JP6380736B2 - 窒化鉄系磁性粉及びそれを用いた磁石 - Google Patents
窒化鉄系磁性粉及びそれを用いた磁石 Download PDFInfo
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- JP6380736B2 JP6380736B2 JP2014077710A JP2014077710A JP6380736B2 JP 6380736 B2 JP6380736 B2 JP 6380736B2 JP 2014077710 A JP2014077710 A JP 2014077710A JP 2014077710 A JP2014077710 A JP 2014077710A JP 6380736 B2 JP6380736 B2 JP 6380736B2
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- 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
- H01F1/032—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 hard-magnetic materials
- H01F1/10—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 hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—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 hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0622—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with iron, cobalt or nickel
-
- 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
- H01F1/032—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 hard-magnetic materials
- H01F1/04—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 hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Description
まず、本実施例及び比較例における測定方法について説明する。原料である酸化鉄及び得られた磁性粉の比表面積値は、窒素によるBET法を用いて測定した。原料である酸化鉄及び得られた磁性粉の組成は、加熱した試料を酸で溶解し、誘導結合プラズマ発光分光分析装置(ICP、島津製作所製ICPS−8100CL)を用いて測定し求めた。原料である酸化鉄及び得られた磁性粉の構成相は、粉末X線回折装置(XRD、リガク製RINT−2500)、メスバウアー分光分析装置により同定を行った。得られた磁性粉の磁気特性は、振動試料型磁力計(VSM、東英工業製VSM−5−20)を用いて296Kにて、0〜20000Oeの磁場中で測定した。得られた磁性粉のメスバウアー測定は、アルゴン雰囲気のグローブボックス中で磁性粉をラミネートパック中に入れて封止した状態で行った。メスバウアースペクトルのピーク解析は、スペクトルを理想線型の足し合わせと仮定してカーブフィッティングを行い、ピーク位置を定めて各成分のピーク面積を算出した。ピークは左右対称のローレンツ型とし、成分毎のピーク半値幅はすべて等しく、対称位置にあるピーク高さはそれぞれ等しいと仮定した。得られた各ピークの相対面積比をそのまま相対組成比として算出し、Fe16N2及びFe4Nの生成比率を求めた。
<出発原料の調整>
比表面積115m2/gの酸化鉄1を硫酸第一鉄、塩化第二鉄、水酸化ナトリウムを用いて作製した。同様に比表面積187m2/gの酸化鉄2を作製した。得られた2種の酸化鉄を分散液の状態で混合し、室温で2時間攪拌を行った。その後、数時間静置して上澄み液を除去した。続けて、得られた試料1gに対して200mL相当の純水を加えて上澄み液を除去する作業を7回繰り返した。85℃の真空乾燥機で乾燥し、乳鉢及び乳棒を用いて解砕を行った。
上記で得られた粉末5gを灰分測定用灰皿(50mm×30mm×深さ10mm)に入れ、熱処理炉に静置した。炉内に窒素ガスを充填した後、水素ガスを1L/minの流量で流しながら、5℃/minの昇温速度で250℃まで昇温し、12時間保持して還元処理を行った。その後、水素ガスの供給を止めて窒素ガスを2L/minの流量で流しながら160℃まで降温した。続いて、アンモニアガスを0.1L/minにて流しながら、160℃で12時間窒化処理を行った。その後、窒素ガスを2L/minの流量で流しながら50℃まで降温し、空気置換を12時間かけて行うことにより試料を得た。
実施例1と同様にして原料となる酸化鉄1及び酸化鉄2を得た。その後、試料1gに対して50mL相当の純水を加えて攪拌しながら、オルトケイ酸ナトリウム水溶液をSiが1.0質量%となるように加えた。得られた試料1gに対して再度200mL相当の純水を加えて数時間静置し、上澄み液を除去することにより洗浄した。続いて、85℃の真空乾燥機で乾燥し、乳鉢及び乳棒を用いて解砕を行った。得られた試料のSi含有量は1.0質量%であった。
実施例1〜14及び比較例1〜10で得られた試料の、メスバウアースペクトルより得られたFe16N2化合物相とFe4N化合物相の割合、比表面積、N量、保磁力について結果を表1に示す。
Claims (3)
- メスバウアースペクトルよりFe16N2化合物相がFe換算で70at%以上95at%以下、Fe4N化合物相が5at%以上30at%以下であり、
比表面積が10m 2 /g以上80m 2 /g以下であることを特徴とする窒化鉄系磁性粉。 - 請求項1の磁性粉であって、N量が3質量%以上6質量%以下であることを特徴とする窒化鉄系磁性粉。
- 請求項1又は請求項2に記載の窒化鉄系磁性粉を用いた磁石。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2014077710A JP6380736B2 (ja) | 2013-06-12 | 2014-04-04 | 窒化鉄系磁性粉及びそれを用いた磁石 |
US14/300,857 US20140370290A1 (en) | 2013-06-12 | 2014-06-10 | Iron nitride based magnetic powder and magnet using the same |
DE102014108271.0A DE102014108271A1 (de) | 2013-06-12 | 2014-06-12 | Magnetisches Pulver auf der Grundlage von Eisennitrid und Magnet, bei dem dasselbe benutzt wird |
CN201410262051.1A CN104240882B (zh) | 2013-06-12 | 2014-06-12 | 氮化铁系磁性粉末以及使用其的磁铁 |
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JP2013123722 | 2013-06-12 | ||
JP2013123722 | 2013-06-12 | ||
JP2014077710A JP6380736B2 (ja) | 2013-06-12 | 2014-04-04 | 窒化鉄系磁性粉及びそれを用いた磁石 |
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JP2015019050A JP2015019050A (ja) | 2015-01-29 |
JP6380736B2 true JP6380736B2 (ja) | 2018-08-29 |
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Country Status (4)
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US (1) | US20140370290A1 (ja) |
JP (1) | JP6380736B2 (ja) |
CN (1) | CN104240882B (ja) |
DE (1) | DE102014108271A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11779083B2 (en) | 2008-11-21 | 2023-10-10 | Boa Technology, Inc. | Reel based lacing system |
Families Citing this family (4)
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US11875934B2 (en) * | 2018-05-28 | 2024-01-16 | Regents Of The University Of Minnesota | Iron-rich permanent magnet |
CN109065318B (zh) * | 2018-07-13 | 2019-08-20 | 江南大学 | 一种基于磁晶各向异性能抵消原理制作高频软磁材料的方法 |
CN109192433A (zh) * | 2018-09-27 | 2019-01-11 | 常州古金磁性材料科技有限公司 | 一种具有高磁感应强度的软磁材料及其制备方法 |
JP6823323B2 (ja) * | 2019-02-01 | 2021-02-03 | 大陽日酸株式会社 | 強磁性粉末、組成物、成形品、強磁性粉末の製造方法 |
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JPH05222483A (ja) * | 1990-12-19 | 1993-08-31 | Nkk Corp | 窒化鉄系高密度焼結体の製造方法 |
JP3848486B2 (ja) | 1999-03-25 | 2006-11-22 | 日立マクセル株式会社 | 磁気記録媒体用窒化鉄系磁性粉末材料及びその製造方法並びに磁気記録媒体 |
JP4146769B2 (ja) * | 2003-08-08 | 2008-09-10 | 日立マクセル株式会社 | 磁気記録媒体 |
EP1548760A3 (en) * | 2003-11-27 | 2007-12-26 | DOWA Electronics Materials Co., Ltd. | Iron nitride magnetic powder and method of producing the powder |
JP2007036183A (ja) * | 2005-06-21 | 2007-02-08 | Fujifilm Holdings Corp | 磁性粒子の製造方法、磁性粒子、磁気記録媒体 |
US8535634B2 (en) * | 2007-05-04 | 2013-09-17 | Advanced Materials Corporation | Iron nitride powders for use in magnetic, electromagnetic, and microelectronic devices |
JP2009249682A (ja) | 2008-04-04 | 2009-10-29 | Nec Tokin Corp | 硬磁性合金およびその製造方法 |
JP4791513B2 (ja) * | 2008-08-05 | 2011-10-12 | 日立マクセル株式会社 | 窒化鉄系磁性粉末、及びそれを用いた磁気記録媒体 |
CN101607701B (zh) * | 2009-07-24 | 2011-01-05 | 东北大学 | 纳米化、强磁场双促进法制备氮化铁材料的方法及装置 |
JP2011129172A (ja) * | 2009-12-15 | 2011-06-30 | Hitachi Maxell Ltd | 窒化鉄系磁性粉末、及びそれを用いた磁気記録媒体 |
JP5822188B2 (ja) * | 2010-09-24 | 2015-11-24 | 戸田工業株式会社 | 強磁性粒子粉末及びその製造法、異方性磁石及びボンド磁石 |
JP5831866B2 (ja) * | 2011-01-21 | 2015-12-09 | 戸田工業株式会社 | 強磁性粒子粉末及びその製造方法、並びに異方性磁石、ボンド磁石及び圧粉磁石 |
EP2693538A4 (en) * | 2011-03-28 | 2015-05-06 | Univ Hyogo | ELECTRODE MATERIAL FOR RECHARGEABLE BATTERY, METHOD FOR PRODUCING ELECTRODE MATERIAL FOR RECHARGEABLE BATTERY, AND RECHARGEABLE BATTERY |
JP5858419B2 (ja) * | 2011-04-27 | 2016-02-10 | 戸田工業株式会社 | 強磁性粒子粉末の製造方法、異方性磁石、ボンド磁石及び圧粉磁石 |
JP5769069B2 (ja) * | 2011-06-03 | 2015-08-26 | 住友電気工業株式会社 | 窒化鉄材及びその製造方法 |
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2014
- 2014-04-04 JP JP2014077710A patent/JP6380736B2/ja active Active
- 2014-06-10 US US14/300,857 patent/US20140370290A1/en not_active Abandoned
- 2014-06-12 DE DE102014108271.0A patent/DE102014108271A1/de not_active Ceased
- 2014-06-12 CN CN201410262051.1A patent/CN104240882B/zh active Active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11779083B2 (en) | 2008-11-21 | 2023-10-10 | Boa Technology, Inc. | Reel based lacing system |
Also Published As
Publication number | Publication date |
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CN104240882B (zh) | 2017-04-12 |
US20140370290A1 (en) | 2014-12-18 |
DE102014108271A1 (de) | 2014-12-18 |
CN104240882A (zh) | 2014-12-24 |
JP2015019050A (ja) | 2015-01-29 |
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