CN117121134A - Composite, molded article, and cured product of composite - Google Patents
Composite, molded article, and cured product of composite Download PDFInfo
- Publication number
- CN117121134A CN117121134A CN202280024658.9A CN202280024658A CN117121134A CN 117121134 A CN117121134 A CN 117121134A CN 202280024658 A CN202280024658 A CN 202280024658A CN 117121134 A CN117121134 A CN 117121134A
- Authority
- CN
- China
- Prior art keywords
- composite
- magnetic powder
- resin composition
- resin
- molded article
- 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.)
- Pending
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- 239000002131 composite material Substances 0.000 title claims abstract description 103
- 239000006247 magnetic powder Substances 0.000 claims abstract description 115
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- 239000011342 resin composition Substances 0.000 claims abstract description 63
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims description 33
- 150000001875 compounds Chemical class 0.000 claims description 26
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- 239000000047 product Substances 0.000 description 34
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- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- HIAAVKYLDRCDFQ-UHFFFAOYSA-L calcium;dodecanoate Chemical compound [Ca+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O HIAAVKYLDRCDFQ-UHFFFAOYSA-L 0.000 description 1
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- ILRSCQWREDREME-UHFFFAOYSA-N dodecanamide Chemical compound CCCCCCCCCCCC(N)=O ILRSCQWREDREME-UHFFFAOYSA-N 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005007 epoxy-phenolic resin Substances 0.000 description 1
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 description 1
- 230000005496 eutectics 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
- FEEPBTVZSYQUDP-UHFFFAOYSA-N heptatriacontanediamide Chemical compound NC(=O)CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC(N)=O FEEPBTVZSYQUDP-UHFFFAOYSA-N 0.000 description 1
- RKVQXYMNVZNJHZ-UHFFFAOYSA-N hexacosanediamide Chemical compound NC(=O)CCCCCCCCCCCCCCCCCCCCCCCCC(N)=O RKVQXYMNVZNJHZ-UHFFFAOYSA-N 0.000 description 1
- HSEMFIZWXHQJAE-UHFFFAOYSA-N hexadecanamide Chemical compound CCCCCCCCCCCCCCCC(N)=O HSEMFIZWXHQJAE-UHFFFAOYSA-N 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
- 239000000314 lubricant Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 235000019808 microcrystalline wax Nutrition 0.000 description 1
- 239000004206 montan acid ester Substances 0.000 description 1
- 235000013872 montan acid ester Nutrition 0.000 description 1
- TXSUIVPRHHQNTM-UHFFFAOYSA-N n'-(3-methylanilino)-n-phenyliminobenzenecarboximidamide Chemical compound CC1=CC=CC(NN=C(N=NC=2C=CC=CC=2)C=2C=CC=CC=2)=C1 TXSUIVPRHHQNTM-UHFFFAOYSA-N 0.000 description 1
- FWFWEABKGWAUSN-UHFFFAOYSA-N n-(hydroxymethyl)docosanamide Chemical compound CCCCCCCCCCCCCCCCCCCCCC(=O)NCO FWFWEABKGWAUSN-UHFFFAOYSA-N 0.000 description 1
- JHOKTNSTUVKGJC-UHFFFAOYSA-N n-(hydroxymethyl)octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCO JHOKTNSTUVKGJC-UHFFFAOYSA-N 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
- 150000004780 naphthols Chemical class 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-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
- WGOROJDSDNILMB-UHFFFAOYSA-N octatriacontanediamide Chemical compound NC(=O)CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC(N)=O WGOROJDSDNILMB-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
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 150000003003 phosphines Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 125000003367 polycyclic group Chemical group 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
- 229920006295 polythiol Polymers 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 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
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000021286 stilbenes Nutrition 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
- 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
- 150000003505 terpenes Chemical class 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 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
- IFNXAMCERSVZCV-UHFFFAOYSA-L zinc;2-ethylhexanoate Chemical compound [Zn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O IFNXAMCERSVZCV-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/28—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder dispersed or suspended in a bonding agent
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The composite of one side of the present invention comprises a resin composition containing an epoxy resin and a curing agent, a non-magnetic powder and a magnetic powder, wherein the content of the magnetic powder is 94 to 98% by mass based on the total amount of the composite, and the minimum melt viscosity at 175 ℃ is 10 to 220 Pa.s.
Description
Technical Field
The present invention relates to a composite, a molded article, and a cured product of the composite.
Background
Composites comprising metal powders and resin compositions are used as raw materials for various industrial products according to physical properties of the metal powders. For example, the composite is used as a raw material for an inductor, a sealing material, an electromagnetic wave shield (EMI shield), a bonded magnet, or the like (refer to patent document 1 below).
Technical literature of the prior art
Patent literature
Patent document 1: japanese patent laid-open publication No. 2014-13803
Disclosure of Invention
Technical problem to be solved by the invention
When an industrial product is manufactured from a composite, a molded body is manufactured by bringing the composite into close contact with a metal member and curing the composite. From the viewpoint of improving reliability, the molded article is required to have excellent mechanical properties (strength at high temperature, strength after moisture resistance test). When the compound is used as a sealing material, it is sometimes required to reduce warpage of a molded article formed of the compound.
The purpose of the present invention is to provide a composite capable of forming a molded body having excellent mechanical properties and reduced warpage, a molded body using the composite, and a cured product of the composite.
Means for solving the technical problems
The composite of one side of the present invention comprises a resin composition containing an epoxy resin and a curing agent, a non-magnetic powder and a magnetic powder, wherein the content of the magnetic powder is 94 to 98% by mass based on the total amount of the composite, and the minimum melt viscosity at 175 ℃ is 10 to 220 Pa.s.
The molded article according to one aspect of the present invention comprises the above-described composite. The cured product of one side of the present invention is a cured product of the above-described composite.
Effects of the invention
According to the present invention, a composite capable of forming a molded article having excellent mechanical properties and reduced warpage, a molded article using the composite, and a cured product of the composite can be provided.
Detailed Description
Hereinafter, preferred embodiments of the present invention will be described. However, the present invention is not limited to the following embodiments.
In the present specification, the numerical range indicated by the term "to" means a range in which numerical values before and after the term "to" are included as a minimum value and a maximum value, respectively. In the numerical ranges described in the present specification in stages, the upper limit value or the lower limit value of the numerical range in one stage may be replaced with the upper limit value or the lower limit value of the numerical range in another stage. In addition, within the numerical ranges described in the present specification, the upper limit value or the lower limit value of the numerical range may be replaced with the value shown in the embodiment. When referring to the amounts of the respective components in the composition in the present specification, in the case where a plurality of substances corresponding to the respective components are present in the composition, the total amount of the plurality of substances present in the composition is referred to unless specified otherwise.
One aspect of the present invention relates to the following composite, molded article, and cured product of the composite.
[1] A composite comprising a resin composition containing an epoxy resin and a curing agent, a non-magnetic powder and a magnetic powder, wherein the content of the magnetic powder is 94 to 98% by mass based on the total amount of the composite, and the minimum melt viscosity at 175 ℃ is 10 to 220 Pa.s.
[2] The complex according to the above [1], wherein,
the content of the non-magnetic powder is 0.10 to 1.50 mass% based on the total amount of the composite.
[3] The complex according to the above [1] or [2], wherein,
the average particle diameter of the non-magnetic powder is 0.3-20 mu m.
[4] The complex according to any one of the above [1] to [3], wherein,
the non-magnetic powder comprises silica.
[5] The complex according to any one of the above [1] to [4], wherein,
the magnetic powder comprises magnetic powder with average particle diameter of 11-45 μm and magnetic powder with average particle diameter of 0.1-9 μm.
[6] A molded article comprising the complex of any one of the above [1] to [5 ].
[7] A cured product of the composite of any one of the above [1] to [5 ].
[ Complex ]
The composite of the present embodiment includes a resin composition, a non-magnetic powder, and a magnetic powder. The resin composition at least contains an epoxy resin and a curing agent. The composite is mixed with a non-magnetic powder, a magnetic powder and a resin composition. The resin composition may further contain a coupling agent, a curing accelerator, a mold release agent, an additive, and the like as other components. The resin composition may be the remaining components (nonvolatile components) other than the organic solvent, the non-magnetic powder, and the magnetic powder, which may contain an epoxy resin, a curing agent, a coupling agent, a curing accelerator, a mold release agent, and an additive. The additive is the rest of components except the resin, the release agent, the curing accelerator and the coupling agent in the resin composition. The additives are, for example, flame retardants, lubricants, etc. The composite may be a powder (composite powder).
The composite may include a non-magnetic powder, a magnetic powder, and a resin composition attached to the surface of each magnetic particle constituting the magnetic powder. The resin composition may cover the entire surface of the magnetic particles or only a part of the surface of the magnetic particles. The composite may also include an uncured resin composition, a non-magnetic powder, and a magnetic powder. The composite may include a prepreg of a resin composition (for example, a B-stage resin composition), a nonmagnetic powder, and a magnetic powder. The composite may also be provided with both an uncured resin composition and a semi-cured resin composition. The composite may be formed of a non-magnetic powder, a magnetic powder, and a resin composition.
The composite of the present embodiment has a minimum melt viscosity of 10 to 220 Pa.s at 175 ℃. The lowest melt viscosity of the composite may be 15pa·s or more, 20pa·s or more, or 25pa·s or more from the viewpoint of reducing burrs of the molded body, and may be 210pa·s or less, 200pa·s or less, or 190pa·s or less from the viewpoint of improving fluidity at the time of molding.
(magnetic powder)
The content of the magnetic powder in the composite is 94-98 mass% based on the total amount of the composite. If the content of the magnetic powder is increased, it is difficult to secure releasability of the molded article, and workability tends to be deteriorated. The content of the magnetic powder in the composite is preferably 94.5 mass% or more, more preferably 94.8 mass% or more, and even more preferably 95.0 mass% or more, from the viewpoint of the magnetic properties of the molded article. The upper limit value of the content of the magnetic powder may be 97.8 mass% or less, 97.5 mass% or less, or 97.0 mass% or less from the viewpoint of fluidity of the composite.
The magnetic powder is magnetic particles having magnetism. The magnetic powder may contain at least one selected from the group consisting of a metal monomer, an alloy, and a metal compound, for example. The magnetic powder may contain, for example, at least one selected from the group consisting of a metal monomer, an alloy, and a metal compound. The alloy may include at least one selected from the group consisting of solid solutions, eutectic (eutec), and intermetallic compounds. The alloy may be, for example, stainless steel (fe—cr-based alloy, fe=ni—cr-based alloy, or the like). The metal compound may be, for example, an oxide such as ferrite. The magnetic powder may contain one metal element or a plurality of metal elements. The metal element contained in the magnetic powder may be, for example, a base metal element, a noble metal element, a transition metal element, or a rare earth element. The composite may contain one kind of magnetic powder or may contain a plurality of kinds of magnetic powder having different compositions.
The metal element contained in the magnetic powder may be, for example, at least one selected from the group consisting of iron (Fe), copper (Cu), titanium (Ti), manganese (Mn), cobalt (Co), nickel (Ni), zinc (Zn), aluminum (Al), tin (Sn), chromium (Cr), niobium (Nb), barium (Ba), strontium (Sr), lead (Pb), silver (Ag), praseodymium (Pr), neodymium (Nd), samarium (Sm), and dysprosium (Dy). The magnetic powder may further contain an element other than the metal element. The magnetic powder may contain, for example, carbon (C), oxygen (O), beryllium (Be), phosphorus (P), sulfur (S), boron (B), or silicon (Si).
The magnetic powder may be a soft magnetic alloy or a ferromagnetic alloy. The magnetic powder may be, for example, a magnetic powder formed of at least one selected from the group consisting of an Fe-Si-based alloy, an Fe-Si-Al-based alloy (Sendust), an Fe-Ni-based alloy (Permalloy), an Fe-Cu-Ni-based alloy (Permalloy), an Fe-Co-based alloy (permadur), an Fe-Cr-Si-based alloy (electromagnetic stainless steel), an Nd-Fe-B-based alloy (rare earth magnet), an Sm-Fe-N-based alloy (rare earth magnet), an Al-Ni-Co-based alloy (Alnico) and ferrite. The ferrite may be, for example, spinel ferrite, hexagonal ferrite or garnet ferrite. The magnetic 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 magnetic powder can also be Fe monomer. The magnetic powder may be an alloy containing iron (Fe-based alloy). The Fe-based alloy may be, for example, an Fe-Si-Cr-based alloy or an Nd-Fe-B-based alloy. The magnetic powder may be at least one of amorphous iron powder and carbonyl iron powder. When the magnetic powder contains at least one of an Fe monomer and an Fe-based alloy, a compact having a high slot-fill ratio (Space factor) and excellent magnetic characteristics can be easily produced from the composite. The magnetic powder can also be Fe amorphous alloy.
As commercial products of the Fe amorphous alloy powder, for example, at least one selected from the group consisting of AW2-08, KUAMET 6B2, KUAMET 9A4-II (trade name manufactured by above Epson Atmix Corporation), DAP MS3, DAP MS7, DAP MSA10, DAP PB, DAP PC, DAP MKV49, DAP 410L, DAP L, DAP HYB series (trade name manufactured by above Daido Steel co., ltd.) and MH45D, MH28D, MH D and MH20D (trade name manufactured by above Kobe Steel, ltd.) can be used.
When a magnetic powder containing iron (ferromagnetic powder) is used as the magnetic powder, the content of iron in the ferromagnetic powder may be 80 mass% or more, and may be 83 to 99 mass%, 84 to 97 mass%, 85 to 95 mass%, or 87 to 93 mass%. By using the ferromagnetic powder containing iron in the above-described range, the composite can be more suitably used as a raw material for an inductor, a sealing material, an electromagnetic wave shield (EMI shield), a bonded magnet, or the like.
The shape of each metal particle constituting the magnetic powder is not limited, and may be, for example, spherical, flat, square or needle-like. The average particle diameter of the magnetic powder is not particularly limited, and may be, for example, 0.1 μm or more, 0.5 μm or more, or 1.0 μm or more, and may be 100 μm or less, 80 μm or less, or 50 μm or less. The average particle diameter can be measured by a particle size distribution meter, for example. The composite may include a plurality of magnetic powders having different average particle diameters. From the viewpoint of improving fluidity and magnetic characteristics, the magnetic powder preferably contains a1 st magnetic powder having an average particle diameter of 11 to 45 μm and a 2 nd magnetic powder having an average particle diameter of 0.1 to 9 μm. The average particle diameter of the 1 st magnetic powder may be 15 to 40. Mu.m, 18 to 35. Mu.m, or 20 to 30. Mu.m. The average particle diameter of the 2 nd magnetic powder may be 0.5 to 6. Mu.m, 0.8 to 5. Mu.m, or 1.0 to 4. Mu.m.
(non-magnetic powder)
The nonmagnetic powder is nonmagnetic particles having no magnetism. By adding the non-magnetic powder, the magnetic powder and the resin component are not easily separated, and the formability of the composite can be improved. The non-magnetic powder may be a non-magnetic powder containing a metal element or a non-magnetic powder containing no metal element.
Examples of the constituent material of the nonmagnetic powder include oxide ceramic materials such as silica, alumina, zirconia, titania, magnesia, and calcia; nitride-based ceramic materials such as silicon nitride and aluminum nitride; carbide-based ceramic materials such as silicon carbide and boron carbide. From the viewpoint of reducing warpage of the molded body, the non-magnetic powder preferably contains silica.
The average particle diameter of the non-magnetic powder of the present embodiment is preferably 0.3 to 20 μm, more preferably 0.4 to 15 μm, and even more preferably 0.5 to 12 μm, from the viewpoint of reducing warpage of the molded article. From the viewpoint of burr reduction, the average particle diameter of the non-magnetic powder may be 10 μm or less, 8 μm or less, or 4 μm or less.
The content of the non-magnetic powder is preferably 0.10 to 1.50% by mass based on the total amount of the composite from the viewpoint of reducing the thermal expansion coefficient of the molded body, may be 0.12% by mass or more, 0.14% by mass or more, or 0.20% by mass or more from the viewpoint of reducing the warpage of the molded body, and may be 1.40% by mass or less, 1.20% by mass or less, or 1.10% by mass or less from the viewpoint of improving the flowability of the composite.
(resin composition)
The resin composition has a function as a binding material (binder) for magnetic particles constituting the magnetic powder, and imparts mechanical strength to a molded body formed of the composite.
For example, when the composite is molded under high pressure using a mold, the resin composition contained in the composite is filled between the magnetic particles, so that the particles are bonded to each other. By curing the resin composition in the molded body, the cured product of the resin composition causes the magnetic particles to adhere more firmly to each other, and the mechanical strength of the molded body is improved.
The resin composition of the present embodiment can improve the fluidity of the composite by containing an epoxy resin as a thermosetting resin. The epoxy resin may be, for example, a resin having 2 or more epoxy groups in 1 molecule. The kind of the epoxy resin is not particularly limited, and may be selected according to desired characteristics of the resin composition, and the like.
Examples of the epoxy resin include the following: biphenyl type epoxy resins, stilbene type epoxy resins, diphenylmethane type epoxy resins, sulfur atom type epoxy resins, novolak type epoxy resins, dicyclopentadiene type epoxy resins, salicylaldehyde type epoxy resins, naphthol type or phenol type copolymerized epoxy resins, aralkyl type novolak type epoxy resins, bisphenol skeleton containing epoxy resins, alcohol type glycidyl ether type epoxy resins, p-xylene and/or m-xylene modified novolak type epoxy resins, terpene modified novolak type epoxy resins, cyclopentadiene type epoxy resins, polycyclic aromatic ring modified novolak type epoxy resins, naphthalene ring containing novolak type epoxy resins, glycidyl ester type epoxy resins, glycidyl type or methyl glycidyl type epoxy resins, alicyclic type epoxy resins, halogenated phenol novolak type epoxy resins, o-cresol novolak type epoxy resins, hydroquinone type epoxy resins, trimethylolpropane type epoxy resins, linear aliphatic epoxy resins obtained by oxidizing olefin bonds with peracetic acid or the like.
From the viewpoint of fluidity, the epoxy resin may contain at least one selected from the group consisting of biphenyl type epoxy resin, o-cresol 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 type epoxy resin.
From the viewpoint of mechanical strength, the epoxy resin may contain at least one selected from the group consisting of biphenylene aralkyl type epoxy resins and o-cresol novolac type epoxy resins.
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 (epoxy resin having high crystallinity) may contain 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, for example.
Examples of the commercially available crystalline epoxy resins include EPICLON 860, EPICLON 1050, EPICLON 1055, EPICLON 2050, EPICLON 3050, EPICLON 4050, EPICLON 7050, EPICLON HM-091, EPICLON HM-101, EPICLON-730A, EPICLON-740, EPICLON-770, EPICLON-775, EPICLON-865, EPICLON HP-4032D, EPICLON HP-7200L, EPICLON HP-7200H, EPICLON HP-4700H, EPICLON HP-4710, EPICLON HP-4770, EPICLON HP-5000, EPICLON HP-6000, EPLON 500 and EPLON 500-500 (trade names of DIC 500 and more); 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, and BREN-10S (above is a trade name manufactured by Nippon Kayaku Co., ltd.); YX-4000, YX-4000H, YL, 4121H and YX-8800 (above is a trade name manufactured by Mitsubishi Chemical Corporation).
The resin composition may contain one of the epoxy resins described above. The resin composition may contain a plurality of epoxy resins as described above. The epoxy resin may contain an epoxy resin having a biphenyl skeleton, an o-cresol novolac type epoxy resin, or a multifunctional epoxy resin having 2 or more epoxy groups.
The curing agents are classified into curing agents that cure epoxy resins in a range from low temperature to room temperature and heat-curable curing agents that cure epoxy resins with heating. Examples of the curing agent for curing the epoxy resin in a range from low temperature to room temperature include aliphatic polyamines, polyaminoamides, and polythiols. Examples of the heat-curable curing agent include aromatic polyamines, acid anhydrides, phenol novolac resins, and dicyandiamide (dic y). The kind of the curing agent is not particularly limited, and may be selected according to the desired properties of the composition, and the like.
When a curing agent for curing an epoxy resin in a range from low temperature to room temperature is used, the glass transition point of the cured product of the epoxy resin is low, and the cured product of the epoxy resin tends to be soft. As a result, the molded article formed of the composite is also easily softened. On the other hand, from the viewpoint of improving the heat resistance of the molded body, the curing agent may be preferably a heat-curable curing agent, more preferably a phenolic resin, and further preferably a phenol novolac resin. In particular, by using a phenol novolac resin as a curing agent, a cured product of an epoxy resin having a high glass transition point can be easily obtained. As a result, the heat resistance and mechanical strength of the molded article can be easily improved.
The phenol resin may include at least one selected from the group consisting of aralkyl type phenol resins, dicyclopentadiene type phenol resins, salicylaldehyde type phenol resins, novolak type phenol resins, copolymerized phenol resins of benzaldehyde type phenol and aralkyl type phenol, para-xylene and/or meta-xylene modified phenol resins, melamine modified phenol resins, terpene modified phenol resins, dicyclopentadiene type naphthol resins, cyclopentadiene modified phenol resins, polycyclic aromatic ring modified phenol resins, biphenyl type phenol resins, and triphenylmethane type phenol resins, for example. The phenolic resin may be a copolymer composed of two or more of the above. As commercial products of the phenol resin, for example, tamanol 758, showa Denko Materials co manufactured by ltd.
The phenol novolac resin may be, for example, a resin obtained by condensing or co-condensing phenols and/or naphthols with aldehydes in the presence of an acidic catalyst. The phenols constituting the phenol novolac resin may contain at least one selected from the group consisting of phenol, cresol, xylenol, resorcinol, catechol, bisphenol a, bisphenol F, phenylphenol, and aminophenol, for example. The naphthol constituting the phenol novolac resin may contain at least one selected from the group consisting of α -naphthol, β -naphthol, and dihydroxynaphthalene, for example. The aldehyde constituting the phenol novolac resin may contain at least one selected from the group consisting of formaldehyde, acetaldehyde, propionaldehyde, benzaldehyde, and salicylaldehyde, for example.
The curing agent may be, for example, a compound having 2 phenolic hydroxyl groups in 1 molecule. The compound having 2 phenolic hydroxyl groups in 1 molecule may contain, for example, at least one selected from the group consisting of resorcinol, catechol, bisphenol a, bisphenol F, and substituted or unsubstituted diphenols.
The resin composition may contain one of the phenolic resins described above. The resin composition may also include a plurality of phenolic resins as described above. The resin composition may contain one of the above curing agents. The resin composition may contain a plurality of curing agents as described above.
The ratio of the active groups (phenolic OH groups) in the curing agent that reacts with the epoxy groups in the epoxy resin may be preferably 0.5 to 1.5 equivalents, more preferably 0.6 to 1.4 equivalents, and even more preferably 0.7 to 1.2 equivalents, relative to 1 equivalent of the epoxy groups in the epoxy resin. When the ratio of the 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. On the other hand, when the ratio of the active groups in the curing agent exceeds 1.5 equivalents, the mechanical strength of the molded article formed of the composite after curing tends to be lowered. However, even in the case where the ratio of the active groups in the curing agent is out of the above range, the effects of the present invention can be obtained.
In order to improve the moldability and releasability of the composite, the resin composition may further contain a curing accelerator (catalyst). By containing the curing accelerator in the resin composition, the mechanical strength of a molded article (for example, an electronic component) produced using the composite is improved, or the storage stability of the composite in a high-temperature/high-humidity environment is improved. The curing accelerator is not limited as long as it is, for example, a composition that reacts with the epoxy resin to accelerate curing of the epoxy resin. The curing accelerator may be, for example, a phosphorus-based curing accelerator, an imidazole-based curing accelerator or a urea-based curing accelerator.
Examples of the phosphorus-based curing accelerator include phosphine compounds and phosphonium salt compounds.
Examples of the commercial products of imidazole-based curing accelerators include 2MZ-H, C11Z, C Z, 1,2DMZ, 2E4MZ, 2PZ-PW, 2P4MZ, 1B2PZ, 2MZ-CN, C11Z-CN, 2E4MZ-CN, 2PZ-CN, C1 1Z-CNS, 2P4MHZ, TPZ and SFZ (trade name manufactured by Shikoku Chemicals Corporation above).
The urea-based curing accelerator is not particularly limited as long as it is a curing accelerator having an ureido group, but is preferably an alkylurea-based curing accelerator having an alkylureido group from the viewpoint of improving storage stability. Examples of the alkyl urea curing accelerator having an alkyl urea group include aromatic alkyl urea and aliphatic alkyl urea. Examples of the commercial product of the alkylurea curing accelerator include U-CAT 35T (trade name, manufactured by San-Apro Ltd., aromatic dimethylurea) and U-CAT3513N (trade name, manufactured by San-Apro Ltd., aliphatic dimethylurea). Among these, aromatic alkyl urea is preferable because the cracking temperature is suitably low, and the composite is easily cured efficiently.
The blending amount of the curing accelerator is not particularly limited as long as the curing accelerator can obtain a curing accelerating effect. The amount of the curing accelerator to be blended may be 0.1 part by mass or more and 20 parts by mass or less, 1 part by mass or more and 15 parts by mass or less or 2 parts by mass or more and 10 parts by mass or less with respect to 100 parts by mass of the epoxy resin from the viewpoint of improving the curability and flowability of the resin composition upon moisture absorption. When the amount of the curing accelerator is 0.1 part by mass or more, a sufficient curing acceleration effect can be easily obtained. When the amount of the curing accelerator is 20 parts by mass or less, the storage stability of the compound is not easily lowered.
The resin composition may further contain a coupling agent. The coupling agent can improve the adhesion between the resin composition and the metal element-containing particles constituting the magnetic powder, and can improve the flexibility and mechanical strength of a molded article (such as an inductor) formed from the composite. The coupling agent may be at least one selected from the group consisting of silane-based compounds (silane coupling agents), titanium-based compounds, aluminum compounds (aluminum chelates), and aluminum/zirconium-based compounds, for example. The silane coupling agent may be at least one selected from the group consisting of an epoxy silane compound, a mercapto silane compound, an aminosilane compound, an alkylsilane compound, an acrylic silane compound, a methacrylic silane compound, an ureido silane compound, an acid anhydride silane compound, and a vinyl silane compound, for example. The complex may include one or more of the above coupling agents.
The content of the coupling agent in the compound of the present embodiment is preferably 0.05 to 0.70 mass%, more preferably 0.10 to 0.60 mass%, and even more preferably 0.12 to 0.50 mass%, based on the total mass of the compound. When the content of the coupling agent is not less than the above lower limit, the flexibility and mechanical strength of the molded article can be easily further improved. When the content of the coupling agent is not more than the above upper limit, a block of the composite is not easily generated. However, even in the case where the content of the coupling agent is outside the above-described range, the effect of the present invention can be obtained.
The resin composition may contain a compound having a siloxane bond (siloxane compound) as an additive, and since the molding shrinkage of the composite is easily reduced, the heat resistance and voltage resistance of the molded article are easily improved. The siloxane bond is a bond containing 2 silicon atoms (Si) and 1 oxygen atom (O) and may be represented by-Si-O-Si-. The compound having a siloxane bond may be a polysiloxane compound.
When a molded body is formed from the compound using a mold, the resin composition may contain wax. The wax improves the fluidity of the compound at the time of molding (e.g., transfer molding) of the compound, 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 may be, for example, a fatty acid selected from the group consisting of montanic acid, stearic acid, 12-hydroxystearic acid (12-oxystearic acid), lauric acid and esters thereof, zinc stearate, calcium stearate, barium stearate, aluminum stearate, magnesium stearate, calcium laurate, zinc linoleate, calcium ricinoleate, fatty acid salts such as zinc 2-ethylhexanoate, stearic acid amide, oleic acid amide, erucic acid amide, behenic acid amide, palmitic acid amide, lauric acid amide, hydroxystearic acid amide, methylenebisstearic acid amide, ethylenebisstearic acid amide, ethylenebislauric acid amide, distearyl adipic acid amide, ethylenebisoleic acid amide, dioleyl adipic acid amide, at least one kind selected from the group consisting of N-stearyl stearamide, N-oleyl stearamide, N-stearyl erucamide, hydroxymethyl stearamide, fatty acid amides such as hydroxymethyl behenamide, fatty acid esters such as butyl stearate, alcohols such as ethylene glycol and stearyl alcohol, polyethers including polyethylene glycol, polypropylene glycol, polytetramethylene glycol and modified products thereof, silicone oils such as silicone oils and silicone grease, fluorine-based oils, fluorine-based grease, fluorine-containing resin powder and other fluorine compounds, and waxes such as paraffin wax, polyethylene wax, amide wax, polypropylene wax, ester wax, carnauba (carnauba) and microcrystalline wax (micro wax).
The compound may contain a flame retardant for the purpose of environmental safety, recyclability, forming processability, and low cost of the compound. The flame retardant may be at least one selected from the group consisting of brominated flame retardants, phosphorus flame retardants, hydrated metal compound flame retardants, silicone flame retardants, nitrogen-containing compounds, hindered amine compounds, organometallic compounds, and aromatic engineering plastics, for example. The resin composition may contain one or more of the above flame retardants.
In producing the composite, the non-magnetic powder, the magnetic powder, and the resin composition (each component constituting the resin composition) are mixed while being heated. For example, the nonmagnetic powder, the magnetic powder and the resin composition are kneaded with a kneader, a roll, a stirrer or the like while being heated. By heating and mixing the non-magnetic powder, the magnetic powder, and the resin composition, the resin composition adheres to a part or the whole of the surface of the metal element-containing particles constituting the magnetic powder to coat the metal element-containing particles, and a part or the whole of the epoxy resin in the resin composition becomes a semi-cured product. As a result, a complex was obtained. The composite may also be obtained by further adding wax to a powder obtained by heating and mixing a non-magnetic powder, a magnetic powder and a resin composition. The resin composition and the wax may be mixed in advance.
In kneading, the non-magnetic powder, the epoxy resin, the curing agent, the curing accelerator and the coupling agent may be kneaded in a tank. The non-magnetic powder, the magnetic powder and the coupling agent may be put into a tank and mixed, and then the epoxy resin, the curing agent and the curing accelerator may be put into the tank and the raw materials in the tank may be kneaded. After kneading the epoxy resin, the curing agent and the coupling agent in the tank, the curing accelerator may be put into the tank, and the raw materials in the tank may be kneaded. The mixed powder (resin mixed powder) of the epoxy resin, the curing agent and the curing accelerator may be prepared in advance, and the non-magnetic powder, the magnetic powder and the coupling agent may be kneaded to prepare a metal mixed powder, and then the metal mixed powder and the resin mixed powder may be kneaded.
The kneading time depends on the type of kneading machine, the volume of the kneading machine, and the amount of the compound produced, and is, for example, preferably 1 minute or more, more preferably 2 minutes or more, and still more preferably 3 minutes or more. The kneading time is preferably 20 minutes or less, more preferably 15 minutes or less, and still more preferably 10 minutes or less. When the kneading time is less than 1 minute, kneading is insufficient, and the formability of the composite is impaired, and the curing degree of the composite varies. When the kneading time exceeds 20 minutes, for example, the resin composition (for example, epoxy resin and phenolic resin) is cured in a tank, and fluidity and moldability of the composite are easily impaired.
When the raw materials in the tank are kneaded by a kneader while being heated, the heating temperature may be, for example, a temperature at which a semi-solid of the epoxy resin (B-stage epoxy resin) is produced and the production of a cured product of the epoxy resin (C-stage epoxy resin) is suppressed. The heating temperature may also be a temperature below the activation temperature of the curing accelerator. The heating temperature is, for example, preferably 50℃or higher, more preferably 60℃or higher, and still more preferably 70℃or higher. The heating temperature is preferably 150℃or lower, more preferably 120℃or lower, and still more preferably 110℃or lower. When the heating temperature is within the above range, the resin composition in the tank is softened and the surfaces of the metal element-containing particles constituting the magnetic powder are easily covered, whereby a semi-solid of the epoxy resin is easily formed and complete curing of the epoxy resin during kneading is easily suppressed.
[ molded article ]
The molded article of the present embodiment may contain the above-described composite. The molded article of the embodiment may contain a cured product of the above-described composite. The molded body may contain at least one selected from the group consisting of an uncured resin composition, a semi-solid of a resin composition (B-stage resin composition), and a cured product of a resin composition (C-stage resin composition). The molded article of the present embodiment can be used as a sealing material for electronic parts or electronic circuit boards. According to the present embodiment, cracking of the molded body caused by a difference in thermal expansion coefficient between a metal member and the molded body (sealing material) provided in the electronic component or the electronic circuit board can be suppressed.
The cured product of the composite is a cured product of a non-magnetic powder, a magnetic powder, and a resin composition. From the viewpoint of improving the strength of the cured product, the bending strength of the cured product at 250℃may be 5.0MPa or more, 5.5MPa or more, or 5.8MPa or more. The upper limit of the bending strength at 250℃is about 10 MPa. The cured product may have a flexural strength at room temperature of 90MPa or more, 95MPa or more, or 100MPa or more. The upper limit of the bending strength at room temperature is about 200 MPa. The cured product of the composite of the present embodiment has excellent mechanical properties even after moisture absorption under a high-temperature and high-humidity environment. For example, the cured product after 20 hours of treatment at 121℃under 100% (saturated) environment may have a flexural strength at room temperature of 48MPa or more, 50MPa or more, or 52MPa or more.
The method for producing a molded article according to the present embodiment may include a step of pressurizing the composite in a mold. The method for producing a molded article may include a step of pressurizing the composite covering a part or the whole of the surface of the metal member in a mold. The method for producing the molded article may include only the step of pressurizing the composite in the mold, or may include other steps in addition to the step. The method for producing a molded article may further include a first step, a second step, and a third step. The details of each step will be described below.
In the first step, a composite is produced by the above method.
In the second step, the composite is pressed in a mold to obtain a molded article (B-stage molded article). In the second step, the composite covering a part or the whole of the surface of the metal member is pressed in a mold to obtain a molded article (B-stage molded article). In the second step, the resin composition is filled between the individual metal element-containing particles constituting the magnetic powder. Further, the resin composition functions as a bonding material (binder) to bond the magnetic powders to each other.
As the second step, transfer molding of the composite may be performed.
In the transfer molding, the composite may be pressurized at a pressure of 5MPa to 50 MPa. The higher the molding pressure, the easier the molded article having excellent mechanical strength tends to be obtained. In consideration of mass productivity of the molded article and life of the mold, the molding pressure is preferably 8MPa or more and 20MPa or less. The density of the molded article formed by transfer molding may be preferably 75% or more and 86% or less, more preferably 80% or more and 86% or less, with respect to the true density of the composite. When the density of the molded article is 75% or more and 86% or less, a molded article excellent in mechanical strength can be easily obtained. In the transfer molding, the second step and the third step may be performed in a lump.
In the third step, the molded body is cured by heat treatment to obtain a molded body in the C stage. The temperature of the heat treatment may be a temperature at which the resin composition in the molded article is sufficiently cured. The temperature of the heat treatment may be preferably 100 ℃ or more and 300 ℃ or less, more preferably 110 ℃ or more and 250 ℃ or less. In order to suppress oxidation of the magnetic powder in the molded body, the heat treatment is preferably performed under an inert atmosphere. When the heat treatment temperature exceeds 300 ℃, the magnetic powder is oxidized or the resin cured product is deteriorated due to a trace amount of oxygen inevitably contained in the heat-treated atmosphere. In order to suppress oxidation of the magnetic powder and degradation of the resin cured product and sufficiently cure the resin composition, the holding time of the heat treatment temperature may be preferably several minutes or more and 10 hours or less, more preferably 3 minutes or more and 8 hours or less.
By using the composite of the present embodiment, a molded article having excellent mechanical properties and reduced warpage can be produced.
Examples
The present invention will be described in further detail with reference to examples, but the present invention is not limited to these examples.
Details of each component used in the preparation of the composites of examples and comparative examples are shown below.
(resin composition)
Epoxy resin 1 (biphenylene aralkyl type epoxy resin, nippon Kayaku Co., ltd. Trade name: NC-3000, epoxy equivalent: 275 g/eq)
Epoxy resin No. 2 (multifunctional epoxy resin, trade name manufactured by Printec Corporation: TECHMORE VG-3101L, epoxy equivalent: 215 g/eq)
Curing agent (phenol novolac resin, meiwa Plastic Industries, ltd. Trade name: HF-3M)
Curing accelerator (trade name: UCAT3 512T manufactured by San-Apro Ltd., aromatic dimethylurea)
Coupling agent (methacryloxyoctyl trimethoxysilane, shin-Etsu Chemical Co., ltd. Trade name: KBM-5803)
Mold release agent (partially saponified montan acid ester wax, clariant Chemicals Co., ltd. Trade name: LICOWAX-OP)
(non-magnetic powder)
Nonmagnetic powder 1 (trade name: SO-25R, average particle diameter: 0.6 μm manufactured by silica, ADMAX Corporation)
Nonmagnetic powder 2 (trade name: SE-2200SEJ, average particle diameter: 0.6 μm manufactured by silica, ADMAX Corporation)
Nonmagnetic powder 3 (trade name: SO-27R, average particle diameter: 0.7 μm, manufactured by silica, ADMAX Corporation)
Nonmagnetic powder 4 (trade name: SO-32R, average particle diameter: 1.4 μm, manufactured by silica, ADMAX Corporation)
Nonmagnetic powder 5 (trade name: FB-5SDX, average particle diameter: 5 μm manufactured by silica, denka Company Limited)
Nonmagnetic powder 6 (trade name: FB-304, average particle diameter: 10 μm manufactured by silica, denka Company Limited)
Nonmagnetic powder 7 (silica, NIPPON AEROSIL CO., LTD. Trade name: AEROSIL R972CF, average particle diameter: 0.2 μm)
(magnetic powder)
No. 1 magnetic powder (amorphous iron powder, trade name: 9A4-II, average particle size: 24 μm manufactured by Epson Atmix Corporation)
2 nd magnetic powder (FeSiCr alloy powder manufactured by SINTOKOGIO, LTD., average particle size: 2.1 μm)
[ preparation of Complex ]
Examples 1 to 9
The epoxy resin, curing agent, curing accelerator and release agent were placed in plastic containers in the amounts (unit: g) shown in Table 1. The resin mixture was prepared by mixing these materials in a plastic container for 10 minutes. The resin mixture corresponds to all the other components in the resin composition except the coupling agent.
The non-magnetic powder and the magnetic powder in the blending amounts (unit: g) shown in table 1 were mixed for 5 minutes by a pressurized biaxial kneader (Nihon Spindle Manufacturing co., ltd., capacity 5L.) and then the coupling agent shown in table 1 was added to the biaxial kneader. Then, the contents of the biaxial kneader were heated to 90℃and mixed for 10 minutes while maintaining the temperature. Then, the above resin mixture was added to the content of the biaxial kneader, and the content was melted/kneaded for 15 minutes while maintaining the temperature of the content at 120 ℃. After cooling the kneaded material obtained by the above melting/kneading to room temperature, the kneaded material was pulverized with a hammer to give a predetermined particle size. The term "melting" means melting at least a part of the resin composition in the content of the biaxial kneader. The non-magnetic powder and the magnetic powder in the compound can not be melted in the preparation process of the compound. The composites of the examples were prepared by the above method. The content of the magnetic powder and the content of the non-magnetic powder based on the total amount of the composite are shown in table 1.
Comparative examples 1 and 2
A compound of comparative example was prepared in the same manner as in example except that the types and blending amounts of the respective components were changed as shown in table 2.
[ evaluation of Complex ]
The following evaluations were performed on the composites obtained in examples and comparative examples. The results are shown in tables 1 to 3.
(melt viscosity)
As a measurement device, CFT-100 (flow tester) manufactured by Shimadzu Corporation was used. As a measurement sample, a columnar tablet having a diameter of 10mm was prepared from 7g of the composite. The lowest melt viscosity of the composite at 175℃was measured using a tablet under the conditions of 175℃waste heat of 10 seconds and a load of 10 kg.
(Burr)
The composite was molded using a mold having a plurality of 5 μm slits at a molding temperature of 175℃under a molding pressure of 6.9MPa for a curing time of 120 seconds.
The maximum value of the distance (mm) from which the compound flowed out to each slit was measured as the burr length.
(bending test)
After the composite was transfer molded at 175℃under a molding pressure of 13.5MPa and a curing time of 360 seconds, post cure (Post cure) was performed at 175℃for 5.5 hours, whereby test pieces 80mm in height by 10mm in width by 3mm in thickness were obtained.
The test piece was subjected to a 3-point support type bending test at room temperature and 250℃using an Autograph with a constant temperature bath. AGS-500A manufactured by Shimadzu Corporation was used as an autoprograph. In the bending test, one of the faces of the test piece was supported by 2 fulcrums. A load was applied at a central position between 2 fulcrums on the other face of the test piece. The load when the test piece was broken was measured. The bending test was carried out under the following conditions: distance between two fulcrums Lv: 64.0.+ -. 0.5mm, head speed: 2.0.+ -. 0.2 mm/min, chart speed: 100 mm/min, chart full scale (Chart full scale): 490N (50 kgf).
The bending strength σ (unit: MPa) was calculated from the following equation (A). In the following expression, "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, and "t" is the thickness (unit: mm) of the test piece.
σ＝(3×P×Lv)/(2×W×t 2 ) (A)
The test piece was subjected to a moisture resistance test at 121℃and a humidity of 100% (saturation) for 20 hours. The same bending test as described above was performed using the test piece after the moisture resistance test, and the bending strength at room temperature was measured.
(thermal expansion Rate)
After the composite was transfer molded at 175℃under a molding pressure of 13.5MPa and a curing time of 360 seconds, the composite was post-cured at 175℃for 5.5 hours, whereby a test piece having a height of 19 mm. Times.3 mm in width. Times.3 mm in thickness was obtained.
The thermal expansion coefficient of the test piece was measured using a thermo-mechanical analysis apparatus (trade name: TMA 8140) manufactured by Rigaku Denki Co., ltd. The measurement was performed at a temperature rise rate of 5℃per minute and at a temperature ranging from 25 to 250℃to determine the thermal expansion rate before and after the glass transition temperature. The coefficient of thermal expansion (CTE 2) above the glass transition temperature is shown in the table.
(warp)
The compound was molded into a shape of 36mm in height, 52mm in width, and 2mm in thickness on a 58mm by 48mm lead frame at a molding temperature of 175℃under a molding pressure of 12MPa for 180 seconds. After molding, the mixture was post-cured at 175℃for 5.5 hours, whereby a molded article in which the cured product of the compound was formed on a lead frame was obtained. The molded article was placed on a table with the surface of the cured product having the composite formed facing upward, and the warpage was measured by measuring the height of the end of the molded article from the table.
TABLE 1
TABLE 2
(Heat resistance)
The composites of examples 1 and 2 and the composite of comparative example 1 were subjected to transfer molding using a mold capable of obtaining a ring shape at a molding temperature of 175 ℃, a molding pressure of 13.5MPa, and a curing time of 360 seconds, and then post-cured at 175 ℃ for 5.5 hours, thereby producing a molded article having dimensions of 20mm in outer diameter, 12mm in inner diameter, and 2mm in thickness.
After the primary winding was wound around the molded body 5 turns and the secondary winding was wound around the molded body 5 turns, the relative permeability μs of the molded body was measured. For the measurement of the relative permeability μs, a B-H analyzer (SY-8218) manufactured by iwotsu Electric co. The frequency at which the relative permeability was measured was 1MHz. Next, the relative permeability μS' of the molded article after heat treatment at 150℃for 1000 hours was measured. The value of μS'/μS represents the retention rate of the relative permeability after the heat treatment, and is used as an index of heat resistance. The results are shown in table 3.
TABLE 3
| Example 1 | Example 2 | Comparative example 1 | |
| μS’/μS | 1.07 | 1.04 | 1.05 |
Claims (7)
1. A composite comprising a resin composition containing an epoxy resin and a curing agent, a non-magnetic powder and a magnetic powder,
the content of the magnetic powder is 94 to 98 mass percent based on the total amount of the compound,
the minimum melt viscosity at 175 ℃ is 10 to 220 Pa.s.
2. The composite of claim 1, wherein,
the content of the non-magnetic powder is 0.10 to 1.50 mass% based on the total amount of the composite.
3. The composite of claim 1, wherein,
the average particle diameter of the non-magnetic powder is 0.3-20 mu m.
4. The composite of claim 1, wherein,
the non-magnetic powder comprises silica.
5. The composite of claim 1, wherein,
the magnetic powder comprises magnetic powder with average particle diameter of 11-45 μm and magnetic powder with average particle diameter of 0.1-9 μm.
6. A shaped body comprising the complex of any one of claims 1 to 5.
7. A cured product of the composite according to any one of claims 1 to 5.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2021098479 | 2021-06-14 | ||
| JP2021-098479 | 2021-06-14 | ||
| PCT/JP2022/023310 WO2022264919A1 (en) | 2021-06-14 | 2022-06-09 | Compound, molded object, and cured compound |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117121134A true CN117121134A (en) | 2023-11-24 |
Family
ID=84527510
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202280024658.9A Pending CN117121134A (en) | 2021-06-14 | 2022-06-09 | Composite, molded article, and cured product of composite |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JPWO2022264919A1 (en) |
| CN (1) | CN117121134A (en) |
| TW (1) | TW202307064A (en) |
| WO (1) | WO2022264919A1 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019102782A (en) * | 2017-11-28 | 2019-06-24 | 住友ベークライト株式会社 | Thermosetting resin composition, coil having magnetic core and/or outer package member, and method for manufacturing molded product |
-
2022
- 2022-06-09 CN CN202280024658.9A patent/CN117121134A/en active Pending
- 2022-06-09 JP JP2023529833A patent/JPWO2022264919A1/ja active Pending
- 2022-06-09 WO PCT/JP2022/023310 patent/WO2022264919A1/en active Application Filing
- 2022-06-10 TW TW111121551A patent/TW202307064A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2022264919A1 (en) | 2022-12-22 |
| TW202307064A (en) | 2023-02-16 |
| WO2022264919A1 (en) | 2022-12-22 |
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