CN109824382A - A kind of heat management SiC/ graphite film laminar composite and preparation method thereof - Google Patents
A kind of heat management SiC/ graphite film laminar composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of heat management SiC/ graphite film laminar composites and preparation method thereof, the composite material presses volume fraction, by 10~50% SiC reinforced phase and 50~90% graphite film matrix phase composition, graphite film and SiC are successively alternately distributed in the composite, and perfect orientations are presented；Preparation method by graphite film surface coated Si/C ceramic layer, surface coated Si/C ceramic layer graphite film it is layer-by-layer stack and pre-molding, the vacuum heating-press sintering of preforming sample and sintering after four steps of subsequent processing of sample complete.The preparation method efficiently solves the problems such as traditional Si C/ graphite composite material sintering densification is difficult and interface bond strength between SiC and graphite is low.The SiC/ graphite film laminar composite prepared using the method for the present invention, not only parallel laminar direction has very high thermal conductivity, and vertical layer direction can obtain the thermal expansion coefficient to match with package substrate, there is low density and high intensity simultaneously, be a kind of very promising new heat pipe reason material.
Description
Technical field
The present invention relates to functional material and preparation method thereof, in particular to a kind of heat management SiC/ graphite film lamellar composite
Material and preparation method thereof.
Background technique
In recent years, it is strided forward with electronics member/device to highly integrated, miniaturization and lightweight direction, for heat management
The research of anisotropic graphite material achieves huge progress.More mainly highly oriented graphite material, institute are studied at present
It is usually graphite fibre, crystalline flake graphite etc. with raw material.Such as document " Laminate squeeze casting of carbon
fiber reinforced aluminum matrix composites”(Materials and Design.67(2015)
154-158), document " In-plane thermal enhancement behaviors of Al matrix composites
With oriented graphite flake alignment " (Composites:Part B 70 (2015) 256-262) etc..
Existing research, which shows graphite degree of orientation in the material, and interface resistance is influences highly oriented graphite material heating conduction
Key factor.Graphite degree of orientation is higher, and interface resistance is smaller, and the thermal conductivity of material is higher.However, due to graphite fibre,
Perfect orientation cannot be presented in highly oriented graphite material for the raw materials such as crystalline flake graphite and there are interface resistances, therefore cannot sufficiently send out
The heating conduction advantage of these graphite raw materials is waved, so that the highly oriented graphite material heating conduction prepared is pre- lower than theoretical
Phase.
High crystallinity graphite film is high with the degree of orientation, degree of graphitization is high, thickness is controllable, planar dimension is big, edgewise is warm
Conductance height (~1800Wm-1·K-1), it is at low cost the advantages that, as a kind of novel two-dimentional highly heat-conductive material, from appearance
Just by the concern of domestic and international researcher, and in the high quantity of heat production such as computer, mobile phone but it is badly in need of in the electronic equipment of heat dissipation
It is widely applied.However, high crystallinity graphite film strength is very low, in order to which the further expansion graphite raw material is in field of heat management
In application, need to usually be prepared into graphite film block materials or the Composites such as itself and metal, ceramics are prepared into graphite film composite wood
Material.
SiC has the excellent properties such as low-density, high intensity, high heat conductance, low thermal coefficient of expansion, and has well with graphite
Chemical compatibility, therefore be highly suitable as the reinforced phase of graphite material.High crystallinity graphite film and SiC ceramic is compound
Change, and SiC/ graphite film laminar composite is prepared by appropriate technique, can not only make graphite film and SiC that perfect orientation be presented
Arrangement so as to give full play to the high thermal conductivity advantage of each composition phase, and then obtains the composite material parallel laminar direction
Very high thermal conductivity, and composite material vertical layer direction thermal expansion system can be realized by the adjusting of SiC volume fraction
Several regulations makes it have the thermal expansion coefficient to match with the electronics member/device that need to be radiated, and in addition the material also has low
Density and high intensity, these performances meet thermal management materials " lightweight, high-strength, thermally conductive predominant direction and thermal expansion matching very much
Direction is perpendicular " application characteristic so that SiC/ graphite film laminar composite is a kind of heat for having very much commercial promise
Management material.However so far, high-thermal conductive metal is concentrated mainly on (such as to the research of graphite film laminar composite both at home and abroad
Al, Cu etc.) enhancing graphite film laminar composite aspect, such as document " Fabrication and thermal
conductivity of copper coated graphite film/aluminum composites for effective
Thermal management " (J.Alloys Compd.711 (2017) 22-30), document " Layer by layer
graphite film reinforced aluminum composites with an enhanced performance of
thermal conduction in the thermal management applications”(J.Alloys Compd.742
(2018) 601-609) etc., there has been no the open source literature reports about SiC ceramic enhancing graphite film laminar composite.
Summary of the invention
The purpose of the present invention is to provide a kind of vertical layer directions to match with electronics member/device thermal expansion coefficient, put down
Row stratiform direction has heat management SiC/ graphite film laminar composite and preparation method thereof of superelevation thermal conductivity.
To achieve the above objectives, heat management of the invention SiC/ graphite film laminar composite, by volume fraction, by
10~50% SiC ceramic phase and 50~90% graphite phase composition block structure, wherein SiC ceramic layer is evenly coated at stone
The surface of ink film, graphite film and SiC ceramic layer are successively alternately distributed in the composite and perfect orientations are presented.
The preparation method of heat management of the present invention SiC/ graphite film laminar composite, which is characterized in that including following steps
It is rapid:
The first step coats SiC ceramic layer in graphite film surface by molten-salt growth method, obtains the stone of surface coated Si/C ceramic layer
Ink film；
The graphite film of surface coated Si/C ceramic layer is placed in graphite jig by second step by the way of successively stacking, and
The pre-molding in the case where pressure is 20MPa, obtains preforming sample；
Third step, by preforming sample vacuum degree lower than 1Pa, sintering temperature be 1800~2000 DEG C, sintering pressure is
30~50MPa, heat preservation 2h carry out vacuum heating-press sintering, obtain block materials after furnace cooling；
The SiC ceramic layer of 4th step, removal vacuum heating-press sintering gained block materials side cladding obtains heat management use
SiC/ graphite film laminar composite.
First step molten-salt growth method coating SiC ceramic layer the following steps are included:
1) it is 1:10~1:2 by Si powder and graphite film molar ratio, takes Si powder；
2) it is that 1:1 takes NaCl and NaF by NaCl and NaF molar ratio, pours into mortar and grind and be uniformly mixed, obtain salt-mixture
Powder；
3) it is 1:5 with the mass ratio for mixing salt fines by Si powder, Si powder and mixing salt fines is poured into mortar and grind and mix
Uniformly, coating powder is obtained；
4) graphite film and coating powder are successively alternately packed into according to the sequence of " coating powder-graphite film-coating powder ... "
In graphite crucible, covers crucible cover and be placed in heat-treatment furnace；
5) argon gas is passed through after vacuumizing heat-treatment furnace, under conditions of flowing argon gas protection, from room temperature to 1200
DEG C and keep the temperature 4 hours, cool to room temperature with the furnace, with distilled water cook out salt and dry after obtain the graphite film of coated Si/C ceramic layer.
The graphite film with a thickness of 12~70 microns.
The partial size of the Si powder is 5 microns.
The graphite crucible is the graphite crucible of inner surface coated Si/C ceramic layer.
Compared with prior art, the present invention has the advantage that
1) SiC/ graphite film laminar composite prepared by the present invention enhances compared to high-thermal conductive metal (such as Al, Cu)
Graphite film laminar composite not only has higher intensity and lower density, but also can be where with electronics member/device
In-plane obtain matching thermal expansion coefficient, while there is higher thermal conductivity in the vertical in-plane, thus
Not only improve the thermal stress reduced between thermal management materials and electronics member/device, but the heat that electronics member/device can be generated and
When remove, guarantee electronics member/normal working efficiency of device and service life, therefore be more able to satisfy the comprehensive of thermal management materials
It can require.
2) SiC/ graphite composite material is prepared compared to SiC is introduced directly in graphite matrix, the present invention uses fused salt
Method forms the SiC of uniformly continuous in graphite film surface in situ, this can not only convert SiC and SiC for the sintering of graphite film and SiC
Between sintering, to be conducive to the sintering of composite material and the raising of consistency；And it is straight with graphite to also significantly increase SiC
Interface bond strength after connecing hot pressed sintering, thus make the composite material comprehensive performance be improved significantly.Meanwhile passing through control
Si powder and graphite film molar ratio in fused salt reaction process processed, can coat thin and continuous SiC, this has very much in graphite film surface
Conducive to high graphite film content is prepared, i.e. the SiC of parallel laminar direction high thermal conductivity enhances graphite film laminar composite.
3) present invention prepares SiC/ graphite film laminar composite by lamination-vacuum hot-pressed sintered technology, not only prepares
It is simple process, at low cost, and graphite film and SiC can be made successively to be alternately distributed in the composite, and perfect orientation row is presented
Column, so as to give full play to the high thermal conductivity advantage in the composite material parallel laminar direction.
Specific embodiment
Embodiment 1:
The first step, the graphite film preparation of surface coated Si/C ceramic layer:
It 1) is 1:2 by Si powder and graphite film molar ratio, taking partial size is 5 microns of Si powder；
2) it is that 1:1 takes NaCl and NaF by NaCl and NaF molar ratio, pours into mortar and grind and be uniformly mixed, obtain salt-mixture
Powder；
3) it is 1:5 with the mass ratio for mixing salt fines by Si powder, Si powder and mixing salt fines is poured into mortar and grind and mix
Uniformly, coating powder is obtained；
4) take graphite film and coating powder with a thickness of 12 microns according to the suitable of " coating powder-graphite film-coating powder ... "
Sequence is successively alternately packed into the graphite crucible of inner surface coated Si/C ceramic layer, is covered crucible cover and is placed in heat-treatment furnace；
5) argon gas is passed through after vacuumizing heat-treatment furnace, under conditions of flowing argon gas protection, from room temperature to 1200
DEG C and keep the temperature 4 hours, cool to room temperature with the furnace, with distilled water cook out salt and dry after obtain the graphite film of coated Si/C ceramic layer
(salt is cooked out using distilled water, the graphite film of adjacent layer coated Si/C ceramic layer can be detached from the stone to form single layer coated Si/C ceramic layer
Ink film)；
The graphite film of surface coated Si/C ceramic layer is placed in graphite jig by second step by the way of successively stacking, and
The pre-molding in the case where pressure is 20MPa, obtains preforming sample；
Third step, by preforming sample vacuum degree lower than 1Pa, sintering temperature be 2000 DEG C, sintering pressure 40MPa,
It keeps the temperature 2h and carries out vacuum heating-press sintering, obtain block materials after furnace cooling；
4th step, the SiC ceramic layer for polishing or cutting away the cladding of block materials side obtained by vacuum heating-press sintering obtain heat
Management SiC/ graphite film laminar composite.
The heat management prepared by the above process SiC/ graphite film laminar composite, by volume fraction, by 50%
SiC ceramic phase and 50% graphite phase composition block structure, wherein SiC ceramic layer is evenly coated at the surface of graphite film, stone
Ink film and SiC ceramic layer are successively alternately distributed in the composite and perfect orientations are presented.
Embodiment 2:
The first step, the graphite film preparation of surface coated Si/C ceramic layer:
It 1) is 2:5 by Si powder and graphite film molar ratio, taking partial size is 5 microns of Si powder；
2) it is that 1:1 takes NaCl and NaF by NaCl and NaF molar ratio, pours into mortar and grind and be uniformly mixed, obtain salt-mixture
Powder；
3) it is 1:5 with the mass ratio for mixing salt fines by Si powder, Si powder and mixing salt fines is poured into mortar and grind and mix
Uniformly, coating powder is obtained；
4) take graphite film and coating powder with a thickness of 50 microns according to the suitable of " coating powder-graphite film-coating powder ... "
Sequence is successively alternately packed into the graphite crucible of inner surface coated Si/C ceramic layer, is covered crucible cover and is placed in heat-treatment furnace；
5) argon gas is passed through after vacuumizing heat-treatment furnace, under conditions of flowing argon gas protection, from room temperature to 1200
DEG C and keep the temperature 4 hours, cool to room temperature with the furnace, with distilled water cook out salt and dry after obtain the graphite film of coated Si/C ceramic layer
(salt is cooked out using distilled water, the graphite film of adjacent layer coated Si/C ceramic layer can be detached from the stone to form single layer coated Si/C ceramic layer
Ink film)；
The graphite film of surface coated Si/C ceramic layer is placed in graphite jig by second step by the way of successively stacking, and
The pre-molding in the case where pressure is 20MPa, obtains preforming sample；
Third step, by preforming sample vacuum degree lower than 1Pa, sintering temperature be 1800 DEG C, sintering pressure 50MPa,
It keeps the temperature 2h and carries out vacuum heating-press sintering, obtain block materials after furnace cooling；
4th step, the SiC ceramic layer for polishing or cutting away the cladding of block materials side obtained by vacuum heating-press sintering obtain heat
Management SiC/ graphite film laminar composite.
The heat management prepared by the above process SiC/ graphite film laminar composite, by volume fraction, by 40%
SiC ceramic phase and 60% graphite phase composition block structure, wherein SiC ceramic layer is evenly coated at the surface of graphite film, stone
Ink film and SiC ceramic layer are successively alternately distributed in the composite and perfect orientations are presented.
Embodiment 3:
The first step, the graphite film preparation of surface coated Si/C ceramic layer:
It 1) is 3:10 by Si powder and graphite film molar ratio, taking partial size is 5 microns of Si powder；
2) it is that 1:1 takes NaCl and NaF by NaCl and NaF molar ratio, pours into mortar and grind and be uniformly mixed, obtain salt-mixture
Powder；
3) it is 1:5 with the mass ratio for mixing salt fines by Si powder, Si powder and mixing salt fines is poured into mortar and grind and mix
Uniformly, coating powder is obtained；
4) take graphite film and coating powder with a thickness of 40 microns according to the suitable of " coating powder-graphite film-coating powder ... "
Sequence is successively alternately packed into the graphite crucible of inner surface coated Si/C ceramic layer, is covered crucible cover and is placed in heat-treatment furnace；
5) argon gas is passed through after vacuumizing heat-treatment furnace, under conditions of flowing argon gas protection, from room temperature to 1200
DEG C and keep the temperature 4 hours, cool to room temperature with the furnace, with distilled water cook out salt and dry after obtain the graphite film of coated Si/C ceramic layer
(salt is cooked out using distilled water, the graphite film of adjacent layer coated Si/C ceramic layer can be detached from the stone to form single layer coated Si/C ceramic layer
Ink film)；
The graphite film of surface coated Si/C ceramic layer is placed in graphite jig by second step by the way of successively stacking, and
The pre-molding in the case where pressure is 20MPa, obtains preforming sample；
Third step, by preforming sample vacuum degree lower than 1Pa, sintering temperature be 1900 DEG C, sintering pressure 30MPa,
It keeps the temperature 2h and carries out vacuum heating-press sintering, obtain block materials after furnace cooling；
4th step, the SiC ceramic layer for polishing or cutting away the cladding of block materials side obtained by vacuum heating-press sintering obtain heat
Management SiC/ graphite film laminar composite.
The heat management prepared by the above process SiC/ graphite film laminar composite, by volume fraction, by 30%
SiC ceramic phase and 70% graphite phase composition block structure, wherein SiC ceramic layer is evenly coated at the surface of graphite film, stone
Ink film and SiC ceramic layer are successively alternately distributed in the composite and perfect orientations are presented.
Embodiment 4:
The first step, the graphite film preparation of surface coated Si/C ceramic layer:
It 1) is 1:5 by Si powder and graphite film molar ratio, taking partial size is 5 microns of Si powder；
2) it is that 1:1 takes NaCl and NaF by NaCl and NaF molar ratio, pours into mortar and grind and be uniformly mixed, obtain salt-mixture
Powder；
3) it is 1:5 with the mass ratio for mixing salt fines by Si powder, Si powder and mixing salt fines is poured into mortar and grind and mix
Uniformly, coating powder is obtained；
4) take graphite film and coating powder with a thickness of 25 microns according to the suitable of " coating powder-graphite film-coating powder ... "
Sequence is successively alternately packed into the graphite crucible of inner surface coated Si/C ceramic layer, is covered crucible cover and is placed in heat-treatment furnace；
5) argon gas is passed through after vacuumizing heat-treatment furnace, under conditions of flowing argon gas protection, from room temperature to 1200
DEG C and keep the temperature 4 hours, cool to room temperature with the furnace, with distilled water cook out salt and dry after obtain the graphite film of coated Si/C ceramic layer
(salt is cooked out using distilled water, the graphite film of adjacent layer coated Si/C ceramic layer can be detached from the stone to form single layer coated Si/C ceramic layer
Ink film)；
The graphite film of surface coated Si/C ceramic layer is placed in graphite jig by second step by the way of successively stacking, and
The pre-molding in the case where pressure is 20MPa, obtains preforming sample；
Third step, by preforming sample vacuum degree lower than 1Pa, sintering temperature be 2000 DEG C, sintering pressure 30MPa,
It keeps the temperature 2h and carries out vacuum heating-press sintering, obtain block materials after furnace cooling；
4th step, the SiC ceramic layer for polishing or cutting away the cladding of block materials side obtained by vacuum heating-press sintering obtain heat
Management SiC/ graphite film laminar composite.
The heat management prepared by the above process SiC/ graphite film laminar composite, by volume fraction, by 20%
SiC ceramic phase and 80% graphite phase composition block structure, wherein SiC ceramic layer is evenly coated at the surface of graphite film, stone
Ink film and SiC ceramic layer are successively alternately distributed in the composite and perfect orientations are presented.
Embodiment 5:
The first step, the graphite film preparation of surface coated Si/C ceramic layer:
It 1) is 1:10 by Si powder and graphite film molar ratio, taking partial size is 5 microns of Si powder；
2) it is that 1:1 takes NaCl and NaF by NaCl and NaF molar ratio, pours into mortar and grind and be uniformly mixed, obtain salt-mixture
Powder；
3) it is 1:5 with the mass ratio for mixing salt fines by Si powder, Si powder and mixing salt fines is poured into mortar and grind and mix
Uniformly, coating powder is obtained；
4) take graphite film and coating powder with a thickness of 70 microns according to the suitable of " coating powder-graphite film-coating powder ... "
Sequence is successively alternately packed into the graphite crucible of inner surface coated Si/C ceramic layer, is covered crucible cover and is placed in heat-treatment furnace；
5) argon gas is passed through after vacuumizing heat-treatment furnace, under conditions of flowing argon gas protection, from room temperature to 1200
DEG C and keep the temperature 4 hours, cool to room temperature with the furnace, with distilled water cook out salt and dry after obtain the graphite film of coated Si/C ceramic layer
(salt is cooked out using distilled water, the graphite film of adjacent layer coated Si/C ceramic layer can be detached from the stone to form single layer coated Si/C ceramic layer
Ink film)；
The graphite film of surface coated Si/C ceramic layer is placed in graphite jig by second step by the way of successively stacking, and
The pre-molding in the case where pressure is 20MPa, obtains preforming sample；
Third step, by preforming sample vacuum degree lower than 1Pa, sintering temperature be 1800 DEG C, sintering pressure 40MPa,
It keeps the temperature 2h and carries out vacuum heating-press sintering, obtain block materials after furnace cooling；
4th step, the SiC ceramic layer for polishing or cutting away the cladding of block materials side obtained by vacuum heating-press sintering obtain heat
Management SiC/ graphite film laminar composite.
The heat management prepared by the above process SiC/ graphite film laminar composite, by volume fraction, by 10%
SiC ceramic phase and 90% graphite phase composition block structure, wherein SiC ceramic layer is evenly coated at the surface of graphite film, stone
Ink film and SiC ceramic layer are successively alternately distributed in the composite and perfect orientations are presented.
Claims (6)
1. a kind of heat management SiC/ graphite film laminar composite, it is characterised in that: volume fraction is pressed, by 10~50%
SiC ceramic phase and 50~90% graphite phase composition block structure, wherein SiC ceramic layer is evenly coated at the table of graphite film
Face, graphite film and SiC ceramic layer are successively alternately distributed in the composite and perfect orientations are presented.
2. a kind of preparation method of heat management as described in claim 1 SiC/ graphite film laminar composite, feature exist
In including the following steps:
The first step coats SiC ceramic layer in graphite film surface by molten-salt growth method, obtains the graphite film of surface coated Si/C ceramic layer；
The graphite film of surface coated Si/C ceramic layer is placed in graphite jig by the way of successively stacking, and pressed by second step
Power is pre-molding under 20MPa, obtains preforming sample；
Third step, by preforming sample vacuum degree lower than 1Pa, sintering temperature be 1800~2000 DEG C, sintering pressure be 30~
50MPa, heat preservation 2h carry out vacuum heating-press sintering, obtain block materials after furnace cooling；
The SiC ceramic layer of 4th step, removal vacuum heating-press sintering gained block materials side cladding obtains heat management SiC/ stone
Ink film laminar composite.
3. the heat management as claimed in claim 2 preparation method of SiC/ graphite film laminar composite, which is characterized in that institute
State the first step molten-salt growth method coating SiC ceramic layer the following steps are included:
1) it is 1:10~1:2 by Si powder and graphite film molar ratio, takes Si powder；
2) it is that 1:1 takes NaCl and NaF by NaCl and NaF molar ratio, pours into mortar and grind and be uniformly mixed, obtain mixing salt fines；
3) it is 1:5 with the mass ratio for mixing salt fines by Si powder, Si powder and mixing salt fines is poured into mortar and grind and be uniformly mixed,
Obtain coating powder；
4) graphite film and coating powder are successively alternately packed into graphite according to the sequence of " coating powder-graphite film-coating powder ... "
In crucible, covers crucible cover and be placed in heat-treatment furnace；
5) argon gas is passed through after vacuumizing heat-treatment furnace, under conditions of flowing argon gas protection, simultaneously from room temperature to 1200 DEG C
Heat preservation 4 hours, cools to room temperature with the furnace, obtains the graphite film of coated Si/C ceramic layer after cooking out salt and drying with distilled water.
4. the heat management as claimed in claim 3 preparation method of SiC/ graphite film laminar composite, it is characterised in that: institute
State graphite film with a thickness of 12~70 microns.
5. the heat management as claimed in claim 3 preparation method of SiC/ graphite film laminar composite, it is characterised in that: institute
The partial size for stating Si powder is 5 microns.
6. the heat management as claimed in claim 3 preparation method of SiC/ graphite film laminar composite, it is characterised in that: institute
State the graphite crucible that graphite crucible is inner surface coated Si/C ceramic layer.
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| CN110369690A (en) * | 2019-08-19 | 2019-10-25 | 西安航空学院 | A kind of graphite film block composite material and preparation method thereof of Al and Ti hybrid buildup |
| CN112125686A (en) * | 2020-09-30 | 2020-12-25 | 郑州大学 | Method for preparing silicon carbide coated graphite by molten salt isolation |
| CN112919912A (en) * | 2021-04-23 | 2021-06-08 | 西安航空学院 | SiC/TiC layered composite material and preparation method thereof |
| CN113511895A (en) * | 2021-04-23 | 2021-10-19 | 西安航空学院 | TiC/graphite film layered composite material and preparation method thereof |
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