CN107116210A - Cu-base composites fin of the oriented laminated arrangement of graphite flake and preparation method thereof - Google Patents

Cu-base composites fin of the oriented laminated arrangement of graphite flake and preparation method thereof Download PDF

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Publication number
CN107116210A
CN107116210A CN201610955113.6A CN201610955113A CN107116210A CN 107116210 A CN107116210 A CN 107116210A CN 201610955113 A CN201610955113 A CN 201610955113A CN 107116210 A CN107116210 A CN 107116210A
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graphite flake
preparation
fin
graphite
oriented laminated
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CN107116210B (en
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郝俊杰
崔倩月
吴成义
郭志猛
王阳
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • 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
    • 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
    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • 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
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides one kind using copper as matrix, using the graphite flake that aligns as composite heat dissipation material of enhanced thermal conduction phase and preparation method thereof, the encapsulating material field applied to integrated electronics.Matrices of composite material selects pure copper powder, and enhanced thermal conduction is mutually from the larger artificial synthesized graphite flake of lateral dimension.Material powder need to be well mixed by batch mixer, add the binding agent being configured to by polyvinyl butyral resin and ethanol solution, it is well mixed, by mixed slurry flow casting molding, through drying, cut, after stacking and degumming, the graphite flake layered and parallel Cu-base composites substrate for being arranged in heat dissipation direction distribution of orientations in the base is obtained using Bidirectional hot press sintering, this composite is high relative to vertical graphite flake orientation 48 times in the thermal conductivity parallel to graphite flake orientation, thermal conductivity parallel to graphite flake orientation relative to the pure copper material for being not added with graphite flake improves 1.1 1.5 times, linear expansion coefficient matches with silicon electronic component.

Description

Cu-base composites fin of the oriented laminated arrangement of graphite flake and preparation method thereof
Technical field
The present invention relates to a kind of Cu-base composites of novel graphite layered arrangement and preparation method thereof, there is provided a kind of profit It is raw material with the flake graphite of anisotropic heat conductivity, the system of layer structure heat dissipation element material is prepared with reference to special preparation technique Preparation Method, belongs to miniaturization integrated electronic encapsulating material field.
Technical background
The heat dispersion of surface-mounted integrated circuit is to ensure the important indicator that each quasi-instrument, living electric apparatus electronic equipment are normally run One of, the package substrate being close to outside integrated circuit electronic element is the critical piece of electronic element radiating.Integrated circuit is in fortune Greatly, the reduction of integrated circuit operation efficiency can be caused or even burn the heat produced during work by failing to scatter in time, electric in addition Subcomponent package substrate and electronic component linear expansion coefficient will have matched well, so just can guarantee that integrated circuit is continual and steady Running.
With electronics industry fast development, electronic information technology is to the miniaturization of electronic product, portability, multi-functional, low Cost proposes requirements at the higher level, and this needs more denseization of integrated circuit, and to meet this requirement, electronic package material has crucial work With.In traditional sense, baseplate material is broadly divided into ceramic substrate, metal substrate and organic polymer substrate.Ceramic substrate such as oxygen Change aluminium, beryllium oxide, aluminium nitride etc., its air-tightness is preferable, high mechanical strength, but sintering precision is poor and expensive, is normally applied In special occasions；Organic polymer sill, predominantly thermosetting plastics, its moisture resistance effect are good and anti-corrosion, but its thermal conductivity compared with Low the problem of, is also to be solved；What metal electron package substrate was commonly used includes copper-based, aluminum matrix composite etc., and thermal conductivity is very It is good, and can mutually improve material and the unmatched problem of electronic component linear expansion coefficient by adding enhancing in the base.
Copper in Cu-base composites, on the one hand as heat conduction substrate, on the other hand plays and bonds and fix graphite flake Effect；Graphite flake is set to align in base plane by using new casting molding processes, greatly enhancing graphite flake row The thermal conductivity of column direction, in addition, large area composite can be made, it is easy to processing cutting.
According to the literature search of last decade, in document [1], polymer-based graphite flake is prepared for using the tape casting and is combined Material, but this kind of material is difficult to electric machining cutting, in document [2], in [3], is prepared for using diamond and graphite fibre Cu-base composites, but the orientation thermal conductivity of this kind of composite is poor；In document [4], single hot pressing sintering method is employed Be prepared for copper-base graphite piece composite, but in this kind of composite graphite flake to align rate relatively low, it is difficult to reach that orientation is high Heat conductivility.
The content of the invention
To improve in above-mentioned material performance deficiency, the present invention from copper powder and graphite flake as raw material, relative to macromolecule Based composites have higher thermal conductivity and more preferable electric machining performance, using casting molding processes, can improve determining for graphite flake To arrangement rate, using Bidirectional hot press sintering process, the consistency of composite can be improved, the more preferable material of heat conductivility is obtained.
A kind of preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake, it is characterised in that：With pure Copper powder is as matrix material, and artificial synthesized graphite flake is as enhanced thermal conduction phase, after former material feed powder is well mixed, through being cast into Type, is dried, and is cut, stacking, degumming, and the oriented laminated arrangement of flake graphite has been made in Bidirectional hot press sintering, in leading for layer structure Thermal anisotropy's composite.
The matrix material further used is tough cathode powder, 5-10 μm of particle diameter, artificial stone ink sheet piece footpath 1-2mm, thick Spend for 20-50 μm, copper powder volume fraction is 30~70% in mixed powder, graphite flake volume fraction is 30~70%；Binding agent is adopted The mixed liquor prepared with polyvinyl butyral resin and ethanol, wherein polyvinyl butyral resin mass fraction are 10%, ethanol quality Fraction is 90%；Raw material powder after dry-mixed 9h, adds binding agent and is sufficiently stirred for as uniform sizing material in V-type batch mixer.
Further flow casting molding step is：Slurry is poured into casting device, regulation blade height is 0.2-0.7mm, stream The operating rate for prolonging band is 4.0-4.4m/min, ensures that the graphite particle of sheet can be on molded membrane plane sufficiently with this Drawout.
Step, which is further dried, is：Molded casting films are placed in drying box, drying temperature is set to 25-45 DEG C, Cut and stacking according to actual requirement after being completely dried.
Further scouring processes are carried out in purity nitrogen atmosphere, to prevent composite material film from aoxidizing, heating rate for 5 DEG C/ Min, to 400 DEG C of insulation 2h.
It further will cut to be placed in graphite jig with the product after stacking and carry out hot pressed sintering, hot pressed sintering is in pure nitrogen gas Carried out in atmosphere, heating rate is 5 DEG C/min, to 950-1000 DEG C of insulation 5-10min, Bidirectional hot press pressure is 5-15MPa.
The composite of the oriented laminated arrangement of further graphite flake need to be oriented the inspection of arrangement rate with SEM Survey, i.e., on defined direction arranged in parallel, transversely arranged rate of the graphite flake arrangement anglec of rotation less than 5 ° is more than 80%, stone Ink sheet percentage of damage is less than 5%.
Obtained sample is oriented the analysis of arrangement rate with SEM, aligns rate degree of orientation κ and broken Broken rate η demarcation, wherein, κ definition is：
κ=Z/Z0× 100% (1)
In formula, Z0For graphite flake sum in visual field, it is that (orientation angular displacement is for graphite flake number arranged in parallel in visual field that Z, which is, ± 3 ° of persons).η is defined as：
η=M/M0In × 100% (2) formula, M0For graphite flake sum in visual field, M is graphite flake broken in visual field Number.
The degree of orientation that the graphite flake of composite is aligned is more than 80%, and graphite flake percentage of damage is less than 5% composite wood Expect for certified products.Specific preparation technology flow such as Fig. 1, flow casting molding process is shown in Fig. 2.
Advantages of the present invention
1. the Cu-base composites fin of the anisotropic heat conductivity of the novel laminate structures prepared, thermal conductivity is compared with fine copper material Expect that fin improves 1.1-1.5 times, density reduces 25%-55% compared with pure copper material, have great for the lightweight research of material Meaning.
2. the casting molding processes used make graphite flake aligning property in Copper substrate more preferably, be combined to further improving The anisotropic thermal conductivity of material can be of great importance.
3. the technique can obtain large area composite fin in a preparation process, operating method is simple and easy to apply, It is easy to electric machining cutting, a large amount of fast industrialization productions can be carried out.
Brief description of the drawings
Fig. 1 is composite fin preparation technology schematic flow sheet,
Fig. 2 is casting molding processes schematic diagram,
1. scraper；2. binding agent；3. graphite flake；4 copper powders
Embodiment
Embodiment 1
A kind of high heat conduction electronic packaging composite material substrate, raw material mixed powder is by 5-10 μm of cathode copper powder and piece footpath 1- The volume fraction of 2mm, the artificial synthesized graphite flake composition of 20-50 μm of thickness, fine copper powder and graphite flake is respectively 60% He 40%.
By above-mentioned each component dispensing in proportion, in miniature batch mixer mixing 9h turns into uniformed powder, adds polyvinyl alcohol Butyral is 1 with ethanol mass ratio:9 binding agent, is sufficiently stirred for as uniform sizing material, and slurry is poured into casting device through curtain coating Film forming, at 400 DEG C after degumming 2h, 1000 DEG C of Bidirectional-pressure sintering, insulation are warming up to during hot pressed sintering with 5 DEG C/min 10min, moulding pressure is 10MPa, obtains copper-based electronic packaging composite material.Reached along the thermal conductivity factor parallel to graphite flake direction 500w/m·k。
Embodiment 2
A kind of high heat conduction electronic packaging composite material substrate, raw material mixed powder is by 5-10 μm of cathode copper powder and piece footpath 1- The volume fraction of 2mm, the artificial synthesized graphite flake composition of 20-50 μm of thickness, fine copper powder and graphite flake is respectively 50% He 50%.
By above-mentioned each component dispensing in proportion, in miniature batch mixer mixing 9h turns into uniformed powder, adds polyvinyl alcohol Butyral is 1 with ethanol mass ratio:9 binding agent, is sufficiently stirred for as uniform sizing material, and slurry is poured into casting device through curtain coating Film forming, at 400 DEG C after degumming 2h, 1000 DEG C of Bidirectional-pressure sintering, insulation are warming up to during hot pressed sintering with 5 DEG C/min 10min, moulding pressure is 15MPa, obtains copper-based electronic packaging composite material.Reached along the thermal conductivity factor parallel to graphite flake direction 550w/m·k。
Bibliography
[1]ZHOU S,Yuan Z H U,DU H,et al.Preparation of oriented graphite/ polymer composite sheets with high thermal conductivities by tape casting [J].New Carbon Materials,2012,27(4):241-249. [2]Guillemet T,Geffroy P M,Heintz J M,et al.An innovative process to fabricate copper/diamond composite films for thermal management applications [J].Composites Part A:Applied Science and Manufacturing,2012,43(10):1746- 1753.
[3]Geffroy P M,Chartier T,Silvain J F.Preparation by tape casting and hot pressing of copper carbon composites films[J].Journal of the European Ceramic Society,2007,27(1):291-299.
[4]Liu Q,He X B,Ren S B,et al.Thermophysical properties and microstructure of graphite flake/copper composites processed by electroless copper coating[J].Journal of Alloys and Compounds,2014,587:255-259.

Claims (7)

1. a kind of preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake, it is characterised in that：Use fine copper Powder is as matrix material, and artificial synthesized graphite flake is as enhanced thermal conduction phase, after former material feed powder is well mixed, through flow casting molding, Dry, cut, stacking, degumming, the oriented laminated arrangement of flake graphite has been made in Bidirectional hot press sintering, each in the heat conduction of layer structure Anisotropy composite.
2. the preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake as claimed in claim 1, its feature It is：The matrix material used is tough cathode powder, 5-10 μm of particle diameter, artificial stone ink sheet piece footpath 1-2mm, and thickness is 20-50 μm, Copper powder volume fraction is 30~70% in mixed powder, and graphite flake volume fraction is 30~70%；Binding agent is contracted using polyvinyl alcohol The mixed liquor that butyraldehyde and ethanol are prepared, wherein polyvinyl butyral resin mass fraction are 10%, and ethanol mass fraction is 90%；It is former Material powder after dry-mixed 9h, adds binding agent and is sufficiently stirred for as uniform sizing material in V-type batch mixer.
3. the preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake as claimed in claim 1, its feature It is that flow casting molding step is：Slurry is poured into casting device, regulation blade height is 0.2-0.7mm, the operation of casting belt Speed is 4.0-4.4m/min, with this ensure sheet graphite particle can on molded membrane plane sufficient drawout.
4. the preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake as claimed in claim 1, its feature It is that drying steps are：Molded casting films are placed in drying box, drying temperature is set to 25-45 DEG C, after being completely dried Cut according to actual requirement and stacking.
5. the preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake as claimed in claim 1, its feature It is that scouring processes are carried out in purity nitrogen atmosphere, to prevent composite material film from aoxidizing, heating rate is 5 DEG C/min, to 400 DEG C of guarantors Warm 2h.
6. the preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake as claimed in claim 1, its feature It is to cut to be placed in graphite jig with the product after stacking to carry out hot pressed sintering, hot pressed sintering enters in pure nitrogen gas atmosphere OK, heating rate is 5 DEG C/min, and to 950 DEG C of -1000 DEG C of insulation 5-10min, Bidirectional hot press pressure is 5-15MPa.
7. the preparation method of the Cu-base composites fin of the oriented laminated arrangement of graphite flake as claimed in claim 1, its feature The detection of arrangement rate need to be oriented with SEM by being the composite of the oriented laminated arrangement of graphite flake, i.e., in regulation Direction arranged in parallel on, the graphite flake arrangement anglec of rotation less than 5 ° of transversely arranged rate more than 80%, graphite flake percentage of damage Less than 5%.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107791616A (en) * 2017-10-26 2018-03-13 北京科技大学 A kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film
CN108396169A (en) * 2018-01-26 2018-08-14 中国科学院兰州化学物理研究所 A kind of copper-base graphite composite seal
CN109175356A (en) * 2018-10-16 2019-01-11 中国科学院兰州化学物理研究所 A kind of graphite-copper laminar composite and preparation method thereof
CN113770347A (en) * 2021-08-24 2021-12-10 西安交通大学 Method for regulating and controlling friction coefficient of copper-graphite composite material through graphite flake orientation

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WO2003095688A2 (en) * 2002-05-09 2003-11-20 Harmonics, Inc Tapecast electro-conductive cermets for high temperature resistive heating systems
CN1944698A (en) * 2006-10-24 2007-04-11 北京科技大学 Super high heat conduction, low heat expansion coefficient composite material and its preparing method
CN103317140A (en) * 2013-06-25 2013-09-25 武汉理工大学 Method for manufacturing gradient composite of W-Cu system by aid of tape casting process
CN104891996A (en) * 2015-05-18 2015-09-09 山东理工大学 Preparation process for highly oriented graphite composite material
CN105218103A (en) * 2015-10-26 2016-01-06 哈尔滨工业大学 The preparation method of a kind of Graphene/ceramic laminar material
CN105483423A (en) * 2016-01-14 2016-04-13 北京科技大学 Manufacturing method of copper/diamond composite material with high thermal conductivity
CN105728719A (en) * 2016-03-18 2016-07-06 北京科技大学 Method for manufacturing high-thermal-conductivity copper-based electronic packaging substrate
CN105803242A (en) * 2016-03-21 2016-07-27 中南大学 Composite enhanced through coupling of flaky and linear thermal conductive materials and preparation method

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EP0767154A1 (en) * 1995-10-03 1997-04-09 SKF Nova AB Method for the production of solid shaped bodies
WO2003095688A2 (en) * 2002-05-09 2003-11-20 Harmonics, Inc Tapecast electro-conductive cermets for high temperature resistive heating systems
CN1944698A (en) * 2006-10-24 2007-04-11 北京科技大学 Super high heat conduction, low heat expansion coefficient composite material and its preparing method
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Publication number Priority date Publication date Assignee Title
CN107791616A (en) * 2017-10-26 2018-03-13 北京科技大学 A kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film
CN107791616B (en) * 2017-10-26 2019-09-10 北京科技大学 A kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film
CN108396169A (en) * 2018-01-26 2018-08-14 中国科学院兰州化学物理研究所 A kind of copper-base graphite composite seal
CN109175356A (en) * 2018-10-16 2019-01-11 中国科学院兰州化学物理研究所 A kind of graphite-copper laminar composite and preparation method thereof
CN113770347A (en) * 2021-08-24 2021-12-10 西安交通大学 Method for regulating and controlling friction coefficient of copper-graphite composite material through graphite flake orientation

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