CN101545057A - Method for preparing diamond/Cu composite material with high heat conductivity - Google Patents
Method for preparing diamond/Cu composite material with high heat conductivity Download PDFInfo
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- CN101545057A CN101545057A CN200910084424A CN200910084424A CN101545057A CN 101545057 A CN101545057 A CN 101545057A CN 200910084424 A CN200910084424 A CN 200910084424A CN 200910084424 A CN200910084424 A CN 200910084424A CN 101545057 A CN101545057 A CN 101545057A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 57
- 239000010432 diamond Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 37
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- 238000001764 infiltration Methods 0.000 claims abstract description 13
- 230000008595 infiltration Effects 0.000 claims abstract description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 7
- 238000004663 powder metallurgy Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000005087 graphitization Methods 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 35
- 239000000463 material Substances 0.000 description 7
- 238000005245 sintering Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
The invention belongs to the field of research of metal-based composite materials, and relates to a method for preparing a diamond/Cu composite material with high heat conductivity. The method is characterized in that: before the composite material is prepared, a Cr-B composite layer of 0.1 to 5mu m is plated on the surface of diamond powder by adopting a magnetron sputtering method, the thickness of the Cr-B composite layer plated on the surface of the diamond is 0.1 to 5mu m, the ratio of the Cr to B is 30-70:70-30, the granularity of the diamond powder is 10 to 150mu m, and the volume ratio of the diamond to Cu is 55-75:45-25. The heat conductivity of diamond/Cu is improved by compounding with Cu through powder metallurgy, heat pressing or infiltration technology; and by establishing a strong chemical bond interface transition layer consisting of diamond, (Cr-B) C and matrix Cu between the diamond and Cu, the heat conductivity of the composite material is improved to more than 500 W/m.K from the prior about 170 W/m.K. The method not only can effectively improve the heat conductivity of the diamond/Cu composite material, but also can prevent high-temperature graphitization of the diamond powder.
Description
Technical field
The invention belongs to field of research of metal, relate to a kind of method for preparing high heat-conductive diamond/Cu matrix material.
Background technology
Along with the high speed development of information technology, the chip integration in the electronic device part is more and more higher, and power is increasing, and is also more and more higher to the heat radiation requirement of packaged material.Simultaneously, the packaged material thermal expansivity also should keep coupling with ceramic substrate and chip, because it is too big that the thermal expansivity of packaged material and ceramic substrate and chip differs, just be easy to cause bursting or the cracking of some solder joint, weld seam of chip and ceramic substrate, thereby cause electron device to lose efficacy.Therefore, thermal conductivity (TC) and thermal expansivity (CTE) are the two big fundamentals that development hyundai electronics packaged material institute must consideration.Traditional metallic substance is difficult to take into account simultaneously above-mentioned various performance demands, and metal-base composites (MMC) can metallic matrix is good heat conductivility and the low-expansion characteristic of stupalith combine, the matrix material that can obtain not only to have thermal conductive resin but also can be in quite wide scope be complementary with the thermal expansivity of multiple differing materials has become the direction of high performance electronic packaging material development.
The thermal conductivity of commonly used wild phase W, Mo and SiC is respectively 168,140 and 65～200Wm-1K-1, and matrix phase Al and Cu thermal conductivity are respectively 221 and 398Wm-1K-1.Diamond has thermal conductivity the highest in all substances (700～2000Wm-1K-1), adopt 60vol.% above diamond particles and copper compound, the thermal conductivity of matrix material is expected to surpass 800Wm-1K-more than 1, in addition, development along with the artificially synthesizing diamond technology, the price of diamond powder significantly reduces (＜2000 yuan/kilogram), the price of unit volume near in addition be lower than refractory metals such as W, Mo.Therefore, diamond-carbon/carbon-copper composite material has become the primary study object of third generation high performance electronic packaging material behind W-Cu first-generation packaged material, SiCp/Al s-generation packaged material.
Yet existing experimental result shows, adopts methods such as powder metallurgy or infiltration directly 60vol% diamond, the pure Cu of 40vol% to be carried out compound tense, and the thermal conductivity of matrix material only is about 170W/mK, well below theoretical value.This mainly be since the thermal conductivity of matrix material except depending on matrix and strengthen the thermal conductivity of body, matrix and the interface bonding state that strengthens body also have very important influence for the heat conduction behavior of matrix material.Because the two is incompatible, also nonwetting for diamond and Cu, its interface junction is combined into weak mechanical-physical combination, makes the thermal resistance increasing that heat transmits between diamond and Cu, thereby has a strong impact on the heat conductivility of matrix material.Therefore, for the thermal characteristics of giving full play to the diamond excellence, the matrix material of the high thermal conductance of preparation, the interface modification of diamond and Cu is the key scientific problems that must solve.
Summary of the invention
The present invention seeks to solve the interface modification problem of diamond and Cu, give full play to the thermal characteristics of diamond excellence, the matrix material of the high thermal conductance of preparation.
A kind of method for preparing high heat-conductive diamond/Cu matrix material, it is characterized in that earlier behind the Cr-B composite bed of the about 0.1-5 μ of bortz powder surface plated thickness m, and then carry out the heat conductivility that composite methods improves diamond/Cu matrix material by SPS (discharge plasma sintering) powder metallurgy, hot pressing or infiltration process and Cu, concrete technology is:
The method that at first adopts magnetron sputtering is the Cr-B composite bed of the diamond powder coating surface 0.1-5 μ m of 10-150 μ m in granularity, wherein Cr:B=30-70:70-30 (mass ratio), and then employing SPS powder metallurgical technique, hot pressing or infiltration process and Cu carry out compound.Adopt the SPS powder metallurgical technique that diamond powder and the Cu of plating Cr-B are carried out compound tense, selected Cu powder size is 30-120 μ m, and temperature is 850-1070 ℃, and pressure is 30-50MPa; Adopt infiltration process that diamond powder and the Cu of plating Cr-B are carried out compound tense, temperature is 900-1100 ℃, and infiltration pressure is 1-3MPa; Adopt heat pressing process that diamond powder and the Cu of plating Cr-B are carried out compound tense, temperature is 800-1000 ℃, and infiltration pressure is 30-70MPa, and atmosphere is argon gas atmosphere or vacuum
The present invention is by before the preparation matrix material, adopt the method for magnetron sputtering earlier behind the plating 0.1-5 μ mCr-B composite bed of bortz powder surface, adopt powder metallurgy, hot pressing or infiltration process and Cu to carry out the heat conductivility that composite methods improves diamond/Cu again, by after setting up by the strong chemical bond interface transition layer that diamond+(Cr-B) C+ matrix Cu forms between diamond and the Cu, the thermal conductivity of matrix material is brought up to more than the 500W/mK about by original 170W/mK.This method not only can improve the thermal conductivity of diamond/Cu matrix material effectively, and can prevent the high temperature graphitization of diamond powder.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
Embodiment 1: adopting the method for magnetron sputtering is Cr-B (the about 40:60 of the mass ratio) composite bed of 4 μ m at bortz powder surface plating thickness, and diamond grit is 50 μ m, Cu powder size 50 μ m, and the volume ratio of diamond and Cu powder is 55:45.
In ball mill, mixed 5 hours with the Cu powder according to the diamond powder of the ratio of setting the plating composite bed, the rotating speed of ball mill is 120 rev/mins, after mixing, powder mix is put into plasma agglomeration stove (SPS) carry out sintering, sintering temperature is 850 ℃, sintering pressure is 40MPa, and temperature rise rate is 35 ℃/minute, soaking time 8 minutes.Adopt the diamond/Cu matrix material thermal conductivity of this prepared to reach 500W/mK, density is higher than 99%.
Embodiment 2: adopting the method for magnetron sputtering is Cr-B (the about 50:50 of the mass ratio) composite bed of 2 μ m at bortz powder surface plating thickness, and diamond grit is 80 μ m, Cu powder size 80 μ m, and the volume ratio of diamond and Cu powder is 60:40.
In ball mill, mixed 4 hours with the Cu powder according to the diamond powder of the ratio of setting plating, the rotating speed of ball mill is 120 rev/mins, after mixing, powder mix is put into graphite jig, and also putting into hot pressing furnace together carries out hot pressed sintering, temperature is 900 ℃, sintering pressure is 40MPa, and atmosphere is argon gas atmosphere, soaking time 5 minutes.Adopt the diamond/Cu matrix material thermal conductivity of this prepared to reach 510W/mK, density is higher than 99%.
Embodiment 3: adopting the method for magnetron sputtering is the Cr-B layer of 3 μ m at bortz powder surface plating thickness, and diamond grit is 90 μ m, and the volume ratio of diamond and Cu powder is 65:35.
The diamond powder of plating Cr-B is put in the graphite grinding tool, and then pure Cu ingot is placed on the top of diamond powder, put into the infiltration stove at last more together, temperature rise rate with 40 ℃/min rises to 1000 ℃, apply the pressure of 1MPa then, fused Cu pressed in the hole be seeped between diamond powder go, the dwell time is 6 minutes.Adopt the diamond/Cu matrix material thermal conductivity of this prepared to reach 505W/mK, density is higher than 99%.
Claims (5)
1. one kind prepares high heat-conductive diamond/Cu composite process, it is characterized in that: after adopting the Cr-B composite deposite of method with diamond surface plating 0.1-5 μ m of magnetron sputtering plating, method and Cu by SPS powder metallurgy, hot pressing or infiltration carries out compound again, the interface of diamond-Cu in conjunction with by original mechanical-physical in conjunction with becoming strong Chemical bond, the thermal conductivity of matrix material is brought up to more than the 500W/mK about by original 170W/mK like this.
2. in accordance with the method for claim 1, it is characterized in that: with Cu carry out compound before, the thickness of diamond surface plating Cr-B composite bed is 0.1-5 μ m, the ratio of Cr and B is 30-70:70-30, the granularity of diamond powder is 10-150 μ m, and the volume ratio of diamond and Cu is 55-75:45-25.
3. in accordance with the method for claim 1, it is characterized in that: adopt the SPS powder metallurgical technique that diamond powder and the Cu of plating Cr-B are carried out compound tense, selected Cu powder size is 30-120 μ m, and temperature is 850-1070 ℃, and pressure is 30-50MPa.
4. in accordance with the method for claim 1, it is characterized in that: adopt infiltration process that diamond powder and the Cu of plating Cr-B are carried out compound tense, temperature is 900-1100 ℃, and infiltration pressure is 1-3MPa.
5. in accordance with the method for claim 1, it is characterized in that: adopt heat pressing process that diamond powder and the Cu of plating Cr-B are carried out compound tense, temperature is 800-1000 ℃, and infiltration pressure is 30-70MPa, and atmosphere is argon gas atmosphere or vacuum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200910084424XA CN101545057B (en) | 2009-05-15 | 2009-05-15 | Method for preparing diamond/Cu composite material with high heat conductivity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910084424XA CN101545057B (en) | 2009-05-15 | 2009-05-15 | Method for preparing diamond/Cu composite material with high heat conductivity |
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| CN101545057A true CN101545057A (en) | 2009-09-30 |
| CN101545057B CN101545057B (en) | 2012-02-29 |
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Cited By (20)
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| CN101985702A (en) * | 2010-06-29 | 2011-03-16 | 北京科技大学 | Super-high thermal conductivity and low thermal expansivity diamond composite material and preparation method thereof |
| CN102383014A (en) * | 2011-11-11 | 2012-03-21 | 华中科技大学 | Method for preparing diamond-copper composite material by virtue of metallization of high-temperature blending surface |
| CN102465213A (en) * | 2010-11-02 | 2012-05-23 | 北京有色金属研究总院 | High-thermal-conductivity diamond heat sink material and preparation method thereof |
| CN102586704A (en) * | 2012-03-23 | 2012-07-18 | 北京科技大学 | High thermal conductivity graphite whisker/copper composite and preparation method thereof |
| CN102586641A (en) * | 2012-03-30 | 2012-07-18 | 北京科技大学 | Method for preparing high-heat-conductivity diamond copper-base composite material through super-high-pressure sintering |
| CN104152740A (en) * | 2014-08-12 | 2014-11-19 | 铜陵国鑫光源技术开发有限公司 | LED packaging material containing mica powder and preparing method thereof |
| CN104630527A (en) * | 2014-12-30 | 2015-05-20 | 北京安泰钢研超硬材料制品有限责任公司 | Method for preparing copper-based diamond composite material |
| CN104674053A (en) * | 2015-01-26 | 2015-06-03 | 北京科技大学 | Method for preparing diamond/Cu electronic packaging composite material with high thermal conductivity |
| CN104726735A (en) * | 2013-12-23 | 2015-06-24 | 北京有色金属研究总院 | Composite-structure highly-oriented heat conducting material and preparation method thereof |
| CN105728695A (en) * | 2014-12-09 | 2016-07-06 | 北京有色金属研究总院 | Preparation method of high-orientation heat conduction material of composite structure |
| CN105886849A (en) * | 2016-06-22 | 2016-08-24 | 哈尔滨工业大学 | Preparation method of W-plated diamond/aluminum composite |
| CN105986158A (en) * | 2015-02-12 | 2016-10-05 | 中国科学院宁波材料技术与工程研究所 | High-thermal-conductivity diamond-metal composite material and preparation method thereof |
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| CN106854750A (en) * | 2016-12-06 | 2017-06-16 | 北京安泰钢研超硬材料制品有限责任公司 | A kind of diamond carbon/carbon-copper composite material and preparation method |
| CN107937783A (en) * | 2017-11-17 | 2018-04-20 | 湖南大学 | Increase the method for binding ability between diamond and metallic matrix |
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- 2009-05-15 CN CN200910084424XA patent/CN101545057B/en not_active Expired - Fee Related
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| CN101985702B (en) * | 2010-06-29 | 2013-02-06 | 北京科技大学 | Super-high thermal conductivity and low thermal expansivity diamond composite material and preparation method thereof |
| CN101985702A (en) * | 2010-06-29 | 2011-03-16 | 北京科技大学 | Super-high thermal conductivity and low thermal expansivity diamond composite material and preparation method thereof |
| CN102465213A (en) * | 2010-11-02 | 2012-05-23 | 北京有色金属研究总院 | High-thermal-conductivity diamond heat sink material and preparation method thereof |
| CN102383014A (en) * | 2011-11-11 | 2012-03-21 | 华中科技大学 | Method for preparing diamond-copper composite material by virtue of metallization of high-temperature blending surface |
| CN102586704A (en) * | 2012-03-23 | 2012-07-18 | 北京科技大学 | High thermal conductivity graphite whisker/copper composite and preparation method thereof |
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| CN104726735A (en) * | 2013-12-23 | 2015-06-24 | 北京有色金属研究总院 | Composite-structure highly-oriented heat conducting material and preparation method thereof |
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| CN111590080A (en) * | 2020-05-21 | 2020-08-28 | 南京航空航天大学 | Method for rapidly preparing titanium-plated diamond copper composite material by SPS |
| CN111500892A (en) * | 2020-06-18 | 2020-08-07 | 哈尔滨锦威科技有限公司 | Preparation method of large-size flaky diamond/copper composite material with ultrahigh thermal conductivity |
| CN111500892B (en) * | 2020-06-18 | 2021-08-31 | 哈尔滨锦威科技有限公司 | Preparation method of large-size flaky diamond/copper composite material with ultrahigh thermal conductivity |
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