CN103276265A - Method for preparing free-standing diamond film-diamond particles-metallic composite material - Google Patents
Method for preparing free-standing diamond film-diamond particles-metallic composite material Download PDFInfo
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Abstract
The invention provides a method for preparing a free-standing diamond film-diamond particles-metallic composite material. The method comprises the steps as follows: firstly, a free-standing diamond film is subjected to laser cutting for forming, and surfaces of diamond particles and free-standing diamond film strips are plated with metal transition layers; then copper powder and the diamond particles are mixed uniformly, in a die which is in a shape of a required radiator, the free-standing diamond film strips are regularly embedded into a mixed material of the copper powder and the diamond particles, and then hot press molding and surface processing are performed; and the composite material is obtained. The method provided by the invention has the main advantages that heat conductivity in a direction of the free-standing diamond film strips is increased remarkably; and meanwhile, by virtue of the metal transition layers on the surfaces of the diamond particles and the free-standing diamond film strips, after sintering, wettability between the diamond particles, the free-standing diamond film strips and copper is improved, interface resistance between copper and the diamond particles and the free-standing diamond film strips is reduced, and the strength of the composite material is improved.
Description
Technical field
The invention belongs to dissipation from electronic devices body technical field of material.A kind of diamond self-supported membrane-diamond particles-metal composite and preparation method thereof particularly is provided.
Background technology
The heat diffusion capabilities of electron device has become the restraining factors of development of electronic devices, as big integrated circuit (IC) chip, High-Power Microwave devices etc., it is integrated with many electronic unit height of high power density device and aerospacecraft to have influence on communications satellite especially, and the miniaturization of electron device.Therefore, the high heat conduction of development of new, low-density novel material become the problem that presses for solution.
Diamond is heat conductivility best material in the nature all material, have the 2000W/mk thermal conductivity, and copper is heat conductivility excellent material in the metal, and the investigator has carried out broad research and exploitation to diamond-copper composite material both at home and abroad.The Lawrence Livermore National Laboratory of the U.S. and Sun Microsystems company have developed diamond-copper composite material as far back as nineteen ninety-five, are referred to as Dymalloy, and the matrix material thermal conductivity of preparation reaches 420W/mk.Japan Sumitomo Electric company adopts the high-pressure sinter technology to prepare DMCH(Diamond Metal Composite Heatsink by name) as heat sink diamond-copper composite material, have the thermal conductivity of 600 W/mk.Domestic, the matrix material of also having carried out diamond and metal is used for the research of thermally conductive material, and as practical new patent, 200920089841.9 1 kinds of radiating elements that adopt the heat radiation of large-particle monocrystal diamond heat sink material are embedded in diamond particles on the copper coin.Other researchs comprise that the metal of use has copper, aluminium, silver etc., utilize methods such as hot pressing, sintering, infiltration with diamond particles and metal forming processing, and the highest thermal conductivity reaches 570 W/mk.Its common characteristic is modification to be carried out on the diamond particles surface handle, and uses diamond particles and carcass material to carry out composite molding.Simultaneously because the size of diamond particles is less, thermal conductivity further improves is subjected to very big restriction.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of diamond self-supported membrane-diamond particles-metal composite of directed super-high heat-conductive, satisfy high-performance HIGH-POWERED MICROWAVES power device, the radiator of height integrated-optic device and high heat conduction, the properties of low density requirement of electronic package material.
The preparation method of the diamond self-supported membrane-diamond particles-metal composite of a kind of directed super-high heat-conductive of the present invention, at first diamond self-supported membrane laser cutting is shaped, to diamond particles and diamond self-supported membrane bar coating surface intermediate metal, copper powder and diamond particles mixed thereafter, in the mould of required radiator shape, diamond self-supported membrane bar rule is buried in the batch mixing of putting copper powder and diamond particles, carry out hot-forming and surface working then.Specifically may further comprise the steps:
1) shaping of diamond self-supported membrane bar: the CVD diamond self-supported membrane that DC arc plasma CVD, microwave plasma CVD or heated filament CVD technology is prepared diameter 60 ~ 300mm, thickness 0.2 ~ 3mm, form with laser cutting then, its length, width and shape can be decided according to the shape of radiator, can be arc, " I " shape, " L " shape, "T"-shaped or " worker " shape, as shown in Figure 1.The thermal conductivity of described diamond self-supported membrane bar is at 1200-2000W/(mK);
2) diamond particles and the surface treatment of diamond self-supported membrane bar: use the combination of magnetron sputtering, arc ion plating or filtered arc method plating any one or they in the material that titanium, tungsten, molybdenum, niobium, tantalum or the chromium on diamond particles and diamond self-supported membrane bar surface are formed, the thickness of coating layer is 0.1-2 μ m;
3) batch mixing: be that raw material mixes and forms the carcass material with copper powder and diamond particles, the size range 30-150 μ m of selected copper powder, the particle size range 1-150 μ m of diamond particles, the content of diamond particles in carcass is 5-65% by mass, copper powder and diamond particles are packed in the urethane abrasive can, mix in the three-dimensional blender machine, mixing time is 0.5-4 hour;
4) diamond self-supported membrane bar is placed: earlier the mixing carcass material of part copper powder and diamond particles is packed in the hot pressing graphite jig of required radiator shape, the height that mixes the carcass material is 1/3 of mold height, then diamond self-supported membrane bar rule is inserted and placed, the mixing carcass material with copper powder and diamond particles fills up again;
5) hot pressed sintering: the hot pressing graphite jig that rule is placed with the mixing carcass material of diamond self-supported membrane bar and copper powder and diamond particles is placed in the vacuum heating-press sintering stove, sintering temperature 500-950 ℃, pressing pressure 5-35MPa, sintering time 0.5-3 hour;
6) materials processing: the cutting of employing line is polished again or direct polishing process is processed into desired shape and size with hot-pressed and sintered product.
Diamond self-supported membrane-diamond particles-the metal composite that makes by preparation method provided by the invention is to be that the compound that metallic matrix and diamond particles form is carcass by copper, the diamond self-supported membrane bar that is distributed in the different shape in the carcass is that heat conduction strengthens body, and the intermediate metal that improves copper and diamond particles and diamond self-supported membrane bar interface bonding state constitutes, the size range 30-150 μ m of selected copper powder, the particle size range 1-150 μ m of diamond particles, the content of diamond particles in carcass is 5-65% by mass, described diamond self-supported membrane bar thickness is 0.2-3mm, thermal conductivity is at 1200-2000W/(mK), described intermediate metal is that plating is in the titanium on diamond particles and diamond self-supported membrane bar surface, tungsten, molybdenum, niobium, in the material that tantalum or chromium are formed any one or their combination.
Copper matrix among the present invention is the supporter of described matrix material, is Application Areas basic material commonly used in the various radiator materials, has high thermal conductivity 398W/(mK).
The diamond particles that adds among the present invention plays the effect that improves the matrix material thermal conductivity, reduces thermal expansivity, improves intensity, and its consumption in carcass is 5-65% in mass, and selected particle size range is 1-150 μ m.The thermal conductivity of single-crystal diamond can reach 2000W/(mK), thermal expansivity at room temperature is 1.0 * 10
-6/ ℃.
The diamond self-supported membrane bar that adds among the present invention is the main body that improves matrix material directional heat conductance, diamond self-supported membrane bar uses DC arc plasma CVD, microwave plasma CVD or heated filament CVD technology to prepare the CVD diamond self-supported membrane of diameter 60 ~ 300mm, thickness 0.2 ~ 3mm, form with laser cutting then, its length and shape can be decided according to the shape of radiator, can be the rectangular of arc, " I " shape, " L " shape, "T"-shaped and " worker " shape, as shown in Figure 1.The thermal conductivity scope of described diamond self-supported membrane bar is at 1200-2000W/(mK).
Intermediate metal described in the present invention is for using the combination of magnetron sputtering, arc ions degree or filtered arc method plating any one or they in the material that titanium, tungsten, molybdenum, niobium, tantalum or the chromium on diamond particles and diamond self-supported membrane bar surface are formed, play in the present invention the effect that improves copper and diamond particles and diamond self-supported membrane bar interface resistance, raising composite material strength.In the Composite Preparation process, these elements can react with the interface of diamond particles and diamond self-supported membrane bar, form corresponding carbide, improve the density of matrix material, reduce voidage, improve the effect of interface bond strength.
The method of diamond particles and diamond self-supported membrane surface metal transition layer plating can be magnetron sputtering, arc ions degree, filtered arc method or their arbitrary combination, the thickness of coating layer is 0.1-2 μ m, and blocked up intermediate metal will increase the thermal resistance at interface.
Major advantage of the present invention is that the diamond self-supported membrane bar of high heat conduction can effectively improve the thermal conductivity of diamond-copper based composites, particularly the direction thermal conductivity at diamond self-supported membrane bar increases significantly, the intermediate metal on while diamond particles and diamond self-supported membrane bar surface, by having improved the wetting property of diamond particles and diamond self-supported membrane bar and copper behind the sintering, reduce the interface resistance between copper and diamond particles and the diamond self-supported membrane bar, improve the intensity of matrix material.
Description of drawings
Fig. 1 is the shape synoptic diagram of diamond self-supported membrane bar.
Embodiment:
The present invention is described in detail below by embodiment,
The diamond self-supported membrane bar that adds among the present invention is the main body that improves matrix material directional heat conductance, diamond self-supported membrane bar uses DC arc plasma CVD, microwave plasma CVD or heated filament CVD technology to prepare the CVD diamond self-supported membrane of diameter 60 ~ 300mm, thickness 0.2 ~ 3mm, form with laser cutting then, its length and shape can be decided according to the shape of radiator, can be the rectangular of arc, " I " shape, " L " shape, "T"-shaped and " worker " shape, as shown in Figure 1.The thermal conductivity scope of described diamond self-supported membrane bar is at 1200-2000W/(mK).
Embodiment 1
(1) DC arc plasma CVD is prepared the CVD diamond self-supported membrane of diameter 100mm, thickness 0.8mm, with " I " shape bar that is laser-cut into length 3 mm, width 1 mm, diamond self-supported membrane bar in the thermal conductivity of length and width at 1940W/(mK), in the thermal conductivity of thickness direction at 1764W/(mK);
(2) the titanium thickness in diamond particles and diamond self-supported membrane bar surface is 1.2 μ m with granularity 50 μ m diamond particles and diamond self-supported membrane bar using electric arc ion plating plating;
(3) be that raw material mixes formation carcass material with diamond particles behind copper powder and the plating, the particle diameter of selected copper powder is 80 μ m, the content of diamond particles in carcass is 55% by mass, copper powder and diamond particles are packed in the urethane abrasive can, mix in the three-dimensional blender machine, mixing time is 3 hours;
(4) earlier the mixing carcass material of diamond particles behind part copper powder and the plating is packed in the hot pressing graphite jig, the height that mixes the carcass material is 1/3 of mold height, then the rule insertion along its length of diamond self-supported membrane bar behind the plating is placed, area occupied is 18% of die area, and the mixing carcass material with diamond particles behind copper powder and the plating fills up again;
(5) rule is placed with behind the plating that the hot pressing graphite jig of the mixing carcass material of diamond particles is placed in the vacuum heating-press sintering stove 850 ℃ of sintering temperatures, pressing pressure 30MPa, sintering time 2 hours behind the diamond self-supported membrane bar and copper powder and plating;
(6) adopt direct polishing process with formed sample surfaces and side polishing, the sample thickness direction is the length direction of diamond strips, and the average conduction that records the thickness of sample direction surpasses 900W/(mK).
Embodiment 2
(1) DC arc plasma CVD is prepared the CVD diamond self-supported membrane of diameter 60mm, thickness 1mm, with " I " shape bar that is laser-cut into length 3 mm, width 1 mm, diamond self-supported membrane bar in the thermal conductivity of length and width at 1900W/(mK), in the thermal conductivity of thickness direction at 1720W/(mK);
(2) the titanium thickness in diamond particles and diamond self-supported membrane bar surface is 1.5 μ m with granularity 80 μ m diamond particles and diamond self-supported membrane bar using electric arc ion plating plating;
(3) selecting behind the particle diameter 40 μ m of copper powder and the plating diamond particles for use is that raw material mixes and forms the carcass material, the content of diamond particles in carcass is 50% by mass, copper powder and diamond particles are packed in the urethane abrasive can, mix in the three-dimensional blender machine, mixing time is 2.5 hours;
(4) earlier partially mixed carcass material is packed in the hot pressing graphite jig, the height that mixes the carcass material is 1/3 of mold height, then the rule insertion along its length of diamond self-supported membrane bar behind the plating is placed, area occupied is 15% of die area, and the mixing carcass material with diamond particles behind copper powder and the plating fills up again;
(5) rule is placed with behind the plating that the hot pressing graphite jig of the mixing carcass material of diamond particles is placed in the vacuum heating-press sintering stove 800 ℃ of sintering temperatures, pressing pressure 25MPa, sintering time 2.5 hours behind the diamond self-supported membrane bar and copper powder and plating;
(6) adopt direct polishing process with formed sample surfaces and side polishing, the sample thickness direction is the length direction of diamond strips, cuts into the specimen size, and the average conduction that records the thickness of sample direction surpasses 850W/(mK).
Embodiment 3
(1) DC arc plasma CVD is prepared the CVD diamond self-supported membrane of diameter 60mm, thickness 0.6mm, with " I " shape bar that is laser-cut into length 3 mm, width 1 mm, diamond self-supported membrane bar in the thermal conductivity of length and width at 2060W/(mK), in the thermal conductivity of thickness direction at 1840W/(mK);
(2) the titanium thickness in diamond particles and diamond self-supported membrane bar surface is 1.0 μ m with granularity 60 μ m diamond particles and diamond self-supported membrane bar using electric arc ion plating plating;
(3) selecting behind the particle diameter 40 μ m of copper powder and the plating diamond particles for use is that raw material mixes and forms the carcass material, the content of diamond particles in carcass is 45% by mass, copper powder and diamond particles are packed in the urethane abrasive can, mix in the three-dimensional blender machine, mixing time is 2.0 hours;
(4) earlier partially mixed carcass material is packed in the hot pressing graphite jig, the height that mixes the carcass material is 1/3 of mold height, then the rule insertion along its length of diamond self-supported membrane bar behind the plating is placed, area occupied is 16% of die area, and the mixing carcass material with diamond particles behind copper powder and the plating fills up again;
(5) rule is placed with behind the plating that the hot pressing graphite jig of the mixing carcass material of diamond particles is placed in the vacuum heating-press sintering stove 750 ℃ of sintering temperatures, pressing pressure 27MPa, sintering time 2 hours behind the diamond self-supported membrane bar and copper powder and plating;
(6) adopt direct polishing process with formed sample surfaces and side polishing, the sample thickness direction is the length direction of diamond strips, cuts into the specimen size, and the average conduction that records the thickness of sample direction surpasses 800W/(mK).
Above embodiment just meets several examples of the technology of the present invention content, does not illustrate that the present invention only limits to the described content of following example, and the technician in the industry all belongs to content of the present invention according to the product of claim item of the present invention manufacturing.
Claims (5)
1. the preparation method of diamond self-supported membrane-diamond particles-metal composite, it is characterized in that: the preparation method of described diamond self-supported membrane-diamond particles-metal composite at first is shaped diamond self-supported membrane laser cutting, to diamond particles and diamond self-supported membrane bar coating surface intermediate metal, copper powder and diamond particles mixed thereafter, in the mould of required radiator shape, diamond self-supported membrane bar rule is buried in the batch mixing of putting copper powder and diamond particles, carry out hot-forming and surface working then; Specifically may further comprise the steps:
1) shaping of diamond self-supported membrane bar: will be with the CVD diamond self-supported membrane of diameter 60 ~ 300mm, the thickness 0.2 ~ 3mm of DC arc plasma CVD, microwave plasma CVD or the preparation of heated filament CVD technology, form with laser cutting then, its length, width and shape can be decided according to the shape of radiator, and the thermal conductivity of described diamond self-supported membrane bar is at 1200-2000W/(mK);
2) diamond particles and the surface treatment of diamond self-supported membrane bar: use the combination of magnetron sputtering, arc ions degree or filtered arc method plating any one or they in the material that titanium, tungsten, molybdenum, niobium, tantalum or the chromium on diamond particles and diamond self-supported membrane bar surface are formed, the thickness of coating layer is 0.1-2 μ m;
3) batch mixing: be that raw material mixes and forms the carcass material with copper powder and diamond particles, the size range 30-150 μ m of selected copper powder, the particle size range 1-150 μ m of diamond particles, the content of diamond particles in carcass is 5-65% by mass, copper powder and diamond particles are packed in the urethane abrasive can, mix in the three-dimensional blender machine, mixing time is 0.5-4 hour;
4) diamond self-supported membrane bar is placed: earlier in the hot pressing graphite jig of the radiator shape of packing into the mixing carcass material of part copper powder and diamond particles required, the height that mixes the carcass material is 1/3 of mold height, then diamond self-supported membrane bar rule is inserted and placed, the mixing carcass material with copper powder and diamond particles fills up again;
5) hot pressed sintering: the hot pressing graphite jig that rule is placed with the mixing carcass material of diamond self-supported membrane bar and copper powder and diamond particles is placed in the vacuum heating-press sintering stove, sintering temperature 500-950 ℃, pressing pressure 5-35MPa, sintering time 0.5-3 hour;
6) materials processing: the cutting of employing line is polished again or direct polishing process is processed into desired shape and size with hot-pressed and sintered product.
2. the preparation method of the diamond self-supported membrane-diamond particles-metal composite of directed super-high heat-conductive according to claim 1, it is characterized in that: described diamond self-supported membrane bar is arc, " I " shape, " L " shape, "T"-shaped or " worker " shape.
3. the preparation method of diamond self-supported membrane-diamond particles according to claim 1-metal composite, it is characterized in that: the described diamond self-supported membrane bar of preparing is the main body that improves matrix material directional heat conductance, diamond self-supported membrane bar uses DC arc plasma CVD, microwave plasma CVD or heated filament CVD technology prepare diameter 60 ~ 300mm, the CVD diamond self-supported membrane of thickness 0.2 ~ 3mm, form with laser cutting then, its length and shape can be decided according to the shape of radiator, can be arcs, " I " shape, " L " shape, "T"-shaped and " worker " shape rectangular.
4. the preparation method of diamond self-supported membrane-diamond particles according to claim 3-metal composite, it is characterized in that: the method for described diamond particles and diamond self-supported membrane surface metal transition layer plating is magnetron sputtering, arc ions degree, filtered arc method or their arbitrary combination, and the thickness of coating layer is 0.1-2 μ m.
5. the preparation method of diamond self-supported membrane-diamond particles according to claim 3-metal composite, it is characterized in that: described matrix material is to be that the compound that metallic matrix and diamond particles form is carcass by copper, the diamond self-supported membrane bar that is distributed in the different shape in the carcass is that heat conduction strengthens body, and the intermediate metal that improves copper and diamond particles and diamond self-supported membrane bar interface bonding state constitutes, the size range 30-150 μ m of selected copper powder, the particle size range 1-150 μ m of diamond particles, the content of diamond particles in carcass is 5-65% by mass, described diamond self-supported membrane bar thickness is 0.2-3mm, thermal conductivity is at 1200-2000W/(mK), described intermediate metal is that plating is in the titanium on diamond particles and diamond self-supported membrane bar surface, tungsten, molybdenum, niobium, in the material that tantalum or chromium are formed any one or their combination.
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| CN105220049A (en) * | 2015-10-12 | 2016-01-06 | 中南大学 | A kind of sheet diamond reinforced metal-base composite material and preparation method |
| CN105695831A (en) * | 2016-03-21 | 2016-06-22 | 中南大学 | Superhigh-thermal-conductivity continuous diamond skeleton reinforced composite material and preparation method |
| CN107419133A (en) * | 2017-05-12 | 2017-12-01 | 南通鑫祥锌业有限公司 | High-volume fractional diamond zinc composite |
| CN107649688A (en) * | 2017-08-21 | 2018-02-02 | 武汉速博酷新材料科技有限公司 | A kind of diamond heat-conducting composite of easy processing and its preparation method and application |
| CN107873063A (en) * | 2015-04-16 | 2018-04-03 | Ii-Vi有限公司 | The thin diamond base material of Optical finishing or window and its manufacture method of high length-diameter ratio |
| CN109128192A (en) * | 2017-06-28 | 2019-01-04 | 深圳先进技术研究院 | Composite polycrystal-diamond and preparation method thereof |
| CN110193600A (en) * | 2019-05-09 | 2019-09-03 | 西安交通大学 | A kind of preparation method of titanium carbide enhancing titanium coated graphite powder |
| CN110394521A (en) * | 2019-08-02 | 2019-11-01 | 太原理工大学 | Diamond film high efficiency and heat radiation material and preparation method thereof |
| CN113146158A (en) * | 2021-01-27 | 2021-07-23 | 北京科技大学 | Preparation method of open type full-diamond heat dissipation structure |
| CN113458395A (en) * | 2021-07-05 | 2021-10-01 | 荣成高时新材料技术有限公司 | Preparation process of diamond tool formed by microwave heating |
| CN114540765A (en) * | 2020-11-25 | 2022-05-27 | 有研工程技术研究院有限公司 | Diamond/copper composite material heat sink coated with metal titanium-copper layer and preparation method thereof |
| CN117020209A (en) * | 2023-10-09 | 2023-11-10 | 赣州金顺科技有限公司 | Heat dissipation substrate and preparation method thereof |
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| CN107873063A (en) * | 2015-04-16 | 2018-04-03 | Ii-Vi有限公司 | The thin diamond base material of Optical finishing or window and its manufacture method of high length-diameter ratio |
| CN105220049A (en) * | 2015-10-12 | 2016-01-06 | 中南大学 | A kind of sheet diamond reinforced metal-base composite material and preparation method |
| CN105220049B (en) * | 2015-10-12 | 2017-03-08 | 中南大学 | A kind of lamellar diamond reinforced metal-base composite material and preparation method |
| CN105695831A (en) * | 2016-03-21 | 2016-06-22 | 中南大学 | Superhigh-thermal-conductivity continuous diamond skeleton reinforced composite material and preparation method |
| CN107419133A (en) * | 2017-05-12 | 2017-12-01 | 南通鑫祥锌业有限公司 | High-volume fractional diamond zinc composite |
| CN109128192A (en) * | 2017-06-28 | 2019-01-04 | 深圳先进技术研究院 | Composite polycrystal-diamond and preparation method thereof |
| CN107649688A (en) * | 2017-08-21 | 2018-02-02 | 武汉速博酷新材料科技有限公司 | A kind of diamond heat-conducting composite of easy processing and its preparation method and application |
| CN110193600B (en) * | 2019-05-09 | 2021-10-08 | 西安交通大学 | Preparation method of titanium carbide reinforced titanium-coated graphite powder |
| CN110193600A (en) * | 2019-05-09 | 2019-09-03 | 西安交通大学 | A kind of preparation method of titanium carbide enhancing titanium coated graphite powder |
| CN110394521A (en) * | 2019-08-02 | 2019-11-01 | 太原理工大学 | Diamond film high efficiency and heat radiation material and preparation method thereof |
| CN110394521B (en) * | 2019-08-02 | 2021-03-23 | 太原理工大学 | Diamond film high-efficiency heat dissipation material and preparation method thereof |
| CN114540765A (en) * | 2020-11-25 | 2022-05-27 | 有研工程技术研究院有限公司 | Diamond/copper composite material heat sink coated with metal titanium-copper layer and preparation method thereof |
| CN113146158A (en) * | 2021-01-27 | 2021-07-23 | 北京科技大学 | Preparation method of open type full-diamond heat dissipation structure |
| CN113458395A (en) * | 2021-07-05 | 2021-10-01 | 荣成高时新材料技术有限公司 | Preparation process of diamond tool formed by microwave heating |
| CN117020209A (en) * | 2023-10-09 | 2023-11-10 | 赣州金顺科技有限公司 | Heat dissipation substrate and preparation method thereof |
| CN117020209B (en) * | 2023-10-09 | 2024-01-26 | 赣州金顺科技有限公司 | Heat dissipation substrate and preparation method thereof |
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