WO2021153688A1 - コンパウンド、成形体、及びコンパウンドの硬化物 - Google Patents
コンパウンド、成形体、及びコンパウンドの硬化物 Download PDFInfo
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- WO2021153688A1 WO2021153688A1 PCT/JP2021/003087 JP2021003087W WO2021153688A1 WO 2021153688 A1 WO2021153688 A1 WO 2021153688A1 JP 2021003087 W JP2021003087 W JP 2021003087W WO 2021153688 A1 WO2021153688 A1 WO 2021153688A1
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- Prior art keywords
- compound
- epoxy resin
- resin
- metal powder
- resin composition
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 108
- 239000003822 epoxy resin Substances 0.000 claims abstract description 92
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 91
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- 239000000843 powder Substances 0.000 claims abstract description 75
- 239000011342 resin composition Substances 0.000 claims abstract description 62
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- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 6
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- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 description 1
- SWSBIGKFUOXRNJ-CVBJKYQLSA-N ethene;(z)-octadec-9-enamide Chemical compound C=C.CCCCCCCC\C=C/CCCCCCCC(N)=O.CCCCCCCC\C=C/CCCCCCCC(N)=O SWSBIGKFUOXRNJ-CVBJKYQLSA-N 0.000 description 1
- ZJOLCKGSXLIVAA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O ZJOLCKGSXLIVAA-UHFFFAOYSA-N 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 235000013872 montan acid ester Nutrition 0.000 description 1
- PECBPCUKEFYARY-ZPHPHTNESA-N n-[(z)-octadec-9-enyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCCCCCCC\C=C/CCCCCCCC PECBPCUKEFYARY-ZPHPHTNESA-N 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- DJWFNQUDPJTSAD-UHFFFAOYSA-N n-octadecyloctadecanamide Chemical compound CCCCCCCCCCCCCCCCCCNC(=O)CCCCCCCCCCCCCCCCC DJWFNQUDPJTSAD-UHFFFAOYSA-N 0.000 description 1
- NXPPAOGUKPJVDI-UHFFFAOYSA-N naphthalene-1,2-diol Chemical compound C1=CC=CC2=C(O)C(O)=CC=C21 NXPPAOGUKPJVDI-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- AJDORVSWJRNUEA-UHFFFAOYSA-N octadecanoyloxymethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCOC(=O)CCCCCCCCCCCCCCCCC AJDORVSWJRNUEA-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 150000003003 phosphines Chemical class 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- IYMSIPPWHNIMGE-UHFFFAOYSA-N silylurea Chemical compound NC(=O)N[SiH3] IYMSIPPWHNIMGE-UHFFFAOYSA-N 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229940098697 zinc laurate Drugs 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- ODNJVAVDJKOYFK-GRVYQHKQSA-L zinc;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Zn+2].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O.CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O ODNJVAVDJKOYFK-GRVYQHKQSA-L 0.000 description 1
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
Definitions
- the present invention relates to a compound, a molded product, and a cured product of the compound.
- Compounds containing metal powders and resin compositions are used as raw materials for various industrial products, depending on the physical characteristics of the metal powders.
- the compound is used as a raw material for an inductor, a sealing material, an electromagnetic wave shield (EMI shield), a bond magnet, or the like (see Patent Document 1 below).
- a molded product When manufacturing an industrial product from a compound, a molded product may be produced by bringing the compound into close contact with a metal member and curing the compound, and then the molded product may be heated. In the step of heating the molded product, cracks are likely to be formed in the molded product due to the difference in the coefficient of thermal expansion between the cured product of the compound and the metal member, steam explosion inside the package, and the like. Therefore, it is required to improve the reflow resistance of the molded product.
- the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a compound capable of forming a molded product having excellent reflow resistance, a molded product using the same, and a cured product of the compound. ..
- the compound according to one aspect of the present invention comprises a metal powder and a resin composition containing an epoxy resin, a curing agent and a plasticizer, and the plasticizer contains core-shell rubber particles.
- the molded product according to one aspect of the present invention includes the above compound.
- the cured product according to one aspect of the present invention is a cured product of the above compound.
- a compound capable of forming a molded product having excellent reflow resistance, a molded product using the compound, and a cured product of the compound are provided.
- the compound according to the present embodiment includes a metal powder and a resin composition.
- the metal powder may contain, for example, at least one selected from the group consisting of elemental metals, alloys, amorphous powders, and metal compounds.
- the resin composition contains at least an epoxy resin, a curing agent and a plasticizer.
- the plasticizer contains core-shell rubber particles. In the compound, metal powder, epoxy resin, curing agent and plasticizer are mixed.
- the resin composition may further contain a curing accelerator, a mold release agent, an additive and the like as other components.
- the resin composition is a component that can include an epoxy resin, a curing agent, a plasticizer, a curing accelerator, a mold release agent, and an additive, and is a remaining component (nonvolatile component) excluding an organic solvent and a metal powder. May be.
- the additive is a component of the rest of the resin composition excluding the resin, the mold release agent, the curing agent, and the curing accelerator. Additives are, for example, coupling agents, flame retardants, lubricants and the like.
- the compound may be a powder (compound powder).
- the compound may include a metal powder and a resin composition adhering to the surface of each metal particle constituting the metal powder.
- the resin composition may cover the entire surface of the particles, or may cover only a part of the surface of the particles.
- the compound may comprise an uncured resin composition and a metal powder.
- the compound may include a semi-cured product of the resin composition (for example, a B-stage resin composition) and a metal powder.
- the compound may comprise both an uncured resin composition and a semi-cured resin composition.
- the compound may consist of a metal powder and a resin composition.
- the content of the metal powder in the compound is preferably 90% by mass or more and less than 100% by mass with respect to the total mass of the compound.
- the content of the metal powder is preferably 90% by mass or more, more preferably 92% by mass or more, further preferably 94% by mass or more, and particularly preferably 96% by mass or more.
- the upper limit of the content of the metal powder may be 99% by mass or less, 98% by mass or less, or 97.5% by mass or less.
- the average particle size of the metal powder is not particularly limited, but may be, for example, 1 ⁇ m or more and 300 ⁇ m or less.
- the average particle size may be measured, for example, by a particle size distribution meter.
- the shape of the individual metal particles constituting the metal powder is not limited, but may be spherical, flat, prismatic, or needle-shaped, for example.
- the compound may include a plurality of types of metal powders having different average particle sizes.
- Various properties such as electromagnetic properties of the molded product formed from the compound are freely controlled according to the composition or combination of the metal powder contained in the compound, and the molded product is used for various industrial products or their raw materials.
- Industrial products manufactured using the compound may be, for example, automobiles, medical equipment, electronic equipment, electrical equipment, information communication equipment, home appliances, audio equipment, and general industrial equipment.
- the compound may be used as a raw material for a bond magnet.
- the compound when the compound contains a soft magnetic powder such as Fe—Si—Cr based alloy or ferrite as the metal powder, the compound may be used as an inductor (for example, an EMI filter) or a raw material for a transformer (for example, a magnetic core).
- a molded product for example, a sheet formed from the compound may be used as an electromagnetic wave shield.
- the resin composition has a function as a binder of metal particles constituting the metal powder, and imparts mechanical strength to the molded product formed from the compound.
- the resin composition contained in the compound is filled between the metal particles when the compound is molded at high pressure using a mold, and the particles are bound to each other.
- the cured product of the resin composition binds the metal particles more firmly to each other, and the mechanical strength of the molded product is improved.
- the resin composition according to the present embodiment can improve the fluidity of the compound by containing an epoxy resin as a thermosetting resin.
- the epoxy resin may be, for example, a resin having two or more epoxy groups in one molecule.
- the type of epoxy resin is not particularly limited and can be selected according to the desired properties of the composition and the like.
- Epoxy resins include, for example, biphenyl type epoxy resin, stillben type epoxy resin, diphenylmethane type epoxy resin, sulfur atom-containing epoxy resin, novolak type epoxy resin, dicyclopentadiene type epoxy resin, salicylaldehyde type epoxy resin, naphthols and phenol.
- Copolymerization type epoxy resin aralkyl type phenol resin epoxidized product, bisphenol type epoxy resin, epoxy resin containing bisphenol skeleton, alcoholic glycidyl ether type epoxy resin, paraxylylene and / or metaxylylene modified phenol resin glycidyl ether Type epoxy resin, glycidyl ether type epoxy resin of terpen-modified phenol resin, cyclopentadiene type epoxy resin, glycidyl ether type epoxy resin of polycyclic aromatic ring-modified phenol resin, glycidyl ether type epoxy resin of naphthalene ring-containing phenol resin, glycidyl ester type Epoxy resin, glycidyl type or methyl glycidyl type epoxy resin, alicyclic epoxy resin, halogenated phenol novolac type epoxy resin, orthocresol novolac type epoxy resin, hydroquinone type epoxy resin, trimethylolpropane type epoxy resin, and ole
- the epoxy resins are biphenyl type epoxy resin, orthocresol novolac type epoxy resin, phenol novolac type epoxy resin, bisphenol type epoxy resin, epoxy resin having a bisphenol skeleton, salicylaldehyde novolac type epoxy resin, and naphthol novolac. It may contain at least one selected from the group consisting of type epoxy resins.
- the epoxy resin may contain at least one selected from the group consisting of biphenylene aralkyl type epoxy resin and orthocresol novolac type epoxy resin.
- the epoxy resin may be a crystalline epoxy resin. Although the molecular weight of the crystalline epoxy resin is relatively low, the crystalline epoxy resin has a relatively high melting point and is excellent in fluidity.
- the crystalline epoxy resin (highly crystalline epoxy resin) may contain, for example, at least one selected from the group consisting of hydroquinone type epoxy resin, bisphenol type epoxy resin, thioether type epoxy resin, and biphenyl type epoxy resin. ..
- Commercially available crystalline epoxy resins include, for example, Epicron 860, Epicron 1050, Epicron 1055, Epicron 2050, Epicron 3050, Epicron 4050, Epicron 7050, Epicron HM-091, Epicron HM-101, Epicron N-730A, Epicron.
- N-740 Epicron N-770, Epicron N-775, Epicron N-865, Epicron HP-4032D, Epicron HP-7200L, Epicron HP-7200, Epicron HP-7200H, Epicron HP-7200HH, Epicron HP-7200HHH, Epicron HP-4700, Epicron HP-4710, Epicron HP-4770, Epicron HP-5000, Epicron HP-6000, N500P-2, and N500P-10 (above, trade names manufactured by DIC Co., Ltd.); NC-3000, NC- 3000-L, NC-3000-H, NC-3100, CER-3000-L, NC-2000-L, XD-1000, NC-7000-L, NC-7300-L, EPPN-501H, EPPN-501HY, EPPN-502H, EOCN-1020, EOCN-102S, EOCN-103S, EOCN-104S, CER-1020, EPPN-201, BREN-S, BREN-10S (above, trade name manufactured by Nippon Kayaku Co., Ltd.);
- the resin composition may contain one of the above epoxy resins.
- the resin composition may contain a plurality of types of epoxy resins among the above.
- the resin composition may contain an epoxy resin containing a biphenyl skeleton, an orthocresol novolac type epoxy resin, and a polyfunctional epoxy resin containing two or more epoxy groups.
- the curing agent is classified into a curing agent that cures the epoxy resin in the range of low temperature to room temperature and a heat curing type curing agent that cures the epoxy resin with heating.
- Hardeners that cure epoxy resins in the low temperature to room temperature range are, for example, aliphatic polyamines, polyaminoamides, and polymercaptans.
- Heat-curing hardeners are, for example, aromatic polyamines, acid anhydrides, phenol novolac resins, and dicyandiamides (DICY).
- the type of curing agent is not particularly limited and can be selected according to the desired properties of the composition and the like.
- the curing agent may be preferably a heat-curing type curing agent, more preferably a phenol resin, and further preferably a phenol novolac resin.
- a phenol novolac resin as a curing agent, it is easy to obtain a cured product of an epoxy resin having a high glass transition point. As a result, the heat resistance and mechanical strength of the molded product are likely to be improved.
- the phenol resin is, for example, an aralkyl type phenol resin, a dicyclopentadiene type phenol resin, a salicylaldehyde type phenol resin, a novolac type phenol resin, a copolymerized phenol resin of a benzaldehyde type phenol and an aralkyl type phenol, a paraxylylene and / or a metaxylylene modification.
- phenol resin From the group consisting of phenol resin, melamine-modified phenol resin, terpen-modified phenol resin, dicyclopentadiene-type naphthol resin, cyclopentadiene-modified phenol resin, polycyclic aromatic ring-modified phenol resin, biphenyl-type phenol resin, and triphenylmethane-type phenol resin. It may contain at least one selected.
- the phenol resin may be a copolymer composed of two or more of the above.
- Tamanol 758 manufactured by Arakawa Chemical Industry Co., Ltd., HP-850N manufactured by Hitachi Kasei Co., Ltd., or the like may be used.
- the phenol novolac resin may be, for example, a resin obtained by condensing or co-condensing phenols and / or naphthols and aldehydes under an acidic catalyst.
- the phenols constituting the phenol novolac resin may include, for example, at least one selected from the group consisting of phenol, cresol, xylenol, resorcin, catechol, bisphenol A, bisphenol F, phenylphenol, and aminophenol.
- the naphthols constituting the phenol novolac resin may include, for example, at least one selected from the group consisting of ⁇ -naphthol, ⁇ -naphthol, and dihydroxynaphthalene.
- the aldehydes constituting the phenol novolac resin may include, for example, at least one selected from the group consisting of formaldehyde, acetaldehyde, propionaldehyde, benzaldehyde, and salicylaldehyde.
- the curing agent may be, for example, a compound having two phenolic hydroxyl groups in one molecule.
- the compound having two phenolic hydroxyl groups in one molecule may contain, for example, at least one selected from the group consisting of resorcin, catechol, bisphenol A, bisphenol F, and substituted or unsubstituted biphenol.
- the resin composition may contain one of the above phenol resins.
- the resin composition may include a plurality of types of phenol resins among the above.
- the resin composition may contain one of the above curing agents.
- the resin composition may contain a plurality of types of curing agents among the above.
- the ratio of active groups (phenolic OH groups) in the curing agent that reacts with the epoxy groups in the epoxy resin is preferably 0.5 to 1.5 equivalents, more preferably 0.5 equivalents, relative to 1 equivalent of the epoxy groups in the epoxy resin. May be 0.6 to 1.4 equivalents, more preferably 0.7 to 1.2 equivalents.
- the ratio of active groups in the curing agent is less than 0.5 equivalent, it is difficult to obtain a sufficient elastic modulus of the obtained cured product.
- the ratio of active groups in the curing agent exceeds 1.5 equivalents, the mechanical strength of the molded product formed from the compound after curing tends to decrease. However, even when the ratio of active groups in the curing agent is out of the above range, the effect according to the present invention can be obtained.
- the resin composition has an excellent balance between the elastic modulus and strength of the molded product, and can improve the reflow resistance.
- the core-shell rubber particles may be at least one selected from the group consisting of butadiene-based rubber particles, acrylic-based rubber particles, silicone-based rubber particles, and silicone-acrylic rubber particles.
- the core-shell rubber particles may be dispersed in a thermosetting resin such as a liquid epoxy resin.
- the average primary particle size of the core-shell rubber particles may be 500 to 1000 nm from the viewpoint of improving the dispersibility in the epoxy resin.
- core-shell rubber particles include, for example, Kaneka MX series manufactured by Kaneka Corporation, Pararoid series manufactured by Daw Chemical Corporation, Metabren S series manufactured by Mitsubishi Chemical Corporation, and KMP series manufactured by Shin-Etsu Chemical Corporation. Can be mentioned.
- the amount of the plasticizer to be blended is 1 part by mass or more and 16 parts by mass or less, 3 parts by mass or more and 14 parts by mass or less, or 5 parts by mass with respect to 100 parts by mass of the epoxy resin. It may be 10 parts or more and 12 parts by mass or less.
- the curing accelerator is not limited as long as it is a composition that reacts with the epoxy resin to accelerate the curing of the epoxy resin, for example.
- the curing accelerator may be, for example, a phosphorus-based curing accelerator, an imidazole-based curing accelerator, or a urea-based curing accelerator.
- a curing accelerator in the resin composition, the moldability and releasability of the compound can be improved.
- the resin composition contains a curing accelerator, the mechanical strength of the molded product (for example, an electronic component) manufactured by using the compound is improved, and the compound is stored in a high temperature and high humidity environment. Stability is improved.
- Examples of the phosphorus-based curing accelerator include phosphine compounds and phosphonium salt compounds.
- imidazole-based curing accelerators include, for example, 2MZ-H, C11Z, C17Z, 1,2DMZ, 2E4MZ, 2PZ-PW, 2P4MZ, 1B2MZ, 1B2PZ, 2MZ-CN, C11Z-CN, 2E4MZ-CN, 2PZ.
- -At least one selected from the group consisting of CN, C11Z-CNS, 2P4MHZ, TPZ, and SFZ above, trade name manufactured by Shikoku Kasei Kogyo Co., Ltd.
- the urea-based curing accelerator is not particularly limited as long as it is a curing accelerator having a urea group, but from the viewpoint of improving storage stability, an alkylurea-based curing accelerator having an alkylurea group is preferable.
- the alkylurea-based curing accelerator having an alkylurea group include aromatic alkylurea and aliphatic alkylurea.
- Examples of commercially available alkylurea-based curing accelerators include U-CAT3512T (trade name, manufactured by San-Apro Co., Ltd., aromatic dimethyl urea) and U-CAT3513N (trade name, manufactured by San-Apro Co., Ltd., aliphatic dimethyl urea). Can be mentioned.
- aromatic alkylurea is preferable because the cleavage temperature is moderately low and the compound can be easily cured efficiently.
- the amount of the curing accelerator to be blended is not particularly limited as long as it can obtain the curing promoting effect.
- the amount of the curing accelerator blended is preferably 0.1 part by mass or more and 30 parts by mass with respect to 100 parts by mass of the epoxy resin.
- it may be more preferably 1 part by mass or more and 15 parts by mass or less.
- the content of the curing accelerator is preferably 0.001 part by mass or more and 5 parts by mass or less with respect to 100 parts by mass in total of the mass of the epoxy resin and the phenol resin.
- the blending amount of the curing accelerator is less than 0.1 parts by mass, it is difficult to obtain a sufficient curing promoting effect.
- the blending amount of the curing accelerator exceeds 30 parts by mass, the storage stability of the compound tends to decrease. However, even when the blending amount and content of the curing accelerator are out of the above range, the effect according to the present invention can be obtained.
- the coupling agent improves the adhesion between the resin composition and the metal element-containing particles constituting the metal powder, and improves the flexibility and mechanical strength of the molded product formed from the compound.
- the coupling agent may be at least one selected from the group consisting of, for example, a silane compound (silane coupling agent), a titanium compound, an aluminum compound (aluminum chelate), and an aluminum / zirconium compound.
- the silane coupling agent may be at least one selected from the group consisting of, for example, epoxysilane, mercaptosilane, aminosilane, alkylsilane, ureidosilane, acid anhydride-based silane, and vinylsilane.
- the resin composition may contain one of the above-mentioned coupling agents, and may contain a plurality of of the above-mentioned coupling agents.
- the resin composition may contain a compound having a siloxane bond (siloxane compound) because the molding shrinkage rate of the compound is easily reduced and the heat resistance and withstand voltage resistance of the molded product are easily improved.
- the siloxane bond is a bond containing two silicon atoms (Si) and one oxygen atom (O), and may be represented by —Si—O—Si—.
- the compound having a siloxane bond may be a polysiloxane compound.
- the compound may contain a flame retardant.
- the flame retardant is selected from the group consisting of, for example, a bromine-based flame retardant, a phosphorus-based flame retardant, a hydrated metal compound-based flame retardant, a silicone-based flame retardant, a nitrogen-containing compound, a hindered amine compound, an organic metal compound, and an aromatic empra. It may be at least one kind.
- the resin composition may contain one of the above flame retardants, and may contain a plurality of the above flame retardants.
- the resin composition may contain wax.
- the wax enhances the fluidity of the compound in the molding of the compound (for example, transfer molding) and functions as a mold release agent.
- the wax may be at least one of fatty acids such as higher fatty acids and fatty acid esters.
- the wax is, for example, fatty acids such as montanic acid, stearic acid, 12-oxystearic acid, laurate or esters thereof; zinc stearate, calcium stearate, barium steaenoate, aluminum stearate, magnesium stearate, calcium laurate, Fatty acid salts such as zinc linoleate, calcium ricinolate, zinc 2-ethylhexoneate; stearic acid amide, oleic acid amide, erucic acid amide, bechenic acid amide, palmitate amide, laurate amide, hydroxystearic acid amide, methylene bisstearate.
- fatty acids such as montanic acid, stearic acid, 12-oxystearic acid, laurate or esters thereof
- zinc stearate calcium stearate, barium steaenoate, aluminum stearate, magnesium stearate, calcium laurate
- Fatty acid salts such as zinc linoleate
- Acid amide ethylene bisstearic acid amide, ethylene bislauric acid amide, distearyl adipate amide, ethylene bisoleic acid amide, diorail adipic acid amide, N-stearyl stearic acid amide, N-oleyl stearic acid amide, N-stearyl Fatty acid amides such as erucate amide, methylol stearic acid amide, methylol bechenic acid amide; fatty acid esters such as butyl stearate; alcohols such as ethylene glycol and stearyl alcohol; polyethylene glycol, polypropylene glycol, polytetramethylene glycol and modifications thereof.
- Polyethers made of materials; Polysiloxanes such as silicone oil and silicon grease; Fluorine compounds such as fluorine oil, fluorine grease, and fluorine-containing resin powder; and paraffin wax, polyethylene wax, amide wax, polypropylene wax, and esters. It may be at least one selected from the group consisting of waxes such as wax, carnauba, and microwax;
- the metal powder may contain, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds.
- the metal powder may consist of, for example, at least one selected from the group consisting of elemental metals, alloys and metal compounds.
- the alloy may include at least one selected from the group consisting of solid solutions, eutectic and intermetallic compounds.
- the alloy may be, for example, stainless steel (Fe—Cr based alloy, Fe—Ni—Cr based alloy, etc.).
- the metal compound may be, for example, an oxide such as ferrite.
- the metal powder may contain one kind of metal element or a plurality of kinds of metal elements.
- the metal element contained in the metal powder may be, for example, a base metal element, a noble metal element, a transition metal element, or a rare earth element.
- the compound may contain one kind of metal element-containing powder, and may contain a plurality of kinds of metal element-containing powders having different compositions.
- the metal powder is not limited to the above composition.
- the metal elements contained in the metal powder are, for example, iron (Fe), copper (Cu), titanium (Ti), manganese (Mn), cobalt (Co), nickel (Ni), zinc (Zn), and aluminum (Al). , Tin (Sn), Chromium (Cr), Niob (Nb), Barium (Ba), Strontium (Sr), Lead (Pb), Silver (Ag), Praseodymium (Pr), Neogym (Nd), Samarium (Sm) , And at least one selected from the group consisting of dysprosium (Dy).
- the metal powder may further contain an element other than the metal element.
- the metal powder may contain, for example, carbon (C), oxygen ( ⁇ ), beryllium (Be), phosphorus (P), sulfur (S), boron (B), or silicon (Si).
- the metal powder may be a magnetic powder.
- the metal powder may be a soft magnetic alloy or a ferromagnetic alloy.
- the metal powder includes, for example, Fe—Si alloy, Fe—Si—Al alloy (Sendust), Fe—Ni alloy (Permalloy), Fe—Cu—Ni alloy (Permalloy), Fe—Co alloy (Permalloy). Menzur), Fe-Cr-Si alloy (electromagnetic stainless steel), Nd-Fe-B alloy (rare earth magnet), Sm-Fe-N alloy (rare earth magnet), Al-Ni-Co alloy (Alnico) It may be a magnetic powder consisting of at least one selected from the group consisting of a magnet) and ferrite.
- the ferrite may be, for example, spinel ferrite, hexagonal ferrite, or garnet ferrite.
- the metal powder may be a copper alloy such as a Cu—Sn-based alloy, a Cu—Sn—P-based alloy, a Cu—Ni-based alloy, or a Cu—Be-based alloy.
- the metal powder may contain one of the above elements and compositions, and may contain a plurality of of the above elements and compositions.
- the metal powder may be Fe alone.
- the metal powder may be an iron-containing alloy (Fe-based alloy).
- the Fe-based alloy may be, for example, a Fe—Si—Cr based alloy or an Nd—Fe—B based alloy.
- the metal element-containing powder may be at least one of amorphous iron powder and carbonyl iron powder. When the metal powder contains at least one of Fe simple substance and Fe-based alloy, it is easy to prepare a molded product having a high space factor and excellent magnetic properties from the compound.
- the metal powder may be an Fe amorphous alloy.
- Fe amorphous alloy powders include, for example, AW2-08, KUAMET-6B2 (above, trade name manufactured by Epson Atmix Co., Ltd.), DAP MS3, DAP MS7, DAP MSA10, DAP PB, DAP PC, DAP MKV49. , DAP 410L, DAP 430L, DAP HYB series (above, product name manufactured by Daido Special Steel Co., Ltd.), MH45D, MH28D, MH25D, and MH20D (above, product name manufactured by Kobe Steel Co., Ltd.). At least one may be used.
- the metal powder and the resin composition are mixed while being heated.
- the metal powder and the resin composition may be kneaded with a kneader, a roll, a stirrer, or the like while being heated.
- the resin composition adheres to a part or the whole of the surface of the metal element-containing particles constituting the metal powder to coat the metal element-containing particles, and the epoxy in the resin composition.
- Part or all of the resin becomes a semi-cured product.
- a compound may be obtained by further adding wax to the powder obtained by heating and mixing the metal powder and the resin composition.
- the resin composition and wax may be mixed in advance.
- metal powder, epoxy resin, curing agent, plasticizer, curing accelerator, and coupling agent may be kneaded in the tank.
- the epoxy resin, the phenol resin, and the curing accelerator may be put into the tank to knead the raw materials in the tank.
- the curing accelerator may be put in the tank, and the raw materials in the tank may be further kneaded.
- a mixed powder of an epoxy resin, a curing agent, and a curing accelerator (resin mixed powder) is prepared in advance, and then a metal powder, a plasticizer, and a coupling agent are kneaded to prepare a metal mixed powder, followed by The metal mixed powder and the above resin mixed powder may be kneaded.
- the kneading time depends on the type of the kneading machine, the volume of the kneading machine, and the production amount of the compound, but for example, it is preferably 1 minute or more, more preferably 2 minutes or more, and 3 minutes or more. Is more preferable.
- the kneading time is preferably 20 minutes or less, more preferably 15 minutes or less, and even more preferably 10 minutes or less. If the kneading time is less than 1 minute, the kneading is insufficient, the moldability of the compound is impaired, and the degree of curing of the compound varies.
- the resin composition for example, epoxy resin and phenol resin
- the heating temperature is, for example, a semi-cured epoxy resin (B-stage epoxy resin) and a cured epoxy resin (C-stage epoxy resin). Any temperature may be used as long as the production of the epoxy is suppressed.
- the heating temperature may be lower than the activation temperature of the curing accelerator.
- the heating temperature is, for example, preferably 50 ° C. or higher, more preferably 60 ° C. or higher, and even more preferably 70 ° C.
- the heating temperature is preferably 150 ° C. or lower, more preferably 120 ° C. or lower, and even more preferably 110 ° C. or lower.
- the resin composition in the tank softens and easily covers the surface of the metal element-containing particles constituting the metal powder, and a semi-cured epoxy resin is easily formed, and is being kneaded. Complete curing of the epoxy resin is likely to be suppressed.
- the molded product according to the present embodiment may include the above-mentioned compound.
- the molded product according to the present embodiment may include a cured product of the above compound.
- the molded product is at least one selected from the group consisting of an uncured resin composition, a semi-cured product of the resin composition (B-stage resin composition), and a cured product of the resin composition (C-stage resin composition). May include.
- the molded product according to this embodiment may be used as a sealing material for an electronic component or an electronic circuit board. According to this embodiment, it is possible to suppress cracks in the molded body due to the difference in the coefficient of thermal expansion between the metal member included in the electronic component or the electronic circuit board and the molded body (sealing material).
- the cured product of the compound is a cured product of the metal powder and the resin composition, and the content of the metal powder is 90% by mass or more and less than 100% by mass.
- the bending strength of the cured product at 250 ° C. may be 5.5 MPa or more, 6.0 MPa or more, or 6.5 MPa or more from the viewpoint of increasing the strength of the cured product.
- the upper limit of the bending strength is about 10 MPa.
- the flexural modulus of the cured product at 250 ° C. may be 1.2 GPa or less, 1.1 GPa or less, or 1.0 GPa or less from the viewpoint of imparting flexibility to the cured product.
- the lower limit of the flexural modulus is about 0.1 GPa.
- the method for producing a molded product according to the present embodiment may include a step of pressurizing the compound in a mold.
- a method for producing a molded product may include a step of pressurizing a compound covering a part or the whole of the surface of a metal member in a mold.
- the method for producing the molded product may include only the step of pressurizing the compound in the mold, and may include other steps in addition to the step.
- the method for producing the molded product may include a first step, a second step, and a third step. The details of each step will be described below.
- the compound is prepared by the above method.
- a molded product (B stage molded product) is obtained by pressurizing the compound in the mold.
- a molded product (B stage molded product) may be obtained by pressurizing a compound covering a part or the entire surface of the metal member in the mold.
- the resin composition is filled between the individual metal element-containing particles constituting the metal element-containing powder. The resin composition then functions as a binder and binds the metal element-containing particles to each other.
- transfer molding of the compound may be carried out.
- the compound may be pressurized at 5 MPa or more and 50 MPa or less.
- the higher the molding pressure the easier it is to obtain a molded product having excellent mechanical strength.
- the molding pressure is preferably 8 MPa or more and 20 MPa or less.
- the density of the molded product formed by transfer molding may be preferably 75% or more and 86% or less, and more preferably 80% or more and 86% or less with respect to the true density of the compound. When the density of the molded product is 75% or more and 86% or less, it is easy to obtain a molded product having excellent mechanical strength.
- the second step and the third step may be carried out collectively.
- the molded product is cured by heat treatment to obtain a C-stage molded product.
- the temperature of the heat treatment may be a temperature at which the resin composition in the molded product is sufficiently cured.
- the temperature of the heat treatment may be preferably 100 ° C. or higher and 300 ° C. or lower, and more preferably 110 ° C. or higher and 250 ° C. or lower.
- the heat treatment temperature exceeds 300 ° C., the metal powder is oxidized or the cured resin product is deteriorated by a small amount of oxygen inevitably contained in the heat treatment atmosphere.
- the heat treatment temperature holding time is preferably several minutes or more and 10 hours or less, more preferably 3 minutes or more 8 It may be less than an hour.
- Imidazole-based curing accelerator (trade name: 2P4MZ manufactured by Shikoku Kasei Kogyo Co., Ltd.) Imidazole-based curing accelerator (trade name: C17Z manufactured by Shikoku Kasei Kogyo Co., Ltd.) (Coupling agent) Methacryloxyoctyltrimethoxysilane (trade name: KBM-5803 manufactured by Shin-Etsu Chemical Co., Ltd.) 3-Mercaptopropyltrimethoxysilane (trade name: KBM-803 manufactured by Shin-Etsu Chemical Co., Ltd.) (Release agent) Zinc laurate (trade name: Powder Base L manufactured by NOF CORPORATION) Partially saponified montanic acid ester wax (trade name: LICOWAX OP manufactured by Clariant Chemicals Co., Ltd.) (Siloxane compound) Caprolactone-modified dimethyl silicone (trade name: DBL-C32 manufactured by Gelest Co.,
- Amorphous iron powder (trade name: 9A4-II manufactured by Epson Atmix Co., Ltd., average particle size 24 ⁇ m)
- Amorphous iron powder (trade name: AW2-08, average particle size 5.3 ⁇ m manufactured by Epson Atmix Co., Ltd.)
- the two types of amorphous iron powder shown in Table 2 were uniformly mixed for 5 minutes with a pressurized twin-screw kneader (manufactured by Nihon Spindle Manufacturing Co., Ltd., capacity 5 L) to prepare a metal powder.
- the coupling agent and the siloxane compound shown in Table 2 were added to the metal powder in the biaxial kneader. Subsequently, the contents of the twin-screw kneader were heated to 90 ° C., and the contents of the twin-screw kneader were mixed for 10 minutes while maintaining the temperature.
- the above resin mixture was added to the contents of the twin-screw kneader, and the contents were melted and kneaded for 15 minutes while maintaining the temperature of the contents at 120 ° C.
- the kneaded product was crushed with a hammer until the kneaded product had a predetermined particle size.
- the above-mentioned "melting” means melting at least a part of the resin composition in the contents of the biaxial kneader.
- the metal powder in the compound does not melt during the compound preparation process.
- the compounds of Examples 1 to 5 were prepared by the above method.
- Comparative Examples 1 and 2 The compounds of Comparative Examples 1 and 2 were prepared by operating in the same manner as in Examples except that the types and blending amounts of each component were changed as shown in Table 3.
- the gel time of the compound was measured by the following method. Using a curast meter (manufactured by JSR Trading Co., Ltd.), the gel time was measured under the conditions of a sample volume of 1.5 mL and 140 ° C. The time at which the torque of the obtained chart started to rise was defined as the gel time. The shorter the gel time, the higher the curability.
- Test piece was obtained by transfer molding the compound under the conditions of a molding die temperature of 140 ° C., a molding pressure of 13.5 MPa, and a curing time of 360 seconds, and then post-curing at 180 ° C. for 2 hours.
- the dimensions of the test piece were 80 mm in length ⁇ 10 mm in width ⁇ 3.0 mm in thickness.
- the bending strength ⁇ (unit: MPa) was calculated based on the following mathematical formula (A).
- the flexural modulus E (unit: GPa) was calculated based on the following mathematical formula (B).
- the bending elongation rate ⁇ (unit:%) was calculated based on the following mathematical formula (C).
- P is the load (unit: N) when the test piece is broken.
- Lv is the distance (unit: mm) between the two fulcrums.
- W is the width (unit: mm) of the test piece.
- T is the thickness (unit: mm) of the test piece.
- F / Y is the gradient (unit: N / mm) of the straight line portion of the load-deflection curve.
- S is the deflection (unit: mm) of the test piece immediately before the test piece is destroyed.
- ⁇ (3 ⁇ P ⁇ Lv) / (2 ⁇ W ⁇ t 2 ) (A)
- E [Lv 3 / (4 x W x t 3 )] x (F / Y) (B)
- ⁇ (600 ⁇ s ⁇ t) / Lv 2 (C)
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Abstract
Description
本実施形態に係るコンパウンドは、金属粉と、樹脂組成物と、を備える。金属粉は、例えば、金属単体、合金、アモルファス粉、及び金属化合物からなる群より選ばれる少なくとも一種を含有してよい。樹脂組成物は、少なくともエポキシ樹脂、硬化剤及び可塑剤を含有する。可塑剤は、コアシェルゴム粒子を含む。コンパウンドにおいて、金属粉、エポキシ樹脂、硬化剤及び可塑剤は混合されている。樹脂組成物は、他の成分として硬化促進剤、離型剤、添加剤等を更に含有してよい。樹脂組成物は、エポキシ樹脂、硬化剤、可塑剤、硬化促進剤、離型剤、及び添加剤を包含し得る成分であって、有機溶媒と金属粉とを除く残りの成分(不揮発性成分)であってよい。添加剤とは、樹脂組成物のうち、樹脂、離型剤、硬化剤、及び硬化促進剤を除く残部の成分である。添加剤は、例えば、カップリング剤、難燃剤、潤滑剤等である。コンパウンドは、粉末(コンパウンド粉)であってよい。
樹脂組成物は、金属粉を構成する金属粒子の結合材(バインダ)としての機能を有し、コンパウンドから形成される成形体に機械的強度を付与する。例えば、コンパウンドに含まれる樹脂組成物は、金型を用いてコンパウンドが高圧で成形される際に、金属粒子の間に充填され、当該粒子を互いに結着する。成形体中の樹脂組成物を硬化させることにより、樹脂組成物の硬化物が金属粒子同士をより強固に結着して、成形体の機械的強度が向上する。
金属粉(金属元素含有粒子)は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種を含有してよい。金属粉は、例えば、金属単体、合金及び金属化合物からなる群より選ばれる少なくとも一種からなっていてよい。合金は、固溶体、共晶及び金属間化合物からなる群より選ばれる少なくとも一種を含んでよい。合金とは、例えば、ステンレス鋼(Fe‐Cr系合金、Fe‐Ni‐Cr系合金等)であってよい。金属化合物とは、例えば、フェライト等の酸化物であってよい。金属粉は、一種の金属元素又は複数種の金属元素を含んでよい。金属粉に含まれる金属元素は、例えば、卑金属元素、貴金属元素、遷移金属元素、又は希土類元素であってよい。コンパウンドは、一種の金属元素含有粉を含んでよく、組成が異なる複数種の金属元素含有粉を含んでもよい。
コンパウンドの製造では、金属粉と樹脂組成物(樹脂組成物を構成する各成分)とを加熱しながら混合する。例えば、金属粉と樹脂組成物とを加熱しながらニーダー、ロール、攪拌機などで混練してよい。金属粉及び樹脂組成物の加熱及び混合により、樹脂組成物が金属粉を構成する金属元素含有粒子の表面の一部又は全体に付着して金属元素含有粒子を被覆し、樹脂組成物中のエポキシ樹脂の一部又は全部が半硬化物になる。その結果、コンパウンドが得られる。金属粉及び樹脂組成物の加熱及び混合によって得られた粉末に、更にワックスを加えることによって、コンパウンドを得てもよい。予め樹脂組成物とワックスとが混合されていてもよい。
本実施形態に係る成形体は、上記のコンパウンドを備えてよい。本実施形態に係る成形体は、上記のコンパウンドの硬化物を備えてよい。成形体は、未硬化の樹脂組成物、樹脂組成物の半硬化物(Bステージの樹脂組成物)、及び樹脂組成物の硬化物(Cステージの樹脂組成物)からなる群より選ばれる少なくとも一種を含んでいてよい。本実施形態に係る成形体は、電子部品又は電子回路基板用の封止材として用いられてよい。本実施形態によれば、電子部品又は電子回路基板が備える金属部材と、成形体(封止材)との熱膨張率差に起因する成形体のクラックを抑制することができる。
本実施形態に係る成形体の製造方法は、コンパウンドを金型中で加圧する工程を備えてよい。成形体の製造方法は、金属部材の表面の一部又は全体を覆うコンパウンドを金型中で加圧する工程を備えてよい。成形体の製造方法は、コンパウンドを金型中で加圧する工程のみを備えてよく、当該工程に加えてその他の工程を備えてもよい。成形体の製造方法は、第一工程、第二工程及び第三工程を備えてもよい。以下では、各工程の詳細を説明する。
トリフェニルメタン型多官能エポキシ樹脂(日本化薬株式会社製のEPPN-501HY、エポキシ当量:169g/eq)
ビフェニレンアラルキル型エポキシ樹脂(日本化薬株式会社製の商品名:NC‐3000、エポキシ当量:275g/eq)
(硬化剤)
トリフェニルメタン型フェノール樹脂(明和化成株式会社製の商品名:MEHC‐7500-3S、水酸基当量:103g/eq)
ビフェニレンアラルキル型フェノール樹脂(明和化成株式会社製の商品名:MEHC‐7851SS、水酸基当量:202g/eq)
表1に示すコアシェルゴム粒子
イミダゾール系硬化促進剤(四国化成工業株式会社製の商品名:2P4MZ)
イミダゾール系硬化促進剤(四国化成工業株式会社製の商品名:C17Z)
(カップリング剤)
メタクリロキシオクチルトリメトキシシラン(信越化学工業株式会社製の商品名:KBM-5803)
3-メルカプトプロピルトリメトキシシラン(信越化学工業株式会社製の商品名:KBM-803)
(離型剤)
ラウリン酸亜鉛(日油株式会社製の商品名:パウダーベースL)
部分ケン化モンタン酸エステルワックス(クラリアントケミカルズ株式会社製の商品名:LICOWAX OP)
(シロキサン化合物)
カプロラクトン変性ジメチルシリコーン(Gelest株式会社製の商品名:DBL‐C32)
アモルファス系鉄粉(エプソンアトミックス株式会社製の商品名:9A4-II、平均粒径24μm)
アモルファス系鉄粉(エプソンアトミックス株式会社製の商品名:AW2‐08、平均粒径5.3μm)
(実施例1~7)
表2に示すエポキシ樹脂、硬化剤、硬化促進剤、離型剤、及び可塑剤を、同表に示す配合量(単位:g)でポリ容器に投入した。これらの材料をポリ容器内で10分間混合することにより、樹脂混合物を調製した。樹脂混合物とは、樹脂組成物のうちシロキサン化合物及びカップリング剤を除く他の全成分に相当する。
各成分の種類及び配合量を表3に示すように変更したこと以外は実施例と同様に操作して、比較例1~2のコンパウンドを調製した。
実施例及び比較例で得られたコンパウンドについて、以下の評価を行った。結果を表2及び3に示す。
流動性の評価は、株式会社島津製作所製のフローテスタCFT-100を用いて行った。コンパウンド7gを成形して、タブレットを作製した。タブレットを用いて、130℃、余熱20秒、荷重100kgの条件にて、流動性の評価を実施した。コンパウンドの流動が停止するまでのプランジャーの押し込み距離(単位:mm)をフローテスターストロークとし、コンパウンドの流動が停止するまでの時間をフロータイムとして測定し、流動性の指標とした。
コンパウンドのゲルタイムを、以下の方法で測定した。キュラストメータ(JSRトレーディング株式会社製)を用い、試料量1.5mL、140℃の条件でゲルタイムを測定した。得られたチャートのトルクの立ち上がり開始の時間をゲルタイムとした。ゲルタイムが短いほど硬化性が高いことを意味する。
コンパウンドを、成形金型温度140℃、成形圧力13.5MPa、硬化時間360秒の条件でトランスファー成形した後、180℃で2時間ポストキュアすることによって、試験片を得た。試験片の寸法は、縦幅80mm×横幅10mm×厚さ3.0mmであった。
2つの支点間の距離Lv: 64.0±0.5mm
ヘッドスピード: 2.0±0.2mm/分
チャートスピード: 100mm/分
チャートフルスケール: 490N(50kgf)
σ=(3×P×Lv)/(2×W×t2) (A)
E=[Lv3/(4×W×t3)]×(F/Y) (B)
ε=(600×s×t)/Lv2 (C)
250℃における曲げ強度(MGa)を250℃における曲げ弾性率(GPa)で除した値を信頼性の評価の指標とした。この値が大きいほど、強度と弾性率とのバランスに優れることを意味する。
トランスファー成形により、銅製の金属部材をコンパウンドで封止して、コンパウンドを硬化することにより成形体を得た。成形体にリフロー処理を施した。リフロー処理における最高加熱温度は、260℃であった。加熱時間は、300秒であった。リフロー処理後、成形体を観察して、成形体におけるクラックの有無を調べた。表中の「A」は、クラックが成形体に形成されていなかったことを意味し、「B」は、クラックが成形体に形成されたことを意味する。
Claims (6)
- 金属粉と、エポキシ樹脂、硬化剤及び可塑剤を含有する樹脂組成物と、を備え、
前記可塑剤が、コアシェルゴム粒子を含む、コンパウンド。 - 前記コアシェルゴム粒子が、ブタジエン系ゴム粒子、アクリル系ゴム粒子、シリコーン系ゴム粒子、及びシリコーン・アクリル系ゴム粒子からなる群より選ばれる少なくとも一種である、請求項1に記載のコンパウンド。
- 前記可塑剤の含有量が、前記エポキシ樹脂の100質量部に対して1質量部以上16質量部以下である、請求項1又は2に記載のコンパウンド。
- 前記金属粉の含有量が、90質量%以上100質量%未満である、請求項1~3のいずれか一項に記載のコンパウンド。
- 請求項1~3のいずれか一項に記載のコンパウンドを含む、成形体。
- 請求項1~3のいずれか一項に記載のコンパウンドの硬化物。
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2021
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- 2021-01-28 JP JP2021574118A patent/JPWO2021153688A1/ja active Pending
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JP2001335689A (ja) * | 2000-05-29 | 2001-12-04 | Taiyo Yuden Co Ltd | 電子材料用ポリサルファイド系硬化性樹脂組成物、電子用品及び電子材料用ポリサルファイド系硬化性樹脂組成物の使用方法 |
JP2009295671A (ja) * | 2008-06-03 | 2009-12-17 | Sony Chemical & Information Device Corp | 磁性シート及び磁性シートの製造方法 |
JP2012532942A (ja) * | 2009-07-08 | 2012-12-20 | ヘンケル・アクチェンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフト・アウフ・アクチェン | 導電性接着剤 |
JP2011181747A (ja) * | 2010-03-02 | 2011-09-15 | Denso Corp | リアクトル |
WO2013150907A1 (ja) * | 2012-04-02 | 2013-10-10 | 株式会社スリーボンド | 導電性組成物 |
JP2014011467A (ja) * | 2012-06-28 | 2014-01-20 | Samsung Electro-Mechanics Co Ltd | インダクタ用の金属−ポリマー複合体フィルム及びインダクタの製造方法 |
JP2018009079A (ja) * | 2016-07-12 | 2018-01-18 | 千住金属工業株式会社 | 導電性接着剤、接合体および継手 |
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