JP5858499B2 - Method for producing amorphous soft magnetic alloy powder - Google Patents
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- 239000000843 powder Substances 0.000 title claims description 81
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims description 32
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- 239000007789 gas Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000009689 gas atomisation Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 9
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000009692 water atomization Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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Description
本発明は、アモルファス軟磁性合金粉末の製造方法に関し、特に高いアモルファス化率の得られる製造方法に関するものである。 The present invention relates to a method for producing an amorphous soft magnetic alloy powder, and more particularly to a method for producing a high amorphization rate.
現在実用化されている軟磁性材料としては、電磁鋼板や水アトマイズ軟磁性粉末が一般的である。代表的な使用分野は、産業機器分野では発電機、超高圧変電所および一次/二次変電所の変圧器、動力用等の各種モーター、道路照明の安定器などがある。また一般民生分野では、蛍光灯の安定器（トランスの一種）をはじめ、家電機器のモーター、テレビの電源トランスなど、様々な装置で使用されている。 Commonly used soft magnetic materials are magnetic steel sheets and water atomized soft magnetic powder. Typical fields of application include generators, ultra-high voltage substations and primary / secondary substation transformers, various motors for power, ballasts for road lighting, etc. in the industrial equipment field. In the general consumer field, it is used in various devices such as fluorescent lamp ballasts (a kind of transformer), motors for home appliances, and power transformers for televisions.
特に、従来から使用されている方向性電磁鋼板は、製造にノウハウがあり、限られたメーカーにより寡占的に供給されていた。最近、水アトマイズ法の合金粉末の製造方法が普及して、水アトマイズ法で得られたアモルファス軟磁性粉末が民生機器分野で使用されてきている。アモルファス粉末は結晶粉末とは異なり、粒界がないので、結晶に比較して優れた磁気特性が得られる長所がある（例えば、特許文献１参照）。 In particular, the grain-oriented electrical steel sheets that have been used in the past have know-how in production and have been supplied exclusively by a limited number of manufacturers. Recently, a method for producing an alloy powder by the water atomizing method has been widespread, and amorphous soft magnetic powder obtained by the water atomizing method has been used in the field of consumer equipment. Unlike the crystal powder, the amorphous powder has no grain boundary, and therefore has an advantage that excellent magnetic properties can be obtained as compared with the crystal (see, for example, Patent Document 1).
しかしながら、水アトマイズ粉末は、アトマイズ時に水が分解して酸素ガスや酸素イオンが発生して、得られたアトマイズ粉末の表面が酸素により酸化したり、酸化が起点として粉末の一部が結晶化したりするなどの問題点がある。 However, water atomized powder decomposes water during atomization to generate oxygen gas and oxygen ions, and the surface of the obtained atomized powder is oxidized by oxygen, or a part of the powder is crystallized starting from oxidation. There are problems such as.
水アトマイズ法の問題点である粉末表面の酸化や結晶化を防ぐ方法として、不活性ガス中で金属の溶湯を噴霧するガスアトマイズ法が開発されている（例えば、特許文献２参照）。 As a method for preventing oxidation and crystallization of the powder surface, which is a problem of the water atomization method, a gas atomization method in which a molten metal is sprayed in an inert gas has been developed (see, for example, Patent Document 2).
しかしながら、ガスアトマイズ法は、水アトマイズ法に比べて冷却速度が格段に遅いという問題点がある。その結果、ガスアトマイズ法では、粉末の一部が結晶化したり、結晶の状態の粉末が得られたりすることとなり、アモルファス粉末の収率が低下するという問題点があった。 However, the gas atomization method has a problem that the cooling rate is much slower than the water atomization method. As a result, the gas atomization method has a problem that a part of the powder is crystallized or a powder in a crystalline state is obtained, and the yield of the amorphous powder is lowered.
本発明は、このような課題に着目してなされたもので、ガスアトマイズ法で得られる、全体がアモルファスになっていない、結晶や一部結晶を含む粉末を、アモルファス化することができるアモルファス軟磁性合金粉末の製造方法を提供することを目的とする。 The present invention has been made paying attention to such a problem, and is obtained by a gas atomization method. Amorphous soft magnetism capable of amorphizing a crystal or a powder containing a part of a crystal which is not entirely amorphous. It aims at providing the manufacturing method of an alloy powder.
本発明者らは、ガスアトマイズ法の冷却速度が遅いことに着目し、ガスアトマイズ処理した粉末を詳細に分析した結果、ガスアトマイズ処理した粉末を一定の大きさでアモルファスと結晶に分離できることを見出し、本発明に至った。 As a result of detailed analysis of the gas atomized powder, the present inventors have found that the gas atomized powder can be separated into amorphous and crystals in a certain size, focusing on the slow cooling rate of the gas atomizing method. It came to.
すなわち、本発明によれば、アモルファス軟磁性合金粉末の製造方法において、軟磁性合金の溶湯に不活性ガスを吹き付けてガスアトマイズして、軟磁性合金の粉末を製造する第一の工程と、次に前記粉末を所定の粒径で二つに分割する第二の工程と、次に、不活性ガスが上方から下方に流れる透明石英管中で、前記所定の粒径より大きい粉末を落下させ、石英管上部の外側に設けた反射型赤外線加熱装置により、落下中の粉末を非接触加熱で再溶解する第三の工程と、しかる後に、前記透明石英管の鉛直下方に設けた不活性ガス冷却部で、再溶解した粉末を急冷固化し、回収する第四の工程とを有することを特徴とするアモルファス軟磁性合金粉末の製造方法が得られる。 That is, according to the present invention, in the method for producing an amorphous soft magnetic alloy powder, the first step of producing a soft magnetic alloy powder by spraying an inert gas onto the molten soft magnetic alloy and gas atomizing, and A second step of dividing the powder into two at a predetermined particle size; and then, in a transparent quartz tube in which an inert gas flows downward from above, the powder having a particle size larger than the predetermined particle size is dropped. A third step of re-dissolving the falling powder by non-contact heating by a reflective infrared heating device provided outside the upper part of the tube, and then an inert gas cooling unit provided vertically below the transparent quartz tube Then, a fourth method of rapidly solidifying and recovering the re-dissolved powder is obtained, and a method for producing an amorphous soft magnetic alloy powder is obtained.
また、本発明によれば、前記第二の工程は、前記粉末を、ＪＩＳ規格３８ミクロンメッシュで篩上と篩下との二つに分割することを特徴とするアモルファス軟磁性合金粉末の製造方法が得られる。 Further, according to the present invention, in the second step, the powder is divided into two parts, a sieve top and a sieve under a JIS standard 38 micron mesh. Is obtained.
また、本発明によれば、前記第一の工程および前記第三の工程の不活性ガスが、３ａｔ％水素−ヘリウムガスであることを特徴とするアモルファス軟磁性合金粉末の製造方法が得られる。３ａｔ％水素以上に水素量を増やすと、水素の爆発限界を超えるので危険であり、水素濃度は３ａｔ％が好ましい。 Further, according to the present invention, there can be obtained a method for producing an amorphous soft magnetic alloy powder, wherein the inert gas in the first step and the third step is 3 at% hydrogen-helium gas. Increasing the amount of hydrogen beyond 3 at% hydrogen is dangerous because it exceeds the explosion limit of hydrogen, and the hydrogen concentration is preferably 3 at%.
更に、本発明によれば、前記軟磁性合金は、Ｆｅを主成分とし、Ｃｏ、Ｎｂ、Ｓｉ、Ｂ、Ｐ、Ｃｕのうちから少なくとも二種以上の合金成分と、その他不可避不純物元素からなることを特徴とするアモルファス軟磁性合金粉末の製造方法が得られる。 Furthermore, according to the present invention, the soft magnetic alloy is mainly composed of Fe, and is composed of at least two alloy components of Co, Nb, Si, B, P, and Cu, and other inevitable impurity elements. A process for producing an amorphous soft magnetic alloy powder characterized by
本発明により、ガスアトマイズ法で得られる、全体がアモルファスになっていない、結晶や一部結晶を含む粉末を、アモルファス化することができるアモルファス軟磁性合金粉末の製造方法を提供することができる。 According to the present invention, it is possible to provide a method for producing an amorphous soft magnetic alloy powder that can be amorphized from a powder that is obtained by a gas atomization method and that is not entirely amorphous and that contains crystals or partially containing crystals.
以下に本発明の実施例について説明するが、本発明の合金組成はこれらの実施例に限定されるものではない。 Examples of the present invention will be described below, but the alloy composition of the present invention is not limited to these examples.
まず、軟磁性合金インゴットとして、［（Ｆｅ０．５Ｃｏ０．５）０．７５Ｓｉ０．０５Ｂ０．２］９６Ｎｂ４から成る組成物を１００ｇ準備し、そのインゴットを３ａｔ％水素−ヘリウムガスの雰囲気のチャンバー内部で、その融点１１８０℃より＋５０℃高い温度に加熱溶融した。次に、チャンバー内で、溶融金属に対して、１０ＭＰａに加圧した３ａｔ％水素−ヘリウムガスをノズルから数秒間噴射し、ガスアトマイズ粉末を製造した。次に、得られたガスアトマイズ粉末を、ＪＩＳ規格３８ミクロンメッシュで篩上と篩下との二つに分割した。しかる後に、３ａｔ％水素−ヘリウムガス雰囲気の外径５０ｍｍ、長さ１５００ｍｍの透明石英管上部に設置した振動式フィーダーに篩上の粉末を投入し、投入粉末を透明石英管中に順次落下させ、透明石英管外側上部に設けた反射型赤外線加熱装置により、落下中に粉末を１５００℃に加熱溶解し、それに続いて鉛直方向の透明石英管下部の３ａｔ％水素−ヘリウムガス中で急速凝固し、アモルファス軟磁性合金粉末を得た。 First, as a soft magnetic alloy ingot, 100 g of a composition composed of [(Fe 0.5 Co 0.5 ) 0.75 Si 0.05 B 0.2 ] 96 Nb 4 was prepared, and the ingot was made into 3 at% hydrogen − Inside the chamber of helium gas atmosphere, it was heated and melted to a temperature higher than its melting point of 1180 ° C. by + 50 ° C. Next, in the chamber, 3 at% hydrogen-helium gas pressurized to 10 MPa was sprayed from the nozzle for several seconds with respect to the molten metal to produce gas atomized powder. Next, the obtained gas atomized powder was divided into two on the sieve and below the sieve with a JIS standard 38 micron mesh. After that, the powder on the sieve was put into a vibrating feeder installed on the top of a transparent quartz tube having an outer diameter of 50 mm and a length of 1500 mm in a 3 at% hydrogen-helium gas atmosphere, and the charged powder was sequentially dropped into the transparent quartz tube, The reflective infrared heating device provided on the outer upper part of the transparent quartz tube heats and dissolves the powder to 1500 ° C. during dropping, and then rapidly solidifies in 3 at% hydrogen-helium gas at the lower part of the transparent quartz tube in the vertical direction. Amorphous soft magnetic alloy powder was obtained.
図１は、本実施例で使用した落下中の加熱と急冷に使用した装置の概略図である。図２と図３は、本実施例でガスアトマイズ粉末をＪＩＳ規格３８ミクロンメッシュで篩上と篩下の二つに分割した、それぞれの粉末のＸ線回折結果である。図２が篩上粉末で、結晶が晶出していることがわかる。また、図３から、篩下の粉末はアモルファスであることが分かる。図４は、落下加熱急冷後の粉末のＸ線回折結果で、アモルファスになっていることが分かる。 FIG. 1 is a schematic view of an apparatus used for heating and quenching during dropping used in this example. FIGS. 2 and 3 are X-ray diffraction results of the respective powders obtained by dividing the gas atomized powder into two on the sieve and below the sieve with a JIS standard 38 micron mesh in this example. FIG. 2 shows the powder on the sieve, and it can be seen that crystals are crystallized. Moreover, it can be seen from FIG. 3 that the powder under the sieve is amorphous. FIG. 4 is an X-ray diffraction result of the powder after dropping and rapid cooling, and it can be seen that the powder is amorphous.
図５は、ガスアトマイズ後の粉末、図６は、ＪＩＳ規格３８ミクロンメッシュで篩上の粉末、図７は、ＪＩＳ規格３８ミクロンメッシュで篩下の粉末のそれぞれのＳＥＭ像である。 5 is a powder after gas atomization, FIG. 6 is a SEM image of a powder on a sieve with a JIS standard 38 micron mesh, and FIG. 7 is a SEM image of a powder on a sieve with a JIS standard 38 micron mesh.
軟磁性合金インゴットとして、Ｆｅ７６Ｓｉ９Ｂ１０Ｐ５から成る組成物を１００ｇ準備し、実施例１と類似の工程でガスアトマイズした。この時の溶湯の温度は、融点１０６０℃より＋１００℃の１１６０℃とした。また、アトマイズ時の３ａｔ％水素−ヘリウムガスのノズル噴射圧力は、１４ＭＰａであった。更に、落下装置の透明石英管上部の反射型赤外線加熱装置の加熱温度は、１３５０℃とした。 As a soft magnetic alloy ingot, 100 g of a composition composed of Fe 76 Si 9 B 10 P 5 was prepared, and gas atomized in the same process as in Example 1. The temperature of the molten metal at this time was 1160 ° C., which is + 100 ° C. from the melting point of 1060 ° C. Further, the nozzle injection pressure of 3 at% hydrogen-helium gas during atomization was 14 MPa. Furthermore, the heating temperature of the reflective infrared heating device on the upper part of the transparent quartz tube of the dropping device was set to 1350 ° C.
図８は、ガスアトマイズ後の粉末、図９は、ＪＩＳ規格３８ミクロンメッシュで篩上の粉末、図１０は、ＪＩＳ規格３８ミクロンメッシュで篩下の粉末のそれぞれのＳＥＭ像である。 FIG. 8 shows SEM images of the powder after gas atomization, FIG. 9 shows the powder on the sieve with a JIS standard 38 micron mesh, and FIG. 10 shows the powder on the sieve with a JIS standard 38 micron mesh.
本発明によれば、高純度のアモルファスの軟磁性合金粉末が得られ、産業機器分野では発電機、超高圧変電所および一次/二次変電所の変圧器、動力用等の各種モーター、道路照明の安定器など、また一般民生分野では、蛍光灯の安定器（トランスの一種）をはじめ、家電機器のモーター、テレビの電源トランスなどの高効率化に寄与することが可能となる。 According to the present invention, a high-purity amorphous soft magnetic alloy powder can be obtained. In the industrial equipment field, generators, ultra-high voltage substations and primary / secondary substation transformers, various motors for power, road lighting, etc. In the general consumer field, it is possible to contribute to higher efficiency of fluorescent ballasts (a kind of transformer), motors for home appliances, power transformers for televisions, and the like.
Claims (4)
軟磁性合金の溶湯に不活性ガスを吹き付けてガスアトマイズして、軟磁性合金の粉末を製造する第一の工程と、
次に前記粉末を所定の粒径で二つに分割する第二の工程と、
次に、不活性ガスが上方から下方に流れる透明石英管中で、前記所定の粒径より大きい粉末を落下させ、石英管上部の外側に設けた反射型赤外線加熱装置により、落下中の粉末を非接触加熱で再溶解する第三の工程と、
しかる後に、前記透明石英管の鉛直下方に設けた不活性ガス冷却部で、再溶解した粉末を急冷固化し、回収する第四の工程とを
有することを特徴とするアモルファス軟磁性合金粉末の製造方法。 In the method for producing amorphous soft magnetic alloy powder,
A first step of producing a soft magnetic alloy powder by spraying an inert gas onto the melt of the soft magnetic alloy and gas atomizing;
Next, a second step of dividing the powder into two with a predetermined particle size,
Next, a powder larger than the predetermined particle size is dropped in a transparent quartz tube in which an inert gas flows downward from above, and the falling powder is reflected by a reflective infrared heating device provided outside the quartz tube. A third step of redissolving with non-contact heating;
Thereafter, a fourth step of rapidly solidifying and recovering the re-dissolved powder in an inert gas cooling section provided vertically below the transparent quartz tube, and producing an amorphous soft magnetic alloy powder, Method.
The soft magnetic alloy is mainly composed of Fe, and includes at least two kinds of alloy components of Co, Nb, Si, B, P, and Cu, and other inevitable impurity elements. A method for producing an amorphous soft magnetic alloy powder according to 2 or 3.
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