CN102732764A - Preparation method for diamond/copper composite material with high heat conductivity and low thermal expansion coefficient - Google Patents
Preparation method for diamond/copper composite material with high heat conductivity and low thermal expansion coefficient Download PDFInfo
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- CN102732764A CN102732764A CN2012102531769A CN201210253176A CN102732764A CN 102732764 A CN102732764 A CN 102732764A CN 2012102531769 A CN2012102531769 A CN 2012102531769A CN 201210253176 A CN201210253176 A CN 201210253176A CN 102732764 A CN102732764 A CN 102732764A
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Abstract
The invention discloses a preparation method for a diamond/copper composite material with high heat conductivity and low heat expansion coefficient, which relates to a preparation method for a diamond/copper composite material, to solve the technical problem of low heat conductivity of the traditional composite material prepared by directly compositing the diamond and pure copper by adopting a powder metallurgy or infiltration method. The preparation method comprises the following steps of: (1) plating copper on the surface of diamond powder by adopting a chemical copper plating method to prepare copper plated diamond powder; (2) mixing the copper plated diamond powder in the step (1) with copper powder by adopting a mechanical powder mixing mode to form mixed powder; and (3) performing cold pressing and molding on the mixed powder prepared in the step (2), and compounding the mixed powder with copper through vacuum hot pressing and sintering to obtain the diamond/copper composite material with high heat conductivity and low heat expansion coefficient. After sintering, the interface bonding of the composite material is better, and the density is higher; and the heat conductivity of the composite material reaches 500W/m.K, and the heat expansion coefficient is reduced to 7.8*10<-6>/K. The preparation method is applied to the field of preparation of diamond/copper composite materials.
Description
Technical field
The invention belongs to field of research of metal, relate to the preparation method of diamond/carbon/carbon-copper composite material.
Background technology
Along with the high speed development of microelectronics, semiconductor integrated circuit package density is increasing, and travelling speed is more and more faster.Yet; High integration and high travelling speed, the heat that makes device send increases sharply, and causes the operating ambient temperature of circuit card to raise; Thereby influence the stability of device; On the other hand, the thermal cycling regular meeting during device work produces bigger stress, and not matching as if thermal expansivity between the material to cause the thermal fatigue failure of microelectronic circuit and device.Research shows: when the coefficient of thermal expansion differences of substrate and chip surpasses 1.2 * 10
-5During/K, bear about 100 thermal cyclings and just occur separating.Existing electronic package material like matrix materials such as W/Cu, Mo/Cu, SiCp/Al, SiCp/Cu, BeO/Cu, all is difficult to satisfy the radiating requirements of following high-power component.Therefore, the superelevation thermal conducting material that matees fully of development thermal expansivity and semiconductor material is significant.
Diamond is the highest material of known occurring in nature thermal conductivity, and the thermal conductivity of single-crystal diamond can reach 2000W/ (mK), and its thermal expansivity (CTE) is 1.1 * 10
-6K, and diamond is an isolator under the room temperature, it also has a lot of good characteristics at aspects such as semi-conductor, optics.But single diamond is difficult for being made into packaged material; And cost is very high, and comparatively ideal is to make metal-base composites with it, and copper is one of important engineering material in the industrial circle; Have good conductivity and high heat conductivility, its thermal expansivity (CTE) is 17 * 10
-6K, thermal conductivity (TC) is 400W/ (mK), meets the low thermal coefficient of expansion of Electronic Packaging substrate material and the use properties requirement of high heat conductance.Therefore, be wild phase with the diamond, copper is that the diamond/carbon/carbon-copper composite material of body material is a kind of novel electron packaged material that has competitive power.This kind novel electron packaged 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 diamond and fine copper to be carried out compound tense, and the thermal conductivity of matrix material is merely 150W/m.K, well below theoretical value.This mainly be since the thermal conductivity of matrix material except depending on matrix and the thermal conductivity that strengthens body, matrix and the interface bonding state that strengthens body also have extremely important influence for the heat conduction behavior of matrix material.Because the two is incompatible, also nonwetting for diamond and copper, its interface is that weak mechanical-physical combines, and the thermal resistance that makes heat between diamond and copper, transmit strengthens, thereby has a strong impact on the heat conductivility of matrix material.Therefore, in order to give full play to the matrix material of the excellent thermal property of diamond, the high heat conduction of preparation, the interface modification of diamond and copper is the key scientific problems that must solve.
Summary of the invention
The present invention will solve the method for existing employing powder metallurgy or infiltration directly diamond and fine copper to be carried out the low technical problem of thermal conductivity of the matrix material of compound preparation, thereby the preparation method of a kind of high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material is provided.
The preparation method of a kind of high heat conduction of the present invention, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material realizes according to the following steps:
One, adopting the method for electroless copper is the copper coating of diamond powder coating surface 0.1 ~ 5 μ m of 1 ~ 200 μ m in granularity, forms the copper facing bortz powder;
Two, the mode that adopts powder mixing machine forms mixed powder copper facing bortz powder and copper powder in the step 1 are mixed;
Three, adopt the mixed powder coldmoulding of graphite jig with the step 2 preparation; Then the mixed powder after the coldmoulding is put into vacuum hotpressing stove together with graphite jig, earlier vacuum hotpressing stove being evacuated to vacuum tightness is 0.001 ~ 0.1Pa, is under 5 ~ 20 ℃/min condition in heating rate then; Vacuum hotpressing stove is warming up to 800 ~ 1000 ℃; Apply pressure to 20 ~ 60MPa simultaneously, the heat-insulation pressure keeping time is 0.5 ~ 2h, promptly obtains high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material;
Wherein, the electroless copper plating method in the step 1 is: earlier with diamond powder alligatoring, sensitization and activation then, and last electroless copper, the volume ratio of diamond and copper powder is 50 ~ 150:1;
Powder mixing machine mode in the step 2 is: steel ball, copper facing bortz powder and copper powder are put into Space cup, and being placed on then rolls on the powder mixing machine machine mixed powder 3 hours; Ball material mass ratio is 1 ~ 5:1; The copper powder granularity that is adopted is 10 ~ 200 μ m.
The present invention is through before the preparation matrix material; Plating one layer thickness is the copper layer of 0.1 ~ 5 μ m to the method for employing electroless copper in the bortz powder surface earlier, adopts vacuum heating-press sintering and copper powder to carry out heat conductivility and reduction thermal expansivity that composite methods improves diamond/carbon/carbon-copper composite material again.Through between diamond and copper powder, setting up the transition copper layer of one deck electroless plating, not only can become the sintering of diamond and copper the sintering of copper and copper, and the interface of matrix material combines better behind such sintering, density is also higher.The thermal conductivity of the matrix material of the present invention's preparation reaches 500W/m.K; And the thermal conductivity of copper facing diamond/carbon/carbon-copper composite material is not merely 170W/m.K; The present invention has not only improved the thermal conductivity of matrix material; And can reduce thermal expansivity through the volume(tric)fraction that increases diamond particles, the thermal expansivity of matrix material of the present invention can reduce to 7.8 * 10
-6/ K, and the thermal expansivity of copper is 17 * 10
-6/ K.
Description of drawings
Fig. 1 is the high heat conduction of test one preparation, the stereoscan photograph of low thermal coefficient of expansion diamond/carbon/carbon-copper composite material.
Embodiment
Embodiment one: the preparation method of a kind of high heat conduction of this embodiment, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material realizes according to the following steps:
One, adopting the method for electroless copper is the copper coating of diamond powder coating surface 0.1 ~ 5 μ m of 1 ~ 200 μ m in granularity, forms the copper facing bortz powder;
Two, the mode that adopts powder mixing machine forms mixed powder copper facing bortz powder and copper powder in the step 1 are mixed;
Three, adopt the mixed powder coldmoulding of graphite jig with the step 2 preparation; Then the mixed powder after the coldmoulding is put into vacuum hotpressing stove together with graphite jig, earlier vacuum hotpressing stove being evacuated to vacuum tightness is 0.001 ~ 0.1Pa, is under 5 ~ 20 ℃/min condition in heating rate then; Vacuum hotpressing stove is warming up to 800 ~ 1000 ℃; Apply pressure to 20 ~ 60MPa simultaneously, the heat-insulation pressure keeping time is 0.5 ~ 2h, promptly obtains high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material;
Wherein, the electroless copper plating method in the step 1 is: earlier with diamond powder alligatoring, sensitization and activation then, and last electroless copper, the volume ratio of diamond and copper powder is 50 ~ 150:1;
Powder mixing machine mode in the step 2 is: steel ball, copper facing bortz powder and copper powder are put into Space cup, and being placed on then rolls on the powder mixing machine machine mixed powder 3 hours; Ball material mass ratio is 1 ~ 5:1; The copper powder granularity that is adopted is 10 ~ 200 μ m.
The present invention is through before the preparation matrix material; Plating one layer thickness is the copper bed thickness of 0.1-5 μ m to the method for employing electroless copper in the bortz powder surface earlier, adopts vacuum heating-press sintering and copper powder to carry out heat conductivility and reduction thermal expansivity that composite methods improves diamond/carbon/carbon-copper composite material again.Through between diamond and copper powder, setting up the transition copper layer of one deck electroless plating, just can become the sintering of diamond and copper the sintering of copper and copper, the interface of matrix material combines better behind the sintering like this, and density is also higher.The thermal conductivity of the matrix material of the present invention's preparation reaches 500W/m.K; And the thermal conductivity of copper facing diamond/carbon/carbon-copper composite material is not merely 170W/m.K; The present invention has not only improved the thermal conductivity of matrix material; And can reduce thermal expansivity through the volume(tric)fraction that increases diamond particles, the thermal expansivity of matrix material of the present invention can reduce to 7.8 * 10
-6/ K, and the thermal expansivity of copper is 17 * 10
-6/ K.
Embodiment two: what this embodiment and embodiment one were different is: the diamond powder granularity in the step 1 is 50 ~ 150 μ m.Other step and parameter are identical with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is: the diamond powder granularity in the step 1 is 100 μ m.Other step and parameter are identical with embodiment one or two.
Embodiment four: what this embodiment was different with one of embodiment one to three is: the copper coating thickness on the diamond powder surface in the step 1 is 1 ~ 4 μ m.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: what this embodiment was different with one of embodiment one to four is: the copper coating thickness on the diamond powder surface in the step 1 is 2.5 μ m.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: what this embodiment was different with one of embodiment one to five is: original pressure 0.01 ~ 0.05Pa in the vacuum hotpressing stove after the vacuumizing in the step 3.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: what this embodiment was different with one of embodiment one to six is: original pressure 0.03Pa in the vacuum hotpressing stove after the vacuumizing in the step 3.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: what this embodiment was different with one of embodiment one to seven is: heating rate is 10 ~ 15 ℃/min in the step 3.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: what this embodiment was different with one of embodiment one to eight is: heating rate is 13 ℃/min in the step 3.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: what this embodiment was different with one of embodiment one to nine is: vacuum hotpressing stove is warming up to 850 ~ 950 ℃ in the step 3.Other step and parameter are identical with one of embodiment one to nine.
Embodiment 11: what this embodiment was different with one of embodiment one to ten is: vacuum hotpressing stove is warming up to 900 ℃ in the step 3.Other step and parameter are identical with one of embodiment one to ten.
Embodiment 12: what this embodiment was different with one of embodiment one to 11 is: exerting pressure in the step 3 is 30 ~ 50MPa.Other step and parameter are identical with one of embodiment one to 11.
Embodiment 13: what this embodiment was different with one of embodiment one to 12 is: exerting pressure in the step 3 is 40MPa.Other step and parameter are identical with one of embodiment one to 12.
Embodiment 14: what this embodiment was different with one of embodiment one to 13 is: the heat-insulation pressure keeping time is 0.8 ~ 1.7h in the step 3.Other step and parameter are identical with one of embodiment one to 13.
Embodiment 15: what this embodiment was different with one of embodiment one to 14 is: the heat-insulation pressure keeping time is 1.5h in the step 3.Other step and parameter are identical with one of embodiment one to 14.
Through following verification experimental verification beneficial effect of the present invention:
Test one: a kind of high heat conduction of this test, the preparation method of low thermal coefficient of expansion diamond/carbon/carbon-copper composite material realize according to the following steps:
One, adopting the method for electroless copper is the copper layer of 1 μ m at bortz powder surface plating thickness, and diamond grit is 100 μ m, forms the copper facing bortz powder;
Two, selecting granularity for use is the copper powder of 90 μ m, is 50:50 by the volume ratio of copper facing bortz powder and copper powder, adopts the mode of powder mixing machine that the copper facing bortz powder in the step 1 was mixed 3 hours with copper powder, the formation mixed powder;
Three, the mixed powder after mixing in the step 2 is put into graphite jig coldmoulding.Then mixed powder is together put into the vacuum heating-press sintering stove together with graphite jig; Earlier vacuum hotpressing stove being evacuated to vacuum tightness is that 0.001Pa is that the speed of 10 ℃/min rises to 900 ℃ with vacuum heating-press sintering stove sintering temperature with temperature rise rate; Sintering pressure is 50MPa, and the heat-insulation pressure keeping time is 0.5h;
Wherein the electroless copper plating method described in the step 1 is specific as follows: step 1: a, roughening treatment: with diamond particles with 10% HNO
3Boil 20min, extremely neutral with distilled water flushing then; B, sensitization are handled: in 40 ℃ water-bath; The diamond particles that will pass through step a roughening treatment joins in the beaker of sensitizing solution that the massfraction that is equipped with by the tin protochloride of 30g/L and 25ml/L is 37% hydrochloric acid preparation; Reaction is 20 minutes under churned mechanically effect; Staticly settle then, upper solution toppled over, with the particle flushing of suction method after with sensitization to neutral; C, activation treatment: in 40 ℃ water-bath; Diamond particles after will passing through step c sensitization and handling adds 30ml zero(ppm) water, the furnishing scattered paste shape, and joining by 50mg/L Palladous chloride and 25ml/L massfraction is in the middle of the activation solution that is mixed with of 37% hydrochloric acid; Reaction 20min under churned mechanically effect; Staticly settle then, upper solution toppled over, with the diamond particles flushing of suction method after with activation to neutral; D, reduction are handled: the diamond particles that will pass through after the step c activation treatment is received solution with 4ml/L formaldehyde solution or ortho phosphorous acid, and heated and stirred 20min under 40 ℃ of water bath condition filters, with distilled water flushing to neutrality, dry for standby; Step 2: diamond particles electroless copper: respectively with 15g CuSO
45H
2O, 30g Na
2EDTA, 20g C
4H
4KNa4H
2O is dissolved in 60 ℃ the zero(ppm) water, and 15gNaOH is dissolved in the cold water; Again CuSO will be housed
45H
2The beaker of O solution is placed in 60 ℃ the water-bath, while stirring with Na
2EDTA solution slowly joins CuSO
45H
2O solution stirred after 20 minutes, added C
4H
4KNa4H
2O solution slowly adds NaOH solution subsequently and strengthens the stirring dynamics; Treat that solution clarification back adds the α of 30mg, α '-dipyridyl, the back that stirs is for use as plating bath to 1L with distilled water diluting; The plating bath for preparing is heated to 65 ℃, and adding 20ml massfraction is 37% formaldehyde, adjustment pH; Plating bath pH is that 10% NaOH dilute solution transfers to 12 by mass concentration; Adding is carried out the electroless copper reaction through the pretreated diamond particles of step 1 under the condition of continuously stirring, thickness of coating is controlled at 3 μ m by the time.
Concrete effect: the diamond/carbon/carbon-copper composite material thermal conductivity of this test one preparation reaches 550W/m.K, and thermal expansivity is 8.2 * 10
-6/ K, density is higher than 99%.And the thermal conductivity of copper facing diamond/carbon/carbon-copper composite material is not 170W/m.K, and thermal expansivity is 8.8 * 10
-6/ K, density is 95%.
Test two: a kind of high heat conduction of this test, the preparation method of low thermal coefficient of expansion diamond/carbon/carbon-copper composite material realize according to the following steps:
One, adopting the method for electroless copper is the copper layer of 2 μ m at bortz powder surface plating thickness, and diamond grit is 120 μ m, and the copper powder granularity is 110 μ m,, form the copper facing bortz powder;
Two, the volume ratio according to copper facing bortz powder and copper powder is the ratio of 60:40, adopts the mode of powder mixing machine that the copper facing diamond powder in the step 1 was mixed 3 hours with copper powder, forms mixed powder;
Three, the mixed powder after mixing in the step 2 is put into graphite jig coldmoulding.Then mixed powder is together put into the vacuum heating-press sintering stove together with graphite jig; Earlier vacuum hotpressing stove is evacuated to 0.001Pa; The speed that with temperature rise rate is 10 ℃/min rises to 900 ℃ with vacuum heating-press sintering stove sintering temperature, and sintering pressure is 50MPa, and the heat-insulation pressure keeping time is 1h.
Electroless copper plating method in this test two is identical with the electroless copper plating method of test one.
Concrete effect: the diamond/carbon/carbon-copper composite material thermal conductivity of this test two preparations reaches 530W/m.K, and thermal expansivity is 8.0 * 10
-6/ K, density is higher than 99%.
Test three: a kind of high heat conduction of this test, the preparation method of low thermal coefficient of expansion diamond/carbon/carbon-copper composite material realize according to the following steps:
One, adopting the method for electroless copper is the copper layer of 5 μ m at bortz powder surface plating thickness, and diamond grit is 150 μ m, and the copper powder granularity is 120 μ m, forms the copper facing bortz powder;
Two, the volume ratio according to copper facing bortz powder and copper powder is the ratio of 70:30, adopts the mode of powder mixing machine that the copper facing bortz powder in the step 1 was mixed 3 hours with copper powder, forms mixed powder;
Three, the mixed powder after mixing in the step 2 is put into graphite jig coldmoulding.Then mixed powder is together put into the vacuum heating-press sintering stove together with graphite jig; Earlier vacuum hotpressing stove is evacuated to 0.001Pa; The speed that with temperature rise rate is 10 ℃/min rises to 1000 ℃ with vacuum heating-press sintering stove sintering temperature, and sintering pressure is 60MPa, and the heat-insulation pressure keeping time is 1.5h.
Electroless copper plating method in this test three is identical with the electroless copper plating method of test one.
Concrete effect: the diamond/carbon/carbon-copper composite material thermal conductivity of this test three preparations reaches 500W/m.K, and thermal expansivity is 7.8 * 10
-6/ K, density is higher than 98%.
Claims (10)
1. the preparation method of a high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material is characterized in that preparing high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material method realizes according to the following steps:
One, adopting the method for electroless copper is the copper coating of diamond powder coating surface 0.1 ~ 5 μ m of 1 ~ 200 μ m in granularity, forms the copper facing bortz powder;
Two, copper facing bortz powder and copper powder in the step 1 are mixed, form mixed powder;
Three, adopt the mixed powder coldmoulding of graphite jig with the step 2 preparation; Then the mixed powder after the coldmoulding is put into vacuum hotpressing stove together with graphite jig, earlier vacuum hotpressing stove being evacuated to vacuum tightness is 0.001 ~ 0.1Pa, is under 5 ~ 20 ℃/min condition in heating rate then; Vacuum hotpressing stove is warming up to 800 ~ 1000 ℃; Apply pressure to 20 ~ 60MPa simultaneously, the heat-insulation pressure keeping time is 0.5 ~ 2h, promptly obtains high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material.
2. the high heat conduction of a kind of preparation according to claim 1, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material method is characterized in that the diamond powder granularity in the step 1 is 50 ~ 150 μ m.
3. the preparation method of a kind of high heat conduction according to claim 1 and 2, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material is characterized in that the copper coating thickness on the diamond powder surface in the step 1 is 1 ~ 4 μ m.
4. the preparation method of a kind of high heat conduction according to claim 3, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material is characterized in that it is 0.01 ~ 0.05Pa that elder generation in the step 3 is evacuated to vacuum tightness with vacuum hotpressing stove.
5. according to the preparation method of claim 1,2 or 4 described a kind of high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material, it is characterized in that heating rate is 10 ~ 15 ℃/min in the step 3.
6. according to the preparation method of claim 1,2 or 4 described a kind of high heat conduction, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material, it is characterized in that vacuum hotpressing stove is warming up to 850 ~ 950 ℃ in the step 3.
7. the high heat conduction of a kind of preparation according to claim 1 and 2, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material method, it is characterized in that exerting pressure in the step 3 is 30 ~ 50MPa.
8. the preparation method of a kind of high heat conduction according to claim 1 and 2, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material, it is characterized in that exerting pressure in the step 3 is 40MPa.
9. the preparation method of a kind of high heat conduction according to claim 1 and 2, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material is characterized in that the heat-insulation pressure keeping time is 0.8 ~ 1.7h in the step 3.
10. the preparation method of a kind of high heat conduction according to claim 1 and 2, low thermal coefficient of expansion diamond/carbon/carbon-copper composite material is characterized in that the heat-insulation pressure keeping time is 1.5h in the step 3.
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