CN102465213A - High heat conduction diamond heat sink material and preparation method thereof - Google Patents
High heat conduction diamond heat sink material and preparation method thereof Download PDFInfo
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- CN102465213A CN102465213A CN2010105342971A CN201010534297A CN102465213A CN 102465213 A CN102465213 A CN 102465213A CN 2010105342971 A CN2010105342971 A CN 2010105342971A CN 201010534297 A CN201010534297 A CN 201010534297A CN 102465213 A CN102465213 A CN 102465213A
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- sink material
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Abstract
The invention relates to a high heat conduction diamond heat sink material. The diamond heat sink material comprises, by mass, 0.1-1.5% of Co, and the balance diamond particles and Cu, wherein the content of the diamond particles in the balance diamond particles and Cu is 70-90% by volume. Raw material powder and a Co-containing alloy base which are assembled to form a sintering component undergo high-temperature high-pressure sintering after adjusting sintering parameters, The composite material which forms a diamond-diamond based strong metallurgy combination interface allows the influence of the heat resistance of a heterogeneous material interface to the heat conductivity to be reduced and the top thermal conductivity of the diamond-Cu heat sink material to be 639W.m<-1>.K<-1>. The diamond-Cu heat sink material prepared in the invention, which has the characteristics of high heat conductivity and adjustable heat expansion coefficient, allows the high heat conductivity to be satisfied and the heat expansion coupling with a substrate material to be improved through adjusting the volume fraction of a reinforced phase.
Description
Technical field
The present invention relates to a kind of diamond heat-sink material and preparation method thereof, be specially diamond-copper composite heat sink material of a kind of high heat conduction, adjustable thermal expansion matching and preparation method thereof.
Background technology
Along with Electronic Packaging system high-density, multi-functional, microminiaturized development, the heat dissipation problem of electron device becomes restriction electronic industry development key problem, and the novel encapsulated that presses for development high heat conductance and thermal expansion matching is used heat sink material.The traditional heat-dissipating material like Cu, Al etc., has high thermal and (is respectively 401Wm
-1K
-1, 218Wm
-1K
-1), but its thermal expansivity is up to 16.7 * 10
-6K
-1, 23 * 10
-6K
-1, differ greatly with substrate materials such as Si, GaAs and (to be respectively 2.5 * 10
-6K
-1, 6.86 * 10
-6K
-1).Stupalith thermal conductivities such as BeO, SiC, AlN are higher relatively, and chemicalstability is good, and thermal expansivity and semiconductor material are approximate, but processing is comparatively difficult, and especially BeO has severe toxicity and cost height.
High quality diamond is the highest material of known in the world thermal conductivity, and natural IIa type diamond thermal conductivity reaches as high as 2200Wm
-1K
-1, it also has characteristics such as high resistivity and high breaking down field strength, low-k, low-thermal-expansion, therefore is with a wide range of applications in the Electronic Packaging field.Diamond mainly contains two kinds of forms as heat sink material, i.e. diamond thin and with metal composite such as diamond and copper, aluminium.It is reported that the diamond thin thermal conductivity can reach 800Wm
-1K
-1Its technology of preparing is ripe relatively at present, but synthesis condition is very harsh, and (CTE is merely 1 * 10 because diamond thin has low-thermal-expansion
-6K
-1), difficult and characteristics such as wetting metal and welding, cause the assembling and the application of diamond thin and other devices and scolder to be very limited.And, realize high thermal conductance and adjustable thermal expansion through regulating the diamond volume(tric)fraction with metal composite such as diamond and copper, aluminium, can satisfy the requirement of system radiating and packaging technology.Therefore diamond-metal composite has become the new lover of domestic and international advanced heat sink material, is described as third generation thermal management materials.
0.Beffort be about 375Wm Deng adopting squeeze casting method to prepare Al/ diamond composite thermal conductivity
-1K
-1, the diamond volume(tric)fraction is between 50%～70%.It is diamond-Cu matrix material of 42% that employing hot-press methods such as Schubert have prepared the diamond volume(tric)fraction, and thermal conductivity reaches 640Wm
-1K
-1Diamond-Cu matrix material thermal conductivity that people such as Yoshida adopt pressure sintering to make diamond volume(tric)fraction 60% is about 395Wm
-1K
-1E.A.Ekimov etc. adopt the diamond composite thermal conductivity of HTHP preparation up to 900Wm
-1K
-1, wherein the diamond volume(tric)fraction is up to 93%～95%.Domestic researchist shows diamond-Cu composite study, adopts the diamond composite heat sink material thermal conductivity of method preparations such as infiltration method, SPS sintering extremely low, is significantly less than theoretical value.The reason that thermal conductivity promotes bottleneck occurs, much relations are arranged with matrix material thermal conductivity influence factor.The net heat transmissibility of matrix material is not only the function of each constituent element thermal conductivity, geometric distribution and volume(tric)fraction thereof, but also receives the tremendous influence of interfacial characteristics between each constituent element.Diamond surface can be extremely low, and with the wetting difficulty of copper, diamond behind the sintering/copper interface is weak mechanical bond, and thermal expansion coefficient difference can cause remarkable interface resistance effect.The interface resistance effect makes net heat conductance or the thermal diffusivity of matrix material reduce one or two order of magnitude, thus havoc the thermal conductivity of diamond-copper.Therefore, in order to give full play to diamond, must under the prerequisite that strengthens interface binding intensity, reduce interface resistance as far as possible at the excellent properties aspect the thermal conduction.
Summary of the invention
One of the object of the invention is to solve the interface bonding and the interface resistance problem of diamond and these two kinds of dissimilar materialss of copper, gives full play to the characteristic of the high heat conduction of diamond, prepares the diamond-copper heat sink material of high thermal conductance, thermal expansion matching.
For realizing above-mentioned purpose, the present invention takes following technical scheme:
A kind of high heat-conductive diamond heat sink material is made up of matrix copper, diamond particles and cobalt, it is characterized in that: the content of cobalt counts 0.1～1.5% with massfraction, and all the other are diamond particles and copper; In diamond particles and copper, said diamond particles content counts 70%～90% with volume percent.
A kind of optimized technical scheme is characterized in that: the particle diameter of diamond particles is 10 μ m～200 μ m.
Another object of the present invention provides a kind of high heat-conductive diamond-copper composite heat sink preparation methods, and diamond and copper powder, cobalt-containing alloy substrate after suction filtration is handled are carried out vacuum heat treatment after assembling by sintering unit wiring layout.Adopt the HTHP sintering method to prepare the diamond-copper heat sink material, utilize the diffusion of cobalt in the alloy substrates to realize the adding of additive, adjustment alloy substrates composition with cobalt element content in the control heat sink material between 0.1%～1.5%.The concrete technical scheme of taking is following:
A kind of preparation method of high heat-conductive diamond heat sink material may further comprise the steps:
1. diamond particles pre-treatment: rare HNO that diamond particles is being boiled respectively
3Respectively boil 30min in solution, the NaOH solution, the cooling back, is carried out suction filtration and is handled to neutral with deionized water rinsing in vacuum apparatus;
2. assemble the sintering unit: grinding and buffing jacket surface, with jacket and pad deoil, ultrasonic cleaning, infrared oven dry; With putting into jacket after diamond particles and the copper powder wet mixing evenly, the substrate of assembling cobalt-containing alloy is assembled into the sintering unit block;
3. HTHP sintering: sintering temperature is 800 ℃～1300 ℃, and sintering pressure is 4GPa～8GPa, and sintering time is 9～15min;
4. following process: adopt the diamond abrasive tool polishing to remove outer jacket, the line cutting processing is downcut diamond-copper composite material from alloy substrates, and grinding machine polishing tangent plane is to light.
A kind of optimized technical scheme is characterized in that: before assembling sintering unit, also comprise copper powder reduction treatment step, be about to copper powder and use hydrogen reducing that reduction temperature is 300 ℃～500 ℃, the time is 1～3h.When the copper powder oxygen level is higher, can select to adopt this step.
A kind of optimized technical scheme is characterized in that: step 1. in, said suction filtration treatment temperature is 400 ℃～600 ℃, the treatment time is 5h～8h, with impurity such as the oxygen of further removal diamond surface absorption, nitrogen, water vapors.
A kind of optimized technical scheme is characterized in that: step 2. in, said vacuum drying oven vacuum tightness is 10
-2Pa, temperature is 120 ℃～300 ℃.
A kind of optimized technical scheme is characterized in that: described cobalt-containing alloy is a YG8 trade mark wimet, and cobalt contents is in massfraction about 8%.Additive cobalt in the heat sink material is from the diffusion of cobalt in the cobalt-containing alloy.The stable catalyst reaction zone that is in diamond sintering unit under the HTHP sintering condition, the additive cobalt impels the diamond-diamond interface that forms low thermal resistance, and effectively improvement bonding phase copper combines with the interface of diamond particles.
The invention has the advantages that:
High thermal conductance diamond heat-sink material of the present invention; Adopt the preparation of HTHP sintering method; Being made up of matrix copper, the additive cobalt that has the wild phase diamond particles of low-thermal-expansion high heat conductance and improve diamond/copper interface bonding state, is the bonding phase with copper, is wild phase with the high thermal conductive diamond stone granulate; Heat sink material forms with diamond-diamond interface and is the master, combines the interface structure tight, that intensity is high, and thermal conductivity reaches as high as 639Wm
-1K
-1The diamond-copper heat sink material of the present invention preparation has thermal conductivity height, characteristics that thermal expansivity is adjustable, can when satisfying the high capacity of heat transmission, improve the thermal expansion matching with baseplate material through adjustment wild phase volume(tric)fraction.
The present invention is under the HTHP sintering condition, and the good wet through additive cobalt realization diamond and copper improves the bonding strength at diamond/copper dissimilar materials interface.Addition with cobalt in the alloy substrates adjustment heat sink material of different cobalt content.Regulating the sintering parameter makes sintering process be stabilized in the diamond catalyst reaction zone; Impelling matrix material to form diamond-diamond lattic structure is main low thermal resistance, strong metallurgical bonding interface; Reduced the influence of dissimilar materials interface resistance to thermal conductivity, the composite heat sink material thermal conductivity reaches as high as 639Wm
-1K
-1This method can be prepared the high diamond of thermal conductivity-Cu composite heat sink material.
Through accompanying drawing and embodiment the present invention is further specified below, but and do not mean that restriction protection domain of the present invention.
Description of drawings
Fig. 1 is a sintering unit wiring layout.
Fig. 2 is a process flow sheet of the present invention.
Fig. 3 is the diamond heat-sink material interface state of embodiment 1 preparation.
Fig. 4 is the diamond heat-sink material interface state of embodiment 2 preparations.
Fig. 5 is the diamond heat-sink material interface state of embodiment 3 preparations.
Fig. 6 is the diamond heat-sink material interface state of embodiment 4 preparations.
Embodiment
Embodiment 1: select 170 orders～200 order diamond single crystal particles (the about 80 μ m of median size) and 325 orders～400 order copper powders for use.In diamond particles and copper, the diamond particles volume(tric)fraction is 80%.
Prepare diamond-copper composite heat sink material according to technical process shown in Figure 2.Rare HNO that the diamond single crystal particle is boiling respectively
3Boil 30min in solution, the NaOH solution, cooling back, is carried out suction filtration and is handled to neutral with deionized water rinsing in vacuum apparatus, and the suction filtration temperature is 500 ℃, and the treatment time is 5h, with impurity such as the oxygen of further removal diamond surface absorption, nitrogen, water vapors.
With diamond particles and copper powder wet mixing 2h in mixer, the wet mixing medium is an alcohol according to preset proportion.After mixing, press the wiring layout assembling of sintering unit.As shown in Figure 1, be sintering of the present invention unit wiring layout, wherein 1 is electrode, and 2 is pad, and 3 is jacket, and 4 is mixed powder, and 5 is the cobalt-containing alloy substrate, and 6 is mould.Elder generation grinding and buffing jacket 3 surfaces, with jacket 3 and pad 2 deoil, ultrasonic cleaning, infrared oven dry; The mixed powder 4 that obtains after diamond particles and the copper powder wet mixing is evenly put into jacket 3, assembling cobalt-containing alloy substrate 5, the YG8 alloy is adopted in cobalt-containing alloy substrate 5, and cobalt contents is 8wt.%.Be assembled into the sintering unit block, vacuum heat treatment places vacuum drying oven (10
-2Pa, 120 ℃～300 ℃) in subsequent use.Carry out the HTHP sintering, 900～1100 ℃ of sintering temperatures, sintering pressure 5.5～8GPa, sintering time 9～11min.Adopt the diamond abrasive tool polishing to remove outer jacket, the line cutting processing is downcut diamond-copper composite material from alloy substrates, and grinding machine polishing tangent plane is to light.
Adopt the diamond-copper heat sink material cobalt contents of this prepared to be about 1.05%, density 4.911g/cm
3, thermal conductivity is about 639Wm
-1K
-1Thermal expansivity 4.044 * 10
-6K
-1, near the thermal expansivity of Si, GaAs.The interfacial state of the diamond heat-sink material of present embodiment preparation is as shown in Figure 3.
Embodiment 2: select 170 orders～200 order diamond single crystal particles (the about 80 μ m of median size) and 325 orders～400 order copper powders for use.In diamond particles and copper, diamond particles volume(tric)fraction 80%.
The diamond single crystal particle is respectively at rare HNO
3Boil 30min in solution, the NaOH solution, cooling back, is carried out suction filtration and is handled to neutral with deionized water rinsing in vacuum apparatus, and the suction filtration temperature is 400 ℃, and the treatment time is 5h～7h, with impurity such as the oxygen of further removal diamond surface absorption, nitrogen, water vapors.
With diamond particles and copper powder wet mixing 2h in mixer, the wet mixing medium is an alcohol according to preset proportion.After mixing, press the assembling of sintering unit wiring layout, first grinding and buffing jacket 3 surfaces, with jacket 3 and pad 2 deoil, ultrasonic cleaning, infrared oven dry; The mixed powder 4 that obtains after diamond particles and the copper powder wet mixing is evenly put into jacket 3, assembling cobalt-containing alloy substrate 5, the YG8 alloy is adopted in cobalt-containing alloy substrate 5, and cobalt contents is 8%w.t..Be assembled into the sintering unit block.Carry out the HTHP sintering, 1000～1200 ℃ of sintering temperatures, sintering pressure 5.5～8GPa, sintering time 9～11min.Adopt the diamond abrasive tool polishing to remove outer jacket, the line cutting processing is downcut diamond-copper composite material from alloy substrates, and grinding machine polishing tangent plane is to light.
Adopt the diamond-Cu heat sink material cobalt contents of this prepared to be about 0.71%, density 4.870g/cm
3, thermal conductivity is about 616Wm
-1K
-1The interfacial state of the diamond heat-sink material of present embodiment preparation is as shown in Figure 4.
Embodiment 3: select 325 orders～400 order diamond single crystal particles (the about 40 μ m of median size) and 325 orders～400 order copper powders for use.In diamond particles and copper, diamond particles volume(tric)fraction 80%.
The diamond single crystal particle is respectively at rare HNO
3Boil 30min in solution, the NaOH solution, to neutral, suction filtration is handled with deionized water rinsing in the cooling back, and the suction filtration temperature is 600 ℃, and the treatment time is 6h.Copper powder is used hydrogen reducing, and reduction temperature is 300 ℃, and the time is 3h.With diamond particles and copper powder wet mixing 2h in mixer, the wet mixing medium is an alcohol according to preset proportion.After mixing, press the wiring layout assembling of sintering unit, be assembled into the sintering unit block.Carry out the HTHP sintering.900～1100 ℃ of sintering temperatures, sintering pressure 4～5.5GPa, sintering time 9～11min.Other operation is with embodiment 1.
Adopt the diamond-Cu heat sink material cobalt contents of this prepared to be about 1.05%, density 4.715g/cm
3, thermal conductivity is about 540Wm
-1K
-1, thermal expansivity 4.403 * 10
-6K
-1The interfacial state of the diamond heat-sink material of present embodiment preparation is as shown in Figure 5.
Embodiment 4: select 70 orders～80 order diamond single crystal particles (the about 200 μ m of median size) and 325 orders～400 order copper powders for use.In diamond particles and copper, diamond particles volume(tric)fraction 70%.
The diamond single crystal particle is respectively at rare HNO
3Boil 30min in solution, the NaOH solution, to neutral, suction filtration is handled with deionized water rinsing in the cooling back, and the suction filtration temperature is 450 ℃, and the treatment time is 8h.Copper powder is used hydrogen reducing, and reduction temperature is 500 ℃, and the time is 1h.With diamond particles and copper powder wet mixing 2h in mixer, the wet mixing medium is an alcohol according to preset proportion.After mixing, press the wiring layout assembling of sintering unit, be assembled into the sintering unit block.Carry out the HTHP sintering, 900～1100 ℃ of sintering temperatures, sintering pressure 4～5.5GPa, sintering time 10～12min.Other operation is with embodiment 1.
Adopt the diamond-Cu heat sink material cobalt contents of this prepared to be about 0.69%, density 4.899g/cm
3, thermal conductivity is about 563Wm
-1K
-1The interfacial state of the diamond heat-sink material of present embodiment preparation is as shown in Figure 6.
Claims (7)
1. a high heat-conductive diamond heat sink material is made up of matrix copper, diamond particles and cobalt, it is characterized in that: the content of cobalt counts 0.1～1.5% with massfraction, and all the other are diamond particles and copper; In diamond particles and copper, said diamond particles content counts 70%～90% with volume percent.
2. high heat-conductive diamond heat sink material according to claim 1 is characterized in that: the particle diameter of diamond particles is 10 μ m～200 μ m.
3. the preparation method of a high heat-conductive diamond heat sink material may further comprise the steps:
1. diamond particles pre-treatment: rare HNO that diamond particles is being boiled respectively
3Respectively boil 30min in solution, the NaOH solution, the cooling back, is carried out suction filtration and is handled to neutral with deionized water rinsing in vacuum apparatus;
2. assemble the sintering unit: grinding and buffing jacket surface, with jacket and pad deoil, ultrasonic cleaning, infrared oven dry; With putting into jacket after diamond particles and the copper powder wet mixing evenly, the substrate of assembling cobalt-containing alloy is assembled into the sintering unit block;
3. HTHP sintering: sintering temperature is 800 ℃～1300 ℃, and sintering pressure is 4GPa～8GPa, and sintering time is 9～15min;
4. following process: adopt the diamond abrasive tool polishing to remove outer jacket, the line cutting processing is downcut diamond-copper composite material from alloy substrates, and grinding machine polishing tangent plane is to light.
4. the preparation method of high heat-conductive diamond heat sink material according to claim 3; It is characterized in that: before assembling sintering unit, also comprise copper powder reduction treatment step, be about to copper powder and use hydrogen reducing; Reduction temperature is 300 ℃～500 ℃, and the time is 1～3h.
5. the preparation method of high heat-conductive diamond heat sink material according to claim 3 is characterized in that: step 1. in, described suction filtration treatment temperature is 400 ℃～600 ℃, the treatment time is 5h～8h.
6. the preparation method of high heat-conductive diamond heat sink material according to claim 3 is characterized in that: step 2. in, said vacuum drying oven vacuum tightness is 10
-2Pa, temperature is 120 ℃～300 ℃.
7. the preparation method of high heat-conductive diamond heat sink material according to claim 3 is characterized in that: described cobalt-containing alloy is the YG8 alloy, and cobalt contents counts 8% with massfraction.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419133A (en) * | 2017-05-12 | 2017-12-01 | 南通鑫祥锌业有限公司 | High-volume fractional diamond zinc composite |
| CN108588529A (en) * | 2018-04-13 | 2018-09-28 | 上海交通大学 | The high heat conduction metal-based composite material and preparation method at graphene modified interface |
| CN110330950A (en) * | 2019-08-02 | 2019-10-15 | 太原理工大学 | Composite heat dissipation material and preparation method thereof containing diamond strips |
| CN112877563A (en) * | 2021-02-23 | 2021-06-01 | 郑州华晶金刚石股份有限公司 | Diamond/copper composite material and preparation method thereof |
| CN114134381A (en) * | 2021-12-06 | 2022-03-04 | 中南大学 | Wear-resistant multi-principal-element alloy-diamond composite material and preparation method and application thereof |
| CN114941132A (en) * | 2022-05-27 | 2022-08-26 | 邵阳市东昇超硬材料有限公司 | Enhanced diamond material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419133A (en) * | 2017-05-12 | 2017-12-01 | 南通鑫祥锌业有限公司 | High-volume fractional diamond zinc composite |
| CN108588529A (en) * | 2018-04-13 | 2018-09-28 | 上海交通大学 | The high heat conduction metal-based composite material and preparation method at graphene modified interface |
| CN110330950A (en) * | 2019-08-02 | 2019-10-15 | 太原理工大学 | Composite heat dissipation material and preparation method thereof containing diamond strips |
| CN112877563A (en) * | 2021-02-23 | 2021-06-01 | 郑州华晶金刚石股份有限公司 | Diamond/copper composite material and preparation method thereof |
| CN112877563B (en) * | 2021-02-23 | 2022-05-10 | 郑州华晶金刚石股份有限公司 | Diamond/copper composite material and preparation method thereof |
| CN114134381A (en) * | 2021-12-06 | 2022-03-04 | 中南大学 | Wear-resistant multi-principal-element alloy-diamond composite material and preparation method and application thereof |
| CN114134381B (en) * | 2021-12-06 | 2022-06-21 | 中南大学 | Wear-resistant multi-principal-element alloy-diamond composite material and preparation method and application thereof |
| CN114941132A (en) * | 2022-05-27 | 2022-08-26 | 邵阳市东昇超硬材料有限公司 | Enhanced diamond material |
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Application publication date: 20120523 |