistency is high, and thermal conductivity is high, thermal expansion system
Number 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 covered metal Nano capsule Al2O3The preparation method of composite substrate, which is characterized in that including as follows
Step:
(1) carbon alclad, carbon nickel coat, carbon copper-clad Nano capsule are 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 obtains the Al/Ni/Cu/Al of nanostructure2O3Composite substrate.
2. a kind of core-shell structure carbon covered metal 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 ultrasound in the step (2) is stirred
Mixing jitter time is 10~60min.
3. a kind of core-shell structure carbon covered metal 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, milling time is 2~30h, and the ball mill makes
Medium is stainless steel ball, and revolving speed is 150~600 revs/min, and ratio of grinding media to material is 5~20:1.
4. a kind of core-shell structure carbon covered metal Nano capsule Al according to claim 12O3The preparation method of composite substrate,
It is characterized in that, the carbon alclad Nano capsule, carbon nickel coat Nano capsule, carbon copper-clad Nano capsule, Al2O3The volume ratio of powder
For 1~3:1~3:1~3:15~75.
5. a kind of core-shell structure carbon covered metal Nano capsule Al according to claim 12O3The preparation method of composite substrate,
It is characterized in that, the bonding agent is polyvinyl butyral, dispersing agent is the castor oil and poly- second two of volume ratio 6~9:4~1
Alcohol, plasticizer is 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 covered metal Nano capsule Al according to claim 12O3The preparation method of composite substrate,
It is characterized in that, the mass ratio of mixed-powder and fluid-mixing is 1~2:1~2 in the step (3).
7. a kind of core-shell structure carbon covered metal Nano capsule Al according to claim 12O3The preparation method of composite substrate,
It is characterized in that, the casting slurry in the step (4) is molded on casting machine and carries out, when molding scraper height be 0.5~
2.0mm。
8. a kind of core-shell structure carbon covered metal Nano capsule Al according to claim 12O3The preparation method of composite substrate,
It is characterized in that, green sintering carries out under inert gas conditions in the step (4), 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 covered metal Nano capsule Al as described in any one of claims 1 to 82O3The system of composite substrate
Composite substrate made from Preparation Method.
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Cited By (2)
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| CN112210324A (en) * | 2020-09-15 | 2021-01-12 | 太仓金煜电子材料有限公司 | Preparation method of conductive adhesive, conductive material and preparation method of conductive material |
| CN115058129A (en) * | 2022-05-24 | 2022-09-16 | 武汉济能纳米流体技术有限公司 | Preparation method and application of functional micro powder for engine coolant |
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