JP5936686B2 - 混合酸化物および永久磁性粒子の製造方法 - Google Patents
混合酸化物および永久磁性粒子の製造方法 Download PDFInfo
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- JP5936686B2 JP5936686B2 JP2014516400A JP2014516400A JP5936686B2 JP 5936686 B2 JP5936686 B2 JP 5936686B2 JP 2014516400 A JP2014516400 A JP 2014516400A JP 2014516400 A JP2014516400 A JP 2014516400A JP 5936686 B2 JP5936686 B2 JP 5936686B2
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- permanent magnetic
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Images
Classifications
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0235—Starting from compounds, e.g. oxides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
-
- 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
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
-
- 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
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0578—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together bonded together
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- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Description
(式中、REはネオジム、サマリウムおよび/またはプラセオジムであり、RE’はイットリウム、ランタン、セリウム、ユウロピウム、ガドリニウム、テルビウム、ジスプロシウム、ホルミウム、エルビウム、ツリウム、イッテルビウムおよびルテチウムから成る群から選択される1種以上の希土類元素である。遷移金属に関して、TMはコバルト、ニッケル、マンガン、クロムおよび銅から成る群から選択される1種以上の遷移金属)
によって表される。
噴霧ダイがスプレーまたはエアロゾルとして微小液滴を発生する熱エネルギー入力を有する反応器に、該親化合物の混合物を導入する工程、
形成した微小液滴を熱分解および燃焼させて、混合酸化物粒子を形成する工程、
形成し、回収した混合酸化物粒子を均一粉体形状で還元して、永久磁性粒子を得る工程
を含むことを特徴とする希土類‐遷移金属型磁性材料を製造するための希土類‐遷移金属をベースとする混合酸化物および永久磁性粒子の製造方法、が記載されている。
本発明の方法によれば、1つの態様は、溶媒と混合してもしなくても、火炎反応器に液状金属親化合物を導入することからなる。他の方法では、上記火炎以外のエネルギー入力手段、それらの中でも例えばプラズマ、温度制御オーブンまたはレーザーを用いてもよい。
Nd0.047Fe0.33B0.024O0.6の好ましい混合酸化物組成の典型的な実験において、上記金属(ネオジム、鉄およびホウ素)を含有する化学量論量の液状親化合物を、適当な溶媒に溶解する。
上記親化合物および溶媒の混合物を熱分解反応器、好ましくは火炎反応器に導入し、ここで上記液状媒体を、噴霧ダイ、ネブライザー、超音波噴霧器または微小液滴を製造可能な他の要素などによって噴霧してスプレーまたはエアロゾルとして微小液滴を形成する。
混合酸化物ナノ粒子を回収して、固体物質粒子をガスから分離する。本発明の方法では、用いられる装置は、固体‐ガス分離法に適している。好ましくは、1つの方法として、バッグフィルターが用いられ、他の適当な方法として、静電集塵機、サイクロン、またはスクラバーなどの液体を用いる回収装置が挙げられる。
スプレー火炎熱分解によって、組成式Nd0.047Fe0.33B0.024O0.6を有する混合酸化物を作製した。キシレンに溶解した、59.3gのネオジムアセチルアセトネート(C15H21NdO6)、875.8gの鉱油中の2‐エチルヘキサン酸鉄(Fe 6%)および15.6gのホウ酸トリ‐n‐ブチル([CH3(CH2)3O]3B)を用いて、液状親化合物の混合物を調製した。キシレンを加えて、合計金属濃度0.8Mを得た。
スプレー火炎熱分解によって、組成式Sm0.04Co0.36B0.024O0.6を有する混合酸化物を作製した。キシレンに溶解した、50gのサマリウムアセチルアセトネートおよび523gの2‐エチルヘキサン酸コバルト(鉱油中65重量%)を用いて、液状親化合物の混合物を調製した。上記混合物の合計金属濃度を0.5Mに調整した。上記液状混合物を、分散ガスO2の供給量100L/分で、口径0.8mmを有するダイを通って、ポンプを用いて50mL/分で供給した。O2の供給量8L/分およびCH4供給量4L/分で、支持炎を形成した。バッグフィルターを用いて、最終組成Sm0.04Co0.36B0.024O0.6を有する混合酸化物粒子を回収した。
Claims (11)
- ホウ素を含有する、または含有しない化学量論量の希土類および遷移金属を含有する溶媒を含有する、または含有しない有機金属親化合物の液状混合物を作製する工程、
噴霧ダイがスプレーまたはエアロゾルとして微小液滴を発生する熱エネルギー入力を有する燃焼炎反応器に、該有機金属親化合物の液状混合物を導入する工程、
燃焼ガスを該燃焼炎反応器へ導入して、酸素および空気から成る群から選択される酸化性ガスを有する支持炎を形成する工程、
形成した微小液滴を熱分解および燃焼させて、混合酸化物粒子を形成する工程、
形成し、回収した混合酸化物粒子を均質な粉体の形で還元して、永久磁性粒子を得る工程
を含むことを特徴とする希土類‐遷移金属型磁性材料を製造するための希土類‐遷移金属をベースとする混合酸化物および永久磁性粒子の製造方法。 - 前記親化合物の溶媒が、アルコール、有機酸、グリコール、アルデヒド、ケトン、エーテル、芳香族化合物、アルカンまたは燃料油、無機溶媒およびそれらの混合物である請求項1記載の混合酸化物および永久磁性粒子の製造方法。
- 前記親化合物の混合物の反応器への導入が、不活性窒素の導入も含んで、スプレーの形成、冷却、希釈およびキャリアとしての用途を達成する請求項1記載の混合酸化物および永久磁性粒子の製造方法。
- 熱分解のための前記親化合物の導入が、熱分解チャンバーまたはその中に到達する前に行われるスプレーの形成以外の蒸発手段によって行われる請求項1記載の混合酸化物および永久磁性粒子の製造方法。
- 前記混合酸化物の組成が、還元後、前記磁性粒子が原子数に対する希土類元素含有率2〜70%を有するように設定され、好ましい希土類元素がネオジム、サマリウムおよび/またはプラセオジム、更に、他の元素からの希土類元素、例えばランタン、セリウム、テルビウム、ジスプロシウム、ホルミウム、エルビウム、ユウロピウム、ガドリニウム、プロメチウム、ツリウム、イッテルビウム、ルテチウムまたはイットリウムおよび/またはそれらの混合物を用いることができ、それらが50%を超えない場合、更に遷移金属15〜98原子%を含有し、そして前記遷移金属は好ましくは、鉄、コバルト、ニッケル、クロム、銅またはマンガンであり、前記磁性粒子にはホウ素を用いてもよく、そのような場合には、50原子%を超えず、10原子%未満の他の元素、ジルコニウム、チタン、バナジウム、ゲルマニウム、ニオビウム、モリブデン、アルミニウム、錫、タンタル、タングステン、アンチモン、炭素、ケイ素および/またはハフニウムを用いる、請求項1記載の混合酸化物および永久磁性粒子の製造方法。
- 前記混合酸化物粒子の粒径が1〜1000nmであり、平均粒径が10〜500nmである、請求項1記載の混合酸化物および永久磁性粒子の製造方法。
- 前記反応器中の微小液滴の発生が、超音波アトマイザーまたはネブライザーによって行われる、請求項1記載の混合酸化物および永久磁性粒子の製造方法。
- 前記混合酸化物が、還元後、原子数に対する希土類元素含有率2〜70%を有する磁性粒子となり、好ましい希土類元素がネオジム、サマリウムおよび/またはプラセオジム、更に、他の元素からの希土類元素、例えばランタン、セリウム、テルビウム、ジスプロシウム、ホルミウム、エルビウム、ユウロピウム、ガドリニウム、プロメチウム、ツリウム、イッテルビウム、ルテチウムまたはイットリウムおよび/またはそれらの混合物を用いることができ、それらが50%を超えない場合、更に遷移金属15〜98原子%を含有し、そして前記遷移金属は好ましくは、鉄、コバルト、ニッケル、クロム、銅またはマンガンであり、前記磁性粒子にはホウ素を用いてもよく、そのような場合には、50原子%を超えず、10原子%未満の他の元素、ジルコニウム、チタン、バナジウム、ゲルマニウム、ニオビウム、モリブデン、アルミニウム、錫、タンタル、タングステン、アンチモン、炭素、ケイ素および/またはハフニウムを用いる、請求項1〜7のいずれか1項記載の混合酸化物および永久磁性粒子の製造方法。
- 請求項1〜8のいずれか1項記載の方法の前記混合酸化物の還元工程の後に永久磁性粒子を製造する工程、および
得られる該永久磁性粒子を永久磁石製造用のインゴットの仕上げ用の原材料として使用する工程
を含むことを特徴とする永久磁石の製造方法。 - 請求項1〜8のいずれか1項記載の方法の前記混合酸化物の還元工程の後に永久磁性粒子を製造する工程、および
得られる該永久磁性粒子を等方性ボンド磁石または異方性磁石の製造用に使用する工程
を含むことを特徴とする等方性ボンド磁石または異方性磁石の製造方法。 - 請求項1〜8のいずれか1項記載の方法の前記混合酸化物の還元工程の後に永久磁性粒子を製造する工程、および
得られる該永久磁性粒子を磁性および非磁性希土類系合金の製造用に使用する工程
を含むことを特徴とする磁性および非磁性希土類系合金の製造方法。
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WO2012159096A2 (en) * | 2011-05-18 | 2012-11-22 | The Regents Of The University Of California | Nanostructured high-strength permanent magnets |
US10229776B2 (en) * | 2013-10-31 | 2019-03-12 | General Electric Company | Multi-phase magnetic component and method of forming |
CN105499561B (zh) * | 2015-12-09 | 2017-08-11 | 西南交通大学 | 一种磁性碳纳米管的制备方法 |
CN108246210B (zh) * | 2018-01-30 | 2023-08-08 | 浙江工业大学 | 一种高温裂解反应装置 |
US11715592B2 (en) * | 2018-09-04 | 2023-08-01 | Lawrence Livermore National Security, Llc | Samarium cobalt and neodymium iron boride magnets and methods of manufacturing same |
FR3105789B1 (fr) * | 2019-12-27 | 2024-01-12 | Oreal | Particules d’oxyde de metal enrobees d’oxyde de terre rare et son procede de preparation par pyrolyse par projection de flamme |
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US11926880B2 (en) | 2021-04-21 | 2024-03-12 | General Electric Company | Fabrication method for a component having magnetic and non-magnetic dual phases |
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