JPH09227901A - Production of rare earth element-iron-nitrogen magnet alloy powder having excellent magnetic property - Google Patents
Production of rare earth element-iron-nitrogen magnet alloy powder having excellent magnetic propertyInfo
- Publication number
- JPH09227901A JPH09227901A JP8030819A JP3081996A JPH09227901A JP H09227901 A JPH09227901 A JP H09227901A JP 8030819 A JP8030819 A JP 8030819A JP 3081996 A JP3081996 A JP 3081996A JP H09227901 A JPH09227901 A JP H09227901A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- powder
- compound
- coarsely
- ingot
- 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.)
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Links
- 239000000843 powder Substances 0.000 title claims abstract description 114
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 107
- 239000000956 alloy Substances 0.000 title claims abstract description 107
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 150000002910 rare earth metals Chemical class 0.000 title 1
- 150000001875 compounds Chemical class 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 30
- 238000005121 nitriding Methods 0.000 claims abstract description 30
- 238000010298 pulverizing process Methods 0.000 claims abstract description 26
- 239000012298 atmosphere Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000005266 casting Methods 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 2
- 238000006467 substitution reaction Methods 0.000 claims 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract description 30
- 239000000203 mixture Substances 0.000 abstract description 4
- 229910001004 magnetic alloy Inorganic materials 0.000 abstract description 3
- 150000001412 amines Chemical class 0.000 abstract description 2
- 125000004093 cyano group Chemical group *C#N 0.000 abstract description 2
- 150000002429 hydrazines Chemical class 0.000 abstract description 2
- 230000004913 activation Effects 0.000 abstract 1
- 229910017464 nitrogen compound Inorganic materials 0.000 abstract 1
- 150000002830 nitrogen compounds Chemical class 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 26
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 description 14
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 description 13
- 229940067157 phenylhydrazine Drugs 0.000 description 12
- 239000002245 particle Substances 0.000 description 8
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- -1 fatty acid amine Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- SWGZHHCRMZDRSN-BTJKTKAUSA-N (Z)-but-2-enedioic acid 1-phenoxypropan-2-ylhydrazine Chemical compound OC(=O)\C=C/C(O)=O.NNC(C)COC1=CC=CC=C1 SWGZHHCRMZDRSN-BTJKTKAUSA-N 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 125000000717 hydrazino group Chemical group [H]N([*])N([H])[H] 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011812 mixed powder 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
- H01F1/032—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
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
- H01F1/0593—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2 of tetragonal ThMn12-structure
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、優れた磁気特性
を有するＲ−Ｆｅ−Ｎ系磁石合金粉末（ただし、Ｒは希
土類元素、以下同じ）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 method for producing an R--Fe--N magnet alloy powder (where R is a rare earth element, the same applies hereinafter) having excellent magnetic properties.
【０００２】[0002]
【従来の技術】従来、Ｒ2 Ｆｅ17Ｎx （ただし、１＜ｘ
＜４）からなるＲ−Ｆｅ−Ｎ系磁石合金粉末を製造する
には、まず、溶解鋳造してＲ2 Ｆｅ17合金鋳塊を製造
し、得られたＲ2 Ｆｅ17合金鋳塊を均質化処理する工
程、均質化処理したＲ2 Ｆｅ17合金鋳塊を５００μｍ以
下に粗粉砕する工程、得られた粗粉砕粉末を当量以上の
窒素を含有する化合物（以下、Ｎ化合物という）と混合
する工程、混合して得られた混合粗粉砕粉末を非酸化性
雰囲気中で温度：３００〜６００℃に加熱することによ
り窒化処理する工程、並びにこの窒化処理した粗粉砕粉
末をさらに微粉砕する工程を経て製造されることは知ら
れており、前記Ｎ化合物は、有機系アミン類（脂肪酸ア
ミン（第１〜第３）、脂環式アミン、芳香族アミン）、
ヒドラジンおよびヒドラジン誘導体（ヒドラジノ化合
物、ヒドラゾ化合物、ヒドラゾノ化合物）、シアノ化合
物（有機系シアン類、無機系シアン類）であることも知
られている（特開平５−２８７３０６号公報参照）。 2. Description of the Related Art Conventionally, R 2 Fe 17 N x (where 1 <x
In order to produce the R-Fe-N-based magnet alloy powder consisting of <4), first, melt casting is performed to produce an R 2 Fe 17 alloy ingot, and the obtained R 2 Fe 17 alloy ingot is homogenized. A step of treating, a step of roughly crushing the homogenized R 2 Fe 17 alloy ingot to 500 μm or less, and a step of mixing the obtained coarsely crushed powder with a compound containing nitrogen in an equivalent amount or more (hereinafter referred to as N compound) Through a step of nitriding the mixed coarsely pulverized powder obtained by mixing by heating at a temperature of 300 to 600 ° C. in a non-oxidizing atmosphere, and a step of further finely pulverizing the coarsely pulverized powder subjected to the nitriding treatment. It is known to be produced, and the N compound is an organic amine (fatty acid amine (first to third), alicyclic amine, aromatic amine),
It is also known that they are hydrazine and hydrazine derivatives (hydrazino compounds, hydrazo compounds, hydrazono compounds) and cyano compounds (organic cyans, inorganic cyans) (see JP-A-5-287306).
【０００３】[0003]
【発明が解決しようとする課題】しかし、前記従来のＲ
−Ｆｅ−Ｎ系磁石合金粉末の製造方法により得られたＲ
−Ｆｅ−Ｎ系磁石合金粉末の磁気特性は予測した値に比
べて低く、製造方法の改良が求められていた。However, the above-mentioned conventional R
R obtained by the method for producing —Fe—N-based magnet alloy powder
Since the magnetic properties of the —Fe—N magnet alloy powder are lower than the predicted values, improvement of the manufacturing method has been demanded.
【０００４】[0004]
【課題を解決するための手段】そこで、本発明者等は、
なお一層優れた磁気特性を有するＲ−Ｆｅ−Ｎ系磁石合
金粉末を得るべく研究を行った結果、（イ）均質化処理
したＲ2 Ｆｅ17合金鋳塊を５００μｍ以下に粗粉砕する
場合に、Ｒ2 Ｆｅ17合金鋳塊をＮ化合物とともに粉砕機
に装入して粗粉砕と混合を同時に行うと、得られたＲ−
Ｆｅ−Ｎ系磁石合金粉末の磁気特性が一層向上する、
（ロ）窒化処理した粗粉砕粉末をＮ化合物とともに微粉
砕すると、得られたＲ−Ｆｅ−Ｎ系磁石合金粉末の磁気
特性が一層向上する、という知見を得たのである。Means for Solving the Problems Accordingly, the present inventors have
As a result of research to obtain an R-Fe-N-based magnet alloy powder having further excellent magnetic characteristics, (a) when the homogenized R 2 Fe 17 alloy ingot is roughly pulverized to 500 μm or less, The R 2 Fe 17 alloy ingot was charged into a crusher together with an N compound, and coarse crushing and mixing were performed at the same time.
The magnetic properties of the Fe-N magnet alloy powder are further improved,
(B) It was found that when the nitriding coarsely pulverized powder is finely pulverized together with the N compound, the magnetic characteristics of the obtained R-Fe-N magnet alloy powder are further improved.
【０００５】この発明は、かかる知見に基づいて成され
たものであって、（ａ） 溶解鋳造して得られたＲ2 Ｆ
ｅ17合金（ただし、Ｒは、希土類元素）鋳塊を均質化処
理する工程、均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉
砕する工程、粗粉砕粉末をＮ化合物と混合する工程、混
合して得られた混合粗粉砕粉末を非酸化性雰囲気中で温
度：３００〜６００℃に加熱して窒化処理する工程、窒
化処理した粗粉砕粉末をさらに微粉砕する工程からなる
Ｒ−Ｆｅ−Ｎ系磁石合金粉末の製造方法において、前記
均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉砕する工程お
よび粗粉砕粉末をＮ化合物と混合する工程を、均質化処
理したＲ2 Ｆｅ17合金鋳塊とＮ化合物を共に粉砕機に装
入して粗粉砕と混合を同時に行う工程に置換する優れた
磁気特性を有するＲ−Ｆｅ−Ｎ系磁石合金粉末の製造方
法、（ｂ） 溶解鋳造して得られたＲ2 Ｆｅ17合金（た
だし、Ｒは、希土類元素）鋳塊を均質化処理する工程、
均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉砕する工程、
粗粉砕粉末をＮ化合物と混合する工程、混合して得られ
た混合粗粉砕粉末を非酸化性雰囲気中で温度：３００〜
６００℃に加熱して窒化処理する工程、窒化処理した粗
粉砕粉末をさらに微粉砕する工程からなるＲ−Ｆｅ−Ｎ
系磁石合金粉末の製造方法において、前記窒化処理した
粗粉砕粉末をさらに微粉砕する工程を、窒化処理した粗
粉砕粉末にさらにＮ化合物を添加して微粉砕したのち加
熱することにより、微粉砕して得られた微粉砕粉末に含
まれるＮ化合物を蒸発させる工程に置換する優れた磁気
特性を有するＲ−Ｆｅ−Ｎ系磁石合金粉末の製造方法、
（ｃ） 溶解鋳造して得られたＲ2 Ｆｅ17合金（ただ
し、Ｒは、希土類元素）鋳塊を均質化処理する工程、均
質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉砕する工程、粗
粉砕粉末をＮ化合物と混合する工程、混合して得られた
混合粗粉砕粉末を非酸化性雰囲気中で温度：３００〜６
００℃に加熱して窒化処理する工程、窒化処理した粗粉
砕粉末をさらに微粉砕する工程をからなるＲ−Ｆｅ−Ｎ
系磁石合金粉末の製造方法において、前記均質化処理し
たＲ2 Ｆｅ17合金鋳塊を粗粉砕する工程および粗粉砕粉
末をＮ化合物と混合する工程を、均質化処理したＲ2 Ｆ
ｅ17合金鋳塊とＮ化合物を共に粉砕機に装入して粗粉砕
と混合を同時に行う工程に置換し、さらに、前記窒化処
理した粗粉砕粉末をさらに微粉砕する工程を、窒化処理
した粗粉砕粉末にＮ化合物を添加して微粉砕したのち加
熱することにより、微粉砕して得られた微粉砕粉末に含
まれるＮ化合物を蒸発させる工程に置換する優れた磁気
特性を有するＲ−Ｆｅ−Ｎ系磁石合金粉末の製造方法、
に特徴を有するものである。The present invention was made on the basis of such findings, and (a) R 2 F obtained by melt casting.
e 17 alloy (where R is a rare earth element) a step of homogenizing the ingot, a step of roughly crushing the homogenized R 2 Fe 17 alloy ingot, a step of mixing the coarsely pulverized powder with an N compound, and mixing R-Fe-N consisting of a step of heating the mixed coarsely pulverized powder obtained in this way to a temperature of 300 to 600 ° C. in a non-oxidizing atmosphere for nitriding treatment and a step of further finely pulverizing the coarsely pulverized powder subjected to nitriding treatment. the method of manufacturing a system magnet alloy powder, the homogenized treated R 2 Fe 17 a step of the process and the coarse pulverized powder coarsely pulverized alloy ingot is mixed with N compounds were homogenized R 2 Fe 17 alloy ingot A method for producing an R-Fe-N-based magnet alloy powder having excellent magnetic properties, in which both the N and N compounds are charged into a crusher and coarse crushing and mixing are performed simultaneously, (b) Obtained by melt casting R 2 Fe 17 alloy (where R is a rare earth Element) step of homogenizing the ingot,
A step of roughly crushing a homogenized R 2 Fe 17 alloy ingot,
Step of mixing coarsely pulverized powder with N compound, mixed coarsely pulverized powder obtained by mixing, in non-oxidizing atmosphere, temperature: 300-
R-Fe-N consisting of a step of heating to 600 ° C. for nitriding treatment and a step of further finely pulverizing the coarsely pulverized powder subjected to nitriding treatment
In the method for producing a magnet-based magnetic alloy powder, the step of further finely pulverizing the coarsely pulverized powder subjected to the nitriding treatment is finely pulverized by further adding an N compound to the coarsely pulverized powder subjected to the nitriding treatment and then finely pulverizing the mixture. A method for producing an R-Fe-N-based magnet alloy powder having excellent magnetic properties, which is replaced by a step of evaporating an N compound contained in the finely pulverized powder obtained by
(C) melting and casting-obtained R 2 Fe 17 alloy (wherein, R represents a rare earth element) a step of rough grinding step, the homogenization treated R 2 Fe 17 alloy ingot to homogenizing the ingot, Step of mixing coarsely pulverized powder with N compound, mixed coarsely pulverized powder obtained by mixing, in non-oxidizing atmosphere, temperature: 300-6
R-Fe-N comprising a step of nitriding treatment by heating to 00 ° C and a step of further finely pulverizing the coarsely pulverized powder subjected to nitriding treatment.
In the method for producing a magnet-based magnet alloy powder, the step of roughly crushing the homogenized R 2 Fe 17 alloy ingot and the step of mixing the coarsely crushed powder with an N compound are homogenized R 2 F
e 17 alloy ingot and N compound were both charged into a pulverizer and replaced with a step of performing coarse pulverization and mixing at the same time, and the step of further finely pulverizing the nitriding-treated coarsely pulverized powder was performed by nitriding coarse R-Fe-having excellent magnetic properties, which is obtained by adding the N compound to the pulverized powder, pulverizing it, and then heating the pulverized powder to replace the N compound contained in the pulverized powder obtained by the pulverization. N-based magnet alloy powder manufacturing method,
It is characterized by the following.
【０００６】この発明で使用する粉砕混合機は、アトラ
イタミル、振動ミル、コロイドミルの内のいずれでも良
い。またこの発明の窒化処理の雰囲気は、水素、窒素、
Ａｒ、Ｈｅなどの非酸化性雰囲気であればいかなる雰囲
気であっても良いが、窒素雰囲気が最も好ましい。The grinding and mixing machine used in the present invention may be any one of an attritor mill, a vibration mill and a colloid mill. The atmosphere of the nitriding treatment of the present invention is hydrogen, nitrogen,
Any atmosphere may be used as long as it is a non-oxidizing atmosphere such as Ar or He, but a nitrogen atmosphere is most preferable.
【０００７】Ｒ2 Ｆｅ17合金とＮ化合物を粉砕混合機に
装入し、粉砕と同時に混合することにより得られた混合
粉末を用いることにより従来よりも磁気特性の優れたＲ
−Ｆｅ−Ｎ系磁石合金粉末が得られる理由として、Ｒ2
Ｆｅ17合金の粗粉砕または微粉砕と同時にＮ化合物を混
合することにより、表面活性化されたＲ2 Ｆｅ17合金の
周囲にＮ化合物が均一に付着するので窒化されやすくな
り、得られたＲ−Ｆｅ−Ｎ系磁石合金粉末は中心部まで
十分に窒化されることによるものと考えられる。By using a mixed powder obtained by charging an R 2 Fe 17 alloy and an N compound into a pulverizing mixer and mixing them at the same time as pulverizing, R having better magnetic properties than before can be obtained.
The reason why the —Fe—N-based magnet alloy powder is obtained is R 2
By mixing N compound at the same time as the coarse grinding or milling of Fe 17 alloy, since N compound is uniformly attached on the periphery of the surface activated R 2 Fe 17 alloy likely to be nitrided, resulting R- It is considered that the Fe-N magnet alloy powder is sufficiently nitrided up to the center.
【０００８】[0008]
実施例１〜４ 溶解鋳造して得られたＳｍ2 Ｆｅ17合金鋳塊を均質化処
理したのち、切断して５ｃｍ以下の角の寸法を有するＳ
ｍ2 Ｆｅ17合金塊を作製し、Ｓｍ2 Ｆｅ17合金塊：１０
０重量部に対してヒドラジン：３．８重量部（実施例
１）、Ｓｍ2 Ｆｅ17合金塊：１００重量部に対してジメ
チルヒドラジン：７．２重量部（実施例２）、Ｓｍ2 Ｆ
ｅ17合金塊：１００重量部に対してフェニルヒドラジ
ン：１３．０重量部（実施例３）、Ｓｍ2 Ｆｅ17合金
塊：１００重量部に対してアニリン：２２．３重量部
（実施例４）の割合でアトライタミルに装入し、２時間
粉砕混合してＳｍ2 Ｆｅ17合金塊を粗粉砕すると同時に
ヒドラジン、ジメチルヒドラジン、フェニルヒドラジン
またはアニリンをそれぞれ混合した平均粒径：５００μ
ｍ以下のＳｍ2 Ｆｅ17合金粗粉砕粉末とＮ化合物との混
合粗粉砕粉末を得た。Examples 1 to 4 Sm 2 Fe 17 alloy ingots obtained by melting and casting were homogenized and then cut to form S having a corner size of 5 cm or less.
An m 2 Fe 17 alloy ingot was prepared, and an Sm 2 Fe 17 alloy ingot: 10
Hydrazine: 3.8 parts by weight based on 0 part by weight (Example 1), Sm 2 Fe 17 alloy ingot: dimethyl hydrazine: 7.2 parts by weight (Example 2) by 100 parts by weight, Sm 2 F
Phenylhydrazine: 13.0 parts by weight per 100 parts by weight of e 17 alloy ingot (Example 3), aniline: 22.3 parts by weight per 100 parts by weight of Sm 2 Fe 17 alloy ingot (Example 4) Was charged into an attritor mill at a ratio of 2 and crushed and mixed for 2 hours to coarsely crush the Sm 2 Fe 17 alloy ingot, and at the same time, hydrazine, dimethylhydrazine, phenylhydrazine or aniline were mixed respectively, and an average particle diameter: 500 μm.
A mixed coarsely pulverized powder of an Sm 2 Fe 17 alloy coarsely pulverized powder of m or less and an N compound was obtained.
【０００９】得られたＳｍ2 Ｆｅ17合金粗粉砕粉末とヒ
ドラジン、ジメチルヒドラジン、フェニルヒドラジンま
たはアニリンとの混合粗粉砕粉末を窒素雰囲気中、温
度：４５０℃、１時間保持の条件の窒化処理することに
よりＳｍ2 Ｆｅ17Ｎx 合金粗粉砕粉末を作製し、このＳ
ｍ2 Ｆｅ17Ｎx 合金粗粉砕粉末をさらにＡｒガス雰囲気
中でジェットミルにより平均粒径：３μｍ以下に微粉砕
することにより、実施例１〜４を実施した。この実施例
１〜４で得られたＳｍ2 Ｆｅ17Ｎx 合金微粉末のｘの値
を求め、さらにＶＳＭ（振動型磁気測定器）により磁気
特性を測定し、その結果を表１に示した。Nitriding the mixed coarsely pulverized powder of the obtained Sm 2 Fe 17 alloy coarsely pulverized powder and hydrazine, dimethylhydrazine, phenylhydrazine or aniline in a nitrogen atmosphere at a temperature of 450 ° C. for 1 hour. Sm 2 Fe 17 N x alloy coarsely pulverized powder was prepared by
Examples 1 to 4 were carried out by further finely pulverizing the m 2 Fe 17 N x alloy coarsely pulverized powder by a jet mill in an Ar gas atmosphere to an average particle diameter of 3 μm or less. The value of x of the Sm 2 Fe 17 N x alloy fine powder obtained in Examples 1 to 4 was determined, and the magnetic characteristics were measured by VSM (vibration type magnetometer). The results are shown in Table 1. .
【００１０】[0010]
【表１】 [Table 1]
【００１１】実施例５〜８ 実施例１で作製した５ｃｍ以下の角の寸法を有するＳｍ
2 Ｆｅ17合金塊を、先ず、アトライタミルに装入して粗
粉砕することにより平均粒径：５００μｍ以下のＳｍ2
Ｆｅ17合金粗粉砕粉末を作製した。得られたＳｍ2 Ｆｅ
17合金粗粉砕粉末：１００重量部に対して、それぞれヒ
ドラジン：３．８重量部、ジメチルヒドラジン：７．２
重量部、フェニルヒドラジン：１３．０重量部、アニリ
ン：２２．３重量部を混合して混合粗粉砕粉末を作製
し、この混合粗粉砕粉末を窒素雰囲気中、温度：４５０
℃、１時間保持の条件の窒化処理することによりＳｍ2
Ｆｅ 17Ｎx 合金粗粉砕粉末を作製した。Examples 5-8 Sm produced in Example 1 having a corner size of 5 cm or less
TwoFe17The alloy ingot was first charged into the attritor mill and roughed.
By crushing, average particle size: Sm of 500 μm or lessTwo
Fe17An alloy coarsely crushed powder was produced. The obtained SmTwoFe
17Coarse crushed alloy powder: 100 parts by weight
Drazine: 3.8 parts by weight, dimethylhydrazine: 7.2
Parts by weight, phenylhydrazine: 13.0 parts by weight, anili
22.3 parts by weight are mixed to prepare a mixed coarsely pulverized powder.
Then, the mixed coarsely pulverized powder was heated in a nitrogen atmosphere at a temperature of 450.
Sm is obtained by nitriding under the condition of 1 ° C for 1 hour.Two
Fe 17NxAn alloy coarsely crushed powder was produced.
【００１２】Ｓｍ2 Ｆｅ17Ｎx 合金粗粉砕粉末：１００
重量部に対してヒドラジン：５０重量部（実施例５）、
Ｓｍ2 Ｆｅ17Ｎx 合金粗粉砕粉末：１００重量部に対し
てジメチルヒドラジン：８０重量部（実施例６）、Ｓｍ
2 Ｆｅ17Ｎx 合金粗粉砕粉末：１００重量部に対してフ
ェニルヒドラジン：１５０重量部（実施例７）、Ｓｍ2
Ｆｅ17Ｎx 合金粗粉砕粉末：１００重量部に対してアニ
リン：５０重量部（実施例８）、の割合でアトライタミ
ルに装入し、４時間粉砕することにより平均粒径：３μ
ｍ以下に微粉砕することによりＳｍ2 Ｆｅ17Ｎx 合金微
粉末とヒドラジン、ジメチルヒドラジン、フェニルヒド
ラジンまたはアニリンの混合微粉末を作製し、ついでこ
の混合微粉末を真空雰囲気中、２００℃に保持すること
によりヒドラジン、ジメチルヒドラジン、フェニルヒド
ラジンまたはアニリンを蒸発させ、実施例５〜８を実施
した。ついでこの実施例５〜８で得られたＳｍ2 Ｆｅ17
Ｎx 合金微粉末のｘの値を求め、さらにこのＲ2 Ｆｅ17
Ｎx 合金微粉末をＶＳＭにより磁気特性を測定し、その
結果を表２に示した。Sm 2 Fe 17 N x alloy coarsely pulverized powder: 100
Hydrazine to 50 parts by weight: 50 parts by weight (Example 5),
Sm 2 Fe 17 N x alloy coarsely pulverized powder: 100 parts by weight dimethylhydrazine: 80 parts by weight (Example 6), Sm
2 Fe 17 N x alloy coarsely pulverized powder: 100 parts by weight of phenylhydrazine: 150 parts by weight (Example 7), Sm 2
An average particle diameter of 3 μ was obtained by charging the Fe 17 N x alloy coarsely pulverized powder: 100 parts by weight to aniline: 50 parts by weight (Example 8) in an attritor mill and pulverizing for 4 hours.
A fine powder of Sm 2 Fe 17 N x alloy and fine powder of Sm 2 Fe 17 N x and hydrazine, dimethylhydrazine, phenylhydrazine or aniline are prepared by finely pulverizing to m or less, and then the fine powder of mixture is kept at 200 ° C. in a vacuum atmosphere. Hydrazine, dimethylhydrazine, phenylhydrazine or aniline were thereby evaporated and Examples 5-8 were carried out. Then, the Sm 2 Fe 17 obtained in Examples 5 to 8 was obtained.
The value of x of the N x alloy fine powder was calculated, and further, this R 2 Fe 17
The magnetic properties of the N x alloy fine powder were measured by VSM, and the results are shown in Table 2.
【００１３】[0013]
【表２】 [Table 2]
【００１４】実施例９〜１２ 溶解鋳造して得られたＳｍ2 Ｆｅ17合金鋳塊を均質化処
理したのち、切断して５ｃｍ以下の角の寸法を有するＳ
ｍ2 Ｆｅ17合金塊を作製し、Ｓｍ2 Ｆｅ17合金塊：１０
０重量部に対してヒドラジン：３．８重量部（実施例
９）、Ｓｍ2 Ｆｅ17合金塊：１００重量部に対してジメ
チルヒドラジン：７．２重量部（実施例１０）、Ｓｍ2
Ｆｅ17合金塊：１００重量部に対してフェニルヒドラジ
ン：１３．０重量部（実施例１１）、Ｓｍ2 Ｆｅ17合金
塊：１００重量部に対してアニリン：２２．３重量部
（実施例１２）の割合でアトライタミルに装入し、２時
間粉砕混合してＳｍ2 Ｆｅ17合金塊を粗粉砕すると同時
にヒドラジン、ジメチルヒドラジン、フェニルヒドラジ
ンまたはアニリンをそれぞれ混合した平均粒径：５００
μｍ以下のＳｍ2 Ｆｅ17合金粗粉砕粉末とＮ化合物を混
合した混合粗粉末を得た。Examples 9 to 12 Sm 2 Fe 17 alloy ingots obtained by melting and casting were homogenized and then cut to form S having a corner size of 5 cm or less.
An m 2 Fe 17 alloy ingot was prepared, and an Sm 2 Fe 17 alloy ingot: 10
Hydrazine: 3.8 parts by weight based on 0 part by weight (Example 9), Sm 2 Fe 17 alloy ingot: Dimethylhydrazine: 7.2 parts by weight (Example 10) by 100 parts by weight, Sm 2
Phenyl hydrazine: 13.0 parts by weight with respect to 100 parts by weight of Fe 17 alloy ingot (Example 11), aniline: 22.3 parts by weight with respect to 100 parts by weight of Sm 2 Fe 17 alloy ingot (Example 12) The mixture was charged into an attritor mill at a ratio of 2 and pulverized and mixed for 2 hours to coarsely pulverize an Sm 2 Fe 17 alloy lump, and at the same time, hydrazine, dimethylhydrazine, phenylhydrazine or aniline were mixed respectively, and an average particle diameter: 500.
A mixed coarse powder was obtained by mixing an Sm 2 Fe 17 alloy coarsely pulverized powder having a size of μm or less and an N compound.
【００１５】得られたＳｍ2 Ｆｅ17合金粗粉砕粉末とヒ
ドラジン、ジメチルヒドラジン、フェニルヒドラジンま
たはアニリンとの混合粗粉砕粉末を窒素雰囲気中、温
度：４５０℃、１時間保持の条件の窒化処理することに
よりＳｍ2 Ｆｅ17Ｎx 合金粗粉砕粉末を作製し、Ｓｍ2
Ｆｅ17Ｎx 合金粗粉砕粉末：１００重量部に対してヒド
ラジン：５０重量部（実施例９）、Ｓｍ2 Ｆｅ17Ｎx 合
金粗粉砕粉末：１００重量部に対してジメチルヒドラジ
ン：８０重量部（実施例１０）、Ｓｍ2 Ｆｅ17Ｎx 合金
粗粉砕粉末：１００重量部に対してフェニルヒドラジ
ン：１５０重量部（実施例１１）、Ｓｍ2 Ｆｅ17Ｎx 合
金粗粉砕粉末：１００重量部に対してアニリン：５０重
量部（実施例１２）、の割合でアトライタミルに装入
し、平均粒径：３μｍ以下に微粉砕することによりＳｍ
2 Ｆｅ17Ｎx 合金微粉末とヒドラジン、ジメチルヒドラ
ジン、フェニルヒドラジンまたはアニリンの混合微粉末
を作製し、ついでこの混合微粉末を真空雰囲気中、２０
０℃に保持することによりヒドラジン、ジメチルヒドラ
ジン、フェニルヒドラジンまたはアニリンを蒸発させ、
実施例９〜１２を実施した。ついでこの実施例９〜１２
で得られたＳｍ2 Ｆｅ17Ｎx 合金微粉末のｘの値を求
め、さらにこのＲ2 Ｆｅ17Ｎx 合金微粉末をＶＳＭによ
り磁気特性を測定し、その結果を表３に示した。Nitriding the mixed coarsely pulverized powder of the obtained Sm 2 Fe 17 alloy coarsely pulverized powder and hydrazine, dimethylhydrazine, phenylhydrazine or aniline in a nitrogen atmosphere at a temperature of 450 ° C. for 1 hour. to prepare a Sm 2 Fe 17 N x alloy coarsely pulverized powder by, Sm 2
Fe 17 N x alloy coarsely pulverized powder: 100 parts by weight, hydrazine: 50 parts by weight (Example 9), Sm 2 Fe 17 N x alloy coarsely pulverized powder: 100 parts by weight, dimethylhydrazine: 80 parts by weight ( Example 10), Sm 2 Fe 17 N x alloy coarsely pulverized powder: 100 parts by weight to phenylhydrazine: 150 parts by weight (Example 11), Sm 2 Fe 17 N x alloy coarsely pulverized powder: 100 parts by weight Aniline: 50 parts by weight (Example 12), charged into an attritor mill, and finely pulverized to an average particle size of 3 μm or less to give Sm.
A mixed fine powder of 2 Fe 17 N x alloy fine powder and hydrazine, dimethylhydrazine, phenylhydrazine or aniline was prepared, and then the mixed fine powder was placed in a vacuum atmosphere for 20
Evaporating hydrazine, dimethylhydrazine, phenylhydrazine or aniline by holding at 0 ° C,
Examples 9-12 were carried out. Then, Examples 9 to 12
The value of x of the Sm 2 Fe 17 N x alloy fine powder obtained in 1. was determined, and the magnetic characteristics of this R 2 Fe 17 N x alloy fine powder were measured by VSM. The results are shown in Table 3.
【００１６】[0016]
【表３】 [Table 3]
【００１７】従来例１〜４ 実施例１で作製した５ｃｍ以下の角の寸法を有するＳｍ
2 Ｆｅ17合金塊を先ずアトライタミルに装入して粗粉砕
して平均粒径：５００μｍ以下のＳｍ2 Ｆｅ17合金粗粉
砕粉末を作製し、得られたＳｍ2 Ｆｅ17合金粗粉砕粉
末：１００部に対して、それぞれヒドラジン：３．８重
量部、ジメチルヒドラジン：７．２重量部、フェニルヒ
ドラジン：１３．０重量部、アニリン：２２．３重量部
を混合して混合粗粉砕粉末を作製し、この混合粗粉砕粉
末を以下実施例１と同じ条件で窒化処理することにより
Ｓｍ2 Ｆｅ17Ｎx 合金粗粉砕粉末を作製し、このＳｍ2
Ｆｅ 17Ｎx 合金粗粉砕粉末をさらにＡｒガス雰囲気中で
ジェットミルにより平均粒径：３μｍ以下に微粉砕する
ことにより従来例１〜４を実施し、ついでこの従来例１
〜４で得られたＳｍ2 Ｆｅ17Ｎx 合金微粉末のｘの値を
求め、さらにこのＲ2Ｆｅ17Ｎx 合金微粉末をＶＳＭに
より磁気特性を測定し、その結果を表４に示した。Conventional Examples 1 to 4 Sm produced in Example 1 and having a corner size of 5 cm or less
TwoFe17The alloy lump is first charged into the attritor mill and coarsely crushed.
And average particle size: Sm of 500 μm or lessTwoFe17Alloy coarse powder
Sm obtained by making crushed powderTwoFe17Coarse crushed powder
End: 100 parts, hydrazine: 3.8 times each
Parts by weight, dimethylhydrazine: 7.2 parts by weight, phenylhydr
Dorazine: 13.0 parts by weight, aniline: 22.3 parts by weight
To produce a mixed coarsely crushed powder.
By nitriding the powder under the same conditions as in Example 1 below
SmTwoFe17NxCoarse crushed powder of alloy is prepared, and this SmTwo
Fe 17NxCoarse crushed powder is further added in Ar gas atmosphere.
Finely pulverize with a jet mill to an average particle size of 3 μm or less
Therefore, the conventional examples 1 to 4 are carried out, and then the conventional example 1
~ Sm obtained in ~ 4TwoFe17NxX value of fine alloy powder
I asked for this RTwoFe17NxFine alloy powder to VSM
The magnetic properties were measured more and the results are shown in Table 4.
【００１８】[0018]
【表４】 [Table 4]
【００１９】[0019]
【発明の効果】表１〜表４に示に示される結果から、Ｓ
ｍ2 Ｆｅ17合金塊とＮ化合物を粉砕機に装入し、粉砕と
同時に混合する工程を含む実施例１〜１２により得られ
たＲ−Ｆｅ−Ｎ系磁石合金粉末は、Ｓｍ2 Ｆｅ17合金塊
を粉砕機に装入して粉砕し、ついでこのＳｍ2 Ｆｅ17合
金粗粉砕粉末とＮ化合物との混合したのち、窒素雰囲気
中で窒化処理する従来例１〜５により得られたＲ−Ｆｅ
−Ｎ系磁石合金粉末に比べて、生成されるＲ2 Ｆｅ17Ｎ
x 合金粉末のＮ含有量が多く、磁気特性が優れているこ
とが分かる。From the results shown in Tables 1 to 4, S
The m 2 Fe 17 alloy ingot and N compounds were charged into the crusher, R-Fe-N based magnet alloy powder obtained by Examples 1 to 12 comprising the step of mixing at the same time as the pulverization, Sm 2 Fe 17 alloy The lump was charged into a crusher and crushed, and then the Sm 2 Fe 17 alloy coarsely crushed powder and the N compound were mixed and then nitrided in a nitrogen atmosphere.
R 2 Fe 17 N produced as compared with the N-based magnet alloy powder
It can be seen that the N content of the x alloy powder is large and the magnetic properties are excellent.
【００２０】上述のように、Ｒ2 Ｆｅ17合金とＮ化合物
と粉砕混合機に装入し、粗粉砕と同時に混合する工程お
よび／またはＲ2 Ｆｅ17Ｎx とＮ化合物を粉砕混合機に
装入し、微粉砕と同時に混合する工程を含むこの発明の
方法によると、従来よりも磁気特性に優れたＲ−Ｆｅ−
Ｎ系磁石合金粉末を製造することができ、産業上優れた
効果を奏するものである。As described above, the step of charging the R 2 Fe 17 alloy, the N compound and the crushing mixer and mixing them simultaneously with the coarse crushing and / or the method of charging the R 2 Fe 17 N x and the N compound into the crushing mixer. According to the method of the present invention including the steps of charging, finely pulverizing and simultaneously mixing, R-Fe
The N-based magnet alloy powder can be produced, and the industrially excellent effect is exhibited.
Claims (3)
金（ただし、Ｒは、希土類元素）鋳塊を均質化処理する
工程、（２）均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉
砕する工程、（３）粗粉砕粉末を当量以上の窒素を含有
する化合物（以下、Ｎ化合物という）と混合する工程、
（４）混合して得られた混合粗粉砕粉末を非酸化性雰囲
気中、温度：３００〜６００℃で加熱することにより窒
化処理する工程、（５）窒化処理した粗粉砕粉末をさら
に微粉砕する工程からなるＲ−Ｆｅ−Ｎ系磁石合金粉末
の製造方法において、 前記（２）均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉砕
する工程および（３）粗粉砕粉末をＮ化合物と混合する
工程を、均質化処理したＲ2 Ｆｅ17合金鋳塊とＮ化合物
を共に粉砕機に装入して粗粉砕と混合を同時に行う工程
に置換することを特徴とする優れた磁気特性を有するＲ
−Ｆｅ−Ｎ系磁石合金粉末の製造方法。1. A step of homogenizing an ingot of R 2 Fe 17 alloy (where R is a rare earth element) obtained by melt casting, (2) a homogenized R 2 Fe 17 alloy Coarsely crushing the ingot, (3) mixing the coarsely crushed powder with a compound containing nitrogen in an equivalent amount or more (hereinafter referred to as N compound),
(4) A step of subjecting the mixed coarsely pulverized powder obtained by mixing to a nitriding treatment by heating at a temperature of 300 to 600 ° C. in a non-oxidizing atmosphere, (5) the coarsely pulverized powder subjected to the nitriding treatment is further finely pulverized. in R-Fe-N-based method for producing a magnet alloy powder comprising the step, it is mixed with the (2) coarsely grinding the homogenization treated R 2 Fe 17 alloy ingot process and (3) coarsely pulverized powder N compound R having excellent magnetic properties, characterized in that the step is replaced by a step of charging both the homogenized R 2 Fe 17 alloy ingot and the N compound into a crusher and simultaneously performing coarse crushing and mixing.
-Method for producing Fe-N magnet alloy powder.
金（ただし、Ｒは、希土類元素）鋳塊を均質化処理する
工程、（２）均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉
砕する工程、（３）粗粉砕粉末をＮ化合物と混合する工
程、（４）混合して得られた混合粗粉砕粉末を非酸化性
雰囲気中、温度：３００〜６００℃で加熱することによ
り窒化処理する工程、（５）窒化処理した粗粉砕粉末を
さらに微粉砕する工程からなるＲ−Ｆｅ−Ｎ系磁石合金
粉末の製造方法において、 前記（５）窒化処理した粗粉砕粉末をさらに微粉砕する
工程を、窒化処理した粗粉砕粉末にさらにＮ化合物を添
加して微粉砕したのち加熱することにより、微粉砕して
得られた微粉砕粉末に含まれるＮ化合物を蒸発させる工
程に置換することを特徴とする優れた磁気特性を有する
Ｒ−Ｆｅ−Ｎ系磁石合金粉末の製造方法。2. A step of homogenizing an ingot of R 2 Fe 17 alloy (where R is a rare earth element) obtained by melting and casting, (2) a homogenized R 2 Fe 17 alloy Coarsely crushing the ingot, (3) mixing the coarsely crushed powder with an N compound, (4) heating the mixed coarsely crushed powder obtained by mixing at a temperature of 300 to 600 ° C. in a non-oxidizing atmosphere In the method for producing an R-Fe-N-based magnet alloy powder, which comprises the step of nitriding treatment by (5) further finely pulverizing the coarsely pulverized powder subjected to nitriding, The step of further finely pulverizing is a step of evaporating the N compound contained in the finely pulverized powder obtained by finely pulverizing by further adding an N compound to the nitriding coarsely pulverized powder, pulverizing and then heating. Excellent magnetic properties characterized by substitution Of the R-Fe-N-based magnet alloy powder having:
金（ただし、Ｒは、希土類元素）鋳塊を均質化処理する
工程、（２）均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉
砕する工程、（３）粗粉砕粉末をＮ化合物と混合する工
程、（４）混合して得られた混合粗粉砕粉末を非酸化性
雰囲気中で温度：３００〜６００℃に加熱することによ
り窒化処理する工程、（５）窒化処理した粗粉砕粉末を
さらに微粉砕する工程からなるＲ−Ｆｅ−Ｎ系磁石合金
粉末の製造方法において、 前記（２）均質化処理したＲ2 Ｆｅ17合金鋳塊を粗粉砕
する工程および（３）粗粉砕粉末をＮ化合物と混合する
工程を、均質化処理したＲ2 Ｆｅ17合金鋳塊とＮ化合物
を共に粉砕機に装入して粗粉砕と混合を同時に行う工程
に置換し、さらに、 前記（５）窒化処理した粗粉砕粉末をさらに微粉砕する
工程を、窒化処理した粗粉砕粉末にさらにＮ化合物を添
加して微粉砕したのち加熱することにより、微粉砕して
得られた微粉砕粉末に含まれるＮ化合物を蒸発させる工
程に置換することを特徴とする優れた磁気特性を有する
Ｒ−Ｆｅ−Ｎ系磁石合金粉末の製造方法。3. A step of homogenizing an ingot of R 2 Fe 17 alloy (where R is a rare earth element) obtained by melting and casting, (2) a homogenized R 2 Fe 17 alloy Coarsely crushing the ingot, (3) mixing the coarsely crushed powder with an N compound, (4) heating the mixed coarsely crushed powder obtained by mixing to a temperature of 300 to 600 ° C. in a non-oxidizing atmosphere In the method for producing an R-Fe-N-based magnet alloy powder, which comprises the step of nitriding treatment by (5) and further finely pulverizing the coarsely pulverized powder subjected to nitriding, (2) the homogenized R 2 Fe The step of roughly crushing the 17 alloy ingot and (3) the step of mixing the coarsely crushed powder with the N compound are homogenized, and the R 2 Fe 17 alloy ingot and the N compound are both charged into a crusher and coarsely crushed. And the step of performing mixing at the same time are replaced, and further (5) nitriding treatment is performed. In the step of further finely pulverizing the pulverized powder, the N compound contained in the finely pulverized powder obtained by finely pulverizing is vaporized by adding the N compound to the nitriding coarsely pulverized powder, pulverizing it and then heating it. The method for producing an R-Fe-N-based magnet alloy powder having excellent magnetic characteristics, characterized by substituting the step of performing the step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8030819A JPH09227901A (en) | 1996-02-19 | 1996-02-19 | Production of rare earth element-iron-nitrogen magnet alloy powder having excellent magnetic property |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8030819A JPH09227901A (en) | 1996-02-19 | 1996-02-19 | Production of rare earth element-iron-nitrogen magnet alloy powder having excellent magnetic property |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09227901A true JPH09227901A (en) | 1997-09-02 |
Family
ID=12314324
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8030819A Withdrawn JPH09227901A (en) | 1996-02-19 | 1996-02-19 | Production of rare earth element-iron-nitrogen magnet alloy powder having excellent magnetic property |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09227901A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004263275A (en) * | 2003-03-04 | 2004-09-24 | Hitachi Metals Ltd | R-Fe-N MAGNET POWDER AND ITS PRODUCTION METHOD |
| WO2021229965A1 (en) * | 2020-05-13 | 2021-11-18 | 株式会社大阪チタニウムテクノロジーズ | Active metal particle surface modification method, and titanium particles or titanium alloy particles |
-
1996
- 1996-02-19 JP JP8030819A patent/JPH09227901A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004263275A (en) * | 2003-03-04 | 2004-09-24 | Hitachi Metals Ltd | R-Fe-N MAGNET POWDER AND ITS PRODUCTION METHOD |
| WO2021229965A1 (en) * | 2020-05-13 | 2021-11-18 | 株式会社大阪チタニウムテクノロジーズ | Active metal particle surface modification method, and titanium particles or titanium alloy particles |
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