WO2022210298A1 - 黒鉛-銅複合材料、それを用いたヒートシンク部材、および黒鉛-銅複合材料の製造方法 - Google Patents
黒鉛-銅複合材料、それを用いたヒートシンク部材、および黒鉛-銅複合材料の製造方法 Download PDFInfo
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- graphite
- composite material
- copper
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- 239000002131 composite material Substances 0.000 title claims abstract description 84
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 73
- 239000010949 copper Substances 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000002245 particle Substances 0.000 claims abstract description 120
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 103
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 100
- 239000010439 graphite Substances 0.000 claims abstract description 100
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000005259 measurement Methods 0.000 claims abstract description 15
- 230000006866 deterioration Effects 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 20
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- 230000000052 comparative effect Effects 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 18
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- 241001424392 Lucia limbaria Species 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/004—Filling molds with powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0425—Copper-based alloys
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/72—Investigating presence of flaws
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3736—Metallic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4871—Bases, plates or heatsinks
Definitions
- the present invention relates to a graphite-copper composite material, a heat sink member using the same, and a method for producing the graphite-copper composite material.
- High thermal conductivity is required for materials for heat dissipation parts of semiconductor equipment.
- copper has a high thermal conductivity, it also has a high coefficient of thermal expansion.
- a metal-graphite composite material has been proposed as a composite material that can be obtained at low cost by reducing the coefficient of thermal expansion without impairing the high thermal conductivity of copper (see, for example, Patent Document 1).
- the metal-graphite composite material of Patent Document 1 is disclosed to have high cooling reliability and a low coefficient of linear expansion.
- an object of the present invention is to provide a graphite-copper composite material in which thermal deterioration after temperature cycling is suppressed, a heat sink member using the same, and a method for producing the graphite-copper composite material.
- the present invention provides a graphite-copper composite material containing a copper layer and scale graphite particles laminated via the copper layer, and having a copper volume fraction of 3 to 30%, wherein, in the laminated cross section, A graphite-copper composite material characterized in that the number of intraparticle gaps N obtained by the following (1a) to (1c) is 5 or less.
- (1a) Defining five measurement fields of 930 ⁇ m ⁇ 1230 ⁇ m in the lamination section.
- the number of gaps having a width of 2 to 5 ⁇ m in the scale-like graphite particles is counted as N 1 to N 5 .
- (1c) Calculate the average value of the number of gaps ((N 1 +N 2 +N 3 +N 4 +N 5 )/5) to obtain the number N of gaps in the particle.
- the present invention also provides a heat sink member using the aforementioned graphite-copper composite material.
- the present invention provides a method for producing the above-described graphite-copper composite material, wherein graphite particles are inserted between a pair of grindstones arranged above and below, and the upper grindstone is rotated at 12 Hz or less to produce graphite particles.
- a step of obtaining scaly graphite particles by subjecting to a pretreatment a step of mixing the scaly graphite particles and the copper particles to obtain a molding raw material, and a molding obtained by molding the molding raw material into a large number of and a step of sintering by an axial current sintering method.
- the present invention it is possible to provide a graphite-copper composite material in which thermal deterioration after temperature cycling is suppressed, a heat sink member using the same, and a method for producing the graphite-copper composite material.
- FIG. 3 shows the measurement field defined in the SEM image of the laminated cross-section of the graphite-copper composite.
- FIG. 4 is a diagram for explaining gaps in flake graphite particles; It is a figure explaining the pretreatment method of a graphite particle. It is a schematic diagram explaining a multi-axis electric current sintering apparatus. It is the schematic explaining a cooling board
- the graphite-copper composite material of the present invention (hereinafter also simply referred to as a composite material) is a sintered body obtained using flake graphite particles and copper particles as raw materials.
- the scale-like graphite particles are laminated via a copper layer.
- "through the copper layer” means that the scale-like graphite particles are connected by the adjacent copper layer. That is, the flake graphite particles in the composite material are electrically continuous.
- the thickness of the copper layer in the composite material is not particularly limited, it is generally about 3 to 25 ⁇ m.
- the volume fraction of copper in the composite material is 3-30%.
- the thermal conductivity of the composite material of the present invention is very high due to the high content of graphite with high thermal conductivity of 70-97%. Copper acts as a binder in the composite.
- the volume ratio of graphite to copper (graphite:copper) in the composite material is preferably 70:30 to 97:3.
- the volume ratio (graphite:copper) is more preferably 84:16 to 95:5.
- the volume fraction of copper in the composite material can be adjusted by adjusting the mixing ratio of the raw materials during production.
- the number of intra-particle gaps N obtained by a predetermined method in the laminated cross section is 5 or less.
- the lamination cross section is a cross section in which the laminated scaly graphite particles are observed. This plane includes the direction in which the graphite particles are pressed.
- the longitudinal direction of the column corresponds to the direction in which the scale-like graphite particles are laminated.
- the intra-particle void number N can be obtained by the following (1a) to (1c).
- (1a) Defining five measurement fields of 930 ⁇ m ⁇ 1230 ⁇ m in the laminated cross-section of the composite.
- the measurement field of view can be arbitrarily defined in an SEM image obtained by observing the laminated cross section of the composite material with a scanning electron microscope (SEM) at a magnification of 100 times.
- SEM scanning electron microscope
- the number of gaps having a width of 2 to 5 ⁇ m in the scale-like graphite particles is counted as N 1 to N 5 .
- the width of the interstices within the flake graphite particles is defined as shown in FIG. That is, the gaps 16 in the scale-like graphite particles 12 are arbitrarily selected and adjusted so that the gaps 16 cross the screen.
- the maximum distance between the two sides L1 and L2 defining the upper and lower sides of the gap 16 is defined as the width w of the gap. This width w is measured by commercially available image processing software, and the number of gaps 16 having 2 to 5 ⁇ m is counted to obtain N 1 to N 5 . If necessary, the contrast of the SEM image is appropriately adjusted for observation.
- the number of intra-particle gaps N is defined to be 5 or less.
- the present inventors have found that the scale-like graphite particles having 5 or less intra-particle gaps have the effect of suppressing thermal deterioration of the composite material after temperature cycles.
- the number of intra-particle gaps N is preferably 5.0 or less, more preferably 3.5 or less, and particularly preferably 2.3 or less.
- the composite material of the present invention preferably has a thermal conductivity of 700 W/(m ⁇ K) or higher.
- the thermal conductivity is a value measured in a direction perpendicular to the direction in which the flake graphite particles are laminated.
- the thermal conductivity is more preferably 750 W/(m ⁇ K) or more.
- the thermal conductivity was measured by cutting out a sample of predetermined dimensions (outer diameter 10 mm x thickness 2.5 mm) from the central part of the composite material and using NETZSCH LFA447 in accordance with the laser flash method (JIS H 7801: 2005). An average of the thermal conductivity of five samples measured and cut from the composite is used.
- the composite material of the present invention preferably has a thermal deterioration rate of 10% or less obtained by the following (2a) to (2c).
- (2a) A sample is prepared by cutting a plate in the direction in which the flake graphite particles are laminated. A sample can be obtained by processing the plate to have an outer diameter of 10 mm and a thickness of 2.5 mm, for example.
- (2b) After determining the thermal diffusivity TD 0 of the sample, repeat the cycle of increasing and decreasing the temperature from -40°C to 220°C, and determine the thermal diffusivity TD 500 after 500 cycles.
- the thermal diffusivity can be obtained by LFA447 manufactured by NETZSCH in accordance with the laser flash method (JIS H 7801:2005).
- (2c) ((TD 0 -TD 500 )/TD 0 )) ⁇ 100) to obtain the thermal deterioration rate.
- the thermal deterioration rate is an index of the resistance of the composite material's thermal diffusivity, and the smaller the value, the better the properties. If the thermal deterioration rate is up to 10%, it can be said that the material is suppressed in thermal deterioration after the temperature cycle.
- the heat deterioration rate is more preferably 5% or less.
- the composite material of the present invention is produced by subjecting graphite particles to a predetermined pretreatment to obtain desired scale-like graphite particles, mixing them with copper particles to form a molding raw material, molding this material, and sintering it under predetermined conditions. be able to. Each step will be described below.
- Graphite pretreatment Pretreatment of the graphite particles is performed by applying stress to the graphite particles.
- Graphite particles inherently have internal voids due to the stresses applied during the manufacturing process.
- the present inventors have found that the number of gaps in graphite particles is involved in the thermal deterioration of composite materials containing graphite particles, and use flaky graphite particles obtained by performing a predetermined pretreatment. As a result, it is possible to suppress the thermal deterioration of the composite material after the temperature cycle.
- the whetstone 30b is a rotatable rotary whetstone.
- the grindstones 30a and 30b have metal plates 31a and 31b, respectively, and abrasive grains 33a and 33b such as diamond are provided on the opposing surfaces.
- the abrasive grains 33a and 33b are fixed by bonding metal members 32a and 32b such as plating, and the graphite particles 23 to be processed are arranged between the abrasive grains 33a and 33b.
- a stress is applied to the graphite particles 23 by rotating the emery wheel 30b at 12 Hz or less.
- a desired effect can be obtained if the rotating speed of the emery wheel 30b is 12 Hz or less.
- the number of rotations of the emery wheel 30b is preferably 10 Hz or less, more preferably 6 Hz or less.
- the conditions for the pretreatment of the graphite particles are not particularly specified as long as the rotating speed of the emery wheel 30b is specified to be 12 Hz or less.
- the pressure can be about 0.2 to 0.8 MPa and the time can be about 10 to 30 seconds.
- the copper particles are not particularly specified, and for example, copper particles having a volume-based median diameter of 1.5 ⁇ m or less can be used.
- the median diameter of the copper particles is preferably 1.0 ⁇ m or less.
- a composite material with stable thermal conductivity and workability can be obtained.
- Copper particles having a median diameter of 1.5 ⁇ m or less can be produced by any method. For example, desired copper particles can be obtained by a chemical reduction method or a physical manufacturing method.
- the scale-like graphite particles obtained by the pretreatment and the copper particles are blended in a predetermined ratio, and wet-mixed with an organic solvent to obtain a forming raw material.
- the mixing ratio of the raw materials is selected so that the volume ratio of graphite to copper (graphite:copper) in the composite material is 70:30 to 97:3.
- the volume ratio (graphite:copper) is preferably selected to be 84:16 to 95:5.
- Suitable organic solvents specifically include toluene and xylene.
- a small amount (approximately 40 g or less) of the molding raw material is filled into a predetermined mold, and compacted at a pressure of approximately 3 to 15 MPa using, for example, a hydraulic hand press.
- a mold for example, a SUS mold having a diameter of 30 mm can be used. Filling of the molding raw material and compaction are repeated to produce a compact of a desired size.
- the multi-axis electric sintering apparatus 40 shown in FIG. 4 has a carbon mold 44 containing a molded body, which is arranged in a vertical direction pressing shafts 45a, 45b, horizontal heating shafts (A) 47a, 47b and heating shafts.
- (B) 49a and 49b can be fixed in the vacuum container 42;
- the heating shafts (A) 47a, 47b and the heating shafts (B) 49a, 49b are configured to be alternately energized.
- the heating shaft (A) is energized in the directions of arrows x1 and x2, and the heating shaft (B) is energized in the directions of arrows y1 and y2.
- pressure shafts 45a, 45b and heating shafts 47a, 47b, 49a, 49b are separated. Specifically, the pressure axes 45a and 45b are in the z-axis direction, the heating axes (A) 47a and 47b are in the x-axis direction, and the heating axes (B) 49a and 49b are in the y-axis direction.
- the pressure inside the vacuum vessel 42 is 100 Pa or less, preferably 50 Pa or less in order to suppress oxidation deterioration of parts in the apparatus. Reduce the pressure to Next, first, the heating shafts (A) 47a and 47b are energized to heat to about 650 to 750.degree. C., preferably about 670 to 730.degree.
- the heating shafts (B) 49a and 49b are switched to heat to about 930 to 980°C, preferably about 940 to 970°C. Further, pressure is applied in the directions of arrows z1 and z2 by vertical pressing shafts 45a and 45b. The pressure at this time is preferably about 10 to 100 MPa, more preferably about 30 to 50 MPa.
- the composite material of the present invention Since it is sintered with a uniform temperature distribution by the multiaxial current sintering method, it is possible to manufacture a composite material with stable quality. Moreover, since scale-like graphite particles obtained by performing a predetermined pretreatment are used together with the copper particles as a raw material, the composite material of the present invention has an intra-particle gap obtained by a predetermined method in the cross section of the laminate. The number is 5 or less. When the number of intra-particle gaps is 5 or less, the composite material of the present invention is inhibited from thermal deterioration after temperature cycles and has a higher thermal conductivity.
- the composite material of the present invention can be suitably used as a radiator plate (heat sink member).
- Heat sink members are used in a wide range of fields such as wireless communication fields, electronic control fields, and optical communication fields. Specific applications include power semiconductor modules, optical communication modules, projectors, Peltier coolers, water coolers, and LED heat dissipation fans.
- Fig. 5 shows an example of a cooling board using a heat sink.
- the cooling substrate 55 includes a heat sink 50 and a cooling layer 54 .
- the heat sink 50 has an electrical insulation layer 52 and a wiring layer 51 that are sequentially laminated on a stress buffer layer 53 .
- a heat-generating element such as a semiconductor element is mounted on the mounting surface 51a of the upper surface of the wiring layer 51.
- the composite material of the present invention can be used for at least one of the stress buffer layer 53 and the wiring layer 51 .
- the heat generated by the exothermic elements mounted on the mounting surface 51a of the radiator plate 50 is conducted sequentially to the wiring layer 51, the electrical insulation layer 52, the stress buffer layer 53, and the cooling layer 54, and is dissipated from the cooling layer 54. . Since the composite material of the present invention is inhibited from thermal deterioration after temperature cycling, it can efficiently cool the exoergic element to lower the temperature, and exhibits its effect stably over a long period of time. .
- Example 1 Commercially available raw material graphite was pretreated by the method described with reference to FIG.
- the upper and lower whetstones were equipped with diamond as abrasive grains, and 5 g of graphite particles were inserted with 2 mL of water between them.
- the grindstone was rotated at 10 Hz to pre-treat the graphite particles for about 20 seconds.
- the pressure at that time was 0.5 MPa.
- the treated graphite particles were classified with a sieve having an opening of 500 ⁇ m, and the graphite particles remaining on the upper surface of the sieve were taken out and dried to obtain flake graphite particles as a raw material.
- copper particles having a median diameter of 1.5 ⁇ m were prepared as the copper particles.
- the molded body that was taken out was placed in a cylindrical carbon mold and sintered by a multiaxial electric current sintering method.
- a carbon mold 44 is placed in the vacuum vessel 42 of the multiaxial electric sintering apparatus 40 shown in FIG. B) Fixed with 45a and 45b.
- the pressure inside the vacuum vessel 42 was reduced to 5 Pa by a rotary pump, and the output of the device power supply was increased to raise the temperature. After heating up to 700° C. with the heating shafts (A) 47a and 47b by raising the temperature, heating was performed up to 950° C. with the heating shafts (B) 49a and 49b.
- Example 2 A composite material of Example 2 was produced in the same manner as in Example 1, except that the molding raw material was changed so that the volume fraction of copper after sintering was 16%.
- Example 3 A composite material of Example 3 was produced in the same manner as in Example 1, except that the molding raw material was changed so that the volume fraction of copper after sintering was 5%.
- Example 4 A composite material of Example 4 was produced in the same manner as in Example 2, except that the rotating speed of the rotary grindstone in the pretreatment of the graphite particles was changed to 5 Hz.
- Comparative example 1 A composite material of Comparative Example 1 was produced in the same manner as in Example 1, except that the rotational speed of the rotary grindstone in the pretreatment of the graphite particles was changed to 20 Hz.
- Comparative example 2 A composite material of Comparative Example 2 was produced in the same manner as in Example 2, except that the rotational speed of the rotary grindstone in the pretreatment of the graphite particles was changed to 20 Hz.
- Comparative Example 3 A composite material of Comparative Example 3 was produced in the same manner as in Example 3, except that the rotational speed of the rotary grindstone in the pretreatment of the graphite particles was changed to 20 Hz.
- Comparative Example 4 A composite material of Comparative Example 4 was produced in the same manner as in Example 2, except that graphite particles without pretreatment were used.
- ⁇ Thermal conductivity> In preparing a sample for thermal conductivity measurement, first, a plate was cut longitudinally from the center of the cylinder of the composite material of the example and the comparative example.
- the vertical direction of the cylinder is the direction in which the scale-like graphite particles are laminated.
- This plate was processed to obtain a sample for thermal conductivity measurement having an outer diameter of 10 mm and a thickness of 2.5 mm.
- the thickness direction of the sample is perpendicular to the direction in which the flake graphite particles are laminated (pressing direction). In this thickness direction, the thermal conductivity of the sample was measured according to the "method for measuring thermal diffusivity of metal by laser flash method (JIS H 7801:2005)".
- the thermal deterioration rate was determined based on the decrease in thermal diffusivity due to the temperature cycle test.
- the thermal diffusivity was measured using the same sample shape and measurement method as in the laser flash method.
- TD 0 After determining the thermal diffusivity TD 0 for each measurement sample, a cycle of increasing and decreasing the temperature from -40°C to 220°C was repeated to determine the thermal diffusivity TD 500 after 500 cycles.
- the thermal deterioration rate was calculated by ((TD 0 -TD 500 )/TD 0 )) ⁇ 100).
- the thermal conductivity of the composite material depends on the composition ratio of graphite and copper, as shown in Examples 1 to 3, the volume fraction of copper decreases and the content of graphite that contributes to heat conduction increases. and the thermal conductivity is improved.
- the thermal conductivity decreases as the rotating speed of the emery grindstone in the pretreatment increases. It is speculated that the graphite particles pretreated at rotation speeds exceeding 12 Hz passed between the grindstones without being subjected to sufficient stress. It was confirmed by shape observation with an optical microscope that the scale-like graphite particles of Comparative Examples 1 to 3 were untreated.
- the thermal conductivity of the composite material using graphite particles without pretreatment (Comparative Example 4) is slightly lower than that of the composite material having the same copper volume fraction (Comparative Example 2).
- FIG. 6 shows the transition of the thermal deterioration rate in the temperature cycle test of the composite material of Example 1. As shown in FIG. Although the thermal deterioration rate increases significantly after 100 temperature cycles, it does not significantly increase even if the temperature cycles are repeated after that, and remains almost constant. A similar tendency was confirmed for the composite materials of Examples 2 to 4.
- SYMBOLS 12 Scale-like graphite particles 14... Copper layer 16... Gap 23... Graphite particles 30a, 30b... Grindstones 31a, 31b... Metal plates 32a, 32b... Joining metal members 33a, 33b... Abrasive grains 40... Multiaxial current sintering apparatus 42... Vacuum vessel 44... Carbon mold DESCRIPTION OF SYMBOLS 45a, 45b... Pressure shaft 47a, 47b... Heating shaft 49a, 49b... Heating shaft 50... Radiation plate 51... Wiring layer 52... Electrical insulation layer 53... Stress buffer layer 54... Cooling layer 55... Cooling substrate
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Abstract
Description
そこで、本発明は、温度サイクル後の熱劣化が抑制された黒鉛-銅複合材料、それを用いたヒートシンク部材、および黒鉛-銅複合材料の製造方法を提供することを目的とする。
(1a)前記積層断面内に930μm×1230μmの測定視野を5つ画定する。
(1b)5つの測定視野それぞれについて、鱗片状黒鉛粒子内における幅2~5μmの隙間の数を計数してN1~N5とする。
(1c)隙間の数の平均値((N1+N2+N3+N4+N5)/5)を算出して、粒子内隙間個数Nを得る。
本発明の黒鉛-銅複合材料(以下、単に複合材料とも称する)は、鱗片状黒鉛粒子と銅粒子とを原料として得られた焼結体である。鱗片状黒鉛粒子は、銅層を介して積層されている。ここで、「銅層を介して」とは、鱗片状黒鉛粒子が隣接する銅層により繋がっていることを意味する。すなわち、複合材料内の鱗片状黒鉛粒子は電気的に連続している。複合材料中の銅層の厚さは特に限定されないが、一般的には3~25μm程度である。
複合材料が円柱状の場合、円柱の縦方向が鱗片状黒鉛粒子の積層された方向に相当するので、まず、円柱の縦方向に厚さ2mm程度の板材を切り出す。切り出した板材の表面を研磨した後、CP(Cross section Polisher)を用いて分析箇所の積層断面が得られる。
(1a)複合材料の積層断面内に、930μm×1230μmの測定視野を5つ画定する。測定視野は、複合材料の積層断面を、走査型電子顕微鏡(SEM:Scanning Electron Microscope)により100倍の倍率で観察して得られたSEM像中に、任意に画定することができる。測定視野においては、図1に示すように銅層14を介して鱗片状黒鉛粒子12が積層されており、鱗片状黒鉛粒子12内には隙間16が確認される。
本発明においては、こうして得られた粒子内隙間個数Nが5個以下に規定される。粒子内隙間個数が5個以下の鱗片状黒鉛粒子は、複合材料の温度サイクル後の熱劣化を抑制する作用を有することが本発明者らにより見出された。粒子内隙間個数Nは、5.0個以下が好ましく、3.5個以下がより好ましく、2.3個以下が特に好ましい。
(2a)鱗片状黒鉛粒子が積層された方向に板を切り出して試料を準備する。
試料は、前記板を、例えば外径10mm厚さ2.5mmに加工して得ることができる。
(2b)前記試料の熱拡散率TD0を求めた後、-40℃から220℃の昇温降下のサイクルを繰り返し、500回後の熱拡散率TD500を求める。
熱拡散率は、レーザーフラッシュ法(JIS H 7801:2005)に準拠してNETZSCH社製LFA447により求めることができる。
(2c)((TD0-TD500)/TD0))×100)により熱劣化率を得る。
本発明の複合材料は、黒鉛粒子に所定の前処理を施して所望の鱗片状黒鉛粒子を得、銅粒子と混合して成形原料とし、これを成形して所定条件で焼結して製造することができる。各工程について、以下に説明する。
黒鉛粒子の前処理は、黒鉛粒子に応力を印加することにより行われる。黒鉛粒子は、製造過程で印加される応力に起因して、本来的に内部に隙間を有している。本発明者らは、黒鉛粒子を含む複合材料の熱劣化には、黒鉛粒子内の隙間の数が関与していることを見出し、所定の前処理を施して得られた鱗片状黒鉛粒子を用いることによって、複合材料の温度サイクル後の熱劣化を抑制することを可能とした。
銅粒子は特に規定されず、例えば、体積基準のメジアン径が1.5μm以下の銅粒子を用いることができる。銅粒子のメジアン径は、1.0μm以下であることが好ましい。メジアン径が1.5μm以下の小さい銅粒子を用いた場合には、安定した熱伝導率や加工性の複合材料を得ることができる。メジアン径が1.5μm以下の銅粒子は、任意の方法により製造することができる。例えば、化学還元法や物理的製法によって、所望の銅粒子が得られる。
前処理を施して得られた鱗片状黒鉛粒子と銅粒子とを所定の割合で配合して、有機溶媒により湿式混合を行って成形原料を得る。原料の配合割合は、複合材料における黒鉛と銅との体積比(黒鉛:銅)は、70:30~97:3となるように選択される。熱伝導率と加工性の観点から、体積比(黒鉛:銅)は、84:16~95:5となるように選択することが好ましい。好適な有機溶媒としては、具体的にはトルエンやキシレンが挙げられる。
まず、少量(40g以下程度)の成形原料を所定の成形型に充填して、例えば油圧ハンドプレスを用いて3~15MPa程度の圧力で圧粉する。成形型としては、例えば直径30mmのSUS製型を用いることができる。成形原料の充填と圧粉とを繰り返して、所望の大きさの成形体を作製する。得られた成形体を、多軸通電焼結法により焼結することで、本発明の複合材料となる焼結体が得られる。
市販の原料黒鉛に、図3を参照して説明した方法により前処理を施した。上下の砥石は、砥粒としてダイヤモンドを備えており、その間に、5gの黒鉛粒子を2mLの水とともに挿入した。10Hzで回転砥石を回転させて、20秒間程度の前処理を黒鉛粒子に施した。その際の圧力は、0.5MPaとした。
処理後の黒鉛粒子を目開き500μmの篩で分級し、篩上面に残った黒鉛粒子を取り出し、乾燥させ、これを原料の鱗片状黒鉛粒子とした。一方、銅粒子としては、メジアン径が1.5μmの銅粒子を用意した。
直径30mmのSUS型に3gの成形原料を投入し、油圧プレスを用いて5MPaの圧力で圧粉した。成形原料の投入、圧粉の作業を10回超える程度に繰り返した成形を行い、SUS型から成形体を取り出した。
真空容器42内をロータリーポンプで5Paまで減圧し、装置電源の出力を上げて昇温させた。昇温により加熱軸(A)47a、47bで700℃まで加熱した後、加熱軸(B)49a,49bに変更して950℃まで加熱した。
同様の操作を5回行って5個の焼結体を作製し、実施例1の複合材料が得られた。
焼結後の銅の体積分率が16%となるように成形原料を変更した以外は、実施例1と同様にして実施例2の複合材料を製造した。
焼結後の銅の体積分率が5%となるように成形原料を変更した以外は、実施例1と同様にして実施例3の複合材料を製造した。
黒鉛粒子の前処理における回転砥石の回転数を5Hzに変更した以外は、実施例2と同様にして、実施例4の複合材料を製造した。
黒鉛粒子の前処理における回転砥石の回転数を20Hzに変更した以外は、実施例1と同様にして比較例1の複合材料を製造した。
黒鉛粒子の前処理における回転砥石の回転数を20Hzに変更した以外は、実施例2と同様にして比較例2の複合材料を製造した。
黒鉛粒子の前処理における回転砥石の回転数を20Hzに変更した以外は、実施例3と同様にして比較例3の複合材料を製造した。
前処理なしの黒鉛粒子を使用した以外は、実施例2と同様にして比較例4の複合材料を製造した。
上述したように、複合材料における積層断面を作製し、(1a)~(1c)にしたがって、粒子内隙間個数Nを求めた。
熱伝導率測定用の試料を作製するに当たって、まず、実施例および比較例の複合材料の円柱中央から、縦方向に板を切り出した。円柱の縦方向は、鱗片状黒鉛粒子が積層された方向である。この板を加工して、外径10mm×厚さ2.5mmの熱伝導率測定用の試料を得た。試料の厚さ方向が、鱗片状黒鉛粒子が積層された方向(加圧方向)に垂直な方向となる。この厚さ方向について、「金属のレーザーフラッシュ法による熱拡散率の測定方法(JIS H 7801:2005)」に準拠して、試料の熱伝導率を測定した。
温度サイクル試験による熱拡散率の低下に基づいて、熱劣化率を求めた。熱拡散率は、レーザーフラッシュ法の場合と同様の測定試料の形状と測定方法により測定した。各測定試料について熱拡散率TD0を求めた後、-40℃から220℃の昇温降下のサイクルを繰り返し、500回時の熱拡散率TD500を求めた。((TD0-TD500)/TD0))×100)により、熱劣化率を算出した。
12Hz以下の回転数で前処理を施して得られた鱗片状黒鉛粒子は、粒子内隙間個数が5個以下に制限されている。この結果から、前処理における回転砥石の回転数が、処理後の鱗片状黒鉛粒子における隙間個数に影響を及ぼしていることがわかる。
比較例1~3の鱗片状黒鉛粒子は、未処理であることが光学顕微鏡による形状観察により確認された。前処理なしの黒鉛粒子を用いた複合材料(比較例4)の熱伝導率は、銅体積分率が同じ複合材料(比較例2)よりも若干低い値となっている。
これらの結果は、複合材料の熱劣化率が、鱗片状黒鉛粒子内の隙間数に起因していることを示している。適切な前処理を施すことにより鱗片状黒鉛粒子内の隙間数を制御でき、こうした鱗片状黒鉛粒子を用いることによって、温度サイクル後の熱劣化が抑制された黒鉛-銅複合材料が得られることが確認された。
30a,30b…砥石 31a,31b…金属板 32a,32b…接合用金属部材
33a,33b…砥粒
40…多軸通電焼結装置 42…真空容器 44…カーボン製型
45a,45b…加圧軸 47a,47b…加熱軸 49a,49b…加熱軸
50…放熱板 51…配線層 52…電気絶縁層 53…応力緩衝層 54…冷却層
55…冷却基板
Claims (5)
- 銅層と、前記銅層を介して積層された鱗片黒鉛粒子とを含み、銅の体積分率が3~30%の黒鉛-銅複合材料であって、積層断面において、下記(1a)~(1c)により得られた粒子内隙間個数Nが5個以下であることを特徴とする黒鉛-銅複合材料。
(1a)前記積層断面内に930μm×1230μmの測定視野を5つ画定する。
(1b)5つの測定視野それぞれについて、鱗片状黒鉛粒子内における幅2~5μmの隙間の数を計数してN1~N5とする。
(1c)隙間の数の平均値((N1+N2+N3+N4+N5)/5)を算出して、粒子内隙間個数Nを得る。 - 前記鱗片状黒鉛粒子が積層された方向に垂直な方向での熱伝導率が700W/(m・K)以上である請求項1に記載の黒鉛-銅複合材料。
- 下記(2a)~(2c)により得られた熱劣化率が10%以下である請求項2に記載の黒鉛-銅複合材料。
(2a)前記鱗片状黒鉛粒子が積層された方向に板を切り出して試料を準備する。
(2b)前記試料の熱拡散率TD0を求めた後、-40℃から220℃の昇温降下のサイクルを繰り返し、500回後の熱拡散率TD500を求める。
(2c)((TD0-TD500)/TD0))×100)により熱劣化率を得る。 - 請求項1~3にいずれかに記載の黒鉛-銅複合材料を用いたヒートシンク部材。
- 請求項1記載の黒鉛-銅複合材料の製造方法であって、
上下に配置された一対の砥石の間に黒鉛粒子を挿入し、上側の砥石を12Hz以下で回転させることにより、前記黒鉛粒子に前処理を施して鱗片状黒鉛粒子を得る工程と、
前記鱗片状黒鉛粒子と銅粒子とを混合して成形原料を得る工程と、
前記成形原料を成形して得られた成形体を多軸通電焼結法により焼結する工程と
を備えることを特徴とする製造方法。
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JP2010248064A (ja) * | 2009-03-26 | 2010-11-04 | Shimane Prefecture | 鱗状黒鉛粉末成形体の製造方法および焼結成形体 |
JP2017128802A (ja) | 2016-01-15 | 2017-07-27 | 昭和電工株式会社 | 金属−黒鉛複合材料及びその製造方法 |
US20190366429A1 (en) * | 2018-05-30 | 2019-12-05 | Korea Institute Of Industrial Technology | Manufacturing method of metal hybrid heat-dissipating materials |
WO2021125196A1 (ja) * | 2019-12-17 | 2021-06-24 | 宇部興産株式会社 | 黒鉛-銅複合材料、それを用いたヒートシンク部材、および黒鉛-銅複合材料の製造方法 |
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EP4317954A1 (en) | 2024-02-07 |
CN117136247A (zh) | 2023-11-28 |
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