CN103589894B - Method for preparing orientation-reinforced Cu composite material for two-dimensional heat dissipation - Google Patents
Method for preparing orientation-reinforced Cu composite material for two-dimensional heat dissipation Download PDFInfo
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- CN103589894B CN103589894B CN201310590655.4A CN201310590655A CN103589894B CN 103589894 B CN103589894 B CN 103589894B CN 201310590655 A CN201310590655 A CN 201310590655A CN 103589894 B CN103589894 B CN 103589894B
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Abstract
The invention discloses a method for preparing a flaky graphite and diamond particle orientation-reinforced Cu-based composite material for two-dimensional heat dissipation, and belongs to the field of metal-based composite materials. Flaky graphite is excellent in two-dimensional heat-dissipation performance; diamond particles are high in heat conductivity. The method comprises the following steps: mixing the flaky graphite with the diamond particles, orientating and arranging graphite flakes on an X-Y plane, and performing infiltrating and compounding on the graphite flakes and copper to prepare the (flaky graphite + diamond particle)/Cu composite material with high heat conductivity on the X-Y plane. According to the method, a certain amount of Cr powder with a certain particle size is also added in the mixing process of the flaky graphite and the diamond particles, can be quenched in a Cu solution in the later Cu infiltrating process, is enriched on the surfaces of the diamond particles and the graphite flakes and produces an interface reaction together with the diamond particles and the graphite flakes, so that mechanical bonding of an interface turns into chemical metallurgical bonding and the heat resistance of the interface is greatly reduced. The composite material prepared by using the method has heat conductivity which exceeds 650 W/mK on the X-Y plane and 200 W/mK on a Z plane.
Description
Technical field
The invention belongs to field of research of metal, invent the method that one prepares two-dimentional heat transmission (flaky graphite+diamond particles) orientational strengthening Cu matrix material.
Background technology
Along with semi-conductor becomes more meticulous the development of technology, the heat that radiator structure is no longer confined to semi-conductor is released is transmitted, in the other end heat release along a direction.Pay attention to widely for the research of the heat radiation structures such as heat two-dimensional diffusion, increase heat release area be have also been obtained.This structure have radiating efficiency high, take up room little, along both direction uniform heat conduction, eliminate the feature such as " focus " region.Do not wish to occur that the notebook computer of localized hyperthermia, high-power LED illumination, flat-panel monitor and other portable communication apparatus are particularly urgent to the demand possessing this structure heat sink material.
Graphite-based reinforcement comprises flaky graphite, graphite fibre etc. and has the excellent performance such as high heat conduction, low density, Cutting free processing, becomes the reinforcement material that Electronic Packaging heat sink material of new generation is desirable.But, compare to the graphite fibre of easily reuniting, having good auto-orientation flaky graphite arranged in parallel and easily disperse is first-selection.When adopting press forming, in reinforcement forming process, the normal vector (Z-direction) in flakey face will keep basically identical with pressure direction, the flakey face (X-Y plane) of powder will perpendicular to the parallel packing arrangement of pressure direction, the orientation of crystalline flake graphite and the high thermal conductivity of X-Y plane can be made full use of like this, realize the transmission at two dimensional surface of heat.Meanwhile, the copper as the widely used a kind of heat sink material in Electronic Packaging field has the features such as thermal conductivity is high, low price, becomes the only choosing of Novel heat dissipation material matrix metal.Therefore, flaky graphite powder and the copper with auto-orientation arrangement are compounded to form matrix material, the heat dispersion of the two excellence can be given full play to, its two-dimentional thermal conductivity theoretical value more than 600W/mk, close to the thermal conductivity of diamond/Cu.Significantly, flaky graphite is easily processed, and gained composite processing performance is good, can fully meet through engineering approaches application requiring.Therefore, flaky graphite powder/carbon/carbon-copper composite material is high-performance electronic equipment one of the most promising heat sink material of new generation.
Summary of the invention
The present invention seeks to for radiating structure semiconducter device the demand with high thermal conductivity, two-dimentional radiator structure; make full use of two-dimentional heat sinking function that flaky graphite has and the high thermal conductivity of diamond particles; select copper as matrix metal; the excellent properties of three is organically combined, prepares flaky graphite and diamond particles hybrid orientation enhancing Cu-base composites.
A kind of method preparing orientation-reinforcCu Cu composite material for two-dimensional heat dissipation, concrete content is: first a certain proportion of flaky graphite, diamond particles, Cr powder are mixed, and then carry out mixing with a certain proportion of solid paraffin, melting temperature 60 ~ 80 DEG C.The quality of flaky graphite and the quality of diamond particles and Cr powder quality ratio control are at (60-65) %:(30-35) %:(5-10) within the scope of %.Flaky graphite median size be 200 ~ 300 μm, average aspect ratio 50 ~ 100, mean thickness 3 ~ 5 μm; The particle diameter of diamond particles is 10-15 μm; Cr powder size is 15-20 μm.The main purpose of adding Cr powder can be dissolved into Cu matrix in later stage infiltration process, and can be enriched in diamond particles surface and with diamond particles and graphite flake generation surface reaction, make interface become enhanced primary treatment from original mechanical bond, thus greatly reduce interface resistance.
Obtain uniform compound through fully mixing, be then broken into the particle of median size 2-3mm, suppress.Compacting adopts the method for unidirectional vertical compacting, first a certain amount of particle is put in compacting tool set, mould is through preheating, temperature is the softening temperature 68 ~ 80 DEG C of paraffin, feeding is made to have good mobility at this temperature, ensure that flaky graphite can fully deflect under pressure, make whole or near whole flakey face arranged in parallel along XY face, and perpendicular to compression aspect (Z-direction).Pressing pressure is 10 ~ 20MPa.
After shaping, then agent is formed to the base substrate be shaped through orientation remove and presintering.Remove binder and presintering is carried out in nitrogen atmosphere, concrete sintering schedule: from room temperature to the temperature rise rate of 400 DEG C be 4-5 DEG C/min, temperature is incubated 30min after rising to 400 DEG C, then rise to 800-850 DEG C (pre-sintering temperature) with 10-15 DEG C/min of speed, the soaking time of pre-sintered state is 30-45 minute.Orientation pressing blank removing and presintering through binder, finally obtains porous (flaky graphite+diamond) preformed blank with some strength.
Porous body is placed in infiltration mould, carries out preheating, adopt pressurization infiltration process that the Cu of molten state and base substrate are carried out compound, obtain the Cu based composites of (flaky graphite+diamond) orientational strengthening.The preheating temperature of base substrate controls 800-900 DEG C of scope, and the teeming temperature of molten state Cu is 1200-1250 DEG C, and infiltration pressure is 20-25MPa, and the dwell time is 20-30 minute.
The invention has the advantages that, in flaky graphite, be mixed into diamond particles can effectively avoid flaky graphite to be superimposed, hinder the infiltration of later stage copper, diamond particles has high thermal conductivity simultaneously, effectively can improve the bulk thermal conductivity of final prepared composite wood.In addition, Cr powder is added in base substrate, can admittedly be fused in Cu liquid in the infiltration process of later stage Cu, Sync enrichment also reacts with it on the surface of diamond particles and flaky graphite, interface is made to become enhanced primary treatment from original mechanical bond, therefore greatly can reduce the interface resistance of matrix material, improve the thermal conductivity of matrix material.Because Cr powder is directly mixed in base substrate, avoid the complicated plating technic such as salt bath, vacuum vapor deposition, therefore greatly reduce the preparation cost of this material.Adopt infiltration process that porous body and Cu are carried out compound, effectively can overcome existing employing powder metallurgy pressing sintering and be difficult to fully dense processing disadvantages.
Accompanying drawing illustrates:
Fig. 1 is process flow sheet of the present invention.
Embodiment:
Embodiment 1: the 70vol%(flaky graphite+diamond of preparation 3cm × 2cm × 0.5cm specification) orientational strengthening Cu matrix material
(1) take 2.8 grams of flaky graphites respectively, 1.4 grams of diamond powders, 0.3 gram of Cr powder mix, wherein the median size of flaky graphite is 200 μm, average aspect ratio 70, mean thickness 4 μm, the mean particle size of diamond powder 10 μm, the mean particle size of Cr powder 15 μm;
(2) mixed powder and 0.8 gram of paraffin are carried out mixing, melting temperature 70 DEG C, mixing evenly after obtain compound, so compound is broken into the particle of 2-3mm;
(3) be encased in by particle in 3cm × 2cm punching block, punching block temperature remains on 70 DEG C, suppresses, pressing pressure 10MPa, and 15 minutes dwell times, particle obtains orientation base substrate through hot pressing orientation;
(4) base substrate is formed in nitrogen atmosphere agent to remove and presintering, heating process is for being 4 DEG C/min from room temperature to 400 DEG C of temperature rise rates, 30 minutes are incubated after temperature rises to 400 DEG C, then 800 DEG C are risen to 10 DEG C/min, be incubated 30 minutes, obtain porous (flaky graphite+diamond) preformed blank with some strength; (5) porous body is inserted in graphite infiltration mould, be preheated to 800 DEG C, then 10 of 1200 DEG C of meltings grams of Cu liquid are cast in mould, pressurize, pressure is 20MPa, carry out decrease temperature and pressure after 20 minutes heat-insulation pressure keeping time, whole operation is carried out under vacuum conditions, finally obtains 70vol%(flaky graphite+diamond) orientational strengthening Cu matrix material.Carry out thermal conductivity test to it, X-Y plane thermal conductivity is that 655W/mK, Z plane thermal conductivity is more than 205W/mK.
Embodiment 2: the 75vol%(flaky graphite+diamond of preparation 5cm × 2cm × 0.8cm specification) orientational strengthening Cu matrix material
(1) take 9 grams of flaky graphites respectively, 4.5 grams of diamond powders, 1.2 grams of Cr powder mix, wherein the median size of flaky graphite is 250 μm, average aspect ratio 100, mean thickness 5 μm, the mean particle size of diamond powder 15 μm, the mean particle size of Cr powder 20 μm;
(2) mixed powder and 1.8 grams of paraffin are carried out mixing, melting temperature 80 DEG C, mixing evenly after obtain compound, so compound is broken into the particle of 2-3mm;
(3) be encased in by particle in 5cm × 2cm punching block, punching block temperature remains on 80 DEG C, suppresses, pressing pressure 20MPa, and 15 minutes dwell times, particle obtains orientation base substrate through hot pressing orientation;
(4) base substrate is formed in nitrogen atmosphere agent to remove and presintering, heating process is for being 5 DEG C/min from room temperature to 400 DEG C of temperature rise rates, 30 minutes are incubated after temperature rises to 400 DEG C, then 800 DEG C are risen to 10 DEG C/min, be incubated 30 minutes, obtain porous (flaky graphite+diamond) preformed blank with some strength; (5) porous body is inserted in graphite infiltration mould, be preheated to 900 DEG C, then 20 of 1200 DEG C of meltings grams of Cu liquid are cast in mould, pressurize, pressure is 25MPa, carry out decrease temperature and pressure after 20 minutes heat-insulation pressure keeping time, whole operation is carried out under vacuum conditions, finally obtains 75vol%(flaky graphite+diamond) orientational strengthening Cu matrix material.Carry out thermal conductivity test to it, X-Y plane thermal conductivity is that 690W/mK, Z plane thermal conductivity is more than 212W/mK.
Claims (1)
1. prepare the method for orientation-reinforcCu Cu composite material for two-dimensional heat dissipation for one kind, it is characterized in that: fully mix with the binder with mobility again after the flaky graphite of certain proportion and granularity is mixed with diamond particles, Cr powder, press forming, in pressing process, graphite flake completes orientations, obtain the preformed blank containing binder, then binder is removed, and carry out presintering, obtain nearly full open aperture, the abundant orientations of flaky graphite, there is the preliminary shaping base substrate of some strength; Porous body is placed in infiltration mould, carries out preheating, and then by pressurization infiltration process, the Cu of molten state and base substrate are carried out compound, finally obtain the Cu based composites that flaky graphite+diamond orientations strengthens; Wherein the quality of flaky graphite and the quality of diamond particles and Cr powder quality ratio control are at (60-65) %:(30-35) %:(5-10) within the scope of %, flaky graphite median size be 200 ~ 300 μm, average aspect ratio 50 ~ 100, mean thickness 3 ~ 5 μm; The particle diameter of diamond particles is 10-15 μm; Cr powder size is 15-20 μm; Concrete technology parameter is:
Binder adopts solid paraffin, by mixed powder and solid paraffin by volume 70%:30% carry out mixing, melting temperature 60 ~ 80 DEG C; Through the abundant mixing compound evenly obtained, the particle being then broken into median size 2-3mm loads mould to be suppressed; Compacting adopts the method for unidirectional vertical compacting, and mould is through preheating, and preheating temperature is 68 ~ 80 DEG C, pressing pressure 10 ~ 20MPa, and compound is heat-insulation pressure keeping time 15-20 minute in a mold;
Pressing blank forms removing of agent and presintering in nitrogen atmosphere, and the stage that removes is 4-5 DEG C/min from room temperature to the temperature rise rate of 400 DEG C, and the sintering temperature in pre-burning stage is 800-850 DEG C, and the dwell time is 30-45 minute;
During pressure infiltration copper, the preheating temperature of base substrate controls 800-900 DEG C of scope, and the teeming temperature of molten state Cu is 1200-1250 DEG C, and infiltration pressure is 20-25MPa, and soaking time is 20-30 minute, and whole operation is carried out under vacuum conditions.
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Families Citing this family (9)
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| CN103924119B (en) * | 2014-04-23 | 2016-01-20 | 北京科技大学 | A kind of super-high heat-conductive graphite flakes/carbon/carbon-copper composite material and preparation method thereof |
| CN106553136A (en) * | 2015-09-28 | 2017-04-05 | 河南工业大学 | Infiltration method prepares metal anchoring agent diamond wheel |
| CN105798311B (en) * | 2016-03-21 | 2018-07-10 | 北京科技大学 | A kind of preparation method of high heat conduction ferrous based powder metallurgical brake block for high-speed train |
| CN108517429B (en) * | 2018-04-04 | 2020-07-17 | 太原理工大学 | Ti2Preparation method of AlC reinforced copper-based composite material |
| CN111170317B (en) * | 2018-11-12 | 2022-02-22 | 有研工程技术研究院有限公司 | Preparation method of graphene modified diamond/copper composite material |
| CN109468490A (en) * | 2019-01-07 | 2019-03-15 | 贵溪红石金属有限公司 | A kind of non-conventional copper bar production technology |
| CN110524442B (en) * | 2019-07-31 | 2021-02-02 | 郑州中南杰特超硬材料有限公司 | Porous diamond polycrystalline abrasive and preparation method thereof |
| CN115138851B (en) * | 2021-03-30 | 2024-03-26 | 西安精微超纯材料科技有限公司 | Preparation method of copper-diamond electronic packaging material integrating heat pipe function |
| CN116550975B (en) * | 2023-07-04 | 2023-09-26 | 赣州金顺科技有限公司 | Preparation method of diamond/copper composite material |
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| CN102628149A (en) * | 2012-03-23 | 2012-08-08 | 北京科技大学 | Preparation method of graphite whisker reinforced copper base composite material |
| CN103343274A (en) * | 2013-07-24 | 2013-10-09 | 上海交通大学 | High-thermal-conductivity graphite-aluminium composite material reinforced by diamond particles in hybrid manner and preparation process for same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102628149A (en) * | 2012-03-23 | 2012-08-08 | 北京科技大学 | Preparation method of graphite whisker reinforced copper base composite material |
| CN103343274A (en) * | 2013-07-24 | 2013-10-09 | 上海交通大学 | High-thermal-conductivity graphite-aluminium composite material reinforced by diamond particles in hybrid manner and preparation process for same |
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