JP3361502B2 - Magnetic material, molded product thereof, high-density ferrite electronic component obtained by using the same, and methods for producing them - Google Patents
Magnetic material, molded product thereof, high-density ferrite electronic component obtained by using the same, and methods for producing themInfo
- Publication number
- JP3361502B2 JP3361502B2 JP2000078750A JP2000078750A JP3361502B2 JP 3361502 B2 JP3361502 B2 JP 3361502B2 JP 2000078750 A JP2000078750 A JP 2000078750A JP 2000078750 A JP2000078750 A JP 2000078750A JP 3361502 B2 JP3361502 B2 JP 3361502B2
- Authority
- JP
- Japan
- Prior art keywords
- ferrite
- density
- fatty acid
- acid ester
- molded body
- 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.)
- Expired - Fee Related
Links
- 229910000859 α-Fe Inorganic materials 0.000 title claims description 101
- 239000000696 magnetic material Substances 0.000 title claims description 33
- 238000000034 method Methods 0.000 title claims description 29
- -1 fatty acid ester Chemical class 0.000 claims description 63
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 49
- 239000000194 fatty acid Substances 0.000 claims description 49
- 229930195729 fatty acid Natural products 0.000 claims description 49
- 239000008187 granular material Substances 0.000 claims description 45
- 238000000465 moulding Methods 0.000 claims description 38
- 238000005245 sintering Methods 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 19
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000000047 product Substances 0.000 description 24
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 21
- 238000005469 granulation Methods 0.000 description 15
- 230000003179 granulation Effects 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- 150000004665 fatty acids Chemical class 0.000 description 10
- 238000005452 bending Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 238000000605 extraction Methods 0.000 description 8
- 150000002148 esters Chemical class 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000004147 Sorbitan trioleate Substances 0.000 description 4
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 235000019337 sorbitan trioleate Nutrition 0.000 description 4
- 229960000391 sorbitan trioleate Drugs 0.000 description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 4
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 3
- 229910017518 Cu Zn Inorganic materials 0.000 description 3
- 229910017752 Cu-Zn Inorganic materials 0.000 description 3
- 229910017943 Cu—Zn Inorganic materials 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 125000002947 alkylene group Chemical group 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 150000002402 hexoses Chemical class 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 235000021313 oleic acid Nutrition 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 description 1
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 1
- IJCWFDPJFXGQBN-RYNSOKOISA-N [(2R)-2-[(2R,3R,4S)-4-hydroxy-3-octadecanoyloxyoxolan-2-yl]-2-octadecanoyloxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCCCCCCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCCCCCCCCCCCC IJCWFDPJFXGQBN-RYNSOKOISA-N 0.000 description 1
- 150000003926 acrylamides Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- BGGDRACWOICIIC-KVVVOXFISA-N dodecanoic acid;(z)-octadec-9-enoic acid Chemical compound CCCCCCCCCCCC(O)=O.CCCCCCCC\C=C/CCCCCCCC(O)=O BGGDRACWOICIIC-KVVVOXFISA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- FBPFZTCFMRRESA-UHFFFAOYSA-N hexane-1,2,3,4,5,6-hexol Chemical compound OCC(O)C(O)C(O)C(O)CO FBPFZTCFMRRESA-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical class C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 239000001570 sorbitan monopalmitate Substances 0.000 description 1
- 235000011071 sorbitan monopalmitate Nutrition 0.000 description 1
- 229940031953 sorbitan monopalmitate Drugs 0.000 description 1
- 239000001587 sorbitan monostearate Substances 0.000 description 1
- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 0.000 description 1
- 239000001589 sorbitan tristearate Substances 0.000 description 1
- 235000011078 sorbitan tristearate Nutrition 0.000 description 1
- 229960004129 sorbitan tristearate Drugs 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000009718 spray deposition Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- 239000001993 wax Substances 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
- H01F1/34—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 non-metallic substances, e.g. ferrites
- H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
- H01F1/37—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 non-metallic substances, e.g. ferrites in the form of particles in a bonding agent
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Soft Magnetic Materials (AREA)
Description
【0001】[0001]
【発明の属する技術分野】本発明は、表面の少なくとも
一部が特定の脂肪酸エステルで被覆されたフェライト造
粒体からなる新規な磁性材料、この磁性材料の製造方
法、この磁性材料の成形体、これを用いて得られる高密
度フェライト電子部品及びその製造方法に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a novel magnetic material consisting of a ferrite granule having at least a part of its surface coated with a specific fatty acid ester, a method for producing this magnetic material, a molded body of this magnetic material, The present invention relates to a high-density ferrite electronic component obtained by using this and a manufacturing method thereof.
【0002】[0002]
【従来の技術】フェライトは、一般的に、耐熱性、耐化
学薬品性、機械的性質などに優れ、かつ電気絶縁性が大
きいなどの性質を有することから、例えば電気絶縁部
品、電子製品部品などの各種電子部品の製造用材料とし
て広く用いられている。2. Description of the Related Art Ferrite generally has excellent heat resistance, chemical resistance, mechanical properties and the like, and has a large electric insulation property. It is widely used as a material for manufacturing various electronic components.
【0003】そして、このようなフェライト電子部品を
製造する方法としては、従来、様々な方法が採用されて
いるが、中でも乾式加圧成形法が一般的に広く行われて
いる。これは、例えば、フェライト粉末とバインダーと
水とから水性スラリーを調製し、これをスプレードライ
ヤーで噴霧乾燥して得られる造粒体、又はフェライト粉
末とバインダー溶液とを撹拌混合し、乾燥とオシレーテ
ィング押出し造粒を繰り返して得られる造粒体を加圧成
形する方法であり、このようにして得た成形体を、次い
で焼結することにより、フェライト電子部品が得られ
る。As a method for manufacturing such a ferrite electronic component, various methods have been conventionally adopted, but among them, the dry pressure molding method is generally widely used. This is, for example, an aqueous slurry prepared from ferrite powder, a binder and water and spray-dried with a spray dryer, or a granulated product obtained by stirring or mixing the ferrite powder and a binder solution, followed by drying and oscillating. This is a method of press-molding a granulated body obtained by repeating extrusion granulation, and by sintering the molded body thus obtained, a ferrite electronic component is obtained.
【0004】このような加圧成形法においては、フェラ
イト造粒体として、流動性が良好で、金型への充填性及
び小さい圧力でつぶれやすいものを使用することが、得
られるフェライト電子部品の品質をよくし、また生産性
を高めるという見地から重要である。ところで、流動性
がよく、小さい圧力でつぶれやすい造粒体を製造する方
法としては、これまで分散剤を用いてスラリーを調製
し、これを造粒する方法(特開平5−159918号公
報、特公平7−17460号公報)、バインダーの偏析
を抑制して造粒する方法(特公平3−31660号公
報、特開平10−59776号公報)などが知られてい
る。In such a pressure molding method, it is necessary to use, as the ferrite granulated material, one having good fluidity, filling in a mold and easily crushed by a small pressure. It is important from the standpoint of improving quality and increasing productivity. By the way, as a method for producing a granule having good fluidity and being easily crushed by a small pressure, a method of preparing a slurry using a dispersant and granulating the slurry has been hitherto disclosed (Japanese Patent Laid-Open No. 5-159918). Japanese Patent Publication No. 7-17460), a method of granulating while suppressing segregation of the binder (Japanese Patent Publication No. 3-31660, Japanese Patent Laid-Open No. 10-59776) and the like are known.
【0005】しかしながら、これらの方法は、一般にス
プレードライヤーを用いた噴霧乾燥造粒法に適用される
技術であって、オシレーティング押出し造粒法に適用し
ても、所定の効果を発揮することができない。その上、
この方法は、造粒体の流動性及び小さい圧力でのつぶれ
やすさは改善されるものの、得られる電子部品製造用成
形体の密度バラツキ、金型からの離型性、スプリングバ
ックによる成形体内部のヒビ、金型の長寿命化について
は、満足しうる効果が得られていない。However, these methods are techniques generally applied to the spray-drying granulation method using a spray dryer, and even when applied to the oscillating extrusion granulation method, a predetermined effect can be exhibited. Can not. Moreover,
This method improves the fluidity of the granules and the ease of crushing under a small pressure, but the density variation of the obtained molded article for electronic component production, the releasability from the mold, the inside of the molded article due to springback No satisfactory effect has been obtained with regard to cracks and longer life of the mold.
【0006】このような欠点を克服するために、本発明
者は、先にフェライト造粒体の表面の少なくとも一部を
高級脂肪酸のヘキシタンエステルにより被覆した高密度
フェライト電子部品製造用材料を提案した(特願平11
−270769号)。この材料は、乾式加圧成形する際
の造粒体の流動性、小さい圧力でのつぶれやすさは改善
され、かつ金型から取り出す際の抜き圧が従来のものよ
りも低下し、スプリングバック(成形体膨張)に起因す
る成形体内部のヒビ割れ発生もある程度抑制されるとい
う効果を奏するものの、得られる成形体の密度のバラツ
キや金型からの離型性の点では、必ずしも満足しうるも
のとはいえない上に、成形体及びそれを焼結して得られ
る電子部品の強度が不十分であった。In order to overcome such drawbacks, the present inventor previously proposed a material for producing high density ferrite electronic parts, in which at least a part of the surface of a ferrite granule is coated with a hexitan ester of a higher fatty acid. Yes (Patent application 11
-270769). This material improves the fluidity of the granules during dry pressure molding, the ease of crushing under a small pressure, and the extraction pressure when removing from the mold is lower than that of the conventional material, resulting in spring back ( Although it has the effect of suppressing the occurrence of cracks inside the molded product due to (expansion of the molded product) to some extent, it is always satisfactory in terms of the density variation of the resulting molded product and the releasability from the mold. Not only that, but the strength of the molded body and the electronic component obtained by sintering the molded body was insufficient.
【0007】[0007]
【発明が解決しようとする課題】本発明は、このような
事情のもとで、金型からの離型性がよく、スプリングバ
ックによるヒビなどの成形不良がなく、かつ均質で優れ
た電磁特性を示し、しかも強度の高い高密度フェライト
電子部品を与える磁性材料を提供することを目的として
なされたものである。Under these circumstances, the present invention has good mold releasability from a mold, is free from molding defects such as cracks due to springback, and is uniform and excellent in electromagnetic characteristics. And a magnetic material that provides a high-density high-density ferrite electronic component.
【0008】[0008]
【課題を解決するための手段】本発明者は、先に提案し
た高級脂肪酸のヘキシタンエステルにより表面の少なく
とも一部が被覆されたフェライト造粒体に比べ、さらに
小さい圧力でつぶれ、金型の摩耗や損傷が少なく、金型
の長寿命化の達成に効果的で、かつスプリングバックに
よるヒビの発生が抑制され、焼結により、より強度の高
い高密度フェライト電子部品を与える磁性材料を開発す
るために鋭意研究した結果、前記高級脂肪酸のヘキシタ
ンエステルの代りに、親水性親油性比(以下HLBと略
記する)14以下のヘキシタン脂肪酸エステルポリオキ
シアルキレン縮合物を用いて、表面の少なくとも一部を
被覆したフェライト造粒体を用いることにより、その目
的を達成しうることを見出し、その知見に基づいて本発
明をなすに至った。Means for Solving the Problems The present inventor has crushed with a much smaller pressure as compared with the previously proposed ferrite granules having at least a part of the surface coated with a hexitane ester of a higher fatty acid, and Develop a magnetic material that has less wear and damage, is effective in achieving a longer mold life, suppresses the occurrence of cracks due to springback, and provides high-density ferrite electronic components with higher strength through sintering. As a result of diligent research for the purpose of using a hexitan ester of a higher fatty acid, a hexitan fatty acid ester polyoxyalkylene condensate having a hydrophilic lipophilicity ratio (hereinafter abbreviated as HLB) of 14 or less was used to replace at least a part of the surface It was found that the object can be achieved by using a ferrite granule coated with, and the present invention has been completed based on that finding.
【0009】すなわち、本発明は、HLB14以下のヘ
キシタン脂肪酸エステルポリオキシアルキレン縮合物に
より表面の少なくとも一部が被覆されたフェライト造粒
体からなる高密度フェライト電子部品製造用磁性材料、
それを型成形してなる高密度フェライト電子部品製造用
成形体、及びその型成形体を焼結してなる高密度フェラ
イト電子部品を提供するものである。そして、前記の磁
性材料は、例えばフェライト粉末にバインダーを加えて
造粒し、得られた造粒体に対し、HLB14以下のヘキ
シタン脂肪酸エステルポリオキシアルキレン縮合物を添
加したのち、両者をよく接触させて、該造粒体の表面の
少なくとも一部に該ヘキシタン脂肪酸エステルポリオキ
シアルキレン縮合物を付着させることにより製造するこ
とができるし、また前記の電子部品は、HLB14以下
のヘキシタン脂肪酸エステルポリオキシアルキレン縮合
物により表面の少なくとも一部が被覆されたフェライト
造粒体を所定の形状に型成形したのち、焼結することに
より製造することができる。That is, the present invention relates to a magnetic material for producing a high density ferrite electronic component, which comprises a ferrite granule having at least a part of its surface coated with a condensate of a hexytan fatty acid ester polyoxyalkylene having an HLB of 14 or less,
The present invention provides a molded product for producing a high-density ferrite electronic component, which is obtained by molding the same, and a high-density ferrite electronic component, which is obtained by sintering the molded product. The magnetic material is granulated by adding a binder to, for example, ferrite powder, and after adding a hexan fatty acid ester polyoxyalkylene condensate having an HLB of 14 or less to the granulated material, the two are well contacted with each other. Can be produced by adhering the hexitane fatty acid ester polyoxyalkylene condensate to at least a part of the surface of the granulated product, and the electronic component can be produced by the hexan fatty acid ester polyoxyalkylene having an HLB of 14 or less. It can be produced by molding a ferrite granulated body, at least a part of the surface of which is covered with a condensate, into a predetermined shape and then sintering the molded body.
【0010】[0010]
【発明の実施の形態】本発明の高密度フェライト電子部
品製造用磁性材料の主材として用いるフェライト造粒体
は、これまで一般に電子部品製造の際に用いられている
フェライト造粒体の場合と同じ方法、例えばスプレード
ライヤーによる噴霧造粒法やオシレーティング押出し造
粒法などにより、フェライト粉末を造粒して製造するこ
とができる。この際用いるフェライトの種類及び粒径に
ついては特に制限はなく、フェライト電子部品の使用目
的や用途に応じて適宜選択することができる。このフェ
ライト粉末の粒径範囲は、通常0.5〜5μmの範囲で
ある。本発明においては、このフェライト粉末は単独で
用いてもよいし、2種以上を組み合わせて用いてもよ
い。BEST MODE FOR CARRYING OUT THE INVENTION The ferrite granules used as the main material of the magnetic material for producing high density ferrite electronic parts of the present invention are the same as those used in the manufacture of electronic parts in general. The ferrite powder can be granulated and produced by the same method, for example, a spray granulation method using a spray dryer or an oscillating extrusion granulation method. The type and particle size of the ferrite used at this time are not particularly limited, and can be appropriately selected depending on the intended use and application of the ferrite electronic component. The particle size range of this ferrite powder is usually in the range of 0.5 to 5 μm. In the present invention, this ferrite powder may be used alone or in combination of two or more kinds.
【0011】このフェライト粉末の造粒に際しては、通
常バインダーが用いられる。このバインダーとしては、
従来フェライト粉末の造粒において一般に使用されてい
る公知のものの中から、任意に選択して用いることがで
きる。このようなバインダーとしては、例えばポリビニ
ルアルコールやポリ酢酸ビニルの部分けん化物、ポリア
クリル酸、メチルセルロース、アクリルアミド類の単独
重合体や共重合体などが挙げられる。これらのバインダ
ーは、フェライト粉末100質量部に対し、通常0.2
〜10質量部、好ましくは0.5〜8質量部、より好ま
しくは0.7〜5質量部の範囲で用いられる。A binder is usually used for granulating the ferrite powder. As this binder,
It is possible to arbitrarily select and use from publicly known ones generally used in granulation of conventional ferrite powder. Examples of such binders include partially saponified products of polyvinyl alcohol and polyvinyl acetate, polyacrylic acid, methyl cellulose, and homopolymers and copolymers of acrylamides. These binders are usually 0.2 per 100 parts by mass of ferrite powder.
It is used in the range of 10 to 10 parts by mass, preferably 0.5 to 8 parts by mass, and more preferably 0.7 to 5 parts by mass.
【0012】また、このフェライト粉末を造粒する際に
は、本発明の目的が損なわれない範囲で、所望により、
各種の公知の添加成分、例えばポリカルボン酸塩、縮合
ナフタレンスルホン酸塩などの分散剤、グリセリン、グ
リコール類、トリオール類などの可塑剤、ワックス、ス
テアリン酸やその塩などの滑剤、さらにはポリエーテル
系、ウレタン変性ポリエーテル系、ポリアクリル酸系、
変性アクリル酸系などの有機系高分子凝集剤、硫酸アル
ミニウム、塩化アルミニウム、硝酸アルミニウムなどの
無機系凝集剤などを添加することができる。このように
して得られるフェライト造粒体は、従来電子部品の製造
に際して、一般に用いられているフェライト造粒体と同
じ範囲内の粒径にすればよく、特に変える必要はない。
この粒径範囲は通常平均粒径で50〜500μm、好ま
しくは70〜300μmの範囲である。When granulating the ferrite powder, if desired, within a range not impairing the object of the present invention, if desired.
Various known additives, for example, polycarboxylic acid salts, dispersants such as condensed naphthalene sulfonates, plasticizers such as glycerin, glycols, triols, waxes, lubricants such as stearic acid and its salts, and polyethers. System, urethane modified polyether system, polyacrylic acid system,
An organic polymer flocculant such as a modified acrylic acid type or an inorganic flocculant such as aluminum sulfate, aluminum chloride or aluminum nitrate may be added. The ferrite granules thus obtained may have a particle size within the same range as the ferrite granules that are generally used in the production of conventional electronic parts, and there is no particular need to change it.
This particle size range is usually an average particle size of 50 to 500 μm, preferably 70 to 300 μm.
【0013】次に、このフェライト造粒体の表面の少な
くとも一部に被覆させるヘキシタン脂肪酸エステルポリ
オキシアルキレン縮合物は、種々の六炭糖、すなわちヘ
キソースを還元して得たヘキシトール、例えばソルビッ
ト、マンニットなどに脂肪酸を反応させてエステル化し
たのち、分子内脱水を行わせて得られるヘキシタン脂肪
酸エステルに、アルキレンオキシド、例えばエチレンオ
キシド、プロピレンオキシドを縮合させたもので、市販
品として容易に入手することができる。Next, the hexitane fatty acid ester polyoxyalkylene condensate with which at least a part of the surface of the ferrite granules is coated, is a hexitol obtained by reducing various hexoses, that is, hexoses, such as sorbitol and mannitol. A hexan fatty acid ester obtained by reacting knit with a fatty acid for esterification and then undergoing intramolecular dehydration, which is obtained by condensing an alkylene oxide such as ethylene oxide or propylene oxide, and is easily available as a commercial product. You can
【0014】上記の脂肪酸としては、炭素数12〜18
の脂肪酸が好ましく、このような脂肪酸の例としては、
ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン
酸、オレイン酸、各天然混合脂肪酸などを挙げることが
できるが、特にパルミチン酸、ステアリン酸及びオレイ
ン酸が好ましい。The above fatty acid has 12 to 18 carbon atoms.
The fatty acids of are preferred, and examples of such fatty acids include:
Examples thereof include lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, natural mixed fatty acids, and the like, with palmitic acid, stearic acid, and oleic acid being particularly preferable.
【0015】本発明において用いるものは、これらの脂
肪酸とヘキシタンとの部分エステルでもよいし完全エス
テルでもよい。また、これらのヘキシタン脂肪酸エステ
ルに縮合させるアルキレンオキシドとしては、例えばエ
チレンオキシドやプロピレンオキシドがある。このアル
キレンオキシドは、通常3〜30個、好ましくは5〜2
0個の範囲で縮合させたものが用いられる。このような
ヘキシタン脂肪酸エステルポリオキシアルキレン縮合物
のうち市販されているものとしては、例えばソルビタン
オレイン酸ラウリン酸混合エステルポリオキシエチレン
縮合物、ソルビタンヘキサオレイン酸エステルポリオキ
シエチレン縮合物、ソルビタン混合脂肪酸エステルポリ
オキシエチレン縮合物、ソルビタンモノラウリン酸エス
テルポリオキシエチレン縮合物、ソルビタンモノパルミ
チン酸エステルポリオキシエチレン縮合物、ソルビタン
モノステアリン酸エステルポリオキシエチレン縮合物、
ソルビタントリステアリン酸エステルポリオキシエチレ
ン縮合物、ソルビタンモノオレイン酸エステルポリオキ
シエチレン縮合物、マンニタンモノパルミチン酸エステ
ルポリオキシエチレン縮合物などを挙げることができ
る。What is used in the present invention may be a partial ester or a complete ester of these fatty acids and hexitane. Further, examples of the alkylene oxide to be condensed with these hexitane fatty acid esters include ethylene oxide and propylene oxide. The alkylene oxide is usually 3 to 30, preferably 5 to 2.
Those condensed in the range of 0 are used. Commercially available products of such a hexitane fatty acid ester polyoxyalkylene condensate include, for example, sorbitan oleic acid lauric acid mixed ester polyoxyethylene condensate, sorbitan hexaoleic acid ester polyoxyethylene condensate, sorbitan mixed fatty acid ester. Polyoxyethylene condensate, sorbitan monolaurate polyoxyethylene condensate, sorbitan monopalmitate polyoxyethylene condensate, sorbitan monostearate polyoxyethylene condensate,
Examples thereof include sorbitan tristearate polyoxyethylene condensate, sorbitan monooleate polyoxyethylene condensate, and mannitane monopalmitate polyoxyethylene condensate.
【0016】本発明において用いるヘキシタン脂肪酸エ
ステルポリオキシアルキレン縮合物は、HLBが14以
下であることが必要である。これが14を超えると、磁
性材料の金型からの離型性及び小さい圧力での加圧成形
性はよいが、成形体強度が低下する。The HLB of the hexitane fatty acid ester polyoxyalkylene condensate used in the present invention must be 14 or less. When it exceeds 14, the releasability of the magnetic material from the mold and the pressure moldability with a small pressure are good, but the strength of the molded body is lowered.
【0017】本発明の高密度フェライト電子部品製造用
磁性材料においては、フェライト造粒体の表面を被覆し
ているヘキシタン脂肪酸エステルポリオキシアルキレン
縮合物の量が、フェライト造粒体の質量に基づき0.1
〜3.0質量%であることが好ましい。In the magnetic material for producing high density ferrite electronic parts of the present invention, the amount of the hexitan fatty acid ester polyoxyalkylene condensate covering the surface of the ferrite granulated product is 0 based on the mass of the ferrite granulated product. .1
It is preferably from 3.0% by mass.
【0018】このヘキシタン脂肪酸エステルポリオキシ
アルキレン縮合物の量がフェライト造粒体の質量に基づ
き0.1質量%未満では、本発明の効果が十分に発揮さ
れないし、また3.0質量%を超えるとその量を増加し
ても効果の向上が認められず、むしろ成形体の強度が大
幅に低下するという不都合が発生し、また経済的にも不
利となる。効果及び経済性を考慮すると、このヘキシタ
ン脂肪酸エステルポリオキシアルキレン縮合物の使用量
は0.2〜2.0質量%の範囲であり、特に0.3〜
1.5質量%の範囲が好適である。If the amount of the hexitan fatty acid ester polyoxyalkylene condensate is less than 0.1% by mass based on the mass of the ferrite granulated product, the effect of the present invention is not sufficiently exhibited, and more than 3.0% by mass. However, even if the amount is increased, the effect is not improved, rather the strength of the molded body is significantly lowered, which is disadvantageous economically. Considering the effect and economical efficiency, the amount of the hexitane fatty acid ester polyoxyalkylene condensate used is in the range of 0.2 to 2.0% by mass, and particularly 0.3 to
A range of 1.5% by mass is suitable.
【0019】次に、本発明方法に従い、ヘキシタン脂肪
酸エステルポリオキシアルキレン縮合物により表面の少
なくとも一部が被覆されたフェライト造粒体を製造する
には、前記のようにしてフェライト粉末を造粒したの
ち、これにHLB14以下のヘキシタン脂肪酸エステル
ポリオキシアルキレン縮合物を接触させることが必要で
ある。造粒前にフェライト粉末にヘキシタン脂肪酸エス
テルポリオキシアルキレン縮合物を配合すると、型成形
の際の金型からの離型性の改善が不十分であり、またス
プリングバックによる成形不良がなく、高強度の成形体
を得ることができない。Next, according to the method of the present invention, in order to produce a ferrite granule having at least a part of its surface coated with a polyoxyalkylene condensate of hexitane fatty acid, the ferrite powder is granulated as described above. After that, it is necessary to bring this into contact with a hexan fatty acid ester polyoxyalkylene condensate having an HLB of 14 or less. When ferrite powder is mixed with hexitan fatty acid ester polyoxyalkylene condensate before granulation, the mold releasability from the mold at the time of mold molding is insufficiently improved, and there is no molding failure due to springback, resulting in high strength. Cannot be obtained.
【0020】フェライト造粒体をヘキシタン脂肪酸エス
テルポリオキシアルキレン縮合物で被覆するには、例え
ばヘキシタン脂肪酸エステルポリオキシアルキレン縮合
物を必要に応じ溶剤、例えばエチルアルコールで1.5
〜3倍に希釈し、これをフェライト造粒体に添加してド
ラムミキサーのような混合装置を用いて混合するか、あ
るいは転動流動層を利用して造粒体を転動させながら、
ヘキシタン脂肪酸エステルポリオキシアルキレン縮合物
と接触させたのち、溶媒を除去することによって行われ
る。そのほか、ヘキシタン脂肪酸エステルポリオキシア
ルキレン縮合物溶液を霧化して添加する方法、固体状の
まま又は溶融状態で添加し、機械的に混合する方法など
も用いることができる。To coat the ferrite granules with the hexitane fatty acid ester polyoxyalkylene condensate, for example, the hexitane fatty acid ester polyoxyalkylene condensate is added with a solvent, such as ethyl alcohol, for 1.5 times.
˜3 times diluted and added to ferrite granules and mixed using a mixing device such as a drum mixer, or while rolling the granules using a rolling fluidized bed,
It is carried out by removing the solvent after contacting with the hexitane fatty acid ester polyoxyalkylene condensate. In addition, a method of atomizing and adding a solution of a polyoxyalkylene condensate of hexitane fatty acid ester, a method of mechanically mixing in a solid state or in a molten state, and the like can be used.
【0021】次に、本発明方法により、高密度フェライ
ト電子部品製造用磁性材料を製造するための好適な実施
態様の1例を説明すると、先ず、フェライト粉末を、例
えば、スプレードライヤー法、噴霧造粒法又はオシレー
ティング押出造粒法により造粒して、平均粒径80〜3
00μmの造粒体を作製し、次いでこれにHLB14以
下のソルビタン脂肪酸エステルポリオキシエチレン縮合
物を所定の割合で加え、十分に接触させることによっ
て、フェライト造粒体表面の少なくとも一部をこれによ
って被覆させる。この際の被覆はフェライト造粒体の表
面全体が均質に覆われるように行うのが好ましいが、そ
の一部例えば表面積の10%以上が覆われていれば十分
である。この際、上記のソルビタン脂肪酸エステルポリ
オキシエチレン縮合物は、その一部がフェライト造粒体
の表層部に浸透することがあるが、特に支障はない。Next, one example of a preferred embodiment for producing a magnetic material for producing high density ferrite electronic parts by the method of the present invention will be described. First, ferrite powder is prepared by, for example, a spray dryer method or a spray forming method. Granulated by a granulation method or an oscillating extrusion granulation method to obtain an average particle size of 80 to 3
At least a part of the surface of the ferrite granules is covered with a urbitan fatty acid ester polyoxyethylene condensate having an HLB of 14 or less at a predetermined ratio by making a granule having a size of 00 μm Let The coating at this time is preferably performed so that the entire surface of the ferrite granule is uniformly covered, but it is sufficient if a part thereof, for example, 10% or more of the surface area is covered. At this time, a part of the sorbitan fatty acid ester polyoxyethylene condensate may penetrate into the surface layer of the ferrite granule, but there is no particular problem.
【0022】このようにして、フェライト造粒体に、H
LB14以下のソルビタン脂肪酸エステルポリオキシエ
チレン縮合物を上記の範囲で含有させることにより、型
成形において滑り性、流動性、圧力伝達性が向上し、金
型への充填が良好となる。また、成形体強度の低減が少
ないため、ヒビ、欠けなどの成形不良の発生を抑制する
ことが可能となる。その結果、低い圧力でバラツキの少
ない成形体を与え得る、高密度フェライト電子部品製造
用磁性材料が得られる。In this way, the ferrite granules were mixed with H
By including the sorbitan fatty acid ester polyoxyethylene condensate having an LB of 14 or less in the above range, slipperiness, fluidity and pressure transferability in mold molding are improved, and filling into a mold becomes good. Further, since the reduction in the strength of the molded body is small, it is possible to suppress the occurrence of molding defects such as cracks and chips. As a result, it is possible to obtain a magnetic material for producing high-density ferrite electronic parts, which can give a molded product with little variation at low pressure.
【0023】次に、このようにして得た表面の少なくと
も一部がHLB14以下のソルビタン脂肪酸エステルポ
リオキシエチレン縮合物で被覆されたフェライト造粒体
を成形して高密度フェライト電子部品製造用成形体を製
造するには、上記のようにして被覆されたフェライト造
粒体を通常の型成形法により所望の形状に成形する。こ
の型成形は、特にフェライト造粒体を金型を用いて乾式
プレス成形を行うのが有利である。この際のプレス圧力
は、通常40〜500MPa、好ましくは80〜400
MPaの範囲で選ばれる。この際使用されるフェライト
造粒体は、良好な離型性を有するため、金型からの成形
体取出時の抜き圧が低く、金型の摩耗や損傷を抑制しう
るという利点がある。さらに、これらの効果により、金
型からの成形体取出時のスプリングバック(成形体膨
張)が減少し、成形体強度も高いまま維持できるため、
ヒビや欠けなどの成形不良の発生が防止される。Next, a ferrite granulated product obtained by coating at least a part of the surface thus obtained with a sorbitan fatty acid ester polyoxyethylene condensate having an HLB of 14 or less is molded to form a molded product for producing high density ferrite electronic parts. In order to manufacture, the ferrite granules coated as described above are molded into a desired shape by a usual molding method. In this mold forming, it is particularly advantageous to dry-mold the ferrite granules using a mold. The pressing pressure at this time is usually 40 to 500 MPa, preferably 80 to 400
It is selected in the range of MPa. Since the ferrite granules used at this time have a good releasability, there is an advantage that the drawing pressure at the time of taking out the molded product from the mold is low and the wear and damage of the mold can be suppressed. Furthermore, due to these effects, spring back (mold body expansion) at the time of taking out the molded body from the mold is reduced, and since the molded body strength can be maintained high,
The occurrence of molding defects such as cracks and chips is prevented.
【0024】このようにして得た、高密度フェライト電
子部品製造用成形体を引き続き焼結すれば、高密度フェ
ライト電子部品が得られる。この際の焼結温度は、フェ
ライトの種類により異なるが、一般的には800〜14
00℃の範囲であり、好ましくは1000〜1300℃
の範囲である。その他の焼結条件及び焼結方法は、従来
のフェライト電子部品を製造する場合と全く同じであ
り、特に変更する必要はない。If the thus obtained molded body for producing high density ferrite electronic parts is subsequently sintered, high density ferrite electronic parts can be obtained. The sintering temperature at this time varies depending on the type of ferrite, but is generally 800 to 14
It is in the range of 00 ° C, preferably 1000 to 1300 ° C.
Is the range. Other sintering conditions and a sintering method are exactly the same as those in the case of manufacturing a conventional ferrite electronic component, and it is not particularly necessary to change them.
【0025】このようにして得られたフェライト電子部
品製造用成形体は、均質で高密度であり、例えばNi−
Cu−Zn系フェライトの場合には、密度2.7〜3.
7g/cm3程度のものとすることができる。また、こ
の電子部品は成形体の離型性がよいため、金型からの取
出時の抜き圧が低い上、排出時のスプリングバックが減
少し、ヒビなどの成形不良の発生が少ないので、電磁特
性が優れたものになる。The thus-obtained molded article for producing a ferrite electronic component is homogeneous and has a high density, and is formed of, for example, Ni-
In the case of Cu-Zn ferrite, the density is 2.7 to 3.
It can be about 7 g / cm 3 . In addition, since this electronic component has a good mold release property, the extraction pressure when removing from the mold is low, and the springback when discharging is reduced, and the occurrence of molding defects such as cracks is less likely to occur The characteristics are excellent.
【0026】[0026]
【実施例】次に、本発明を実施例により、さらに詳細に
説明するが、本発明は、これらの例によってなんら限定
されるものではない。EXAMPLES The present invention will now be described in more detail with reference to examples, but the present invention is not limited to these examples.
【0027】実施例1
Ni−Cu−Zn系フェライト粉末(平均粒径1μm)
66質量部、水34質量部、バインダー(ポリビニルア
ルコール)1.0質量部、分散剤(ポリカルボン酸アン
モニウム塩)0.25質量部を、湿式粉砕混合機で混合
して、フェライトスラリーを調製した。次に、このスラ
リーをスプレードライヤーを用いて噴霧造粒し、平均粒
径150μmの球形造粒体を得た。次いで、ソルビタン
トリオレイン酸エステルポリオキシエチレン縮合物(H
LB11)の50質量%エチルアルコール溶液を、上記
造粒体に対して0.6質量%の割合で添加し、ドラムミ
キサーで回転混合し、凝集粉の無いフェライト造粒体を
調製した。Example 1 Ni-Cu-Zn ferrite powder (average particle size 1 μm)
66 parts by mass, 34 parts by mass of water, 1.0 part by mass of binder (polyvinyl alcohol), and 0.25 parts by mass of dispersant (polycarboxylic acid ammonium salt) were mixed by a wet pulverization mixer to prepare a ferrite slurry. . Next, this slurry was spray-granulated using a spray dryer to obtain spherical granules having an average particle diameter of 150 μm. Then, sorbitan trioleate polyoxyethylene condensate (H
A 50 mass% ethyl alcohol solution of LB11) was added at a ratio of 0.6 mass% with respect to the above-mentioned granulated body, and the mixture was rotatively mixed with a drum mixer to prepare a ferrite granulated body having no aggregated powder.
【0028】次に、このようにして得た高密度フェライ
ト電子部品製造用磁性材料を所定の金型に充填し、成形
圧力300MPaで乾式プレス成形することにより、均
質で高密度のヒビのない円柱コア製造用成形体(直径
1.5mm、長さ1.8mm)を得た。この際の金型か
らの抜き圧は、従来のフェライト造粒体を用いた場合よ
りも低く、またスプリングバックも減少していた。この
円柱コア製造用成形体の製造では金型の損傷は認められ
ず、また摩耗も少ないため120万ショットの連続成形
を行うことができた。また、別に前記の高密度フェライ
ト電子部品製造用磁性材料1.5gを直径6mmの金型
に充填し、成形圧力を49〜294MPaの間で変化さ
せ、乾式プレス成形することにより、直径6mm、長さ
16〜19mmの円柱コア製造用成形体を製造した。こ
のサンプルについての成形圧力と成形体密度との関係を
示すグラフを図1(a)に、成形体密度と金型からの抜
き圧との関係を示すグラフを図2(a)に、成形体密度
と膨張率との関係(スプリングバックの変化)を示すグ
ラフを図3(a)にそれぞれ実線で示す。Next, the magnetic material for producing high-density ferrite electronic parts thus obtained is filled in a predetermined mold and subjected to dry press molding at a molding pressure of 300 MPa to obtain a homogeneous, high-density crack-free cylinder. A molded body for core production (diameter 1.5 mm, length 1.8 mm) was obtained. The drawing pressure from the mold at this time was lower than that in the case of using a conventional ferrite granulated body, and the spring back was also reduced. In the production of this molded body for producing a cylindrical core, damage to the mold was not recognized, and wear was small, so 1.2 million shots could be continuously molded. Separately, 1.5 g of the above-mentioned magnetic material for producing high-density ferrite electronic parts was filled in a mold having a diameter of 6 mm, the molding pressure was changed between 49 and 294 MPa, and dry press molding was performed to obtain a diameter of 6 mm and a length of 6 mm. A molded body for producing a cylindrical core having a size of 16 to 19 mm was manufactured. A graph showing the relationship between the molding pressure and the density of the molded body for this sample is shown in Fig. 1 (a), and a graph showing the relationship between the density of the molded body and the drawing pressure from the mold is shown in Fig. 2 (a). A graph showing the relationship between the density and the expansion coefficient (change in springback) is shown by a solid line in FIG.
【0029】実施例2〜4
表1に示すソルビタン脂肪酸エステルポリオキシエチレ
ン縮合物及びソルビタン脂肪酸エステルの添加量を用
い、実施例1と同様にして高密度フェライト電子部品製
造用磁性材料を調製し、それを実施例1と同様に直径6
mmの金型を用いて型成形して円柱コア製造用成形体を
製造した。これらの成形圧力と成形体密度との関係、成
形体密度と金型からの抜き圧との関係、成形体密度と膨
張率との関係は、実施例1の場合とほとんど同じであっ
た。Examples 2 to 4 Using the amounts of sorbitan fatty acid ester polyoxyethylene condensate and sorbitan fatty acid ester added shown in Table 1, magnetic materials for producing high density ferrite electronic parts were prepared in the same manner as in Example 1, The diameter is 6 as in the first embodiment.
A cylindrical core manufacturing body was manufactured by molding using a mm die. The relationship between the molding pressure and the molded body density, the relationship between the molded body density and the extraction pressure from the mold, and the relationship between the molded body density and the expansion coefficient were almost the same as in the case of Example 1.
【0030】比較例1
実施例1と同様にして、平均粒径150μmの球形フェ
ライト造粒体を製造した。この造粒体を、そのまま実施
例1と同様の直径6mmの金型を用いて型成形し、円柱
コア製造用成形体を製造した。このようにして得たソル
ビタン脂肪酸エステルポリオキシエチレン縮合物で被覆
しない成形体は、滑り性、圧力伝達性が悪い上、低圧で
は密度が低い成形体が得られるにすぎなかった。また、
このものは金型からの抜き圧が実施例1の場合よりもか
なり高く、高圧での成形では、成形体取出時に金型鳴き
が発生し、成形体に断層ヒビが認められた。実施例1と
同様にして調べた成形圧力と成形体密度との関係を示す
グラフを図1(a)に、成形体密度と金型からの抜き圧
との関係を示すグラフを図2(a)に、成形体密度と膨
張率との関係(スプリングバックの変化)を示すグラフ
を図3(a)にそれぞれ破線で示す。Comparative Example 1 In the same manner as in Example 1, a spherical ferrite granule having an average particle diameter of 150 μm was produced. This granulated product was molded as it was using a mold having a diameter of 6 mm as in Example 1 to manufacture a molded product for manufacturing a cylindrical core. The molded product not coated with the sorbitan fatty acid ester polyoxyethylene condensate obtained in this manner had poor slipperiness and pressure transferability, and at low pressures, only a low density molded product was obtained. Also,
In this case, the extraction pressure from the mold was considerably higher than that in Example 1, and in molding at high pressure, squeaking of the mold occurred at the time of taking out the molded body, and a fault crack was observed in the molded body. A graph showing the relationship between the molding pressure and the density of the molded body examined in the same manner as in Example 1 is shown in FIG. 1 (a), and a graph showing the relationship between the density of the molded body and the drawing pressure from the mold is shown in FIG. 2 (a). ), A graph showing the relationship between the density of the molded body and the expansion coefficient (change in springback) is shown by broken lines in FIG.
【0031】比較例2
実施例1におけるソルビタン脂肪酸エステルポリオキシ
エチレン縮合物の50質量%エチルアルコール溶液の代
わりに、ステアリン酸亜鉛微粉末を、造粒体に対し0.
1質量%の割合で添加し、それ以外は実施例1と同様に
してフェライト造粒体を調製し、これを実施例1と同じ
直径6mmの金型を用いて型成形した。ステアリン酸亜
鉛の添加により、離型性が付与され、金型からの抜き圧
は低下したが、低圧での成形体密度が低く、密度バラツ
キも大きい成形体が得られた。また、円柱状成形体(直
径1.5mm、長さ1.8mm)の連続成形では、金型
の損傷は無いものの、摩耗が多く、70万ショットで寸
法及び外観の規格を外れる成形体を生じた。実施例1と
同様にして調べた成形圧力と成形体密度との関係、成形
体密度と膨張率との関係(スプリングバックの変化)は
比較例1の場合とほとんど同じであった。成形体密度と
金型からの抜き圧との関係を示すグラフを図2(a)に
点線で示す。Comparative Example 2 Instead of the 50% by mass ethyl alcohol solution of the sorbitan fatty acid ester polyoxyethylene condensate in Example 1, zinc stearate fine powder was added to the granulated product in an amount of 0.
1% by mass was added, and a ferrite granule was prepared in the same manner as in Example 1 except for the above, and this was molded using the same die having a diameter of 6 mm as in Example 1. By the addition of zinc stearate, mold releasability was imparted and the drawing pressure from the mold was reduced, but a compact having a low density at low pressure and a large density variation was obtained. Further, in continuous molding of a cylindrical molded body (diameter 1.5 mm, length 1.8 mm), although there is no damage to the mold, a large amount of wear causes a molded body that deviates from the specifications of dimensions and appearance in 700,000 shots. It was The relationship between the molding pressure and the density of the molded body and the relationship between the density of the molded body and the expansion coefficient (change in springback) examined in the same manner as in Example 1 were almost the same as those in Comparative Example 1. A graph showing the relationship between the density of the molded body and the drawing pressure from the mold is shown by the dotted line in FIG.
【0032】実施例5
Ni−Cu−Zn系フェライト粉末(平均粒径1μm)
100質量部に、固形分濃度6質量%のポリビニルアル
コール水溶液17質量部を添加し、撹拌造粒機TMミキ
サー(三井鉱山社製)で混合撹拌して造粒を行い、造粒
原料を調製した。この造粒原料をベルト式乾燥機で乾燥
処理し、オシレーティング造粒解砕機(日本精機社製)
で押出し造粒を行い、シフターで整粒し、平均粒径25
0μmのオシレーティング押出しにより造粒体を得た。
次いで、実施例1と同様に、HLB11のソルビタント
リオレイン酸エステルポリオキシエチレン縮合物の50
質量%エチルアルコール溶液を、上記造粒体に対し0.
6質量%の割合で添加し、ドラムミキサーで回転混合し
て、凝集粉を含まない高密度フェライト電子部品製造用
磁性材料を調製した。Example 5 Ni-Cu-Zn type ferrite powder (average particle size 1 μm)
17 parts by mass of an aqueous polyvinyl alcohol solution having a solid content of 6% by mass was added to 100 parts by mass, and the mixture was mixed and stirred by a stirring granulator TM mixer (manufactured by Mitsui Mining Co., Ltd.) for granulation to prepare a granulation raw material. . This granulation raw material is dried with a belt dryer and then oscillating granulator and crusher (manufactured by Nippon Seiki Co., Ltd.)
Extruded and granulated with a sifter, and sized with a shifter
Granules were obtained by 0 μm oscillating extrusion.
Then, as in Example 1, 50 parts of sorbitan trioleate polyoxyethylene condensate of HLB11 was obtained.
A mass% ethyl alcohol solution was added to the above granules in an amount of 0.
A magnetic material for producing high-density ferrite electronic parts containing no agglomerated powder was prepared by adding 6 mass% and rotating and mixing with a drum mixer.
【0033】次に、この磁性材料1.5gを用い、実施
例1と同様に、成形圧力を49〜294MPaに変化さ
せて乾式加圧成形することにより、均質で高密度でヒビ
のない円柱状成形体(直径6mm、長さ16〜19m
m)を得た。この際、金型からの抜き圧が低下し、スプ
リングバックも実施例1〜4のスプレードライヤーで造
粒した磁性材料を用いた場合よりもさらに減少した。Next, using 1.5 g of this magnetic material, as in Example 1, by changing the molding pressure to 49 to 294 MPa and performing dry pressure molding, a homogeneous, high-density, crack-free columnar shape was obtained. Molded body (diameter 6 mm, length 16-19 m
m) was obtained. At this time, the extraction pressure from the mold was lowered, and the spring back was further reduced as compared with the case where the magnetic material granulated by the spray dryer of Examples 1 to 4 was used.
【0034】この例における成形圧力と成形体密度との
関係を示すグラフを図1(b)に、成形体密度と金型か
らの抜き圧との関係を示すグラフを図2(b)に、成形
体密度と膨張率との関係(スプリングバックの変化)を
示すグラフを図3(b)に、それぞれ実線で示す。A graph showing the relationship between the molding pressure and the density of the molded body in this example is shown in FIG. 1 (b), and a graph showing the relationship between the density of the molded body and the drawing pressure from the mold is shown in FIG. 2 (b). A graph showing the relationship between the density of the molded body and the expansion coefficient (change in springback) is shown by a solid line in FIG.
【0035】比較例3
実施例5と同様にして、平均粒径250μmの造粒体を
調製した。この造粒体をそのまま型成形し、これを用い
ること以外は実施例5と同様にして成形体を製造した。
このようにして、ソルビタントリオレイン酸エステルポ
リオキシエチレン縮合体による被覆処理を行わない造粒
体を用いた場合は、滑り性、圧力伝達性が悪い上、低圧
での成形体密度が低く、かつ密度バラツキの大きい成形
体となった。また、金型からの抜き圧が高く、高圧での
成形では、成形体取出時に金型鳴きが発生し、得られた
成形体に断層ヒビが認められた。成形圧力と成形体密度
との関係を示すグラフを図1(b)に、成形体密度と金
型からの抜き圧との関係を示すグラフを図2(b)に、
成形体密度と膨張率との関係(スプリングバックの変
化)を示すグラフを図3(b)に、それぞれ破線で示
す。Comparative Example 3 In the same manner as in Example 5, a granule having an average particle size of 250 μm was prepared. A molded body was produced in the same manner as in Example 5 except that this granulated body was directly molded and used.
In this way, when using the granules that are not subjected to the coating treatment with the sorbitan trioleate polyoxyethylene condensate, the slipperiness and pressure transferability are poor, and the compact density at low pressure is low, and A molded product with a large variation in density was obtained. In addition, the mold was squeaked when the molded product was taken out when the molding was taken out at a high pressure because of the high extraction pressure from the mold, and a crack was observed in the resulting molded product. A graph showing the relationship between the molding pressure and the density of the molded body is shown in Fig. 1 (b), and a graph showing the relationship between the density of the molded body and the drawing pressure from the mold is shown in Fig. 2 (b).
A graph showing the relationship between the density of the molded body and the expansion coefficient (change in springback) is shown by broken lines in FIG. 3 (b).
【0036】比較例4
実施例5におけるソルビタントリオレイン酸エステルポ
リオキシエチレン縮合物の50質量%エチルアルコール
溶液の代わりに、ステアリン酸亜鉛微粉末を、造粒体に
対し0.1質量%の割合で添加した以外は、実施例5と
同様にして高密度フェライト電子部品製造用磁性材料を
調製し、次いでこれを型成形して成形体を製造した。ス
テアリン酸亜鉛の添加により、離型性が付与され、金型
からの抜き圧は低下したが、低圧での成形体密度が低
く、密度バラツキも大きい成形体となった。成形圧力と
成形体密度との関係は、比較例3の場合とほとんど同じ
であった。また成形体密度と金型からの抜き圧との関係
を示すグラフを図2(b)に、成形体密度と膨張率との
関係(スプリングバックの変化)を示すグラフを図3
(b)にそれぞれ点線で示す。Comparative Example 4 Zinc stearate fine powder was used in place of the 50 mass% ethyl alcohol solution of the sorbitan trioleate polyoxyethylene condensate in Example 5 in a proportion of 0.1 mass% with respect to the granules. A magnetic material for producing a high-density ferrite electronic component was prepared in the same manner as in Example 5 except that the compound was added in step 5, and then this was molded into a molded body. By the addition of zinc stearate, mold releasability was imparted and the drawing pressure from the mold was reduced, but the density of the compact at low pressure was low, and the density of the compact was large. The relationship between the molding pressure and the density of the molded body was almost the same as in Comparative Example 3. Further, FIG. 2B is a graph showing the relationship between the compact density and the drawing pressure from the mold, and FIG. 3 is a graph showing the relationship between the compact density and the expansion rate (change in springback).
Each is indicated by a dotted line in (b).
【0037】比較例5、6
表1に示すソルビタン脂肪酸エステルポリオキシエチレ
ン縮合物と添加量を用いた以外は、実施例1と同様にし
て高密度フェライト電子部品製造用磁性材料を調製し、
それを実施例1と同様に型成形して円柱コア製造用成形
体を製造した。これらの成形圧と成形体密度との関係、
成形体密度と金型からの抜き圧との関係、成形体密度と
膨張率との関係は、実施例1の場合とほとんど同じであ
った。Comparative Examples 5 and 6 A magnetic material for producing high density ferrite electronic parts was prepared in the same manner as in Example 1 except that the sorbitan fatty acid ester polyoxyethylene condensate shown in Table 1 and the addition amount were used.
It was molded in the same manner as in Example 1 to produce a molded body for producing a cylindrical core. The relationship between these molding pressures and the density of the molded body,
The relationship between the molded body density and the drawing pressure from the mold, and the relationship between the molded body density and the expansion coefficient were almost the same as in the case of Example 1.
【0038】実施例6
前記実施例1、2及び比較例5、6で得た高密度フェラ
イト電子部品製造用磁性材料を、それぞれ49〜147
MPaの圧力でプレス成形し、長さ55mm、幅12m
m、高さ3mmの直方体状のブロック成形体を製造し
た。このブロック成形体の抗折強度を、荷重試験機(ア
イコーエンジニアリング社製)を用いてJIS R16
01に従い測定した。この成形体密度と抗折強度の関係
を示すグラフを図4として示す。HLB14以下の実施
例1、2で得たフェライト磁性材料成形体では、被覆に
よる抗折強度の低減はなく、高い強度が維持できている
が、HLB15以上の比較例5、6で得たフェライト磁
性材料成形体では、抗折強度が低く、ヒビが発生しやす
いものであった。以上実施例1〜5及び比較例1〜6の
フェライト造粒体について造粒方法、被覆成分、その添
加量(フェライト造粒体に対する50%溶液としての質
量%)をまとめて表1に示す。Example 6 The magnetic materials for producing high density ferrite electronic parts obtained in Examples 1 and 2 and Comparative Examples 5 and 6 were 49 to 147, respectively.
Press-formed with a pressure of MPa, length 55 mm, width 12 m
A rectangular parallelepiped block molded body having m and a height of 3 mm was manufactured. The bending strength of this block molded body was measured by JIS R16 using a load tester (manufactured by Aiko Engineering Co., Ltd.).
It measured according to 01. A graph showing the relationship between the density of the molded body and the bending strength is shown in FIG. In the ferrite magnetic material compacts obtained in Examples 1 and 2 having HLB of 14 or less, the bending strength is not reduced by the coating and high strength can be maintained, but the ferrite magnetic materials obtained in Comparative Examples 5 and 6 having HLB of 15 or more are obtained. The molded article was low in flexural strength and was likely to crack. Table 1 collectively shows the granulation method, coating components, and the amount of addition (mass% as a 50% solution to the ferrite granules) of the ferrite granules of Examples 1 to 5 and Comparative Examples 1 to 6 described above.
【0039】[0039]
【表1】 [Table 1]
【0040】実施例7
前記実施例1〜4で得た高密度フェライト電子部品製造
用磁性材料を、それぞれ98MPaの圧力でプレス成形
し、外径21mm、内径12mm、厚さ7mmのリング
状成形体を製造した。次いで、これらを1030℃、1
060℃、1090℃の温度において2時間焼結し、リ
ング状コアを製造した。次に、これらのリング状コアの
密度をアルキメデス法に準じた方法で測定した。また、
これらのリング状コアについて100kHzにおける初
透磁率を、LCRメーター4274A(ヒューレット・
パッカード社製、商品名)により測定した。このように
して得た電子部品の焼結温度と密度との関係を示すグラ
フ及び焼結温度と初透磁率との関係を示すグラフをそれ
ぞれ図5及び図6に実線グラフA〜Cとして示す。図中
Aは、実施例1、Bは実施例2、Cは実施例3のフェラ
イト造粒体成形体を用いた結果である。なお、実施例4
の成形体を用いた電子部品の焼結温度と焼結体密度との
関係を示すグラフは実施例1のグラフAとほとんど同じ
であった。また、実施例2〜4の成形体を用いた電子部
品の焼結温度と初透磁率との関係を示すグラフは実施例
1のグラフAとほとんど同じであった。Example 7 The magnetic materials for producing high-density ferrite electronic parts obtained in Examples 1 to 4 were press-molded at a pressure of 98 MPa, and a ring-shaped molded body having an outer diameter of 21 mm, an inner diameter of 12 mm and a thickness of 7 mm. Was manufactured. Then, these are 1030 ℃, 1
A ring-shaped core was manufactured by sintering at a temperature of 060 ° C and 1090 ° C for 2 hours. Next, the densities of these ring-shaped cores were measured by a method according to the Archimedes method. Also,
The initial permeability at 100 kHz of these ring-shaped cores was measured by LCR meter 4274A (Hewlett
It was measured by Packard, trade name). A graph showing the relationship between the sintering temperature and the density of the electronic component thus obtained and a graph showing the relationship between the sintering temperature and the initial magnetic permeability are shown as solid line graphs A to C in FIGS. 5 and 6, respectively. In the figure, A is the result of using the ferrite granule compact of Example 1, B is Example 2, and C is Example 3. In addition, Example 4
The graph showing the relationship between the sintering temperature and the density of the sintered body of the electronic component using the molded body of was almost the same as the graph A of Example 1. The graph showing the relationship between the sintering temperature and the initial magnetic permeability of the electronic components using the molded bodies of Examples 2 to 4 was almost the same as the graph A of Example 1.
【0041】比較例7
前記比較例1、2で得たフェライト造粒体の成形体を用
い、実施例7と同様にして密度及び初透磁率を測定し、
このようにして得た電子部品の焼結温度と密度との関係
及び焼結温度と初透磁率との関係をそれぞれ図5及び図
6に破線グラフG、Hとして示す。Comparative Example 7 Using the molded ferrite granules obtained in Comparative Examples 1 and 2, the density and the initial magnetic permeability were measured in the same manner as in Example 7.
The relationship between the sintering temperature and the density and the relationship between the sintering temperature and the initial magnetic permeability of the thus obtained electronic component are shown as broken line graphs G and H in FIGS. 5 and 6, respectively.
【0042】実施例8
前記実施例1〜4で得た高密度フェライト電子部品製造
用磁性材料をそれぞれ98MPaの圧力でプレス成形
し、長さ55mm、幅12mm、高さ5mmの直方体状
のブロック成形体を得た。このブロック成形体を103
0℃、1060℃又は1090℃の温度において2時間
焼結し、ブロックコアを製造した。このようにして得た
電子部品について、荷重試験機を用いて測定した。これ
らのものの焼結温度と抗折強度の関係を図7に実線グラ
フA〜Dとして示す。Example 8 The magnetic materials for producing high-density ferrite electronic parts obtained in Examples 1 to 4 were press-molded at a pressure of 98 MPa to form a rectangular parallelepiped block having a length of 55 mm, a width of 12 mm and a height of 5 mm. Got the body This block molded body is
The block core was manufactured by sintering at a temperature of 0 ° C., 1060 ° C. or 1090 ° C. for 2 hours. The electronic components thus obtained were measured using a load tester. The relationship between the sintering temperature and the bending strength of these materials is shown as solid line graphs A to D in FIG.
【0043】比較例8
前記比較例1、2で得たフェライト造粒体を用い、実施
例8と同様にして成形、焼結することによりブロックコ
アを製造した。このようにして得たブロックコアについ
て、実施例8と同様にして抗折強度を測定した。これら
のものの焼結温度と抗折強度の関係を図7に破線グラフ
G、Hとして示す。Comparative Example 8 Using the ferrite granules obtained in Comparative Examples 1 and 2, molding and sintering were performed in the same manner as in Example 8 to produce a block core. The bending strength of the block core thus obtained was measured in the same manner as in Example 8. The relationship between the sintering temperature and the bending strength of these materials is shown as broken line graphs G and H in FIG.
【0044】比較例9
ソルビタン脂肪酸エステルポリオキシエチレン縮合物の
50質量%エチルアルコール溶液の同量を最初からフェ
ライト粉末に添加して造粒したこと以外は、実施例5と
同様にして高密度フェライト電子部品製造用磁性材料を
調製した。この高密度フェライト電子部品製造用磁性材
料と実施例5で得たものとをそれぞれ用いて実施例7及
び8と同様にして成形体を製造し、それぞれ1030℃
において2時間焼成した。このようにして得た電子部品
について実施例7及び8と同様にして密度及び抗折温度
を測定した結果を表2に示す。Comparative Example 9 High-density ferrite was prepared in the same manner as in Example 5 except that the same amount of a 50% by mass ethyl alcohol solution of a sorbitan fatty acid ester polyoxyethylene condensate was added to ferrite powder from the beginning for granulation. A magnetic material for manufacturing electronic parts was prepared. A molded body was manufactured in the same manner as in Examples 7 and 8 using the magnetic material for producing a high-density ferrite electronic component and the material obtained in Example 5, respectively, and at 1030 ° C.
Was baked for 2 hours. Table 2 shows the results of measuring the density and bending temperature of the electronic components thus obtained in the same manner as in Examples 7 and 8.
【0045】[0045]
【表2】 [Table 2]
【0046】この表から分かるように、ソルビタン脂肪
酸エステルポリオキシエチレン縮合物をフェライト粉末
にあらかじめ添加して造粒した場合と造粒後添加した場
合は明らかに後者の方が優れた物性を示す。As can be seen from this table, when the sorbitan fatty acid ester polyoxyethylene condensate is added to the ferrite powder in advance and granulated, and when added after granulation, the latter clearly shows better physical properties.
【0047】[0047]
【発明の効果】本発明によれば、乾式加圧成形の際、滑
り性、流動性、圧力伝達性、金型への充填性がよく、し
かも低い圧力でもバラツキが少なく、均質な成形体を与
える高密度フェライト電子部品製造用磁性材料が得られ
る。そして、この磁性材料を用いると、離型性が向上
し、金型からの取り出し時の抜き圧が低下する結果、金
型の摩耗や損傷が減少するという利点がある上に、金型
から取り出す際に伴うスプリングバックが減少し、ヒビ
のような成形不良の発生がなく、かつ成形体強度の低下
を抑制しうるという効果を奏する。EFFECTS OF THE INVENTION According to the present invention, during dry pressure molding, a slipperiness, fluidity, pressure transferability, and mold filling property are excellent, and there is little variation even at a low pressure, and a homogeneous molding is obtained. A high density ferrite magnetic material for producing electronic parts can be obtained. Further, when this magnetic material is used, the releasability is improved, and the extraction pressure at the time of taking out from the mold is reduced. As a result, wear and damage of the mold are reduced, and at the same time, it is taken out from the mold. This brings about the effects that the springback accompanying the decrease is reduced, molding defects such as cracks do not occur, and the reduction in the strength of the molded body can be suppressed.
【図1】 実施例1、5及び比較例1、3で得た成形体
の成形圧力と成形体密度との関係を示すグラフ。FIG. 1 is a graph showing the relationship between the molding pressure and the density of the molded bodies obtained in Examples 1 and 5 and Comparative Examples 1 and 3.
【図2】 実施例1、5及び比較例1〜4で得た成形体
の成形体密度と金型からの抜き圧との関係を示すグラ
フ。FIG. 2 is a graph showing the relationship between the compact density of the compacts obtained in Examples 1 and 5 and Comparative Examples 1 to 4 and the extraction pressure from the mold.
【図3】 実施例1、5及び比較例1、3、4で得た成
形体密度と膨張率との関係を示すグラフ。FIG. 3 is a graph showing the relationship between the density and the expansion coefficient of the molded bodies obtained in Examples 1 and 5 and Comparative Examples 1, 3 and 4.
【図4】 実施例6で得た成形体の成形体密度と成形体
抗折強度との関係を示すグラフ。FIG. 4 is a graph showing the relationship between the molded body density and the molded body bending strength of the molded body obtained in Example 6.
【図5】 実施例7及び比較例7で得た電子部品の焼結
温度と密度との関係を示すグラフ。FIG. 5 is a graph showing the relationship between the sintering temperature and the density of the electronic components obtained in Example 7 and Comparative Example 7.
【図6】 実施例7及び比較例7で得た電子部品の焼結
温度と初透磁率との関係を示すグラフ。FIG. 6 is a graph showing the relationship between the sintering temperature and the initial magnetic permeability of the electronic components obtained in Example 7 and Comparative Example 7.
【図7】 実施例8及び比較例8で得た電子部品の焼結
温度と抗折強度との関係を示すグラフ。FIG. 7 is a graph showing the relationship between the sintering temperature and the bending strength of the electronic components obtained in Example 8 and Comparative Example 8.
Claims (6)
キシタン脂肪酸エステルポリオキシアルキレン縮合物に
より表面の少なくとも一部が被覆されたフェライト造粒
体からなる高密度フェライト電子部品製造用磁性材料。1. A magnetic material for producing a high-density ferrite electronic component, which comprises a ferrite granule having at least a part of its surface coated with a hexitane fatty acid ester polyoxyalkylene condensate having a hydrophilic lipophilicity ratio (HLB) of 14 or less.
ルキレン縮合物の量がフェライト造粒体の質量に基づき
0.1〜3.0質量%の範囲にある請求項1記載の高密
度フェライト電子部品製造用磁性材料。2. The magnetic material for producing a high-density ferrite electronic component according to claim 1, wherein the amount of the hexytan fatty acid ester polyoxyalkylene condensate is in the range of 0.1 to 3.0% by mass based on the mass of the ferrite granulated product. material.
粒し、得られた造粒体に対し、親水性親油性比(HL
B)14以下のヘキシタン脂肪酸エステルポリオキシア
ルキレン縮合物を添加したのち、両者をよく接触させ
て、該造粒体の表面の少なくとも一部に該ヘキシタン脂
肪酸エステルポリオキシアルキレン縮合物を付着させる
ことを特徴とする高密度フェライト電子部品製造用磁性
材料の製造方法。3. A ferrite powder to which a binder is added and granulated, and the resulting granules have a hydrophilic lipophilicity ratio (HL).
B) After adding 14 or less hexitane fatty acid ester polyoxyalkylene condensate, contact them well and attach the hexitane fatty acid ester polyoxyalkylene condensate to at least a part of the surface of the granule. A method for producing a magnetic material for producing high-density ferrite electronic parts, which is characterized.
キシタン脂肪酸エステルポリオキシアルキレン縮合物に
より表面の少なくとも一部が被覆されたフェライト造粒
体を型成形してなる高密度フェライト電子部品製造用成
形体。4. Production of high-density ferrite electronic parts obtained by molding a ferrite granule having at least a part of its surface coated with a hexitane fatty acid ester polyoxyalkylene condensate having a hydrophilic lipophilicity ratio (HLB) of 14 or less. Molded body for.
キシタン脂肪酸エステルポリオキシアルキレン縮合物に
より表面の少なくとも一部が被覆されたフェライト造粒
体の型成形体を焼結してなる高密度フェライト電子部
品。5. A high density obtained by sintering a die-molded body of a ferrite granule, at least a part of the surface of which is coated with a hexitane fatty acid ester polyoxyalkylene condensate having a hydrophilic-lipophilic ratio (HLB) of 14 or less. Ferrite electronic components.
キシタン脂肪酸エステルポリオキシアルキレン縮合物に
より表面の少なくとも一部が被覆されたフェライト造粒
体を所定の形状に型成形したのち、焼結することを特徴
とする高密度フェライト電子部品の製造方法。6. A ferrite granule having at least a part of its surface coated with a hexitane fatty acid ester polyoxyalkylene condensate having a hydrophilic lipophilicity ratio (HLB) of 14 or less is molded into a predetermined shape and then sintered. A method for manufacturing a high-density ferrite electronic component, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000078750A JP3361502B2 (en) | 2000-03-21 | 2000-03-21 | Magnetic material, molded product thereof, high-density ferrite electronic component obtained by using the same, and methods for producing them |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000078750A JP3361502B2 (en) | 2000-03-21 | 2000-03-21 | Magnetic material, molded product thereof, high-density ferrite electronic component obtained by using the same, and methods for producing them |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001267116A JP2001267116A (en) | 2001-09-28 |
| JP3361502B2 true JP3361502B2 (en) | 2003-01-07 |
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ID=18596118
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000078750A Expired - Fee Related JP3361502B2 (en) | 2000-03-21 | 2000-03-21 | Magnetic material, molded product thereof, high-density ferrite electronic component obtained by using the same, and methods for producing them |
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| JP (1) | JP3361502B2 (en) |
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|---|---|---|---|---|
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- 2000-03-21 JP JP2000078750A patent/JP3361502B2/en not_active Expired - Fee Related
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