CN113631504B - Method for manufacturing heat sink - Google Patents
Method for manufacturing heat sink Download PDFInfo
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- CN113631504B CN113631504B CN201980094566.6A CN201980094566A CN113631504B CN 113631504 B CN113631504 B CN 113631504B CN 201980094566 A CN201980094566 A CN 201980094566A CN 113631504 B CN113631504 B CN 113631504B
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- compound
- heat sink
- thermosetting
- composition layer
- manufacturing
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims description 86
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 147
- 150000001875 compounds Chemical class 0.000 claims abstract description 144
- 239000000203 mixture Substances 0.000 claims abstract description 132
- 239000002245 particle Substances 0.000 claims abstract description 85
- 150000004767 nitrides Chemical class 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- -1 phenol compound Chemical class 0.000 claims description 54
- 239000004593 Epoxy Substances 0.000 claims description 16
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 13
- 229910052582 BN Inorganic materials 0.000 claims description 12
- 239000012948 isocyanate Substances 0.000 claims description 6
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- 239000011256 inorganic filler Substances 0.000 claims description 4
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 4
- 238000001723 curing Methods 0.000 description 45
- 239000003795 chemical substances by application Substances 0.000 description 27
- 239000003822 epoxy resin Substances 0.000 description 18
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- 238000000576 coating method Methods 0.000 description 15
- 238000001035 drying Methods 0.000 description 15
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- SFHYNDMGZXWXBU-LIMNOBDPSA-N 6-amino-2-[[(e)-(3-formylphenyl)methylideneamino]carbamoylamino]-1,3-dioxobenzo[de]isoquinoline-5,8-disulfonic acid Chemical compound O=C1C(C2=3)=CC(S(O)(=O)=O)=CC=3C(N)=C(S(O)(=O)=O)C=C2C(=O)N1NC(=O)N\N=C\C1=CC=CC(C=O)=C1 SFHYNDMGZXWXBU-LIMNOBDPSA-N 0.000 description 2
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
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- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 229930003836 cresol Natural products 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011342 resin composition Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000001029 thermal curing Methods 0.000 description 2
- 125000003396 thiol group Chemical group [H]S* 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- FBHPRUXJQNWTEW-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=CN1CC1=CC=CC=C1 FBHPRUXJQNWTEW-UHFFFAOYSA-N 0.000 description 1
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 1
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
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- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- DOIHHHHNLGDDRE-UHFFFAOYSA-N azanide;copper;copper(1+) Chemical compound [NH2-].[Cu].[Cu].[Cu+] DOIHHHHNLGDDRE-UHFFFAOYSA-N 0.000 description 1
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 description 1
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 description 1
- QCLQZCOGUCNIOC-UHFFFAOYSA-N azanylidynelanthanum Chemical compound [La]#N QCLQZCOGUCNIOC-UHFFFAOYSA-N 0.000 description 1
- GPBUGPUPKAGMDK-UHFFFAOYSA-N azanylidynemolybdenum Chemical compound [Mo]#N GPBUGPUPKAGMDK-UHFFFAOYSA-N 0.000 description 1
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 description 1
- AJXBBNUQVRZRCZ-UHFFFAOYSA-N azanylidyneyttrium Chemical compound [Y]#N AJXBBNUQVRZRCZ-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Substances FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001244 carboxylic acid anhydrides Chemical group 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000007765 extrusion coating Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 125000000466 oxiranyl group Chemical group 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
-
- 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
-
- 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
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
- Epoxy Resins (AREA)
- Cooling Or The Like Of Electrical Apparatus (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a manufacturing method of a radiating fin, which sequentially comprises the following steps: a step of forming a composition layer by applying a composition containing a solvent, a thermosetting compound, and inorganic nitride particles to a substrate; a step of maintaining the surface temperature T of the composition layer within a range of Tm < T < Ts, where T is the surface temperature of the composition layer, tm is the melting point of the thermosetting compound, and Ts is the starting temperature of the thermosetting reaction of the thermosetting compound; and a step of thermally curing the thermosetting compound in the composition layer to form a cured layer.
Description
Technical Field
The invention relates to a manufacturing method of a radiating fin.
Background
With the increase in performance of electronic devices, it is necessary to efficiently release heat generated in various components constituting the electronic devices. For example, a power device, a CPU (Central Processing Unit: central processing unit), or a light emitting diode (LED: light Emitting Diode) backlight has a device for generating heat at 150 ℃. If heat generated from the heating element as described above is accumulated in the electronic device, malfunction of the electronic device may occur. Accordingly, various techniques have been studied for releasing heat emitted from the heating element.
For example, japanese patent application laid-open No. 2018-115275 discloses a method for producing a curable material, which includes the steps of: the curable material is obtained by blending a curable compound and boron nitride agglomerated particles having a compressive strength of 2.7MPa or more when compressed by 30% as agglomerates of primary particles of boron nitride having an aspect ratio of 11 or more, and not blending boron nitride agglomerated particles as agglomerates of primary particles of boron nitride having an aspect ratio of less than 11.
Japanese patent application laid-open No. 2011-181650 discloses a method for manufacturing a heat dissipating substrate, comprising: a disposing step of disposing an uncured composition containing an uncured thermosetting resin containing a crystalline epoxy resin and an inorganic filler, a lead frame, and a wiring board on a metal plate; an embedding step of heating the uncured composition on the metal plate to embed the lead frame and the wiring board into the uncured composition; a convection step of heating at least the uncured composition to at least one of the crystallization temperature and the melting point of the crystalline epoxy resin to form a liquid state, thereby causing convection between the inorganic fillers; and a heat curing step of heat curing the uncured composition to form a heat conductive layer, wherein the inorganic filler is contained in an amount of 66vol% or more and 90vol% or less, and the wiring board and the lead frame are embedded in the heat conductive layer in a state of being in contact with each other via 1 or more contact portions.
In international publication No. 2017/111115, there is disclosed a semi-curable heat conductive film formed by: the solvent is removed from a resin composition comprising a curable compound (alpha), a curing agent (beta), a liquid crystal polymer (gamma) forming a liquid crystal phase at 190 ℃ or lower, and a filler (delta), and a casting of the resin composition.
Disclosure of Invention
Technical problem to be solved by the invention
In the conventional fin, voids (pores) having low thermal conductivity may be formed. If the proportion of voids contained in the heat sink increases, there is a possibility that the heat conductivity of the heat sink decreases. Further, inorganic nitride particles are known as a material having high thermal conductivity. However, since the affinity of the inorganic nitride particles with the resin binder is low, the proportion of voids generated in the heat sink containing the inorganic nitride particles as the heat conductive material tends to be high. Therefore, it is considered that, for example, even by the conventional methods described in Japanese patent application laid-open No. 2018-115275 and International publication No. 2017/111115, it is particularly difficult to sufficiently reduce the voids of the heat sink containing the inorganic nitride particles.
The present invention has been made in view of the above circumstances.
An object of one embodiment of the present invention is to provide a method for manufacturing a heat sink capable of forming a heat sink with few voids.
Means for solving the technical problems
The following means are included in the method for solving the above-described problems.
< 1 > a method for manufacturing a heat sink, comprising in order: a step of forming a composition layer by applying a composition containing a solvent, a thermosetting compound, and inorganic nitride particles to a substrate; a step of maintaining the surface temperature T of the composition layer within a range of Tm < T < Ts, where T is the surface temperature of the composition layer, tm is the melting point of the thermosetting compound, and Ts is the starting temperature of the thermosetting reaction of the thermosetting compound; and a step of thermally curing the thermosetting compound in the composition layer to form a cured layer.
2 the method for manufacturing a heat sink according to 1, wherein,
the step of forming the composition layer and the step of holding include a step of adjusting a residual rate of the solvent contained in the composition layer to 1 to 10 mass%.
< 3 > the method for manufacturing a heat sink according to < 1 > or < 2 >, wherein,
In the step of maintaining, the surface temperature T of the composition layer further satisfies the relation [ (Tm+Ts)/2 ]. Ltoreq.T < Ts.
A method for manufacturing a heat sink according to any one of < 1 > to < 3 >, wherein,
in the step of maintaining, the surface temperature T of the composition layer further satisfies the relationship of (Ts-10 ℃ C.) to T < Ts.
A method for manufacturing a heat sink according to any one of < 1 > to < 4 >, wherein,
the holding time in the holding step is 30 seconds or longer.
A method for manufacturing a heat sink according to any one of < 1 > to < 5 >, wherein,
the inorganic nitride particles have an average aspect ratio of 5 or more.
A method for manufacturing a heat sink according to any one of < 1 > to < 6 >, wherein,
the inorganic nitride particles have an average particle diameter of 30 μm or more.
A method for manufacturing a heat sink according to any one of < 1 > to < 7 >, wherein,
the inorganic nitride particles are boron nitride particles.
A method for manufacturing a heat sink according to any one of < 1 > to < 8 >, wherein,
the thermosetting compound contains at least 1 selected from the group consisting of an epoxy compound, a phenol compound, an imide compound, a melamine compound, an isocyanate compound, a urethane compound, an acrylate compound, and a methacrylate compound.
Effects of the invention
According to one aspect of the present invention, a method for manufacturing a heat sink in which a heat sink having a small space can be formed can be provided.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail. The present invention is not limited to the following embodiments, and can be appropriately modified and implemented within the scope of the object of the present invention.
In the present invention, a numerical range expressed by "to" means a range including numerical values described before and after "to" as a lower limit value and an upper limit value. In the numerical ranges described in stages in the present invention, the upper limit or the lower limit described in a certain numerical range may be replaced with the upper limit or the lower limit of the numerical range described in other stages. In the numerical ranges described in the present invention, the upper limit value or the lower limit value described in a certain numerical range may be replaced with the value shown in the embodiment.
In the present invention, the amounts of the respective components in the composition, when a plurality of substances corresponding to the respective components are present in the composition, refer to the total amount of the plurality of substances present in the composition unless otherwise specified.
In the present invention, a combination of 2 or more preferred modes is a more preferred mode.
In the present invention, the term "process" includes not only an independent process but also a process which cannot be clearly distinguished from other processes, as long as the intended purpose of the process can be achieved.
In the present invention, "mass%" and "weight%" have the same meaning, and "parts by mass" and "parts by weight" have the same meaning.
In the present invention, "total solid component mass" means the total mass of components other than the solvent.
Method for manufacturing heat sink
The manufacturing method of the radiating fin comprises the following steps in sequence: a step of forming a composition layer by applying a composition containing a solvent, a thermosetting compound, and inorganic nitride particles to a substrate (hereinafter referred to as a "forming step"); a step (hereinafter referred to as a "holding step") of holding the surface temperature T of the composition layer in a range of Tm < T < Ts, where T is the surface temperature of the composition layer, tm is the melting point of the thermosetting compound, and Ts is the start temperature of the thermosetting reaction of the thermosetting compound; and a step of forming a cured layer by thermally curing the thermosetting compound in the composition layer (hereinafter referred to as "thermal curing step").
According to the method for manufacturing a heat sink of the present invention, a heat sink with few voids can be formed. The reason why the method for manufacturing a fin according to the present invention exhibits the above-described effects is not clear, but is presumed as follows.
The method for manufacturing a heat sink according to the present invention includes a step of maintaining the surface temperature (T) of the composition layer within a specific temperature range (Tm < T < Ts), that is, within a temperature range exceeding the melting point (Tm) of the thermosetting compound and less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound, whereby the fluidity of the thermosetting compound can be improved while suppressing the thermosetting of the thermosetting compound. Further, the affinity between the thermosetting compound having improved fluidity and the surface of the inorganic nitride particle is also improved. Therefore, it is considered that by keeping the surface temperature (T) of the composition layer within a specific temperature range (Tm < T < Ts), voids in the composition layer (for example, voids formed between inorganic nitride particles and voids formed around the inorganic nitride particles) can be filled. In the method for producing a heat sink according to the present invention, it is considered that the heat sink with small voids can be formed by reducing voids in the composition layer in the holding step and then thermally curing the thermosetting compound in the composition layer with small voids.
Hereinafter, each step of the method for manufacturing a heat sink according to the present invention will be described.
[ Forming Process ]
The method for producing a heat sink according to the present invention includes a step (forming step) of forming a composition layer by applying a composition containing a solvent, a thermosetting compound, and inorganic nitride particles to a substrate.
[ composition ]
The composition used in the present invention contains a solvent, a thermosetting compound, and inorganic nitride particles. A preferred embodiment of the above composition is a coating liquid.
(solvent)
The solvent is not limited, and a known solvent can be used. The solvent is preferably an organic solvent from the viewpoint of solubility of the thermosetting compound. Examples of the organic solvent include ethyl acetate, methyl ethyl ketone, methylene chloride and tetrahydrofuran.
The composition may contain 1 solvent alone or 2 or more solvents.
The content of the solvent is not limited, and may be appropriately set according to the composition of each component contained in the composition and the coating method, for example. The content of the solvent is preferably 30 to 80% by mass, more preferably 50 to 70% by mass, relative to the total mass of the composition.
(thermosetting Compound)
The thermosetting compound is a compound capable of being cured by a chemical reaction under heating conditions, and includes a compound that forms a molecular skeleton of a product (i.e., a cured product) in a thermosetting reaction unless otherwise specified. The thermosetting compound may be 1 kind of compound to be thermally cured alone, may be a compound to be thermally cured by using 2 or more kinds in combination, or may be a compound to be thermally cured in the presence of a known additive.
The form of the thermosetting compound is not limited to monomers, and includes, for example, oligomers, prepolymers, and polymers. The thermosetting compound is preferably a monomer from the viewpoint of easiness of adding functions such as heat resistance.
The thermosetting compound is not limited, and a known thermosetting compound can be used. Examples of the thermosetting compound include epoxy compounds, phenol compounds, imide compounds, melamine compounds, isocyanate compounds, urethane compounds, acrylate compounds, and methacrylate compounds. The above-mentioned compounds also contain a thermosetting resin described later.
From the viewpoint of curability and film quality, the thermosetting compound preferably contains at least 1 selected from the group consisting of an epoxy compound, a phenol compound, an imide compound, a melamine compound, an isocyanate compound, a urethane compound, an acrylate compound, and a methacrylate compound, more preferably contains at least 1 selected from the group consisting of an epoxy compound, a phenol compound, an acrylate compound, and a methacrylate compound, still more preferably contains at least 1 selected from the group consisting of an epoxy compound and a phenol compound, and particularly preferably contains an epoxy compound.
From the viewpoint of curability and film quality, the thermosetting compound is preferably at least 1 selected from the group consisting of an epoxy compound, a phenol compound, an imide compound, a melamine compound, an isocyanate compound, a urethane compound, an acrylate compound, and a methacrylate compound, more preferably at least 1 selected from the group consisting of an epoxy compound, a phenol compound, an acrylate compound, and a methacrylate compound, still more preferably at least 1 selected from the group consisting of an epoxy compound and a phenol compound, and particularly preferably an epoxy compound.
The epoxy compound is not limited as long as it is a compound having an oxirane group. From the viewpoints of curability and film quality, the epoxy compound is preferably a compound having at least 2 ethylene oxide groups in one molecule, more preferably an aromatic compound having at least 2 ethylene oxide groups in one molecule, and particularly preferably a compound represented by the following formula (I).
[ chemical formula 1]
In the formula (I), R 1 、R 2 、R 3 、R 4 、R 5 、R 6 、R 7 R is R 8 Each independently represents a hydrogen atom or an alkyl group.
In the formula (I), R is 1 、R 2 、R 3 、R 4 、R 5 、R 6 、R 7 R is R 8 The alkyl group is preferably an alkyl group having 1 to 6 carbon atoms, more preferably an alkyl group having 1 to 3 carbon atoms, and particularly preferably a methyl group.
In formula (I), R is preferably 1 、R 4 、R 5 R is R 8 Each independently represents a hydrogen atom or an alkyl group having 1 to 3 carbon atoms, R 2 、R 3 、R 6 R is R 7 Is a hydrogen atom. In formula (I), R is more preferably 1 、R 4 、R 5 R is R 8 Each independently is a hydrogen atom or a methyl group, R 2 、R 3 、R 6 R is R 7 Is a hydrogen atom.
The compound represented by the above formula (I) can be obtained, for example, as YX4000 manufactured by Mitsubishi Chemical Corpora tion.
In the case where the composition used in the present invention contains an epoxy compound, the composition preferably further contains a phenol compound from the viewpoint of curability. That is, the thermosetting compound preferably contains at least an epoxy compound and a phenol compound.
The phenol compound is not limited as long as it is a compound having a phenolic hydroxyl group. The phenol compound is preferably a polyhydric phenol compound, more preferably a compound represented by the following formula (II), from the viewpoints of curability and film quality.
[ chemical formula 2]
In the formula (II), R 11 R is R 12 Each independently represents a hydrogen atom, an alkyl group or a hydroxyl group, R 13 、R 14 、R 15 R is R 16 Each independently represents a hydrogen atom or an alkyl group.
In the formula (II), R 11 R is R 12 Each independently is preferably a hydrogen atom, an alkyl group having 1 to 3 carbon atoms, or a hydroxyl group, and more preferably a hydrogen atom or a hydroxyl group.
In the formula (II), R 13 、R 14 、R 15 R is R 16 Each independently is preferably a hydrogen atom or an alkyl group having 1 to 3 carbon atoms, and more preferably a methyl group.
The compound represented by the above formula (II) can be obtained, for example, as QE-2405 manufactured by Combi-Blocks Inc.
Examples of the thermosetting compound include an epoxy resin monomer and an acrylic resin monomer described in paragraph 0028 of Japanese patent application No. 4118691, an epoxy compound described in paragraphs 0006 to 0011 of Japanese patent application laid-open No. 2008-13759, and an epoxy resin monomer described in paragraphs 0032 to 0100 of Japanese patent application laid-open No. 2013-227451.
As the thermosetting compound, a thermosetting resin is also included. The thermosetting resin is not limited, and a known thermosetting resin can be used. Examples of the thermosetting resin include epoxy resin, phenolic resin, polyimide resin, cresol resin, melamine resin, unsaturated polyester resin, isocyanate resin, and thermosetting urethane resin.
Among the above, the thermosetting resin is preferably an epoxy resin from the viewpoints of small thermal expansion coefficient and excellent heat resistance and adhesion.
The epoxy resin is not limited, and a known epoxy resin can be used. Examples of the epoxy resin include difunctional epoxy resins and novolak epoxy resins.
Examples of the difunctional epoxy resin include bisphenol a type epoxy resin, bisphenol F type epoxy resin and bisphenol S type epoxy resin.
Examples of the novolak type epoxy resin include phenol novolak type epoxy resin and cresol novolak type epoxy resin.
The thermosetting compound preferably has a polymerizable group. The polymerizable group in the thermosetting compound is preferably at least 1 polymerizable group selected from the group consisting of an acryl group, a methacryl group, an ethylene oxide group, and a vinyl group, and more preferably an ethylene oxide group.
The thermosetting compound may have 1 kind of polymerizable group alone or 2 or more kinds of polymerizable groups. The number of polymerizable groups in the thermosetting compound may be 1 or 2 or more. The number of polymerizable groups in the thermosetting compound is preferably 2 or more, more preferably 3 or more, from the viewpoint of excellent heat resistance of the cured product. The upper limit of the number of polymerizable groups in the thermosetting compound is not limited. The number of polymerizable groups in the polymerizable monomer is usually 8 or less.
The thermosetting compound preferably contains a compound having at least 1 polymerizable group selected from the group consisting of an acryl group, a methacryl group, an ethylene oxide group, and a vinyl group, and more preferably contains a compound having an ethylene oxide group.
The molecular weight of the thermosetting compound is preferably 10,000 or less, more preferably 5,000 or less, further preferably 1,00 or less, and particularly preferably 600 or less, from the viewpoint of facilitating the addition of functions such as heat resistance.
The lower limit of the molecular weight of the thermosetting compound is not limited. The molecular weight of the thermosetting compound may be appropriately set, for example, in a range of 100 or more, preferably 200 or more.
The composition may contain 1 kind of thermosetting compound alone or 2 or more kinds of thermosetting compounds.
From the viewpoints of the heat conductivity of the heat sink, the dispersibility of the inorganic nitride particles, and the film quality, the content of the thermosetting compound is preferably 10 to 50% by mass, more preferably 20 to 50% by mass, and particularly preferably 20 to 40% by mass, relative to the total solid content mass in the composition.
(inorganic nitride particles)
Examples of the inorganic nitride constituting the inorganic nitride particles include Boron Nitride (BN) and carbon nitride (C 3 N 4 ) Silicon nitride (Si) 3 N 4 ) Gallium nitride (GaN), indium nitride (InN), aluminum nitride (AlN), chromium nitride (Cr) 2 N), copper nitride (Cu 3 N), iron nitride (Fe 4 N or Fe 3 N), lanthanum nitride (La N), lithium nitride (Li) 3 N), magnesium nitride (Mg 3 N 2 ) Molybdenum nitride (Mo) 2 N), niobium nitride (NbN), tantalum nitride (TaN), titanium nitride (TiN), tungsten nitride (W) 2 N、WN 2 Or WN), yttrium Nitride (YN), and zirconium nitride (ZrN).
From the standpoint of the thermal conductivity of the heat sink, the inorganic nitride particles are preferably inorganic nitride particles containing at least 1 atom selected from the group consisting of boron atoms, aluminum atoms, and silicon atoms, more preferably inorganic nitride particles containing at least 1 atom selected from the group consisting of boron atoms and aluminum atoms, and particularly preferably inorganic nitride particles containing boron atoms.
From the standpoint of the thermal conductivity of the heat sink, the inorganic nitride particles are preferably at least 1 kind of inorganic nitride particles selected from the group consisting of boron nitride particles, aluminum nitride particles, and silicon nitride particles, more preferably at least 1 kind of inorganic nitride particles selected from the group consisting of boron nitride particles and aluminum nitride particles, and particularly preferably boron nitride particles.
Average aspect ratio-
The average aspect ratio of the inorganic nitride particles is preferably 3 or more, more preferably 5 or more, and particularly preferably 8 or more. The average aspect ratio of the inorganic nitride particles is 3 or more, whereby the heat conductivity of the heat sink can be improved.
The upper limit of the average aspect ratio of the inorganic nitride particles is not limited. The average aspect ratio of the inorganic nitride particles is preferably 20 or less, more preferably 15 or less, from the viewpoint of particle dispersibility in the composition.
The average aspect ratio of the inorganic nitride particles was measured by the following method.
(1) Images of randomly selected 100 inorganic nitride particles were obtained using a Scanning Electron Microscope (SEM).
(2) The long diameter and the short diameter of each of the above-mentioned inorganic nitride particles were measured. In the present invention, the term "long diameter of the inorganic nitride particles" means the length of the longest line segment among line segments between any two points on the contour line connecting the inorganic nitride particles. For example, in the case where the inorganic nitride particles are perfect circles in the image, the long diameter of the inorganic nitride particles refers to the diameter of the inorganic nitride particles. In the present invention, the term "short diameter of the inorganic nitride particles" refers to the length of the longest line segment among line segments that are orthogonal to the line segments defining the long diameter and connect any two points on the contour line of the inorganic nitride particles.
(3) The ratio of the long diameter to the short diameter (long diameter/short diameter) of each inorganic nitride particle was obtained.
(4) The arithmetic average of the obtained values was taken as the average aspect ratio of the inorganic nitride particles.
Average particle size-
The average particle diameter of the inorganic nitride particles is preferably 10 μm or more, more preferably 20 μm or more, still more preferably 30 μm or more, and particularly preferably 50 μm or more. The heat conductivity of the heat sink can be further improved by the inorganic nitride particles having an average particle diameter of 10 μm or more.
The average particle diameter of the inorganic nitride particles is preferably 200 μm or less, more preferably 150 μm or less. The inorganic nitride particles have an average particle diameter of 200 μm or less, so that surface irregularities of the heat sink can be reduced, and as a result, heat dissipation of the heat sink increases.
In the present invention, the average particle diameter of the inorganic nitride particles is the particle diameter (D50, median particle diameter) at which the number-based accumulation becomes 50% in the number-based particle diameter distribution measured using a laser diffraction particle size distribution measuring apparatus (for example, manufactured by MT3300II, microtracBEL Corporation).
The composition may contain 1 kind of inorganic nitride particles alone or 2 or more kinds of inorganic nitride particles.
From the viewpoint of the heat conductivity of the heat sink, the content of the inorganic nitride particles is preferably 50 to 80 mass%, more preferably 60 to 80 mass%, relative to the total solid content mass in the composition.
From the viewpoint of the heat conductivity of the heat sink, the content of the inorganic nitride particles is preferably 200 to 400 parts by mass, more preferably 250 to 350 parts by mass, relative to 100 parts by mass of the thermosetting compound.
(other Components)
The composition may contain other components in addition to the thermosetting compound and the inorganic nitride particles. Examples of the other components include a curing agent, a curing accelerator, and a polymerization initiator. From the viewpoint of promoting the curing reaction, the composition preferably contains at least 1 selected from the group consisting of a curing agent, a curing accelerator, and a polymerization initiator.
Curing agent-
The curing agent is not limited, and a known curing agent can be used. The curing agent is preferably a compound having at least 1 functional group selected from the group consisting of a hydroxyl group, an amino group, a thiol group, an isocyanate group, a carboxyl group, an acryl group, a methacryl group, and a carboxylic anhydride group, and more preferably a compound having at least 1 functional group selected from the group consisting of a hydroxyl group, an acryl group, a methacryl group, an amino group, and a thiol group.
The curing agent is preferably a compound having 2 or more of the above-mentioned functional groups, more preferably a compound having 2 or 3 of the above-mentioned functional groups.
Specific examples of the curing agent include amine-based curing agents, phenol-based curing agents, guanidine-based curing agents, imidazole-based curing agents, naphthol-based curing agents, acrylic-based curing agents, acid anhydride-based curing agents, active ester-based curing agents, benzoxazine-based curing agents, and cyanate-based curing agents. Among the above, the curing agent is preferably an imidazole-based curing agent, an acrylic-based curing agent, a phenol-based curing agent or an amine-based curing agent.
The composition may contain 1 kind of curing agent alone or 2 or more kinds of curing agents.
When the composition contains a curing agent, the content of the curing agent is preferably 1 to 50% by mass, more preferably 1 to 30% by mass, based on the total solid content mass in the composition.
Curing accelerator-
The curing accelerator is not limited, and a known curing accelerator can be used. Examples of the curing accelerator include triphenylphosphine, 2-ethyl-4-methylimidazole, boron trifluoride amine complex and 1-benzyl-2-methylimidazole.
The composition may contain 1 kind of curing accelerator alone or 2 or more kinds of curing accelerators.
When the composition contains a curing accelerator, the content of the curing accelerator is preferably 0.1 to 20% by mass based on the total mass of solid components in the composition.
Polymerization initiator-
The polymerization initiator is not limited, and a known polymerization initiator can be used. When the thermosetting compound has an acryl or methacryl group, the polymerization initiator is preferably a polymerization initiator described in paragraph 0062 of JP 2010-125782 or a polymerization initiator described in paragraph 0054 of JP 2015-052710.
The composition may contain 1 kind of polymerization initiator alone or 2 or more kinds of polymerization initiators.
In the case where the composition contains a polymerization initiator, the content of the polymerization initiator is preferably 0.1 to 50% by mass relative to the total solid content mass in the composition.
(method for producing composition)
Examples of the method for producing the composition include a method of mixing the above components. For example, the composition can be obtained by mixing a solvent, a thermosetting compound, and inorganic nitride particles. The mixing method is not limited, and a known method can be used.
[ substrate ]
The substrate is not limited, and a known substrate can be used. Examples of the base material include a metal substrate and a release liner.
Examples of the metal substrate include an iron substrate, a copper substrate, a stainless steel substrate, an aluminum substrate, an alloy substrate containing magnesium, and an alloy substrate containing aluminum. Among the above, the metal substrate is preferably a copper substrate.
Examples of the release liner include paper (e.g., kraft paper, cellophane, and high-quality paper), resin film (e.g., polyolefin and polyester), and laminated paper obtained by laminating paper and resin film. Examples of the polyolefin include polyethylene and polypropylene. Examples of the polyester include polyethylene terephthalate (PET).
The paper used as the release liner may be a paper subjected to a release treatment. The paper subjected to the peeling treatment can be formed by further subjecting one or both surfaces of the paper subjected to the sealing treatment to the peeling treatment, for example. The sealing treatment can be performed using clay or polyvinyl alcohol, for example. The peeling treatment can be performed using, for example, a silicone resin.
The thickness of the base material is not limited, and may be appropriately set in a range of 10 μm to 300 μm, for example.
[ coating method ]
The coating method is not limited, and a known method can be used. Examples of the coating method include roll coating, gravure coating, spin coating, wire bar coating, extrusion coating, direct gravure coating, reverse gravure coating, die coating, spray coating, and inkjet coating.
The coating amount of the composition is not limited, and may be appropriately set according to the composition of the composition, the coating method, and the thickness of the target composition layer, for example. The coating amount of the composition after drying is preferably 50cm 3 /m 2 ～400cm 3 /m 2 More preferably 100cm 3 /m 2 ～250cm 3 /m 2 。
[ holding step ]
The method for manufacturing a heat sink according to the present invention includes a step (holding step) of holding the surface temperature T of the composition layer in a range of Tm < T < Ts, where T is the surface temperature of the composition layer, tm is the melting point of the thermosetting compound, and Ts is the starting temperature of the thermosetting reaction of the thermosetting compound. It is considered that the method for manufacturing a heat sink according to the present invention includes the above-described holding step, and can suppress progress of heat curing of the thermosetting compound and improve fluidity of the thermosetting compound, so that voids in the composition layer can be filled. Therefore, a fin with few voids can be formed.
In the present invention, the unit of the surface temperature (T) of the composition layer, the melting point (Tm) of the thermosetting compound, and the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound is "°c" unless otherwise specified.
In the method for manufacturing a heat sink according to the present invention, the start point of the holding step is a point of time when the surface temperature (T) of the composition layer reaches a range of Tm < T < Ts.
The surface temperature (T) of the composition layer preferably satisfies the relation [ (Tm+Ts)/2 ]. Ltoreq.T < Ts on the basis of satisfying the above-mentioned relation (Tm < T < Ts), more preferably satisfies the relation (Ts-20 ℃ C.) T < Ts, still more preferably satisfies the relation (Ts-10 ℃ C.) T < Ts, particularly preferably satisfies the relation (Ts-5 ℃ C.) T < Ts. In the holding step, the smaller the difference between the surface temperature (T) of the composition layer and the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound, the more the voids contained in the heat sink can be reduced. In addition, the film quality of the heat sink can be improved.
The relation represented by [ (Tm+Ts)/2 ]. Ltoreq.T < Ts means that the surface temperature (T) of the composition layer is equal to or higher than the intermediate temperature of the melting point (Tm) of the thermosetting compound and the starting temperature (Ts) of the thermosetting compound for the thermosetting reaction and is smaller than the starting temperature (Ts) of the thermosetting compound for the thermosetting reaction.
The relationship represented by (Ts-20 ℃) T < Ts means that the surface temperature (T) of the composition layer is a temperature 20 ℃ or more lower than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound and less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound.
The relationship represented by (Ts-10 ℃ C. Ltoreq.T < Ts means that the surface temperature (T) of the composition layer is a temperature which is 10 ℃ or more lower than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound and less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound.
The relationship represented by (Ts-5 ℃ C. Ltoreq.T < Ts means that the surface temperature (T) of the composition layer is a temperature which is 5 ℃ or more lower than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound and less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound.
The surface temperature (T) of the composition layer is preferably 70 to 150 ℃, more preferably 80 to 145 ℃, still more preferably 100 to 145 ℃, particularly preferably 120 to 145 ℃, and most preferably 130 to 140 ℃ on the basis of satisfying the above-mentioned relation (Tm < T < Ts). By the surface temperature (T) of the composition layer being within the above range, the voids contained in the heat sink can be further reduced. In addition, the film quality of the heat sink can be improved.
The method for measuring the surface temperature (T) of the composition layer is not limited, and a known method can be used. As a method for measuring the surface temperature (T) of the composition layer, a method using a noncontact thermometer (for example, a radiation thermometer or the like) is preferable.
The melting point (Tm) of the thermosetting compound is measured by the method described in the following (1) or (2).
(1) In the case where the composition layer contains 1 thermosetting compound alone, the melting point of the thermosetting compound is determined by Differential Scanning Calorimetry (DSC).
(2) In the case where the composition layer contains a plurality of thermosetting compounds, the melting point of the thermosetting compounds refers to the temperature measured by the following method. First, each thermosetting compound is prepared to be weighed according to the content ratio of each thermosetting compound in the composition layer. Next, after each thermosetting compound was added to the petri dish, the mixture of each thermosetting compound was warmed using METTLER TOLEDO (METTLER toldo). The temperature at which the mixture of the respective thermosetting compounds added to the dish was melted to be transparent was used as the melting point of the thermosetting compound.
The starting temperature (Ts) of the thermosetting reaction of the thermosetting compound was measured by the following method.
(1) The DSC curve of the composition layer was obtained by Differential Scanning Calorimetry (DSC). Wherein the content of the solvent in the composition layer used as a measurement sample is 10 mass% or less. As the measurement device, a known differential scanning calorimeter can be used.
(2) From the DSC curve, the temperature at which a peak (for example, a heat generation peak) due to the heat curing reaction of the thermosetting compound starts to occur was obtained. Here, the "temperature at which the peak starts to occur" refers to a temperature at which a straight line extending the base line on the low temperature side to the high temperature side intersects a tangential line drawn at a point of the curve on the low temperature side of the peak where the gradient is the largest.
(3) The temperature at which the peak starts to occur is taken as the starting temperature of the thermosetting reaction of the thermosetting compound.
In the holding step, the temperature at which the active species are generated as the starting point of the thermosetting reaction of the thermosetting compound or the temperature at which the thermosetting reaction of the thermosetting compound is started can be used as an index of the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound. For example, in the case where the composition layer before thermosetting contains a polymerization initiator, the pyrolysis temperature of the polymerization initiator can be used as an index of the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound. The temperature conditions in the holding step can be appropriately set according to the above-mentioned index.
The method for maintaining the surface temperature (T) of the composition layer within the above-mentioned respective temperature ranges is not limited, and a known method can be used. Examples of the method include a method of adjusting the temperature of the atmosphere, a method of blowing warm air to the composition layer, and a method of irradiating electromagnetic waves (for example, infrared rays) to the composition layer. Examples of the apparatus used in the above method include an electric furnace, a fan heater, and an Infrared (IR) heater. Among the above, the method of keeping the surface temperature (T) of the composition layer within the above-mentioned respective temperature ranges is preferably a method of heating with warm air.
The holding time is not limited, and may be appropriately set according to the temperature of the surface temperature (T) of the composition layer in the holding step. The holding time is preferably 10 seconds or more, more preferably 20 seconds or more, and particularly preferably 30 seconds or more. By keeping the holding time at 10 seconds or longer, the voids contained in the heat sink can be further reduced. In the present invention, the term "holding time" means a time for which the surface temperature (T) of any one of the composition layers is maintained within the above-mentioned specific temperature range (for example, tm < T < Ts).
The holding time is preferably 120 seconds or less, more preferably 60 seconds or less, from the viewpoints of productivity and equipment cost.
In the method for manufacturing a heat sink according to the present invention, the holding step may be performed as many times as necessary without departing from the spirit of the present invention. In the case where the holding step is performed a plurality of times, the conditions of the holding steps may be the same or different from each other.
[ Heat curing Process ]
The method for producing a heat sink according to the present invention includes a step of forming a cured layer by thermally curing the thermosetting compound in the composition layer (thermal curing step). In the method for manufacturing a heat sink according to the present invention, the thermosetting compound in the composition layer is thermally cured after the holding step, so that a heat sink with few voids can be formed.
The method of heat curing is not limited as long as the thermosetting compound can be heat cured, and known methods can be used. Examples of the method of thermosetting include a method of adjusting the temperature of the atmosphere, a method of blowing warm air to the composition layer, and a method of irradiating electromagnetic waves (for example, infrared rays) to the composition layer. Examples of the apparatus used in the above method include an electric furnace, a fan heater, and an Infrared (IR) heater. Among the above, the method of heat curing is preferably a method of heating using warm air.
The heating temperature in the heat curing step is not limited as long as it is a temperature at which the thermosetting compound can be heat cured, and is set appropriately according to the composition of the composition layer, for example. The heating temperature in the thermosetting step is preferably not less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound from the viewpoint of efficiently carrying out the thermosetting reaction. The heating temperature in the heat curing step may be appropriately set, for example, in the range of 50 to 200 ℃. The heating time in the heat curing step is not limited, and may be appropriately set according to the heating temperature.
And, the curing reaction may be a semi-curing reaction. That is, the cured layer obtained may be in a so-called B-stage state (semi-cured state).
In the method for manufacturing a heat sink according to the present invention, the heat curing step may be performed as many times as necessary without departing from the spirit of the present invention. In the case where the heat curing process is performed a plurality of times, the conditions of the respective heat curing processes may be the same or different from each other.
[ drying Process ]
The method for manufacturing a heat sink according to the present invention preferably includes a step of adjusting the residual rate of the solvent contained in the composition layer to 0.5 to 12 mass% (hereinafter, also referred to as a "drying step") between the step of forming the composition layer (forming step) and the step of holding (holding step). By adjusting the residual rate of the solvent in the composition layer to 0.5 to 12 mass%, the surface temperature (T) of the composition layer can be easily adjusted to a temperature higher than the melting point (Tm) of the thermosetting compound in the holding step. Therefore, the void included in the heat sink can be further reduced.
In the case where the method for manufacturing a heat sink according to the present invention includes the drying step, the drying step and the holding step are not limited to the independent steps, and may be performed continuously. As described above, the starting point of the holding step when the drying step and the holding step are continuously performed is a time point when the surface temperature (T) of the composition layer reaches a range of Tm < T < Ts.
In the drying step, the residual ratio of the solvent contained in the composition layer is more preferably 1 to 10% by mass, still more preferably 1 to 6% by mass, and particularly preferably 1 to 4% by mass. By adjusting the residual rate of the solvent contained in the composition layer to be within the above range, the surface temperature (T) of the composition layer can be easily increased to a temperature higher than the melting point (Tm) of the thermosetting compound in the holding step. Therefore, the void included in the heat sink can be further reduced. Further, the residual rate of the solvent in the obtained heat sink can be reduced, and therefore the film quality of the heat sink can be improved.
The residual rate of the solvent contained in the composition layer is represented by the ratio of the content of the solvent to the total mass of the composition layer. The content of solvent was determined by gas chromatography-mass spectrometry (GC-MS).
In the drying step, a method for adjusting the residual rate of the solvent contained in the composition layer is not limited, and a known method can be used. As the above method, a method of blowing (preferably, warm air) the composition layer is preferable. In the method of blowing the composition layer, the temperature of the wind is preferably 23 to 140 ℃. The time of blowing is not limited as long as it is appropriately set according to the temperature.
The surface temperature (T) of the composition layer in the drying step is preferably in a range of less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound. By the surface temperature (T) of the composition layer being in a range less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound, the voids contained in the heat sink can be further reduced.
In the method for manufacturing a heat sink according to the present invention, the drying step may be performed as many times as necessary without departing from the spirit of the present invention. In the case where the drying process is performed a plurality of times, the conditions of the drying processes may be the same or different from each other.
< Heat sink >)
The heat sink produced by the method for producing a heat sink according to the present invention has a small number of voids and therefore has excellent heat dissipation. Therefore, the heat sink formed by the method for manufacturing a heat sink according to the present invention can efficiently release heat generated in the heat generating element by contact with various heat generating elements. For example, by bringing the heat sink into contact with various components constituting the electronic device, heat generated in the components can be efficiently released. Examples of the components include a power device and a CPU. The heat sink formed by the method for manufacturing a heat sink according to the present invention may be disposed between a heat generating body such as a power device and a heat radiating body such as a heat sink.
The thickness of the heat sink is not limited, and may be appropriately set according to the application, for example. From the standpoint of thermal conductivity, the thickness of the heat sink is preferably in the range of 50 μm to 200 μm.
Examples
Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto. Unless otherwise specified, "parts" and "%" are mass references. Hereinafter, the surface temperature (T) of the composition layer in the holding step is referred to as "holding temperature".
Example 1 >
[ preparation of composition A ]
Composition a was prepared by mixing the following ingredients.
(composition)
Thermosetting compound A1 (compound having the following structure, molecular weight 372.42, manufactured by QE-2405, combi-Blocks Inc.): 17 parts by mass
[ chemical formula 3]
Thermosetting compound B (compound having the following structure, manufactured by molecular weight 354.45,YX4000,Mi tsubishi Chemical Corporation): 34 parts by mass
[ chemical formula 4]
Methyl ethyl ketone: 65 parts by mass
TPP (triphenylphosphine: cure accelerator): 0.6 part by mass
Boron nitride particles (inorganic nitride particles, manufactured by HP-40MF100,MIZUSHIMA FERROALLOY CO, ltd.): 51 parts by mass
[ production of Heat sink ]
The above composition a was applied to the release surface of a polyester film (NP-100A, thickness 100 μm, PANAC co., ltd. Manufactured) using an applicator so that the thickness after drying became 250 μm, and then dried with warm air at 120 ℃ for 5 minutes, thereby forming a coating film (i.e., a composition layer). The residual rate of the solvent in the dried coating film is shown in table 1. Then, the coating film was heated by warm air under the conditions of a holding temperature of 80℃and a holding time of 10 seconds. Then, the coating film was cured at 180℃for 1 hour, whereby a heat sink with a polyester film was produced.
Example 2 >
A fin was manufactured in the same manner as in example 1 except that the drying time was changed to 10 minutes in example 1.
Example 3 >
A fin was manufactured in the same manner as in example 1 except that the drying time was changed to 1 minute in example 1.
Example 4 >
A fin was produced in the same manner as in example 1 except that the holding temperature was changed to 105 ℃ in example 1.
Example 5 >
A heat sink was produced in the same manner as in example 1, except that the holding temperature was changed to 130 ℃.
Example 6 >
A fin was produced in the same manner as in example 1 except that the holding temperature was changed to 137 ℃.
Example 7 >
A fin was produced in the same manner as in example 1 except that in example 1, the thermosetting compound A1 to be used was changed to the thermosetting compound A2 (molecular weight 340.42) described below and the holding time was changed to 30 seconds.
The structure of the thermosetting compound A2 is shown below.
[ chemical formula 5]
Example 8 >
A fin was produced in the same manner as in example 1, except that in example 1, the average particle diameter (D50) of the boron nitride particles used was changed to the value described in table 1 by the classification operation.
Example 9 >
A fin was produced in the same manner as in example 1, except that in example 1, the average particle diameter (D50) of the boron nitride particles used was changed to the value described in table 1 by the classification operation.
Comparative example 1 >
A fin was produced in the same manner as in example 1 except that the holding temperature was changed to 65 ℃ in example 1.
Comparative example 2 >
A heat sink was produced in the same manner as in example 1, except that the holding temperature was changed to 140 ℃.
< evaluation >
The void ratio and the film quality of each fin were evaluated by the following methods.
[ void fraction ]
The void fractions of the respective fins were measured according to the procedures described in the following (1) to (4), and the obtained void fractions were evaluated according to the following criteria. The evaluation results are shown in table 1 below.
(1) The heat sink is cut by irradiating a Focused Ion Beam (FIB).
(2) A Scanning Electron Microscope (SEM) was used to obtain a cross-sectional image of the above-described heat sink. Specifically, 5 field-of-view images were obtained in the cross section of the above-described heat sink. At 20,000 μm 2 ～200,000μm 2 Is adjusted so that the cross-sectional area and the void area can be appropriately calculated.
(3) From the above images, the ratio of the void area to the cross-sectional area (void area/cross-sectional area) was obtained.
(4) The obtained values were arithmetically averaged and then converted into percentages, whereby the void ratio of the fin was obtained.
(Standard)
A: less than 5%
B: more than 5 percent and less than 10 percent
C: more than 10 percent and less than 30 percent
D: more than 30% or not
[ membranous ]
The film quality of each fin was evaluated according to the following criteria. In the following standards, the substrate is referred to as a polyester film (NP-100A). The evaluation results are shown in table 1 below.
(Standard)
A: the heat sink can be peeled off from the substrate without breaking even when the heat sink is bent at a bending radius of 5cm or less by 90 degrees.
B: the heat sink can be peeled off from the base material, but if the heat sink is bent at 90 degrees with a bending radius of 5cm or less, the heat sink breaks.
C: the heat sink can be peeled off from the substrate, but the heat sink breaks as long as it is slightly bent.
D: the heat sink cannot be peeled off from the substrate, or the film itself cannot be formed.
TABLE 1
In table 1, "Tm" represents the melting point of the thermosetting compound.
In table 1, "Ts" represents the starting temperature of the thermosetting reaction of the thermosetting compound.
As is clear from table 1, the fins of examples 1 to 9 have smaller voids than the fins of comparative examples 1 to 2. It is also known that each of the fins of examples 1 to 9 has superior film quality as compared with each of the fins of comparative examples 1 to 2.
The invention of japanese patent application No. 2019-061230, filed on 3/27 in 2019, is incorporated by reference in its entirety into this specification. All documents, patent applications, and technical standards described in the present specification are incorporated by reference into the present specification to the same extent as if each document, patent application, and technical standard were specifically and individually described to be incorporated by reference.
Claims (8)
1. A method of manufacturing a heat sink, wherein the method comprises, in order:
a step of forming a composition layer by applying a composition containing a solvent, a thermosetting compound, and an inorganic filler, which is only an inorganic nitride particle, to a substrate;
a step of maintaining the surface temperature T of the composition layer within a range of Tm < T < Ts, with T being the surface temperature of the composition layer, tm being the melting point of the thermosetting compound, and Ts being the starting temperature of the thermosetting reaction of the thermosetting compound; and
A step of thermally curing the thermosetting compound in the composition layer to form a cured layer;
the step of forming the composition layer and the step of holding include a step of adjusting the residual rate of the solvent contained in the composition layer to 4.9 to 12 mass%.
2. The method for manufacturing a heat sink according to claim 1, wherein,
in the step of maintaining, the surface temperature T of the composition layer further satisfies the relation [ (Tm+Ts)/2 ]. Ltoreq.T < Ts.
3. The method for manufacturing a heat sink according to claim 1, wherein,
In the step of maintaining, the surface temperature T of the composition layer further satisfies the relationship of (Ts-10 ℃ C.). Ltoreq.T < Ts.
4. The method for manufacturing a heat sink according to claim 1, wherein,
the holding time in the holding step is 30 seconds or longer.
5. The method for manufacturing a heat sink according to claim 1, wherein,
the inorganic nitride particles have an average aspect ratio of 5 or more.
6. The method for manufacturing a heat sink according to claim 1, wherein,
the inorganic nitride particles have an average particle diameter of 30 μm or more.
7. The method for manufacturing a heat sink according to claim 1, wherein,
the inorganic nitride particles are boron nitride particles.
8. The method for manufacturing a heat sink according to claim 1, wherein,
the thermosetting compound contains at least 1 selected from the group consisting of an epoxy compound, a phenol compound, an imide compound, a melamine compound, an isocyanate compound, a urethane compound, an acrylate compound, and a methacrylate compound.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2019-061230 | 2019-03-27 | ||
| JP2019061230 | 2019-03-27 | ||
| PCT/JP2019/046395 WO2020194868A1 (en) | 2019-03-27 | 2019-11-27 | Method for manufacturing heat dissipation sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113631504A CN113631504A (en) | 2021-11-09 |
| CN113631504B true CN113631504B (en) | 2024-02-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201980094566.6A Active CN113631504B (en) | 2019-03-27 | 2019-11-27 | Method for manufacturing heat sink |
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| Country | Link |
|---|---|
| JP (1) | JP7167310B2 (en) |
| CN (1) | CN113631504B (en) |
| WO (1) | WO2020194868A1 (en) |
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| CN102140332A (en) * | 2010-01-29 | 2011-08-03 | 日东电工株式会社 | Thermally conductive sheet |
| CN102169856A (en) * | 2010-01-29 | 2011-08-31 | 日东电工株式会社 | Heat dissipation structure body |
| JP2011181650A (en) * | 2010-03-01 | 2011-09-15 | Panasonic Corp | Heat dissipation substrate and method of manufacturing the same |
| CN102770956A (en) * | 2010-02-23 | 2012-11-07 | 三菱电机株式会社 | Thermosetting resin composition, b-stage thermally conductive sheet, and power module |
| CN104024332A (en) * | 2011-11-02 | 2014-09-03 | 日立化成株式会社 | Epoxy resin composition, semi-hardened epoxy resin composition, hardened epoxy resin composition, resin sheet, prepreg, laminate sheet, metal substrate, wiring board, method for producing semi-hardened epoxy resin composition, and method for producing |
| JP2014196403A (en) * | 2013-03-29 | 2014-10-16 | 三菱電機株式会社 | Thermosetting resin composition, heat conductive resin sheet and its manufacturing method, and power module |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5423783B2 (en) | 2009-02-25 | 2014-02-19 | パナソニック株式会社 | Thermally conductive composition and heat dissipation plate, heat dissipation substrate, circuit module, and method for producing thermal conductive composition using the same |
| JP2017135150A (en) * | 2016-01-25 | 2017-08-03 | 日東シンコー株式会社 | Heat dissipation member and semiconductor module |
| JP6706100B2 (en) * | 2016-03-10 | 2020-06-03 | ナミックス株式会社 | Thermally conductive adhesive, dispensing adhesive, screen printing adhesive, and semiconductor device |
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2019
- 2019-11-27 CN CN201980094566.6A patent/CN113631504B/en active Active
- 2019-11-27 WO PCT/JP2019/046395 patent/WO2020194868A1/en active Application Filing
- 2019-11-27 JP JP2021508722A patent/JP7167310B2/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140332A (en) * | 2010-01-29 | 2011-08-03 | 日东电工株式会社 | Thermally conductive sheet |
| CN102169856A (en) * | 2010-01-29 | 2011-08-31 | 日东电工株式会社 | Heat dissipation structure body |
| CN102770956A (en) * | 2010-02-23 | 2012-11-07 | 三菱电机株式会社 | Thermosetting resin composition, b-stage thermally conductive sheet, and power module |
| JP2011181650A (en) * | 2010-03-01 | 2011-09-15 | Panasonic Corp | Heat dissipation substrate and method of manufacturing the same |
| CN104024332A (en) * | 2011-11-02 | 2014-09-03 | 日立化成株式会社 | Epoxy resin composition, semi-hardened epoxy resin composition, hardened epoxy resin composition, resin sheet, prepreg, laminate sheet, metal substrate, wiring board, method for producing semi-hardened epoxy resin composition, and method for producing |
| JP2014196403A (en) * | 2013-03-29 | 2014-10-16 | 三菱電機株式会社 | Thermosetting resin composition, heat conductive resin sheet and its manufacturing method, and power module |
Also Published As
| Publication number | Publication date |
|---|---|
| JP7167310B2 (en) | 2022-11-08 |
| WO2020194868A1 (en) | 2020-10-01 |
| JPWO2020194868A1 (en) | 2021-11-25 |
| CN113631504A (en) | 2021-11-09 |
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