JP6530164B2 - Nanocrystalline soft magnetic alloy powder and dust core using the same - Google Patents
Nanocrystalline soft magnetic alloy powder and dust core using the same Download PDFInfo
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- 229910001004 magnetic alloy Inorganic materials 0.000 title claims description 42
- 239000000428 dust Substances 0.000 title description 18
- 239000013078 crystal Substances 0.000 claims description 50
- 239000000203 mixture Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
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- 239000007788 liquid Substances 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910000510 noble metal Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 description 52
- 229910000859 α-Fe Inorganic materials 0.000 description 20
- 238000001556 precipitation Methods 0.000 description 16
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- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
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- 238000000634 powder X-ray diffraction Methods 0.000 description 1
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Description
本発明は、トランス、チョークコイル、リアクトル等のインダクタに用いられるナノ結晶軟磁性合金粉末とその製造方法、およびナノ結晶軟磁性合金粉末を用いた圧粉磁芯に関する。 The present invention relates to a nanocrystalline soft magnetic alloy powder used for an inductor such as a transformer, a choke coil, and a reactor, a method of producing the same, and a dust core using the nanocrystalline soft magnetic alloy powder.
アモルファス相中に微小なαＦｅ（−Ｓｉ）結晶相が析出したナノ結晶軟磁性合金は、高飽和磁束密度と低磁歪の両立が可能なため、トランスなどのコアとして用いた場合、コア損失を低減できる優れた軟磁性材料である。 A nanocrystalline soft magnetic alloy in which a minute α-Fe (-Si) crystal phase is precipitated in an amorphous phase can achieve both high saturation magnetic flux density and low magnetostriction, so core loss is reduced when it is used as a core of a transformer etc. It is an excellent soft magnetic material that can
また、近年の電子機器の小型化や高周波化の要求に対応し、チョークコイルやリアクトルなどのコアに使用することを目的として、ナノ結晶軟磁性合金粉末と絶縁性の良い樹脂バインダを混合して成形した圧粉磁芯が開発されている。 In addition, in response to the recent demand for miniaturization and high frequency of electronic devices, it is mixed with nanocrystalline soft magnetic alloy powder and resin binder with good insulation for the purpose of using it as core for choke coil, reactor etc. Molded dust cores have been developed.
例えば、特許文献１には、ナノ結晶組織を有するナノ結晶磁性粉末、または熱処理によりナノ結晶組織を発現可能な組成の非晶質軟磁性粉末のいずれかに、バインダーとガラス粉末を添加して加圧成形し、ガラスの軟化点以上６００℃以下で熱処理して得られる圧粉磁芯およびその製造方法が開示されている。 For example, in Patent Document 1, a binder and a glass powder are added to either a nanocrystalline magnetic powder having a nanocrystalline structure or an amorphous soft magnetic powder having a composition capable of expressing a nanocrystalline structure by heat treatment. The powder magnetic core obtained by pressure-forming and heat-processing above 600 degreeC of softening points of glass, and its manufacturing method are disclosed.
αＦｅ（−Ｓｉ）結晶相を析出させたナノ結晶軟磁性合金粉末を加圧成形した圧粉磁芯は、加圧成形時に粉末粒子に歪みを生じさせる。この歪みは、Ｆｅ−ＢやＦｅ−Ｐなどの化合物相が析出しない温度領域では十分に除去ができないため、コア損失が大きくなり、良好な軟磁気特性が得られない問題がある。 A powder magnetic core obtained by pressure-molding a nanocrystalline soft magnetic alloy powder in which an α-Fe (-Si) crystal phase is precipitated causes distortion in powder particles during pressure-molding. This distortion can not be sufficiently removed in a temperature range in which compound phases such as Fe-B and Fe-P do not precipitate, so the core loss becomes large and there is a problem that good soft magnetic characteristics can not be obtained.
また、アモルファス相の軟磁性合金粉末を、加圧成形して圧粉体を作製後、αＦｅ（−Ｓｉ）結晶相を析出させる熱処理を行うと、αＦｅ（−Ｓｉ）結晶相の析出による発熱によって熱暴走を起こしやすく、Ｆｅ−ＢやＦｅ−Ｐなどの化合物相が析出して比透磁率が低下し、圧粉磁芯として良好な軟磁気特性が得られない問題がある。 In addition, when the soft magnetic alloy powder of the amorphous phase is pressure-formed to produce a green compact, heat treatment is performed to precipitate the α-Fe (-Si) crystal phase, which generates heat due to the precipitation of the α-Fe (-Si) crystal phase. There is a problem that thermal runaway is likely to occur, compound phases such as Fe-B and Fe-P precipitate and the relative permeability decreases, and good soft magnetic characteristics can not be obtained as a dust core.
本発明の課題は、上記従来技術による圧粉磁芯の軟磁気特性を改善することを目的とし、優れた軟磁気特性が得られるナノ結晶軟磁性合金粉末とそれを用いた圧粉磁芯を提供することである。 An object of the present invention is to improve the soft magnetic properties of a powder magnetic core according to the above-mentioned prior art, and to provide a nanocrystalline soft magnetic alloy powder capable of obtaining excellent soft magnetic characteristics and a powder magnetic core using the same. It is to provide.
上記の目的を達成するため、本発明は、αＦｅ（−Ｓｉ）結晶相がアモルファス相中に析出したナノ結晶軟磁性合金粉末において、前記αＦｅ（−Ｓｉ）結晶相の結晶化度が４％以上７０％以下であることを特徴とする。 In order to achieve the above object, according to the present invention, in the nanocrystalline soft magnetic alloy powder in which the αFe (-Si) crystal phase is precipitated in the amorphous phase, the crystallinity of the αFe (-Si) crystal phase is 4% or more It is characterized by 70% or less.
本発明では、前記ナノ結晶軟磁性合金粉末の組成が、組成式 ＦｅａＢｂＳｉｃＰｘＣｙＣｕｚで表され、７９．０≦ａ≦８６．０、５．０≦ｂ≦１３．０、０．０≦ｃ≦８．０、１．０≦ｘ≦１０．０、０．０≦ｙ≦５．０、０．４≦ｚ≦１．４および０．０６≦ｚ／ｘ≦１．２０で、、Ｆｅの一部をＴｉ、Ｚｒ、Ｈｆ、Ｎｂ，Ｔａ、Ｍｏ、Ｗ、Ｃｒ、Ｃｏ、Ｎｉ、Ａｌ、Ｍｎ、Ｚｎ、Ｓ、Ｓｎ、Ａｓ、Ｓｂ、Ｂｉ、Ｎ、Ｏ、Ｃａ、Ｖ、Ｍｇおよび希土類元素、貴金属元素のうち１種類以上の元素で、組成全体の３ａｔ％以下を置換し、Ｆｅとの合計が７９．０ａｔ％以上、８６．０ａｔ％以下であることが望ましい。 In the present invention, the composition of the nanocrystalline soft magnetic alloy powder is represented by a composition formula Fe a B b Si c P x C y Cu z, 79.0 ≦ a ≦ 86.0,5.0 ≦ b ≦ 13 .0, 0.0 ≦ c ≦ 8.0, 1.0 ≦ x ≦ 10.0, 0.0 ≦ y ≦ 5.0, 0.4 ≦ z ≦ 1.4 and 0.06 ≦ z / x ≦ 1.20, part of Fe is Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Co, Ni, Al, Mn, Zn, S, Sn, As, Sb, Bi, N, 3 at% or less of the whole composition is replaced with one or more elements of O, Ca, V, Mg and rare earth elements and noble metal elements, and the total with Fe is 79.0 at% or more and 86.0 at% or less Is desirable.
また、前記ナノ結晶軟磁性合金粉末の粒子のアスペクト比が、１．０を超え２．６以下であることが望ましい。 Further, the aspect ratio of the particles of the nanocrystalline soft magnetic alloy powder is preferably more than 1.0 and 2.6 or less.
本発明では、アモルファス相の合金組成物を熱処理してαＦｅ（−Ｓｉ）結晶相を析出させ、αＦｅ（−Ｓｉ）結晶相の結晶化度を４％以上７０％以下とし、その後に前記合金組成物を粉砕することによって粉末化することを特徴とするナノ結晶軟磁性合金粉末の製造方法が得られる。 In the present invention, the alloy composition of the amorphous phase is heat-treated to precipitate the α-Fe (-Si) crystal phase, and the α-Fe (-Si) crystal phase is made to have a crystallinity of 4% to 70%. A method for producing a nanocrystalline soft magnetic alloy powder is provided, which is characterized by pulverizing a substance.
また、前記合金組成物が、薄帯であることが望ましい。 Moreover, it is desirable that the said alloy composition is a thin strip.
さらに本発明では、ナノ結晶軟磁性合金粉末とバインダとを混合したものを、加圧成形した後、熱処理を行ってαＦｅ（−Ｓｉ）結晶相を追加析出させたことを特徴とする圧粉磁芯が得られる。 Furthermore, in the present invention, a mixture of nanocrystalline soft magnetic alloy powder and a binder is pressure-formed and then heat-treated to additionally precipitate an α-Fe (-Si) crystal phase. A core is obtained.
本発明のナノ結晶軟磁性合金粉末は、αＦｅ（−Ｓｉ）結晶相を部分的に析出させたもので、αＦｅ（−Ｓｉ）結晶相の結晶化度を４％以上とすることで、圧粉磁芯の作製における熱処理時に、追加析出するαＦｅ（−Ｓｉ）結晶相の析出量を減少させることができる。したがって、αＦｅ（−Ｓｉ）結晶相の析出によって放出される熱量を低減し、熱処理時の熱暴走を防ぐことが可能となる。これによりＦｅ−ＢやＦｅ−Ｐなどの化合物相の析出を抑制し、比透磁率に優れた良好な軟磁気特性を有する圧粉磁芯が実現できる。 The nanocrystalline soft magnetic alloy powder of the present invention is obtained by partially precipitating the αFe (-Si) crystal phase, and the green compact is obtained by setting the crystallinity of the αFe (-Si) crystal phase to 4% or more. At the time of heat treatment in the preparation of the magnetic core, the amount of precipitation of the additionally precipitated α-Fe (-Si) crystal phase can be reduced. Therefore, it is possible to reduce the amount of heat released by the precipitation of the α-Fe (-Si) crystal phase, and to prevent the thermal runaway during the heat treatment. Thereby, precipitation of a compound phase such as Fe-B or Fe-P can be suppressed, and a dust core having excellent soft magnetic properties and excellent in relative magnetic permeability can be realized.
また、αＦｅ（−Ｓｉ）結晶相の結晶化度を７０％以下とすることで、圧粉磁芯の作製で行う熱処理時に、αＦｅ（−Ｓｉ）結晶相が追加析出できる余地を残すことができる。このためαＦｅ（−Ｓｉ）結晶粒子の成長に伴って、加圧成形時にナノ結晶軟磁性合金粉末粒子に生じた歪みを緩和することが可能となる。これによりコア損失が小さい良好な軟磁気特性を有する圧粉磁芯が実現できる。 Further, by setting the crystallinity of the αFe (-Si) crystal phase to 70% or less, it is possible to leave room for additional precipitation of the αFe (-Si) crystal phase during the heat treatment performed in the production of the dust core. . Therefore, along with the growth of the α-Fe (—Si) crystal particles, it is possible to relieve the strain generated in the nanocrystalline soft magnetic alloy powder particles during pressure forming. As a result, a dust core having good soft magnetic characteristics with small core loss can be realized.
以上述べた様に、本発明のナノ結晶軟磁性合金粉末を使用することにより、比透磁率が高くコア損失の小さい優れた軟磁気特性を有する圧粉磁芯を得ることができる。 As described above, by using the nanocrystalline soft magnetic alloy powder of the present invention, it is possible to obtain a dust core having excellent soft magnetic characteristics, which has a high relative magnetic permeability and a small core loss.
本発明のナノ結晶軟磁性合金粉末の製造方法は、以下の通りである。まず、αＦｅ（−Ｓｉ）結晶相の微細結晶を析出する合金組成物を、高周波加熱などによって融解し、液体急冷法でアモルファス相の薄帯または薄片を作製する。次に、このアモルファス相の薄帯または薄片を、熱処理（以下、この熱処理を、１次熱処理と言う。）してαＦｅ（−Ｓｉ）結晶相を部分的に析出させる。その後、αＦｅ（−Ｓｉ）結晶相が部分的に析出した薄帯または薄片を粉砕して粉末化する。 The method for producing the nanocrystalline soft magnetic alloy powder of the present invention is as follows. First, an alloy composition for precipitating fine crystals of an α-Fe (-Si) crystal phase is melted by high frequency heating or the like, and a ribbon or a thin piece of an amorphous phase is produced by a liquid quenching method. Next, the amorphous phase ribbon or flake is heat-treated (hereinafter, this heat treatment is referred to as primary heat treatment) to partially precipitate an α-Fe (-Si) crystal phase. Thereafter, the ribbon or flake in which the αFe (-Si) crystal phase is partially precipitated is pulverized into powder.
アモルファス相の薄帯を作製する液体急冷法としては、Ｆｅ基アモルファス薄帯の製造などに使用される単ロール式のアモルファス製造装置や、双ロール式のアモルファス製造装置を使用することができる。 As a liquid quenching method for producing an amorphous phase ribbon, a single roll type amorphous production apparatus or a twin roll type amorphous production apparatus used for production of an Fe-based amorphous ribbon or the like can be used.
１次熱処理の方法は、汎用的な手法を適用することができる。例えば、抵抗加熱、赤外線加熱、溶融塩などへの浸漬、加熱された金属やセラミックスなどの固体に直接接触させる方法、レーザー光を照射する方法などがある。 A general-purpose method can be applied to the method of the primary heat treatment. For example, there are methods such as resistance heating, infrared heating, immersion in molten salt, direct contact with heated solids such as metals and ceramics, and laser light irradiation.
１次熱処理において、熱処理温度と熱処理時間を調整することで、αＦｅ（−Ｓｉ）結晶相を部分的に析出させ、目的とする結晶化度を有するナノ結晶軟磁性合金粉末を得ることができる。 In the primary heat treatment, by adjusting the heat treatment temperature and the heat treatment time, it is possible to partially precipitate the α-Fe (-Si) crystal phase, and to obtain a nanocrystalline soft magnetic alloy powder having a desired degree of crystallinity.
本発明によるナノ結晶軟磁性合金粉末は、αＦｅ（−Ｓｉ）結晶相の結晶化度が４％以上７０％以下であることにより、圧粉磁芯の作製時における熱処理（以下、この熱処理を２次熱処理と言う。）において、熱暴走に起因する化合物相の析出を抑制し、かつ圧粉磁芯の作製時の加圧成形において生じた粉末粒子の歪みを緩和することができる。 The nanocrystalline soft magnetic alloy powder according to the present invention has a crystallinity of 4% to 70% of the αFe (-Si) crystal phase, so that the heat treatment at the time of producing the dust core (hereinafter, this heat treatment In the next heat treatment, precipitation of a compound phase caused by thermal runaway can be suppressed, and distortion of powder particles generated in pressure forming at the time of production of a dust core can be alleviated.
αＦｅ（−Ｓｉ）結晶相の結晶化度が１４％以上であれば、２次熱処理におけるαＦｅ（−Ｓｉ）結晶相の析出による発熱はさらに減少する。このため熱暴走が起こる可能性はほとんど無くなり、熱処理温度が適切で有れば、化合物相の析出をほとんど抑止することができるのでより好ましい。またαＦｅ（−Ｓｉ）結晶相の結晶化度が５０％未満であれば、２次熱処理におけるαＦｅ（−Ｓｉ）結晶相の析出余地が十分に確保されるので、加圧成形において粉末粒子に生じる歪みをより効果的に緩和することができるのでより好ましい。 If the crystallinity of the αFe (-Si) crystal phase is 14% or more, the heat generation due to the precipitation of the αFe (-Si) crystal phase in the secondary heat treatment is further reduced. For this reason, the possibility of thermal runaway is almost eliminated, and if the heat treatment temperature is appropriate, it is more preferable because the precipitation of the compound phase can be almost suppressed. In addition, if the crystallinity of the αFe (-Si) crystal phase is less than 50%, room for the precipitation of the αFe (-Si) crystal phase in the secondary heat treatment is sufficiently ensured, so that powder particles are generated during pressure forming. It is more preferable because distortion can be alleviated more effectively.
さらに、αＦｅ（−Ｓｉ）結晶相の結晶化度が１４％以上３０％未満であるのが最も好ましく、高い比透磁率と、小さなコア損失を有する圧粉磁芯を得ることができる。 Furthermore, it is most preferable that the crystallinity of the α-Fe (-Si) crystal phase is 14% or more and less than 30%, and a dust core having high relative magnetic permeability and small core loss can be obtained.
ナノ結晶軟磁性合金粉末におけるαＦｅ（−Ｓｉ）結晶相の結晶化度は、粉末Ｘ線回折によって求めることができる。具体的には、Ｘ線回折装置（ＸＲＤ）によって得られた粉末試料のＸ線回折パターンから、バックグラウンドと装置に起因する回折の非対称性を補正した後、αＦｅ（−Ｓｉ）結晶相の回折パターンと、アモルファス相に特有のブロードな回折パターンを分離し、それぞれの回折強度を求めた後、全回折強度に対するαＦｅ（−Ｓｉ）結晶相の回折強度の比を計算することによって得られる。 The crystallinity of the α-Fe (-Si) crystal phase in the nanocrystalline soft magnetic alloy powder can be determined by powder X-ray diffraction. Specifically, from the X-ray diffraction pattern of the powder sample obtained by the X-ray diffractometer (XRD), after correcting the asymmetry of the diffraction caused by the background and the instrument, the diffraction of the αFe (-Si) crystal phase It is obtained by separating the pattern and a broad diffraction pattern peculiar to the amorphous phase, determining the respective diffraction intensities, and calculating the ratio of the diffraction intensity of the α-Fe (-Si) crystal phase to the total diffraction intensity.
αＦｅ（−Ｓｉ）結晶相が部分的に析出した薄帯または薄片の粉砕は、一般的な粉砕装置を使用できる。例えば、ボールミル、スタンプミル、遊星ミル、サイクロンミル、ジェットミルなどが使用できる。 The grinding of the ribbon or flakes in which the αFe (-Si) crystal phase is partially precipitated can be performed using a common grinding device. For example, a ball mill, a stamp mill, a planetary mill, a cyclone mill, a jet mill and the like can be used.
また、粉砕して得られた粉末をふるいを用いて分級することにより、所望のアスペクト比の粒子を有するナノ結晶軟磁性合金粉末が得られる。 Also, by classifying the powder obtained by grinding using a sieve, a nanocrystalline soft magnetic alloy powder having particles of a desired aspect ratio can be obtained.
本発明によるナノ結晶軟磁性合金粉末では、粒子のアスペクト比を１．０を超え２．６以下とすることにより、特に高周波領域における渦電流損失の増加が抑制されるのでコア損失の低減に効果がある。 In the nanocrystalline soft magnetic alloy powder according to the present invention, by setting the aspect ratio of the particles to 1.0 or more and 2.6 or less, an increase in eddy current loss particularly in a high frequency region is suppressed, which is effective in reducing core loss. There is.
αＦｅ（−Ｓｉ）結晶相の結晶化度が４％未満では、２次熱処理でのαＦｅ（−Ｓｉ）結晶相の析出による発熱量が大きく、熱暴走による化合物相が析出する可能性が大きくなるので望ましくない。さらに粉砕による粉末化が著しく困難になる問題がある。この場合、仮に時間をかけて粉砕したとしても、ほとんどの粒子がアスペクト比で２．６を超えるため好ましくない。 If the crystallinity of the αFe (-Si) crystal phase is less than 4%, the calorific value due to the precipitation of the αFe (-Si) crystal phase in the secondary heat treatment is large, and the possibility of precipitation of the compound phase due to thermal runaway increases. So undesirable. Furthermore, there is a problem that pulverization by grinding becomes extremely difficult. In this case, even if it takes a long time to grind, it is not preferable because most particles have an aspect ratio of more than 2.6.
ナノ結晶軟磁性合金粉末の組成としては、組成式ＦｅａＢｂＳｉｃＰｘＣｙＣｕｚで表され、７９．０≦ａ≦８６．０、５≦ｂ≦１３、０≦ｃ≦８、１≦ｘ≦１０、０≦ｙ≦５、０．４≦ｚ≦１．４および０．０６≦ｚ／ｘ≦１．２０である組成が適用できる。 The composition of nanocrystalline soft magnetic alloy powder, the composition formula Fe a B b Si c P x C y is represented by Cu z, 79.0 ≦ a ≦ 86.0,5 ≦ b ≦ 13,0 ≦ c ≦ 8 The compositions can be applied where 1 ≦ x ≦ 10, 0 ≦ y ≦ 5, 0.4 ≦ z ≦ 1.4 and 0.06 ≦ z / x ≦ 1.20.
Ｆｅ元素は、磁性を担う主たる元素であるので、その含有量は飽和磁束密度向上のためには多い方が好ましく、特に８１ａｔ％以上で有ることが望ましい。しかしながら８６ａｔ％を超えると、アモルファス相の形成能が低下するので好ましくない。 Since the Fe element is a main element responsible for magnetism, its content is preferably as large as possible in order to improve the saturation magnetic flux density, and in particular, it is desirable to be 81 at% or more. However, if it exceeds 86 at%, the ability to form an amorphous phase is reduced, which is not preferable.
また、耐食性の改善や電気抵抗の調整などを目的として、Ｆｅの一部をＴｉ、Ｚｒ、Ｈｆ、Ｎｂ，Ｔａ、Ｍｏ、Ｗ、Ｃｒ、Ｃｏ、Ｎｉ、Ａｌ、Ｍｎ、Ｚｎ、Ｓ、Ｓｎ、Ａｓ、Ｓｂ、Ｂｉ、Ｎ、Ｏ、Ｃａ、Ｖ、Ｍｇおよび希土類元素、貴金属元素のうち１種類以上の元素で、組成全体の３ａｔ％以下を置換し、Ｆｅとの合計が７９．０ａｔ％以上、８６．０ａｔ％以下としても良い。 In addition, for the purpose of improving the corrosion resistance and adjusting the electrical resistance, etc., part of Fe is Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Co, Ni, Al, Mn, Zn, S, Sn, As, Sb, Bi, N, O, Ca, V, Mg and one or more of rare earth elements and noble metal elements, 3 at% or less of the whole composition is replaced, and the total with Fe is 79.0 at% or more And may be 86.0 at% or less.
本発明によるナノ結晶軟磁性合金粉末の製造方法としては、上述の方法以外に、ガスアトマイズ法あるいは水アトマイズ法などで、アモルファス相の粉末を作製し、１次熱処理を行ってαＦｅ（−Ｓｉ）結晶相を部分的に析出させ、目的とする結晶化度を有するナノ結晶軟磁性合金粉末を得ることもできる。 As a method of producing a nanocrystalline soft magnetic alloy powder according to the present invention, in addition to the above-mentioned method, powder of an amorphous phase is produced by gas atomization method or water atomization method, etc., and primary heat treatment is performed to obtain αFe (-Si) crystal. It is also possible to partially precipitate the phase to obtain a nanocrystalline soft magnetic alloy powder having a desired degree of crystallinity.
この場合の熱処理も、アモルファス相の薄帯を１次熱処理する場合と同様に、熱処理温度と熱処理時間を調整することでαＦｅ（−Ｓｉ）結晶相の結晶化度が４％以上７０％以下であるナノ結晶軟磁性合金粉末を得ることができる。 Also in this case, the heat treatment temperature and the heat treatment time are adjusted in the same manner as in the primary heat treatment of the thin ribbon of the amorphous phase, and the crystallinity of the αFe (-Si) crystal phase is 4% or more and 70% or less A nanocrystalline soft magnetic alloy powder can be obtained.
本発明における圧粉磁芯の作製は、２次熱処理工程を除いては、一般的な方法を採用することができる。例えば、αＦｅ（−Ｓｉ）結晶相が部分的に析出したナノ結晶軟磁性合金粉末と、フェノール樹脂やシリコーン樹脂などの絶縁性が良好で耐熱性が高いバインダーとを混合して造粒粉を作製する。次に造粒粉を所望の形状を有する金型に充填し、加圧成形して圧粉体を得る。その後、圧粉体を２次熱処理してαＦｅ（−Ｓｉ）結晶相を追加析出させる。２次熱処理では、バインダーの加熱硬化も同時に行う。 The production of the powder magnetic core in the present invention can adopt a general method except for the secondary heat treatment step. For example, a granulated soft magnetic alloy powder is prepared by mixing a nanocrystalline soft magnetic alloy powder in which an α-Fe (-Si) crystal phase is partially precipitated with a binder having good insulation and high heat resistance such as phenol resin or silicone resin. Do. Next, the granulated powder is filled in a mold having a desired shape and pressed to obtain a green compact. Thereafter, the green compact is subjected to secondary heat treatment to additionally precipitate the αFe (-Si) crystal phase. In the secondary heat treatment, the binder is simultaneously heated and cured.
２次熱処理におけるαＦｅ（−Ｓｉ）結晶相の析出量は、従来のアモルファス相から析出させる場合と比較して、１次熱処理で析出した分だけ減少しているので、αＦｅ（−Ｓｉ）結晶相析出に伴う発熱による熱暴走は抑制される。２次熱処理において、熱処理温度は、αＦｅ（−Ｓｉ）結晶相の析出が進行し、かつＦｅ−Ｂ、Ｆｅ−Ｐなどの化合物相が析出しない温度範囲を設定すれば良い。また熱処理時間は、αＦｅ（−Ｓｉ）結晶相が十分に析出できる時間を設定すれば良い。 The amount of precipitation of the α-Fe (-Si) crystal phase in the secondary heat treatment is reduced by the amount deposited in the first heat treatment as compared to the case of precipitation from the conventional amorphous phase, so the α-Fe (-Si) crystal phase Thermal runaway due to heat generation accompanying precipitation is suppressed. In the secondary heat treatment, the heat treatment temperature may be set to a temperature range in which the precipitation of the α-Fe (-Si) crystal phase proceeds and the compound phase such as Fe-B or Fe-P does not precipitate. Moreover, what is necessary is just to set the heat processing time as the time which can fully precipitate the (alpha) Fe (-Si) crystal phase.
圧粉磁芯の作製方法としては、加圧成形と２次熱処理を同時に行えるホットプレス等でも良い。またバインダーと混合した後に、射出成形などの方法で圧粉体を作製し、その後２次熱処理を行っても良い。 As a method of producing a dust core, a hot press or the like which can simultaneously perform pressure molding and secondary heat treatment may be used. Alternatively, after being mixed with a binder, a green compact may be produced by a method such as injection molding, and then secondary heat treatment may be performed.
（第１の実施例）
原料としてＦｅ、Ｆｅ−Ｂ、Ｆｅ−Ｐ、Ｃｕを用い、組成式でＦｅ８４．３Ｂ６．０Ｐ９．０Ｃｕ０．７となるように秤量し、高周波加熱炉で融解して合金組成物を得た。その後、単ロール型の液体急冷装置にてアモルファス相の薄帯を作製した。作製した薄帯の厚さは約２５μｍ、幅は約１５ｍｍである。
(First embodiment)
Using Fe, Fe-B, Fe-P, and Cu as raw materials, measure so as to be Fe 84.3 B 6.0 P 9.0 Cu 0.7 according to the composition formula, and melt in a high frequency heating furnace to obtain an alloy The composition was obtained. Thereafter, a thin ribbon of an amorphous phase was produced by a single roll type liquid quenching apparatus. The produced ribbon has a thickness of about 25 μm and a width of about 15 mm.
次に、得られた薄帯を、抵抗加熱型の熱処理炉に投入し、アルゴン雰囲気中で１次熱処理を行い、αＦｅ（−Ｓｉ）結晶相を部分的に析出させた。熱処理温度は、実施例１から実施例８では４２０℃から４６０℃とし、熱処理時間は４０秒である。また、１次熱処理を行わない場合を、比較例１とした。比較例２から４では、熱処理温度はそれぞれ４００℃、４１０℃、４７５℃とし、熱処理時間はそれぞれ６０秒、４０秒、４０秒である。 Next, the obtained thin ribbon was put into a resistance heating type heat treatment furnace, and was subjected to primary heat treatment in an argon atmosphere to partially precipitate an αFe (-Si) crystal phase. The heat treatment temperature is set to 420 ° C. to 460 ° C. in Examples 1 to 8 and the heat treatment time is 40 seconds. Moreover, the case where primary heat treatment was not performed was set as Comparative Example 1. In Comparative Examples 2 to 4, the heat treatment temperatures are 400 ° C., 410 ° C., and 475 ° C., respectively, and the heat treatment times are 60 seconds, 40 seconds, and 40 seconds, respectively.
上述の１次熱処理を行った薄帯をステンレス製のポットミルを用いて粉砕し、αＦｅ（−Ｓｉ）結晶相が部分的に析出したナノ結晶軟磁性合金粉末を得た。なお実施例１から実施例８では、薄帯の粉砕による粉末化は容易であったが、比較例１および比較例２の薄帯は、粉末化することができなかった。 The ribbon subjected to the above-mentioned primary heat treatment was crushed using a stainless steel pot mill to obtain a nanocrystalline soft magnetic alloy powder in which an αFe (-Si) crystal phase was partially precipitated. In Examples 1 to 8, although pulverization of the ribbon by pulverization was easy, the ribbons of Comparative Example 1 and Comparative Example 2 could not be powdered.
得られたナノ結晶軟磁性合金粉末は、Ｘ線回折装置（ＸＲＤ）を用いて結晶化度の測定を行った。粉砕することができなかった比較例１と比較例２の薄帯は、薄帯の状態で結晶化度の測定を行った。 The degree of crystallinity of the obtained nanocrystalline soft magnetic alloy powder was measured using an X-ray diffractometer (XRD). The ribbons of Comparative Example 1 and Comparative Example 2 which could not be ground were subjected to measurement of the degree of crystallinity in the state of ribbons.
得られたナノ結晶軟磁性合金粉末に対して、重量比で３％の熱硬化性シリコーン樹脂をバインダーとして混合し、造粒を行い造粒粉を作製した。次に、造粒粉を金型に投入し、９８０ＭＰａで加圧成形を行って圧粉体を作製した。圧粉体の寸法は、外径２０ｍｍ、内径１３ｍｍ、厚さ８ｍｍである。 With respect to the obtained nanocrystalline soft magnetic alloy powder, 3% by weight of a thermosetting silicone resin was mixed as a binder, and the mixture was granulated to prepare granulated powder. Next, the granulated powder was put into a mold and pressure-molded at 980 MPa to produce a green compact. The dimensions of the green compact are an outer diameter of 20 mm, an inner diameter of 13 mm, and a thickness of 8 mm.
作製した圧粉体を、赤外線加熱装置を用いて、熱処理温度４２５℃、熱処理時間２０分で２次熱処理を行い、αＦｅ（−Ｓｉ）結晶相の追加析出と熱硬化性シリコーン樹脂の硬化を行い圧粉磁芯を得た。 The compacts thus prepared are subjected to secondary heat treatment at a heat treatment temperature of 425 ° C. and a heat treatment time of 20 minutes using an infrared heating device to carry out additional precipitation of the αFe (-Si) crystal phase and curing of the thermosetting silicone resin. A dust core was obtained.
作製した圧粉磁芯に巻線を行い、磁気特性を測定した。比透磁率μの測定は、インピーダンスアナライザーを用い、周波数２０ｋＨｚで行った。またＢ−Ｈアナライザーを用いて周波数２０ｋＨｚ、磁束密度１００ｍＴにおけるコア損失を測定した。 Winding was performed on the produced dust core, and the magnetic characteristics were measured. The relative permeability μ was measured using an impedance analyzer at a frequency of 20 kHz. Also, core loss at a frequency of 20 kHz and a magnetic flux density of 100 mT was measured using a BH analyzer.
表１に、第１の実施例におけるナノ結晶軟磁性合金粉末の結晶化度と圧粉磁芯の軟磁気特性を、比較例と共に示す。表１より、αＦｅ（−Ｓｉ）結晶相の結晶化度が４％以上７０％以下のナノ結晶軟磁性合金粉末を用いた圧粉磁芯は、比透磁率が２０ｋＨｚで３０以上を有し、コア損失が２０ｋＨｚ、１００ｍＴで５００ｍＷ／ｃｍ ３ 未満の良好な軟磁気特性を持つことが判る。なお比較例１と比較例２は、先に述べた様に粉末化ができなかったので、圧粉磁芯の作製と磁気特性の測定は実施できなかった。 In Table 1, the crystallinity degree of the nanocrystalline soft magnetic alloy powder in the first example and the soft magnetic properties of the dust core are shown together with the comparative example. From Table 1, the powder magnetic core using the nanocrystalline soft magnetic alloy powder having a crystallinity of 4% to 70% of the αFe (-Si) crystal phase has a relative permeability of 30 or more at 20 kHz, It can be seen that the core loss has good soft magnetic properties of less than 500 mW / cm 3 at 20 kHz and 100 mT. As Comparative Examples 1 and 2 could not be powdered as described above, the production of the dust core and the measurement of the magnetic characteristics could not be carried out.
（第２の実施例）
第１の実施例と同様にして、組成式がＦｅ８４．３Ｂ６．０Ｐ９．０Ｃｕ０．７であるアモルファス相の薄帯を作製し、１次熱処理を行ってαＦｅ（−Ｓｉ）結晶相を部分的に析出させた。熱処理温度は４２５℃、熱処理時間は４０秒である。
Second Embodiment
In the same manner as in the first embodiment, a thin ribbon of an amorphous phase having a composition formula of Fe 84.3 B 6.0 P 9.0 Cu 0.7 is prepared, and subjected to primary heat treatment to form αFe (-Si ) Crystalline phase was partially precipitated. The heat treatment temperature is 425 ° C., and the heat treatment time is 40 seconds.
上述の１次熱処理を行った薄帯をステンレス製のポットミルを用いて粉砕し、αＦｅ（−Ｓｉ）結晶相が部分的に析出したナノ結晶軟磁性合金粉末を得た。 The ribbon subjected to the above-mentioned primary heat treatment was crushed using a stainless steel pot mill to obtain a nanocrystalline soft magnetic alloy powder in which an αFe (-Si) crystal phase was partially precipitated.
得られたナノ結晶軟磁性合金粉末は、Ｘ線回折装置（ＸＲＤ）を用いて結晶化度の測定を行った。本実施例のαＦｅ（−Ｓｉ）結晶相の結晶化度は、１０％であった。 The degree of crystallinity of the obtained nanocrystalline soft magnetic alloy powder was measured using an X-ray diffractometer (XRD). The crystallinity of the αFe (-Si) crystal phase of this example was 10%.
次に、得られたナノ結晶軟磁性合金粉末を、目開き１５０μｍ、９０μｍ、４５μｍのふるいを重ねた多段ふるいに通した。目開き１５０μｍのふるいを通り、目開き９０μｍのふるいを通らなかった粉末を比較例５とし、同様に９０μｍを通り４５μｍを通らなかった粉末を実施例９、４５μｍを通った粉末を実施例１０とした。 Next, the obtained nanocrystalline soft magnetic alloy powder was passed through a multistage sieve in which sieves with openings of 150 μm, 90 μm and 45 μm were stacked. The powder which passed through a 150 μm sieve and which did not pass through a 90 μm sieve was regarded as Comparative Example 5, and the powder which passed through 90 μm and did not pass 45 μm was similarly Example 9; did.
粉末粒子のアスペクト比は走査型電子顕微鏡（ＳＥＭ）を用いて観察した。任意の３０個の粒子について、短径の長径に対する比を測定し、３０個の粒子の平均値を求めてアスペクト比とした。 The aspect ratio of the powder particles was observed using a scanning electron microscope (SEM). The ratio of the minor axis to the major axis was measured for any 30 particles, and the average value of the 30 particles was determined as the aspect ratio.
第１の実施例と同様に、圧粉磁芯を作製した後に巻線を行い、磁気特性を測定した。比透磁率の測定は、周波数１ＭＨｚで行った。またコア損失は、周波数３００ｋＨｚ、磁束密度５０ｍＴで行った。 As in the first embodiment, a powder magnetic core was produced and then wound, and magnetic characteristics were measured. The relative permeability was measured at a frequency of 1 MHz. The core loss was performed at a frequency of 300 kHz and a magnetic flux density of 50 mT.
表２に、第２の実施例におけるナノ結晶軟磁性合金粉末の結晶化度とアスペクト比および圧粉磁芯の比透磁率とコア損失を、比較例と共に示す。表２より、本発明による、粒子のアスペクト比が１．０を超え２．６以下であるナノ結晶軟磁性合金粉末を使用した圧粉磁芯は、アスペクト比が４．８である比較例と比べてコア損失が小さく、３００ｋＨｚの高周波領域で良好な軟磁気特性を有していることが判る。 Table 2 shows the crystallinity and the aspect ratio of the nanocrystalline soft magnetic alloy powder in the second example, and the relative permeability and core loss of the dust core, together with the comparative example. From Table 2, according to the present invention, a powder magnetic core using a nanocrystalline soft magnetic alloy powder having an aspect ratio of particles of more than 1.0 and 2.6 or less and a comparative example having an aspect ratio of 4.8 and In comparison, core loss is small, and it can be seen that it has good soft magnetic characteristics in a high frequency region of 300 kHz.
以上述べたように、本発明は、αＦｅ（−Ｓｉ）結晶相の結晶化度を４％以上７０％以下であるナノ結晶軟磁性合金粉末を使用することにより、比透磁率が高くコア損失が小さい優れた軟磁気特性を有する圧粉磁芯を得ることができる。 As described above, according to the present invention, the relative magnetic permeability is high and the core loss is high by using the nanocrystalline soft magnetic alloy powder having the crystallinity of the αFe (-Si) crystal phase of 4% or more and 70% or less. A dust core having small and excellent soft magnetic properties can be obtained.
本発明は、以上説明した実施例に限定されるものではなく、本発明の技術的思想内で当分野において通常の知識を有する者により多くの変形が可能である。 The present invention is not limited to the embodiments described above, and many modifications can be made by those skilled in the art within the technical concept of the present invention.
Claims (3)
７９．０≦ａ≦８６．０、５．０≦ｂ≦１３．０、０．０≦ｃ≦８．０、１．０≦ｘ≦１０．０、０．０≦ｙ≦５．０、０．４≦ｚ≦１．４および０．０６≦ｚ／ｘ≦１．２０で、
Ｆｅの一部をＴｉ、Ｚｒ、Ｈｆ、Ｎｂ，Ｔａ、Ｍｏ、Ｗ、Ｃｒ、Ｃｏ、Ｎｉ、Ａｌ、Ｍｎ、Ｚｎ、Ｓ、Ｓｎ、Ａｓ、Ｓｂ、Ｂｉ、Ｎ、Ｏ、Ｃａ、Ｖ、Ｍｇおよび希土類元素、貴金属元素のうち１種類以上の元素で、組成全体の３ａｔ％以下を置換し、Ｆｅとの合計が７９．０ａｔ％以上、８６．０ａｔ％以下である請求項１に記載のナノ結晶軟磁性合金粉末の製造方法。 The composition of the alloy composition is represented by a composition formula Fe a B b Si c P x C y Cu z,
79.0 ≦ a ≦ 86.0, 5.0 ≦ b ≦ 13.0, 0.0 ≦ c ≦ 8.0, 1.0 ≦ x ≦ 10.0, 0.0 ≦ y ≦ 5.0, 0.4 ≦ z ≦ 1.4 and 0.06 ≦ z / x ≦ 1.20
A part of Fe is Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Co, Ni, Al, Mn, Zn, S, Sn, As, Sb, Bi, N, O, Ca, V, Mg and rare earth elements, at least one element among the noble metal elements, replace following 3at% of the total composition, the sum of Fe is 79.0At% or more, the nano according to claim 1 or less 86.0At% Method for producing crystalline soft magnetic alloy powder.
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| RU2791679C1 (en) * | 2022-06-30 | 2023-03-13 | Федеральное государственное автономное образовательное учреждение высшего образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Amorphous magnetic alloy based on the iron-silicon system |
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| JP2018167298A (en) * | 2017-03-30 | 2018-11-01 | Ｂｉｚｙｍｅ有限会社 | METHOD FOR PRODUCING Fe-Si-B-BASED NANOCRYSTAL ALLOY |
| JP6460276B1 (en) * | 2017-08-07 | 2019-01-30 | Tdk株式会社 | Soft magnetic alloys and magnetic parts |
| JP6439884B6 (en) | 2018-01-10 | 2019-01-30 | Tdk株式会社 | Soft magnetic alloys and magnetic parts |
| CN111971761A (en) * | 2018-03-29 | 2020-11-20 | 新东工业株式会社 | Iron-based soft magnetic powder and method for producing same, and article comprising iron-based soft magnetic alloy powder and method for producing same |
| CN109576608B (en) * | 2018-11-14 | 2020-11-10 | 江苏科技大学 | In-situ generated cladding structure iron-based block amorphous alloy composition and preparation method thereof |
| CN109295401A (en) * | 2018-12-11 | 2019-02-01 | 广东工业大学 | A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof |
| CN109825781B (en) * | 2019-04-08 | 2021-02-05 | 东北大学 | Method for continuously preparing iron-based amorphous thin strip |
| JP7419127B2 (en) * | 2020-03-23 | 2024-01-22 | 株式会社トーキン | Powder magnetic core and its manufacturing method |
| JP7424164B2 (en) * | 2020-03-30 | 2024-01-30 | Tdk株式会社 | Soft magnetic alloys, magnetic cores, magnetic components and electronic equipment |
| JP7207551B2 (en) | 2020-06-19 | 2023-01-18 | Ｊｆｅスチール株式会社 | Iron-based powder for dust core, dust core, and method for producing dust core |
| CN115961203B (en) * | 2022-12-31 | 2024-05-24 | 创明(韶关)绿色能源材料技术研究院有限公司 | Ultralow-aluminum nanocrystalline master alloy and preparation method thereof |
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| JP2003213331A (en) * | 2002-01-25 | 2003-07-30 | Alps Electric Co Ltd | METHOD FOR MANUFACTURING SOFT MAGNETIC Fe ALLOY, AND SOFT MAGNETIC Fe ALLOY |
| JP4638310B2 (en) * | 2005-09-16 | 2011-02-23 | Ｎｅｃトーキン株式会社 | Amorphous soft magnetic alloy pulverized powder manufacturing method, amorphous soft magnetic alloy pulverized powder, and compacted magnetic core |
| JP5445888B2 (en) * | 2005-09-16 | 2014-03-19 | 日立金属株式会社 | Soft magnetic alloy, method for producing the same, and magnetic component |
| WO2008133302A1 (en) * | 2007-04-25 | 2008-11-06 | Hitachi Metals, Ltd. | Soft magnetic thin strip, process for production of the same, magnetic parts, and amorphous thin strip |
| JP5305126B2 (en) * | 2007-04-25 | 2013-10-02 | 日立金属株式会社 | Soft magnetic powder, method of manufacturing a dust core, dust core, and magnetic component |
| WO2010095496A1 (en) * | 2009-02-20 | 2010-08-26 | アルプス・グリーンデバイス株式会社 | Compressed powder core |
| WO2011122589A1 (en) * | 2010-03-29 | 2011-10-06 | 日立金属株式会社 | Initial ultrafine crystal alloy, nanocrystal soft magnetic alloy and method for producing same, and magnetic component formed from nanocrystal soft magnetic alloy |
| TWI441929B (en) * | 2011-01-17 | 2014-06-21 | Alps Green Devices Co Ltd | Fe-based amorphous alloy powder, and a powder core portion using the Fe-based amorphous alloy, and a powder core |
| JP6041207B2 (en) * | 2012-12-27 | 2016-12-07 | 日立金属株式会社 | Nanocrystalline soft magnetic alloy and magnetic component using the same |
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