CN113631504A - Method for manufacturing heat sink - Google Patents
Method for manufacturing heat sink Download PDFInfo
- Publication number
- CN113631504A CN113631504A CN201980094566.6A CN201980094566A CN113631504A CN 113631504 A CN113631504 A CN 113631504A CN 201980094566 A CN201980094566 A CN 201980094566A CN 113631504 A CN113631504 A CN 113631504A
- Authority
- CN
- China
- Prior art keywords
- compound
- heat sink
- thermosetting
- composition layer
- manufacturing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims description 77
- 150000001875 compounds Chemical class 0.000 claims abstract description 147
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 144
- 239000000203 mixture Substances 0.000 claims abstract description 131
- 239000002245 particle Substances 0.000 claims abstract description 86
- 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 21
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- -1 phenol compound Chemical class 0.000 claims description 60
- 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
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 239000012948 isocyanate Substances 0.000 claims description 6
- 238000001723 curing Methods 0.000 description 45
- 239000003795 chemical substances by application Substances 0.000 description 28
- 239000003822 epoxy resin Substances 0.000 description 18
- 229920000647 polyepoxide Polymers 0.000 description 18
- 238000001035 drying Methods 0.000 description 14
- 239000003505 polymerization initiator Substances 0.000 description 14
- 229920005989 resin Polymers 0.000 description 12
- 239000011347 resin Substances 0.000 description 12
- 238000001029 thermal curing Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 10
- 125000000217 alkyl group Chemical group 0.000 description 9
- 239000000123 paper Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 238000013007 heat curing Methods 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 5
- 238000007664 blowing Methods 0.000 description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 125000000466 oxiranyl group Chemical group 0.000 description 5
- 239000011800 void material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 206010040844 Skin exfoliation Diseases 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 229920003986 novolac Polymers 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 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
- 150000001412 amines Chemical class 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 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
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007756 gravure coating Methods 0.000 description 2
- 239000004615 ingredient Substances 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
- 229920006267 polyester film 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
- 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
- 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
- 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
- 229920000178 Acrylic resin Polymers 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 229910017389 Fe3N 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
- 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
- 150000008065 acid anhydrides 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
- 239000012298 atmosphere Substances 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
- 238000007611 bar coating method Methods 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
- 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
- 230000001186 cumulative effect Effects 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 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
- 238000007646 gravure printing Methods 0.000 description 1
- 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 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910052742 iron Inorganic materials 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
- 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
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000005011 phenolic resin Substances 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
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 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
- 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
- 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
Abstract
The invention provides a manufacturing method of a radiating fin, which sequentially comprises the following steps: a step of coating a composition containing a solvent, a thermosetting compound, and inorganic nitride particles on a substrate to form a composition layer; a step of maintaining the surface temperature T of the composition layer within a range of Tm < T < Ts, where T represents the surface temperature of the composition layer, Tm represents the melting point of the thermosetting compound, and Ts represents 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.
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, there are devices that generate heat of 150 ℃ or higher in a power device, a CPU (Central Processing Unit), or a Light Emitting Diode (LED) backlight. If heat generated from the heating element is accumulated inside the electronic device, a malfunction of the electronic device may occur. Therefore, various techniques have been studied in order to release heat emitted from the heat generating body.
For example, japanese patent application laid-open No. 2018-115275 discloses a method for producing a curable material, which includes the steps of: a curable material is obtained by blending a curable compound and boron nitride aggregated particles which are aggregates of primary particles of boron nitride having an aspect ratio of 11 or more and have a compressive strength of 2.7MPa or more when compressed by 30%, and not blending boron nitride aggregated particles which are aggregates of primary particles of boron nitride having an aspect ratio of less than 11.
Jp 2011-181650 a discloses a method for manufacturing a heat dissipation substrate, which includes: 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 in the uncured composition; a convection step of heating the uncured composition to at least one of a crystallization temperature and a melting point of the crystalline epoxy resin or higher to form a liquid state, and causing convection between the inorganic fillers; and a thermosetting step of thermally curing the uncured composition to form a heat conductive layer, wherein the content of the inorganic filler is 66 Vol% or more and 90 Vol% or less, and the lead frame are embedded in the heat conductive layer in a state of being in contact with each other through 1 or more contact portions.
International publication No. 2017/111115 discloses a semi-curable heat conductive film formed through the following steps: a resin composition comprising a curable compound (alpha), a curing agent (beta), a liquid crystal polymer (gamma) which forms a liquid crystal phase at 190 ℃ or lower, and a filler (delta), and a cast product of the resin composition are freed from the solvent.
Disclosure of Invention
Technical problem to be solved by the invention
In the conventional heat sink, voids (pores) having low thermal conductivity may be formed. If the proportion of voids included in the heat sink increases, the thermal conductivity of the heat sink may decrease. 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 it is difficult to sufficiently reduce the voids of the heat sink containing the inorganic nitride particles particularly by the conventional methods described in, for example, japanese patent application laid-open nos. 2018-115275 and 2017/111115.
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 that can form a heat sink with few voids.
Means for solving the technical problem
The following means are included in the means for solving the above problems.
< 1 > a method of manufacturing a heat sink, comprising in sequence: a step of coating a composition containing a solvent, a thermosetting compound, and inorganic nitride particles on a substrate to form a composition layer; a step of maintaining the surface temperature T of the composition layer within a range of Tm < T < Ts, where T represents the surface temperature of the composition layer, Tm represents the melting point of the thermosetting compound, and Ts represents 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.
< 2 > the method for manufacturing a heat sink according to < 1 >, wherein,
the method further includes a step of adjusting the residual ratio of the solvent contained in the composition layer to 1 to 10 mass% between the step of forming the composition layer and the step of holding.
< 3 > the method for manufacturing a heat sink according to < 1 > or < 2 >, wherein,
in the holding step, the surface temperature T of the composition layer further satisfies the relationship of [ (Tm + Ts)/2] T < Ts.
< 4 > the production method of a heat sink according to any one of < 1 > to < 3 >, wherein,
in the holding step, the surface temperature T of the composition layer further satisfies the relationship (Ts-10 ℃) T < Ts.
< 5 > the production method of a heat sink according to any one of < 1 > to < 4 >, wherein,
the holding time in the holding step is 30 seconds or more.
< 6 > the production method of 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.
< 7 > the production method of 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.
< 8 > the production method of a heat sink according to any one of < 1 > to < 7 >, wherein,
the inorganic nitride particles are boron nitride particles.
< 9 > the production method of 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 an aspect of the present invention, a method for manufacturing a heat sink can be provided, which can form a heat sink with few voids.
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 implemented by appropriately changing the embodiments within the scope of the object of the present invention.
In the present invention, the numerical range expressed by the term "to" refers to a range including numerical values before and after the term "to" as a lower limit value and an upper limit value. In the numerical ranges recited in the present invention, the upper limit or the lower limit recited in a certain numerical range may be replaced with the upper limit or the lower limit recited in another numerical range recited in a stepwise manner. In the numerical ranges of the present invention, the upper limit or the lower limit described in a certain numerical range may be replaced with the values shown in the examples.
In the present invention, the amount of each component in the composition refers to the total amount of a plurality of substances present in the composition unless otherwise specified, when a plurality of substances corresponding to each component are present in the composition.
In the present invention, a combination of 2 or more preferred embodiments is a more preferred embodiment.
In the present invention, the term "process" includes not only an independent process but also a process that can achieve the intended purpose of the process even when it cannot be clearly distinguished from other processes.
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 content mass" means the total mass of components other than the solvent.
< manufacturing method of heat sink >
The manufacturing method of the radiating fin related by the invention sequentially comprises the following steps: a step of applying a composition containing a solvent, a thermosetting compound, and inorganic nitride particles onto a substrate to form a composition layer (hereinafter referred to as "forming step"); a step of maintaining the surface temperature T of the composition layer within a range of Tm < T < Ts, where T is a surface temperature of the composition layer, Tm is a melting point of the thermosetting compound, and Ts is a start temperature of a thermosetting reaction of the thermosetting compound (hereinafter referred to as "maintaining step"); 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 heat sink sheet according to the present invention exerts the above-described effects is not clear, but is presumed as follows.
The method for manufacturing a heat sink sheet 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 being less than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound, thereby improving the fluidity of the thermosetting compound while suppressing thermosetting of the thermosetting compound. Further, the affinity between the thermosetting compound having improved fluidity and the surface of the inorganic nitride particles is also improved. Therefore, it is considered that voids in the composition layer (for example, voids formed between the inorganic nitride particles and voids formed around the inorganic nitride particles) can be filled by maintaining the surface temperature (T) of the composition layer within a specific temperature range (Tm < T < Ts). In the method for manufacturing a heat sink sheet according to the present invention, it is considered that the thermosetting compound in the composition layer having a small number of voids is thermally cured after the voids in the composition layer are reduced in the holding step, and therefore a heat sink sheet having a small number of voids can be formed.
The respective steps of the method for manufacturing the heat sink sheet according to the present invention will be described below.
[ Forming Process ]
The method for manufacturing a heat sink according to the present invention includes a step (forming step) of applying a composition containing a solvent, a thermosetting compound, and inorganic nitride particles onto a base material to form a composition layer.
[ 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 kind of solvent alone or 2 or more kinds of solvents.
The content of the solvent is not limited, and may be appropriately set according to, for example, the composition of each component contained in the composition and the coating method. The content of the solvent is preferably 30 to 80% by mass, more preferably 50 to 70% by mass, based on the total mass of the composition.
(thermosetting compound)
The thermosetting compound is a compound that can be cured by a chemical reaction under heating, and unless otherwise specified, includes a compound that forms a molecular skeleton of a product (i.e., a cured product) during the thermal curing reaction. The thermosetting compound may be 1 kind of compound that is thermally cured alone, may be a compound that is thermally cured by using 2 or more kinds of compounds in combination, or may be a compound that is thermally cured in the presence of a known additive.
The form of the thermosetting compound is not limited to a monomer, and includes, for example, an oligomer, a prepolymer, and a polymer. The thermosetting compound is preferably a monomer from the viewpoint of easy addition of 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 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. Each of the compounds described above further contains 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, further 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 viewpoint of curability and film quality, the epoxy compound is preferably a compound having at least 2 oxirane groups in one molecule, more preferably an aromatic compound having at least 2 oxirane groups in one molecule, and particularly preferably a compound represented by the following formula (I).
[ chemical formula 1]
In the formula (I), R1、R2、R3、R4、R5、R6、R7And R8Each independently represents a hydrogen atom or an alkyl group.
In the formula (I), from R1、R2、R3、R4、R5、R6、R7And R8The 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 the formula (I), R is preferred1、R4、R5And R8Each independently represents a hydrogen atom or an alkyl group having 1 to 3 carbon atoms, R2、R3、R6And R7Is a hydrogen atom. In the formula (I), R is more preferred1、R4、R5And R8Each independently is a hydrogen atom or a methyl group, R2、R3、R6And R7Is a hydrogen atom.
The compound represented by the above formula (I) can be obtained, for example, as YX4000 manufactured by Mitsubishi Chemical Corporation.
When 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, and more preferably a compound represented by the following formula (II), from the viewpoint of curability and film quality.
[ chemical formula 2]
In the formula (II), R11And R12Each independently represents a hydrogen atom, an alkyl group or a hydroxyl group, R13、R14、R15And R16Each independently represents a hydrogen atom or an alkyl group.
In the formula (II), R11And R12Each independently preferably represents a hydrogen atom, an alkyl group having 1 to 3 carbon atoms, or a hydroxyl group, and more preferably represents a hydrogen atom or a hydroxyl group.
In the formula (II), R13、R14、R15And R16Each independently preferably represents a hydrogen atom or an alkyl group having 1 to 3 carbon atoms, and more preferably represents 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 epoxy resin monomers and acrylic resin monomers described in paragraph 0028 of japanese patent No. 4118691, epoxy compounds described in paragraphs 0006 to 0011 of japanese patent application laid-open No. 2008-13759, and epoxy resin monomers 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 resins, phenol resins, polyimide resins, cresol resins, melamine resins, unsaturated polyester resins, isocyanate resins, and thermosetting polyurethane resins.
Among the above, the thermosetting resin is preferably an epoxy resin from the viewpoint of a small thermal expansion coefficient and excellent heat resistance and adhesiveness.
The epoxy resin is not limited, and a known epoxy resin can be used. Examples of the epoxy resin include a bifunctional epoxy resin and a novolac-type epoxy resin.
Examples of the bifunctional epoxy resin include a bisphenol a type epoxy resin, a bisphenol F type epoxy resin, and a bisphenol S type epoxy resin.
Examples of the novolak type epoxy resin include a phenol novolak type epoxy resin and a 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 acryloyl group, a methacryloyl group, an ethylene oxide group and a vinyl group, and an ethylene oxide group is more preferred.
The thermosetting compound may have 1 kind of polymerizable group alone or 2 or more kinds of polymerizable groups. The number of the 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, and more preferably 3 or more, from the viewpoint of excellent heat resistance of the cured product. The upper limit of the number of the 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 acryloyl group, a methacryloyl group, an oxirane group, and a vinyl group, and more preferably contains a compound having an oxirane group.
From the viewpoint of easy addition of functions such as heat resistance, 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.
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, within a range of 100 or more, preferably 200 or more.
The composition may contain 1 kind of the thermosetting compound alone or 2 or more kinds of the thermosetting compounds.
From the viewpoint of the thermal 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 mass%, more preferably 20 to 50 mass%, and particularly preferably 20 to 40 mass%, based on 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)3N4) Silicon nitride (Si)3N4) Gallium nitride (GaN), indium nitride (InN), aluminum nitride (AlN), chromium nitride (Cr)2N), copper nitride (Cu)3N), iron nitride (Fe)4N or Fe3N), lanthanum nitride (Lan), lithium nitride (Li)3N), magnesium nitride (Mg)3N2) Molybdenum nitride (Mo)2N), niobium nitride (NbN), tantalum nitride (TaN), titanium nitride (TiN), tungsten nitride (W)2N、WN2Or WN), Yttrium Nitride (YN), and zirconium nitride (ZrN).
From the viewpoint 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 viewpoint 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 thermal conductivity of the heat sink can be improved.
The upper limit of the average aspect ratio of the inorganic nitride particles is not limited. From the viewpoint of particle dispersibility in the composition, the average aspect ratio of the inorganic nitride particles is preferably 20 or less, and more preferably 15 or less.
The average aspect ratio of the inorganic nitride particles is measured by the following method.
(1) Using a Scanning Electron Microscope (SEM), images of 100 inorganic nitride particles randomly selected were obtained.
(2) The major and minor diameters of the inorganic nitride particles were measured. In the present invention, the "major axis of the inorganic nitride particle" refers to the length of the longest line segment among line segments connecting arbitrary two points on the contour line of the inorganic nitride particle. For example, in the case where the inorganic nitride particles are perfect circles in the above image, the major axis of the inorganic nitride particles means the diameter of the inorganic nitride particles. In the present invention, the "minor axis of the inorganic nitride particle" refers to the length of the longest line segment among line segments that are orthogonal to the line segment defining the major axis and that connect arbitrary two points on the contour line of the inorganic nitride particle.
(3) The ratio of the major axis to the minor axis (major axis/minor axis) of each of the inorganic nitride particles was determined.
(4) The arithmetic mean 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 average particle diameter of the inorganic nitride particles is 10 μm or more, whereby the thermal conductivity of the heat sink can be further improved.
The average particle diameter of the inorganic nitride particles is preferably 200 μm or less, and more preferably 150 μm or less. When the average particle diameter of the inorganic nitride particles is 200 μm or less, the surface irregularities of the heat sink can be reduced, and as a result, the heat dissipation property of the heat sink is increased.
In the present invention, the average particle diameter of the inorganic nitride particles is a particle diameter (D50, median particle diameter) at which the number-based cumulative particle diameter becomes 50% in a number-based particle diameter distribution measured using a laser diffraction-type particle diameter distribution measuring apparatus (for example, MT3300II, manufactured by microtrac bel Corporation).
The composition may contain 1 kind of inorganic nitride particle alone, or may contain 2 or more kinds of inorganic nitride particles.
From the viewpoint of the thermal conductivity of the heat sink, the content of the inorganic nitride particles is preferably 50 to 80 mass%, more preferably 60 to 80 mass%, with respect to the total solid content mass in the composition.
From the viewpoint of the thermal conductivity of the heat sink, the content of the inorganic nitride particles is preferably 200 to 400 parts by mass, and more preferably 250 to 350 parts by mass, with respect 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 accelerating 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 agents
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 acryloyl group, a methacryloyl 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 acryloyl group, a methacryloyl group, an amino group, and a thiol group.
The curing agent is preferably a compound having 2 or more of the above functional groups, and more preferably a compound having 2 or 3 of the above 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 curing agent, an acrylic curing agent, a phenol curing agent or an amine curing agent.
The composition may contain 1 curing agent alone or 2 or more 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 in the composition.
Curing accelerators
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 single curing accelerator or 2 or more 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 solid content in the composition.
Polymerization initiators
The polymerization initiator is not limited, and a known polymerization initiator can be used. When the thermosetting compound has an acryloyl group or a methacryloyl group, the polymerization initiator is preferably the polymerization initiator described in paragraph 0062 of jp 2010-125782 a or the polymerization initiator described in paragraph 0054 of jp 2015-052710 a.
The composition may contain 1 polymerization initiator alone or 2 or more polymerization initiators.
When the composition contains a polymerization initiator, the content of the polymerization initiator is preferably 0.1 to 50% by mass based on the total solid content 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 substrate 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 paper, and high-quality paper), resin film (e.g., polyolefin and polyester), and laminated paper in which paper and resin film are laminated. Examples of the polyolefin include polyethylene and polypropylene. Examples of the polyester include polyethylene terephthalate (PET).
The paper used as the release liner paper may be paper subjected to a release treatment. The paper subjected to the peeling treatment can be formed by further performing the peeling treatment on one or both surfaces of the paper subjected to the sealing treatment, for example. The sealing treatment can be performed using, for example, clay or polyvinyl alcohol. The peeling treatment can be performed using, for example, a silicone resin.
The thickness of the base material is not limited, and may be set appropriately within a range of, for example, 10 to 300. mu.m.
[ coating method ]
The coating method is not limited, and a known method can be used. Examples of the coating method include a roll coating method, a gravure printing method, a spin coating method, a bar coating method, an extrusion coating method, a direct gravure coating method, a reverse gravure coating method, a die coating method, a spray coating method, and an ink jet method.
The coating amount of the composition is not limited, and may be appropriately set according to, for example, the composition of the composition, the coating method, and the thickness of the target composition layer. The coating amount of the composition after drying is preferably 50cm3/m2～400cm3/m2More preferably 100cm3/m2～250cm3/m2。
[ holding step ]
The method for manufacturing a heat sink sheet according to the present invention includes a step (holding step) of holding the surface temperature T of the composition layer within a range of Tm < T < Ts, where T represents the surface temperature of the composition layer, Tm represents the melting point of the thermosetting compound, and Ts represents the start temperature of the thermosetting reaction of the thermosetting compound. It is considered that, by the manufacturing method of a heat sink sheet according to the present invention including the holding step, the fluidity of the thermosetting compound can be improved while suppressing the progress of thermosetting of the thermosetting compound, and therefore, the voids in the composition layer can be filled. Therefore, the heat sink with less 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 start 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 starting point of the holding step is a point of time when the surface temperature (T) of the composition layer falls within a range of Tm < T < Ts.
The surface temperature (T) of the composition layer preferably satisfies the relationship [ (Tm + Ts)/2] T < Ts, more preferably (Ts-20 ℃) T < Ts, still more preferably (Ts-10 ℃) T < Ts, and particularly preferably (Ts-5 ℃) T < Ts, on the basis of satisfying the above relationship (Tm < T < Ts). In the holding step, the smaller the difference between the surface temperature (T) of the composition layer and the start temperature (Ts) of the thermosetting reaction of the thermosetting compound, the more the voids included in the heat sink can be reduced. Furthermore, the film quality of the heat sink can be improved.
The relationship represented by [ (Tm + Ts)/2] ≦ 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 thermal curing reaction of the thermosetting compound and is less than the starting temperature (Ts) of the thermal curing reaction of the thermosetting compound.
The relationship represented by (Ts-20 ℃) T < Ts means that the surface temperature (T) of the composition layer is a temperature which is 20 ℃ or more lower than the starting temperature (Ts) of the thermal curing reaction of the thermosetting compound and is less than the starting temperature (Ts) of the thermal curing reaction of the thermosetting compound.
The relationship represented by (Ts-10 ℃) 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 thermal curing reaction of the thermosetting compound and is less than the starting temperature (Ts) of the thermal curing 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 thermal curing reaction of the thermosetting compound and is less than the starting temperature (Ts) of the thermal curing 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 relationship (Tm < T < Ts). When the surface temperature (T) of the composition layer is within the above range, voids contained in the heat sink can be further reduced. Furthermore, 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 of measuring using a non-contact thermometer (e.g., 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 compound means a temperature measured by the following method. First, each thermosetting compound weighed according to the content ratio of each thermosetting compound in the composition layer is prepared. Next, after each thermosetting compound was added to the petri dish, the mixture of each thermosetting compound was heated using METTLER TOLEDO (METTLER TOLEDO). The melting point of the thermosetting compound is defined as the temperature at which the mixture of the respective thermosetting compounds added to the petri dish is melted to be transparent.
The starting temperature (Ts) of the thermosetting reaction of the thermosetting compound is measured by the following method.
(1) The DSC curve of the composition layer was obtained by Differential Scanning Calorimetry (DSC). The content of the solvent in the composition layer used as the 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) caused by the thermosetting reaction of the thermosetting compound starts to occur is determined. Here, the "temperature at which the peak starts to be generated" refers to a temperature at an intersection of a straight line extending from a base line on the low temperature side to the high temperature side and a tangent line drawn at a point of the curve on the low temperature side of the peak where the slope is the largest.
(3) The temperature at which the peak starts to occur is defined as the starting temperature of the thermosetting reaction of the thermosetting compound.
In the holding step, the temperature at which the reactive species are generated, which becomes the starting point of the thermosetting reaction of the thermosetting compound, or the temperature at which the starting reaction of the thermosetting compound is generated 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 thermal curing contains a polymerization initiator, the pyrolysis temperature of the polymerization initiator can be used as an index of the start temperature (Ts) of the thermal curing reaction of the thermosetting compound. The temperature condition in the holding step can be appropriately set according to the index.
The method of maintaining the surface temperature (T) of the composition layer within the above-described temperature ranges is not limited, and a known method can be used. Examples of the above method include a method of adjusting an atmospheric temperature, a method of blowing warm air to the composition layer, and a method of irradiating the composition layer with electromagnetic waves (for example, infrared rays). 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 maintaining the surface temperature (T) of the composition layer within the above-described respective temperature ranges is preferably a method of heating with warm air.
The holding time is not limited as long as it is 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 setting the holding time to 10 seconds or more, the voids included in the heat sink can be further reduced. In the present invention, the "holding time" refers to a time for which the surface temperature (T) at any one of the composition layers is held within the above-mentioned specific temperature range (for example, Tm < T < Ts).
From the viewpoint of productivity and facility cost, the holding time is preferably 120 seconds or less, and more preferably 60 seconds or less.
In the method for manufacturing the 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 manufacturing a heat sink sheet according to the present invention includes a step (thermosetting step) of thermosetting the thermosetting compound in the composition layer to form a cured layer. In the method for manufacturing a heat sink sheet according to the present invention, the thermosetting compound in the composition layer is thermally cured after the holding step, and therefore a heat sink sheet with few voids can be formed.
The method of heat curing is not limited as long as it is a method capable of heat curing the thermosetting compound, and a known method can be used. Examples of the method of heat curing include a method of adjusting the temperature of an atmosphere, a method of blowing warm air to the composition layer, and a method of irradiating the composition layer with electromagnetic waves (e.g., infrared rays). 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 heat curing method is preferably a method of heating with warm air.
The heating temperature in the thermosetting step is not limited as long as it is a temperature at which the thermosetting compound can be thermally cured, and may be appropriately set according to the composition of the composition layer, for example. From the viewpoint of efficiently performing the thermosetting reaction, the heating temperature in the thermosetting step is preferably not lower than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound. The heating temperature in the thermosetting step may be set appropriately, for example, within a range of 50 to 200 ℃. The heating time in the thermosetting step is not limited, and may be appropriately set according to the heating temperature.
Also, the curing reaction may be a semi-curing reaction. That is, the obtained cured layer 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 thermosetting step may be performed as many times as necessary without departing from the spirit of the present invention. In the case where the thermosetting step is performed a plurality of times, the conditions of the respective thermosetting steps may be the same or different from each other.
[ drying Process ]
The method for manufacturing a heat sink sheet according to the present invention preferably includes a step (hereinafter, also referred to as "drying step") of adjusting the residual ratio of the solvent contained in the composition layer to 0.5 to 12 mass% between the step (forming step) of forming the composition layer and the step (holding step) of holding. By adjusting the residual ratio 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 voids included in the heat sink can be further reduced.
When the method for manufacturing a heat sink sheet according to the present invention includes a drying step, the drying step and the holding step are not limited to separate 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 the point when the surface temperature (T) of the composition layer reaches the 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 ratio 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 voids included in the heat sink can be further reduced. Further, since the residual ratio of the solvent in the obtained heat dissipating sheet can be reduced, the film quality of the heat dissipating sheet can be improved.
The residual ratio 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 the solvent was determined by gas chromatography-mass spectrometry (GC-MS).
In the drying step, a method for adjusting the residual ratio 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) to the composition layer is preferable. In the method of blowing air to the composition layer, the temperature of the air is preferably 23 to 140 ℃. The time of the air 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 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 smaller than the starting temperature (Ts) of the thermosetting reaction of the thermosetting compound, voids contained in the heat sink can be further reduced.
In the method for manufacturing the heat sink sheet 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 step is performed a plurality of times, the conditions of the drying steps may be the same or different from each other.
< Heat sink >
The heat sink formed by the method for manufacturing a heat sink according to the present invention has excellent heat dissipation properties because of few voids. 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 contacting with various heat generating elements. For example, by bringing the heat sink into contact with various components constituting the electronic apparatus, heat generated in the components can be efficiently released. Examples of the components include a power device and a CPU. The heat sink sheet formed by the method for manufacturing a heat sink sheet according to the present invention may be used by being disposed between a heat generating body such as a power device and a heat radiating body such as a heat sink sheet.
The thickness of the heat sink is not limited, and may be set appropriately according to the purpose, for example. The thickness of the heat sink is preferably in the range of 50 μm to 200 μm from the viewpoint of thermal conductivity.
Examples
The present invention will be described in detail below with reference to examples, but the present invention is not limited thereto. Unless otherwise specified, "part" and "%" are based on mass. 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.
(ingredient)
Thermosetting compound a1 (compound having the following structure, molecular weight 372.42, QE-2405, manufactured by Combi-Blocks inc.): 17 parts by mass
[ chemical formula 3]
Thermosetting compound B (compound having the following structure, molecular weight 354.45, YX4000, manufactured by Mitsubishi Chemical Corporation): 34 parts by mass
[ chemical formula 4]
Methyl ethyl ketone: 65 parts by mass
TPP (triphenylphosphine: curing accelerator): 0.6 part by mass
Boron nitride particles (inorganic nitride particles, HP-40MF100, MIZUSHIMA ferrocoalloy co., ltd., manufactured): 51 parts by mass
[ production of Heat radiating fins ]
The above-mentioned composition a was applied to a release surface of a polyester film (NP-100A, thickness 100 μm, PANAC co., ltd., manufactured) using an applicator so that the dried thickness became 250 μm, and then dried with warm air at 120 ℃ for 5 minutes, thereby forming a coating film (i.e., composition layer). The residual ratio of the solvent in the dried coating film is shown in table 1. Subsequently, the coating film was heated with warm air at a holding temperature of 80 ℃ for 10 seconds. Then, the coating film was cured at 180 ℃ for 1 hour to produce a polyester film-attached heat sink.
< example 2 >
A heat sink was produced in the same manner as in example 1, except that the drying time was changed to 10 minutes in example 1.
< example 3 >
A heat sink was produced in the same manner as in example 1, except that the drying time was changed to 1 minute in example 1.
< example 4 >
A heat sink 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 heat sink was produced in the same manner as in example 1, except that the holding temperature was changed to 137 ℃ in example 1.
< example 7 >
A heat sink was produced in the same manner as in example 1, except that the thermosetting compound a1 used in example 1 was changed to the following thermosetting compound a2 (molecular weight 340.42) 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 heat sink was produced in the same manner as in example 1, except that the average particle diameter (D50) of the boron nitride particles used in example 1 was changed to the value shown in table 1 by classification.
< example 9 >
A heat sink was produced in the same manner as in example 1, except that the average particle diameter (D50) of the boron nitride particles used in example 1 was changed to the value shown in table 1 by classification.
< comparative example 1 >
A heat sink 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 porosity and film quality of each of the heat dissipating fins were evaluated by the following methods.
[ void fraction ]
The porosity of each fin was measured according to the procedures described in the following (1) to (4), and the obtained porosity was evaluated according to the following criteria. The evaluation results are shown in table 1 below.
(1) The heat sink was cut by irradiating a Focused Ion Beam (FIB).
(2) A cross-sectional image of the above-described heat sink was obtained using a Scanning Electron Microscope (SEM). Specifically, 5 fields of view images were obtained in the cross section of the above-described fin. At 20,000 μm2～200,000μm2Is adjusted so that the cross-sectional area and the void area can be appropriately calculated.
(3) From the 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, thereby obtaining the void ratio of the fin.
(Standard)
A: less than 5 percent
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 cannot be determined
[ film quality ]
The film quality of each fin was evaluated according to the following criteria. In the following standards, the substrate is a polyester film (NP-100A). The evaluation results are shown in table 1 below.
(Standard)
A: the heat sink sheet can be peeled from the base material without breaking even if the heat sink sheet is bent at 90 degrees with a bending radius of 5cm or less.
B: the heat sink can be peeled off from the base material, but when the heat sink is bent 90 degrees at a bending radius of 5cm or less, the heat sink is broken.
C: the heat sink can be peeled off from the base material, but the heat sink is broken by slightly bending the heat sink.
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 heat curing reaction of the thermosetting compound.
As is apparent from table 1, the fins of examples 1 to 9 have fewer voids than the fins of comparative examples 1 to 2. It is also known that the heat dissipating fins of examples 1 to 9 have superior film qualities as compared with the heat dissipating fins of comparative examples 1 to 2.
The invention of japanese patent application No. 2019-061230, filed on 27.3.2019, is incorporated in its entirety into this specification by reference. 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 was specifically and individually incorporated by reference.
Claims (9)
1. A method of manufacturing a heat sink, wherein the method of manufacturing comprises, in order:
a step of coating a composition containing a solvent, a thermosetting compound, and inorganic nitride particles on a substrate to form a composition layer;
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
and a step of forming a cured layer by thermally curing the thermosetting compound in the composition layer.
2. The method of manufacturing a heat sink according to claim 1,
the method further includes a step of adjusting the residual ratio of the solvent contained in the composition layer to 1 to 10 mass% between the step of forming the composition layer and the step of holding.
3. The method of manufacturing a heat sink according to claim 1 or 2,
in the step of holding, the surface temperature T of the composition layer further satisfies the relationship [ (Tm + Ts)/2] ≦ T < Ts.
4. The method of manufacturing a heat sink according to any one of claims 1 to 3,
in the step of carrying out the holding, the surface temperature T of the composition layer further satisfies the relationship (Ts-10 ℃) T < Ts.
5. The method of manufacturing a heat sink according to any one of claims 1 to 4,
the holding time in the holding step is 30 seconds or more.
6. The method of manufacturing a heat sink according to any one of claims 1 to 5,
the inorganic nitride particles have an average aspect ratio of 5 or more.
7. The method of manufacturing a heat sink according to any one of claims 1 to 6,
the inorganic nitride particles have an average particle diameter of 30 [ mu ] m or more.
8. The method of manufacturing a heat sink according to any one of claims 1 to 7,
the inorganic nitride particles are boron nitride particles.
9. The method of manufacturing a heat sink according to any one of claims 1 to 8,
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 true CN113631504A (en) | 2021-11-09 |
| CN113631504B 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 |
Family Cites Families (3)
| 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 JP JP2021508722A patent/JP7167310B2/en active Active
- 2019-11-27 WO PCT/JP2019/046395 patent/WO2020194868A1/en active Application Filing
- 2019-11-27 CN CN201980094566.6A patent/CN113631504B/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 |
|---|---|
| JPWO2020194868A1 (en) | 2021-11-25 |
| WO2020194868A1 (en) | 2020-10-01 |
| CN113631504B (en) | 2024-02-09 |
| JP7167310B2 (en) | 2022-11-08 |
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