CN102244051B - High-performance directional heat conduction copper-base diamond composite material and preparation method thereof - Google Patents

High-performance directional heat conduction copper-base diamond composite material and preparation method thereof Download PDF

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CN102244051B
CN102244051B CN 201110169998 CN201110169998A CN102244051B CN 102244051 B CN102244051 B CN 102244051B CN 201110169998 CN201110169998 CN 201110169998 CN 201110169998 A CN201110169998 A CN 201110169998A CN 102244051 B CN102244051 B CN 102244051B
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diamond
copper
rod
matrix
column
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CN 201110169998
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CN102244051A (en
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魏秋平
余志明
刘学璋
尹登峰
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中南大学
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L2924/00Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001Technical content checked by a classifier
    • H01L2924/0002Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Abstract

The invention discloses a high-performance directional heat conduction copper-base diamond composite material and a preparation method thereof. A plurality of diamond sticks are distributed on a copper base body in parallel in the same direction; the diameters of the diamond sticks are 0.5 to 10 millimeters; and distances among the diamond sticks are 0.5 to 50 millimeters. As the plurality of columnar diamond sticks with high heat conduction rate are arranged in the copper base body in the same direction, the composite material has high directional heat conduction performance along the direction; and the composite material can be used as electronic package, heat sink materials and the like and can solve the problem of package of high-temperature, high-frequency and high-power electronic devices.

Description

A kind of high-performance directional heat conduction copper-base diamond composite material and preparation method thereof

Technical field

The present invention relates to a kind of diamond composite, particularly relate to a kind of high-performance directional heat conduction copper-base diamond composite material, the invention still further relates to the preparation method of this high-performance directional heat conduction copper-base diamond composite material.

Background technology

The permission operating temperature range of large scale integrated circuit is generally 0~70 ℃, and reliable serviceability temperature scope is 0~40 ℃.When the semiconductor device heating surface temperature rose to 100 ℃, performance began to descend; Temperature is during by 25 ℃ of 100 ℃ of every risings, and failure rate will increase by 5~6 times.But because the circuit heat that produces that runs up even can make the circuit local temperature reach 400 ℃.In recent years, noticeable take high temperature semiconductors material SiC, GaN, AlN and doped diamond as the exploitation of the wide bandgap semiconductor device of representative, they have the characteristics such as energy gap is large, breakdown electric field is high, thermal conductivity is large, carrier mobility is high, dielectric constant is little, capability of resistance to radiation is strong, and being described as is third generation semi-conducting material after Si, GaAs.Have broad application prospects in high temperature, high frequency, great-power electronic field, this class device mostly is operated in hot environment, need special encapsulation, the past people note seldom the encapsulation of high-temperature device, but along with the development of high-temperature electronic device (as the GaN high-temperature device, its working temperature can reach more than 600 ℃), conventional electronic package material such as glass epoxide circuit board, coppered wire and plumber's solder etc. can not be suitable for fully, even the encapsulation of the aluminium oxide ceramics of standard can not meet the demands, in the urgent need to new encapsulating material and technology.

The materials such as semiconductor package reload request substrate, casing and cover plate all must have good heat conductivity, to guarantee that the golf calorific value that electronic device in use causes can in time distribute, the semiconductor and other elements that prevent temperature-sensitive are destroyed, the premature failure of macroscopic view cracking, torsional deformation, layering and other electricity and mechanical mechanics property that the minimizing thermal stress causes.Diamond is except having valuable aesthetic values as diamond, the physical and chemical performance that also has a series of excellences, comprising the highest hardness, modulus of elasticity, high disruptive field intensity, thermal conductivity, carrier mobility, extremely low coefficient of linear expansion, coefficient of friction, very wide forbidden band, optical transmittance, extraordinary chemical stability and biocompatibility, pure diamond is good insulating body, can become good semiconductor after doping and even may become superconductor etc.Adamantine thermal conductivity is high, and during room temperature, the thermal conductivity of II type natural uni-crystal diamond is 4~5 times of copper.Reach 2200WK -1M -1Adamantine thermal coefficient of expansion (1.0~2.0) * 10 -6K -1Suitable with third generation semi-conducting material, density ratio traditional metal encapsulating material is little, has good high-temperature behavior, radiation resistance and chemical stability, is suitable for the high heat conduction requirement of high temperature, high frequency, high-power electronic device encapsulation.

At present, a lot of researchs concentrate on diadust and metal composite, utilize adamantine high thermal conductivity to improve the thermal conductance of composite material, but the thermal conductivity of the acquisition of the method mostly are 200~600WK -1M -1, far below diamond.Along with updating of the deepening continuously of CVD growing diamond film research, technology of preparing, quality and the deposition rate of preparation diamond film improve gradually.By controlling adamantine institutional framework, the thermal conductivity of CVD diamond film has reached 1000~2200WK -1M -1, near the level of II type natural diamond.

Copper has high-melting-point (1356K), low-resistance coefficient (1.72 μ Ω cm), high heat conductance (401WK -1M -1), high resistance electron transfer ability, resistance to oxidation and corrosion, higher mechanical strength, good ductility and plasticity, easy machining, the easily characteristics such as welding.diamond has high thermal conductivity, copper has high conductivity, if make the abundant combination of both advantages, exploitation can be used for high temperature, high frequency, the high thermal conductance of high power semi-conductor electronic device, high electricity is led, the low-power consumption encapsulating material, can greatly advance high temperature, high frequency, the development of high-power Wide Bandgap Semiconductor Technology, promote the progress of high-temperature electronic technology, realize that third generation high temperature half waveguide technology is at the Aero-Space pyrostat, the high temperature intense radiation environment of universe exploration, the highly reliable radio-frequency devices of Radar-Communication system, the application in the fields such as the high temperature detection of nuclear reactor and monitoring.

Summary of the invention

First technical problem to be solved by this invention is to provide a kind of high-performance directional heat conduction copper-base diamond composite material that can realize the directed heat conduction of high-performance.

Second technical problem to be solved by this invention provides a kind of preparation method who realizes this high-performance directional heat conduction copper-base diamond composite material.

For solving above-mentioned first technical problem, high-performance directional heat conduction copper-base diamond composite material of the present invention, comprise the copper matrix, cocurrent and parallel is distributed with some diamond rods on described copper matrix, the diameter of described diamond rod is 0.5~10mm, and the spacing of described diamond rod is 0.5~50mm.

Described diamond rod adopts matrix to arrange.

The center of described diamond rod is axially arranged with linear core, and the diameter of described linear core is 0.1~30mm, and described linear core is selected thread or bar-shaped copper, tungsten, molybdenum or titanium.

In order to solve above-mentioned second technical problem, the preparation method of high-performance directional heat conduction copper-base diamond composite material provided by the invention, cocurrent and parallel is distributed with some diamond rods on the copper matrix, the diameter of diamond rod is 0.5~10mm, the spacing of diamond rod is 0.5~50mm, comprises the following steps:

(1), take thickness as 0.1~30mm copper coin as matrix, bore a series of column through holes that are parallel to each other on the copper matrix, through-hole diameter is 0.5~10mm;

(2), adopt chemical vapour deposition technique depositing high-quality diamond in the column through hole, make diamond fill all column through holes, form diamond rod array.

Before adopting the chemical vapour deposition diamond rod, the copper matrix is placed in the acetone suspension-turbid liquid of fine diamond powder, carry out the preliminary treatment of ultrasonic oscillation plantation seed crystal.

The preparation method of high-performance directional heat conduction copper-base diamond composite material provided by the invention, cocurrent and parallel is distributed with some diamond rods on the copper matrix, and the center of described diamond rod is axially arranged with linear core, comprises the following steps:

(1), the thread or bar-shaped copper take diameter as 0.1~30mm, tungsten, molybdenum or titanium material are as linear core, adopting chemical vapour deposition technique is the diamond film of 0.25~5mm at the continuous thickness of linear wicking surface growth, thereby obtains the cylindric core diamond rod that has;

(2), take thickness as 0.1~100mm copper coin as matrix, boring a series of spacings on the copper matrix is the parallel column through hole of 0.5~50mm, column through-hole diameter and diamond rod are complementary;

(3), diamond rod is inserted in the column through hole of copper matrix, and make copper matrix generation plastic deformation by extruding, thereby make copper contact coupling fully with the diamond rod.

Before adopting the chemical vapour deposition diamond rod, the copper matrix is placed in the acetone suspension-turbid liquid of fine diamond powder, carry out the preliminary treatment of ultrasonic oscillation plantation seed crystal.

The preparation method of high-performance directional heat conduction copper-base diamond composite material provided by the invention, cocurrent and parallel is distributed with some diamond rods on the copper matrix, and the center of described diamond rod is axially arranged with linear core, comprises the following steps:

(1), copper, tungsten, molybdenum or the titanium thread or bar-shaped take diameter as 0.1~30mm be as linear core, adopting chemical vapour deposition technique is the diamond film of 0.25~5mm at the continuous thickness of linear wicking surface growth, thereby obtains the cylindric core diamond rod that has;

(2), take thickness as 0.0001~1mm scale copper or Copper Foil as matrix, bore a series of parallel column through hole on the copper matrix, hole diameter and diamond rod are complementary;

(3), diamond rod is inserted in the column through hole of copper matrix, then by electro-deposition techniques at copper sheet along diamond rod direction deposited copper, make the complete cladding diamond rod of copper, contact coupling fully with diamond;

(4), the copper base diamond composite material is carried out homogenizing annealing heat treatment, the gas hole defect (heat treatment temperature is 300~900 ℃, and heat treatment time size is per sample determined) that elimination is inner.

Before adopting the chemical vapour deposition diamond rod, the copper matrix is placed in the acetone suspension-turbid liquid of fine diamond powder, carry out the preliminary treatment of ultrasonic oscillation plantation seed crystal.

Described employing electro-deposition techniques during along diamond rod direction deposited copper, adopts unidirectional deposited copper at copper sheet, or copper sheet is placed in diamond rod center, in copper sheet both sides along the two-way deposited copper of diamond rod direction.

Described chemical vapour deposition technique comprises all CVD methods, and for example, filament CVD, microwave plasma CVD technique, RF plasma CVD method, flame combustion CVD method, electron cyclotron accelerate resonance wave CVD, laser CVD method or direct current and spray the CVD method.

Adopt high-performance directional heat conduction copper-base diamond composite material of technique scheme and preparation method thereof, make this composite material have in the direction good directed heat conductivility by assembling in the same way some column diamond rod arrays with high heat conductance in the copper matrix, realize the directed heat conduction of high-performance, this composite material can be used as Electronic Packaging and heat sink material etc., solved the encapsulation problem of high temperature, high frequency, high-power electronic device.This composite material can realize that the directed heat conduction of high-performance is based on following characteristics: (1) diamond has the highest thermal conductivity in all known materials, is about 2200WK -1M -1(2) copper has the best thermal conductivity in the known metal material, is about 401WK -1M -1(3) some column diamond rod arrays with high heat conductance have been assembled in composite material; (4) diamond crystals in the diamond rod is fine and close continuously; (5) all diamond rods are arranged in parallel in the same direction.These characteristics make each root diamond rod become a quick conductive district, and heat is distributed rapidly along diamond column direction, and the joint effect of all diamond rods just makes this composite material have good directed heat conductivility.Copper has high-melting-point, low-resistance coefficient, good ductility and plasticity, easy machining, easy characteristics such as welding make the exploitation of this composite material can be used for that the high thermal conductance of high temperature, high frequency, high power semi-conductor electronic device, high electricity are led, the low-power consumption encapsulating material.

Description of drawings

Fig. 1 is that copper coin is at the schematic diagram that drills through array front and back, hole;

Fig. 2 is the schematic diagram of hot-wire chemical gas-phase deposition gained copper base diamond composite material;

Fig. 3 is the schematic diagram of the diamond SEM picture of hot-wire chemical gas-phase deposition gained copper base diamond composite material;

Fig. 4 is for adopting the hot-wire chemical gas-phase deposition technology at the schematic diagram of linear wicking surface depositing high-quality diamond rod; Fig. 4 label declaration: 1-gas cracking heated filament, 2-fixing support rack, 3-driven tooth wheels, 4-brace table, 5-gas feed device, the movable support of 6-, the linear matrix of 7-, 8-driving gear fixed mount, 9-driving gear and axle, 10-shaft coupling, 11-driving snake, 12-gas collector;

Fig. 5 is the structure chart that core diamond rod is arranged;

Fig. 6 is the surperficial SEM picture of diamond rod that core diamond rod is arranged;

Fig. 7 is the diamond rod section S EM picture that core diamond rod is arranged;

Fig. 8 is for adopting extrusion modling to prepare the assembling schematic diagram of copper base diamond composite material;

Fig. 9 is a kind of assembling mode that core diamond rod is arranged on copper sheet or Copper Foil;

Figure 10 is for adopting the unidirectional electrical deposition technique to prepare the schematic diagram of copper base diamond composite material;

Figure 11 is the another kind assembling mode that core diamond rod is arranged on copper sheet or Copper Foil;

Figure 12 is for adopting two-way electro-deposition techniques to prepare the schematic diagram of copper base diamond composite material.

Embodiment

The present invention will be described in detail below in conjunction with drawings and Examples.

Embodiment 1:

At first, with copper coin as copper matrix 13, as shown in Figure 1, bore a series of column through holes 14 that are parallel to each other on copper matrix 13, the spacing of column through hole 14 is 0.5~50mm, and wherein the thickness of copper matrix 13 is 0.1~30mm, and the diameter of column through hole 14 is 0.5~10mm; Then, adopt chemical vapour deposition technique depositing diamond rod 15 in the column through hole, make diamond fill all column through holes 14, form column diamond array, as shown in Figure 2, Fig. 3 is the schematic diagram of the diamond SEM picture of hot-wire chemical gas-phase deposition gained copper base diamond composite material.

With bortz powder acetone suspension-turbid liquid, sample is carried out ultrasonic wave and process 5~60min, clean sample surfaces and dry up with blower fan with acetone before carrying out chemical vapour deposition (CVD), and then adopt the hot-wire chemical gas-phase deposition technology to carry out the preparation of diamond thin.

Embodiment 2:

At first, as shown in Figure 4, with tungsten filament as linear core 16, adopt chemical vapour deposition technique at the continuous diamond film 17 of wicking surface growth, thereby obtain the cylindric core diamond rod 18 that has, the diameter of linear core 16 is 0~30mm, the thickness of diamond rod is 0.25~5mm, as shown in Figure 5, Fig. 6 is the surperficial SEM picture of diamond rod that core diamond rod is arranged, and Fig. 7 is the diamond rod section S EM picture that core diamond rod is arranged; Then, as copper matrix 13, bore a series of parallel column through hole 14 with copper coin on copper matrix 13, the spacing of column through hole 14 is 0.5~50mm, the diameter of column through hole 14 and cylindricly have core diamond rod 18 to be complementary, wherein the thickness of copper matrix 13 is 0.1~100mm; Then, have in the column through hole 14 that core diamond rod 18 is pressed into copper matrix 13 cylindric, and make copper matrix generation plastic deformation by extruding, thereby make copper contact coupling fully with the diamond rod, as shown in Figure 8.

With bortz powder acetone suspension-turbid liquid, sample is carried out ultrasonic wave and process 5~60min, clean sample surfaces and dry up with blower fan with acetone before carrying out chemical vapour deposition (CVD), and then adopt the hot-wire chemical gas-phase deposition technology to carry out the preparation of diamond thin.

Embodiment 3:

At first, as shown in Figure 4, with thread or bar-shaped copper, tungsten, molybdenum or titanium as linear core 16, adopt chemical vapour deposition technique at the continuous diamond film 17 of wicking surface growth, thereby obtain the cylindric core diamond rod 18 that has, the diameter of linear core 16 is 0.1~30mm, and the thickness of diamond film is 0.25~5mm, as shown in Figure 5; Then, as matrix, bore a series of parallel column through hole with scale copper 19 on matrix, hole diameter and cylindricly have core diamond rod 18 to be complementary, wherein scale copper 19 thickness are 0.0001~1mm; Then, as shown in Figure 9, have in the column through hole that core diamond rod 18 is pressed into scale copper 19 cylindric, cylindric have core diamond rod 18 1 ends concordant with scale copper 19, the other end exceeds scale copper 19, then by electro-deposition techniques at copper sheet along diamond rod direction unidirectional electrical deposited copper, make copper coat the cylindric core diamond rod 18 that has fully, contact coupling fully with diamond, as shown in figure 10; At last, the copper base diamond composite material is carried out homogenizing annealing heat treatment, eliminate the inner defectives such as pore.

As shown in figure 11, have in the column through hole that core diamond rod 18 is pressed into scale copper 19 cylindric, cylindric have core diamond rod 18 two ends all to exceed scale copper 19, be that scale copper 19 is placed in cylindric core diamond rod 18 centers of having, as shown in figure 12, along cylindric the core diamond rod 18 two-way deposited coppers of direction are arranged in scale copper 19 both sides.

With bortz powder acetone suspension-turbid liquid, sample is carried out ultrasonic wave and process 5~60min, clean sample surfaces and dry up with blower fan with acetone before carrying out chemical vapour deposition (CVD), and then adopt the hot-wire chemical gas-phase deposition technology to carry out the preparation of diamond thin.

Claims (4)

1. the preparation method of a high-performance directional heat conduction copper-base diamond composite material, cocurrent and parallel is distributed with some diamond rods on the copper matrix, the diameter of diamond rod is 0.5~10 mm, and the spacing of diamond rod is 0.5~50 mm, it is characterized in that: comprise the following steps:
(1), take thickness as 0.1~30mm copper coin as matrix, bore a series of column through holes that are parallel to each other on the copper matrix, through-hole diameter is 0.5~10 mm;
(2), before adopting the chemical vapour deposition diamond rod, the copper matrix is placed in the acetone suspension-turbid liquid of fine diamond powder, carry out the preliminary treatment of ultrasonic oscillation plantation seed crystal, adopt chemical vapour deposition technique depositing high-quality diamond in the column through hole, make diamond fill all column through holes, form diamond rod array.
2. the preparation method of a high-performance directional heat conduction copper-base diamond composite material, cocurrent and parallel is distributed with some diamonds rods on the copper matrix, and the center of described diamond rod is axially arranged with linear core, it is characterized in that: comprise the following steps:
(1), the thread or bar-shaped copper take diameter as 0.1~30 mm, tungsten, molybdenum or titanium material are as linear core, before adopting the chemical vapour deposition diamond rod, the copper matrix is placed in the acetone suspension-turbid liquid of fine diamond powder, carry out the preliminary treatment of ultrasonic oscillation plantation seed crystal, adopting chemical vapour deposition technique is the diamond film of 0.25~5mm at the continuous thickness of linear wicking surface growth, thereby obtains the cylindric core diamond rod that has;
(2), take thickness as 0.1~100mm copper coin as matrix, boring a series of spacings on the copper matrix is the parallel column through hole of 0.5~50 mm, column through-hole diameter and diamond rod are complementary;
(3), diamond rod is inserted in the column through hole of copper matrix, and make copper matrix generation plastic deformation by extruding, thereby make copper contact coupling fully with the diamond rod.
3. the preparation method of a high-performance directional heat conduction copper-base diamond composite material, cocurrent and parallel is distributed with some diamonds rods on the copper matrix, and the center of described diamond rod is axially arranged with linear core, it is characterized in that: comprise the following steps:
(1), take diameter as the thread or bar-shaped copper of 0.1~30 mm, tungsten, molybdenum or titanium as linear core, before adopting the chemical vapour deposition diamond rod, the copper matrix is placed in the acetone suspension-turbid liquid of fine diamond powder, carry out the preliminary treatment of ultrasonic oscillation plantation seed crystal, adopting chemical vapour deposition technique is the diamond film of 0.25~5mm at the continuous thickness of linear wicking surface growth, thereby obtains the cylindric core diamond rod that has;
(2), take thickness as 0.0001~1mm scale copper or Copper Foil as matrix, bore a series of parallel column through hole on the copper matrix, hole diameter and diamond rod are complementary;
(3), diamond rod is inserted in the column through hole of copper matrix, then by electro-deposition techniques at copper sheet along diamond rod direction deposited copper, make the complete cladding diamond rod of copper, contact coupling fully with diamond;
(4), the copper base diamond composite material is carried out homogenizing annealing heat treatment, eliminate inner gas hole defect, wherein heat treatment temperature is 300~900 ℃, and heat treatment time size is per sample determined.
4. the preparation method of directional heat conduction copper-base diamond composite material as claimed in claim 3, it is characterized in that: described employing electro-deposition techniques is at copper sheet during along diamond rod direction deposited copper, adopt unidirectional deposited copper, or copper sheet is placed in diamond rod center, in copper sheet both sides along the two-way deposited copper of diamond rod direction.
CN 201110169998 2011-06-22 2011-06-22 High-performance directional heat conduction copper-base diamond composite material and preparation method thereof CN102244051B (en)

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US20090269521A1 (en) * 2008-04-24 2009-10-29 3M Innovative Properties Company Porous structured thermal transfer article
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CN201587973U (en) * 2009-12-28 2010-09-22 北京有色金属研究总院 Integrated device for preparing copper-based composite material with high thermal conductivity

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