JP3058675B2 - Ultra-microcrystalline magnetic alloy - Google Patents
Ultra-microcrystalline magnetic alloyInfo
- Publication number
- JP3058675B2 JP3058675B2 JP2316551A JP31655190A JP3058675B2 JP 3058675 B2 JP3058675 B2 JP 3058675B2 JP 2316551 A JP2316551 A JP 2316551A JP 31655190 A JP31655190 A JP 31655190A JP 3058675 B2 JP3058675 B2 JP 3058675B2
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- magnetic
- crystal grains
- element selected
- heat treatment
- 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.)
- Expired - Lifetime
Links
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims description 15
- 239000013078 crystal Substances 0.000 claims description 46
- 229910045601 alloy Inorganic materials 0.000 claims description 40
- 239000000956 alloy Substances 0.000 claims description 40
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 25
- 229910052758 niobium Inorganic materials 0.000 claims description 12
- 239000006104 solid solution Substances 0.000 claims description 12
- 229910052735 hafnium Inorganic materials 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- 229910052726 zirconium Inorganic materials 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- 229910052748 manganese Inorganic materials 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 229910052715 tantalum Inorganic materials 0.000 claims description 10
- 229910052721 tungsten Inorganic materials 0.000 claims description 10
- 229910052720 vanadium Inorganic materials 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 229910052788 barium Inorganic materials 0.000 claims description 6
- 229910052790 beryllium Inorganic materials 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052698 phosphorus Inorganic materials 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 229910052712 strontium Inorganic materials 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 5
- 230000004907 flux Effects 0.000 description 15
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 14
- 239000011162 core material Substances 0.000 description 10
- 230000035699 permeability Effects 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000005096 rolling process Methods 0.000 description 4
- 239000000306 component Substances 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910002796 Si–Al Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000000700 radioactive tracer Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910018125 Al-Si Inorganic materials 0.000 description 1
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 1
- 229910018520 Al—Si Inorganic materials 0.000 description 1
- 229910017082 Fe-Si Inorganic materials 0.000 description 1
- 229910017133 Fe—Si Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910020018 Nb Zr Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、優れた磁気特性を有するとともに磁気特性
の安定性に優れた、組織の大半が超微細な結晶粒からな
る磁心部品、特に磁気ヘッド等に好適な超微結晶軟磁性
合金に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a magnetic core component having excellent magnetic properties and excellent stability of magnetic properties, the majority of the structure being composed of ultrafine crystal grains, and particularly to a magnetic component. The present invention relates to a microcrystalline soft magnetic alloy suitable for a head or the like.
［従来の技術］ 従来、磁気ヘッドを始めとする磁性部品に用いられる
磁心材料としては渦電流損が小さく周波数特性が比較的
良好なフェライトが主に用いられていた。しかし、フェ
ライトは飽和磁束密度が低く、磁気ヘッドに用いた場合
は近年の磁気記録再生装置の高記録密度化に対しては十
分な特性ではない。近年、高密度磁気記録用の高保磁力
を有する磁気記録媒体の特性を十分発揮するために、よ
り高飽和磁束密度で高透磁率を示す磁心材料の要求が高
まっている。このような要求に対して、近年Fe−Al−Si
系合金や、Co−Nb−Zr系非晶質合金薄膜等が検討されて
いる。このような試みは、例えば柴谷らによりNHK技報2
9（２）,51〜106（1977），広田らにより機能材料1986
年８月号p68等に報告されている。[Prior Art] Conventionally, as a magnetic core material used for a magnetic component such as a magnetic head, ferrite having a small eddy current loss and a relatively good frequency characteristic has been mainly used. However, ferrite has a low saturation magnetic flux density, and when it is used for a magnetic head, it does not have sufficient characteristics for a recent increase in recording density of a magnetic recording / reproducing apparatus. In recent years, in order to sufficiently exhibit the characteristics of a magnetic recording medium having a high coercive force for high-density magnetic recording, there is an increasing demand for a magnetic core material having a higher saturation magnetic flux density and a higher magnetic permeability. In response to such demands, Fe-Al-Si
Based alloys, Co—Nb—Zr based amorphous alloy thin films and the like have been studied. Such attempts have been made by, for example, NHK Technical Report 2
9 (2), 51-106 (1977), Functional material 1986 by Hirota et al.
August, p68.
［発明が解決しようとする課題］ しかしながら、Fe−Al−Si合金においては、高透磁率
を得るには磁歪λｓと結晶磁気異方性Ｋが共に零付近に
ある必要があり、このような組成では、飽和磁束密度は
12kG程度が限界である。このような問題があるため、現
在更に高飽和磁束密度で磁歪の小さいFe−Si合金等も検
討されているが、耐食性の問題や軟磁気特性の点で不十
分である。Co基アモルファス合金の場合は高飽和磁束密
度組成では結晶化しやすくなり耐熱性が悪いためガラス
ボンディング等が難しく工程上かなり制約を受ける。ま
た、最近になって，高飽和磁束密度で高透磁率を磁すFe
−Ｍ−Ｃ（Ｍ＝Ti,Zr,Hf）膜が信学技報MR89−12,p9等
に報告されている。しかし、Ｃを含む合金はＣ原子が動
き易いため磁気余効が起こり易く信頼性の点で問題があ
る。[Problems to be Solved by the Invention] However, in the Fe—Al—Si alloy, both magnetostriction λs and crystal magnetic anisotropy K need to be near zero in order to obtain high magnetic permeability. Then, the saturation magnetic flux density is
The limit is about 12kG. Because of these problems, Fe-Si alloys and the like having a high saturation magnetic flux density and a small magnetostriction are currently being studied, but are insufficient in terms of corrosion resistance and soft magnetic characteristics. In the case of a Co-based amorphous alloy, a composition having a high saturation magnetic flux density tends to be crystallized and has poor heat resistance, so that glass bonding or the like is difficult and the process is considerably restricted. Also, recently, Fe with high saturation magnetic flux density and high permeability
-MC (M = Ti, Zr, Hf) films are reported in IEICE Technical Report MR89-12, p9 and the like. However, alloys containing C have a problem in reliability because magnetic aftereffects are apt to occur because C atoms are easy to move.
そこで本発明は、優れた磁気特性を有し、かつ耐熱
性、信頼性に優れた合金の提供を課題とする。Therefore, an object of the present invention is to provide an alloy having excellent magnetic properties and excellent heat resistance and reliability.
［課題を解決するための手段］ 上記目的に鑑み鋭意研究の結果、本願発明者はFe,M,B
を基本成分としＭとＢを必ず含むFe基磁性合金であって
（M:Ti,Zr,Hf,V,Nb,Mo,Ta,Cr,W,Mnから選ばれる少なく
とも１種の元素）、結晶化熱処理することにより非晶質
相からbcc構造のFe固溶体からなる結晶粒を形成させ、
組織の少なくとも50％を粒径500Å以下の微細結晶粒と
した超微結晶磁性合金が高飽和磁束密度で高透磁率を有
するとともに耐熱性、磁気ヘッド等の磁心材として最適
であることを見出し本発明に想到した。[Means for Solving the Problems] In view of the above objects, as a result of intensive research, the present inventor has found that Fe, M, B
Is a Fe-based magnetic alloy containing M and B as essential components (M: at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W and Mn), and Crystal grains made of Fe solid solution of bcc structure from amorphous phase by heat treatment
Find out that ultra-microcrystalline magnetic alloys with at least 50% of the microcrystal grains having a grain size of 500 mm or less have high saturation magnetic flux density and high magnetic permeability, as well as heat resistance and are ideal for magnetic core materials such as magnetic heads. Invented the invention.
すなわち、本発明の超微結晶磁性合金は、 組成式： で表され、ここでＭはTi,Zr,Hf,V,Nb,Mo,Ta,Cr,W,Mnか
ら選ばれる少なくとも１種の元素であり、ＭとＢを必ず
含み、４≦ｘ≦15、２≦ｙ≦25、７≦ｘ＋ｙ≦35の関係
の組成を有する合金であって、結晶化熱処理により非晶
質相からbcc構造のFe固溶体からなる結晶粒を形成さ
せ、組織の少なくとも50％を粒径500Å以下の微細結晶
粒とした超微結晶磁性合金である。That is, the ultra-microcrystalline magnetic alloy of the present invention has a composition formula: Where M is at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, and Mn, and always includes M and B, and 4 ≦ x ≦ 15 An alloy having a composition of 2 ≦ y ≦ 25 and 7 ≦ x + y ≦ 35, wherein crystal grains formed of a bcc-structured Fe solid solution from an amorphous phase are formed by a crystallization heat treatment, and at least 50% of the structure Is a microcrystalline magnetic alloy having fine crystal grains having a particle size of 500 mm or less.
本発明において、Ｂは必須の元素であり、結晶粒の微
細化および、bccFe中に固溶し、磁歪や結晶磁気異方性
の調整に効果がある。またＢがbccFe中に固溶していな
いものも本発明に含まれる。In the present invention, B is an essential element, and has an effect on refining crystal grains and dissolving in bccFe to adjust magnetostriction and magnetocrystalline anisotropy. In addition, those in which B is not dissolved in bccFe are also included in the present invention.
Ｍは必須の元素でありTi,Zr,Hf,V,Nb,Mo,Ta,Cr,W,Mn
から選ばれる少なくとも１種の元素である。ＭはＢとの
複合添加により、結晶粒を微細化する効果を有するとと
もに、耐熱性を向上する効果を有する。M is an essential element and Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, Mn
At least one element selected from M has an effect of refining crystal grains and an effect of improving heat resistance by being added in combination with B.
Ｍ量x,B量ｙ及びＭとＢの総和ｘ＋ｙをそれぞれ４≦
ｘ≦15,2≦ｙ≦25,7≦ｘ＋ｙ≦35に限定したのは下限を
はずれると耐熱性が劣化し、一方上限をはずれると飽和
磁束密度の低下や軟磁気特性の劣化が起こるためであ
る。特に耐熱性の点で望ましい範囲は、７≦ｘ≦15,10
＜ｙ≦20,15＜ｘ＋ｙ≦30である。The M amount x, the B amount y and the sum x + y of M and B are each 4 ≦
The reason for limiting to x ≦ 15,2 ≦ y ≦ 25,7 ≦ x + y ≦ 35 is that the heat resistance is degraded if the lower limit is deviated, while the saturation magnetic flux density and the soft magnetic properties are degraded if deviated from the upper limit. is there. A particularly desirable range in terms of heat resistance is 7 ≦ x ≦ 15,10
<Y ≦ 20, 15 <x + y ≦ 30.
また、本発明はSi,Ge,P,Ga,Al,Nからなる群から選ば
れた少なくとも一種の元素（組成式ではＸで示す）、更
にAg,Au,白金族元素,Co,Ni,Sn,Be,Mg,Ca,Sr,Baからなる
群から選ばれた少なくとも一種の元素を（組成式ではＮ
で示す）適宜含有することを許容する。Further, the present invention relates to at least one element selected from the group consisting of Si, Ge, P, Ga, Al, and N (indicated by X in the composition formula), and further includes Ag, Au, a platinum group element, Co, Ni, Sn , Be, Mg, Ca, Sr, Ba at least one element selected from the group consisting of
(Shown as).
すなわち、 組成式： で表され、ここでＭはTi,Zr,Hf,V,Nb,Mo,Ta,Cr,W,Mnか
ら選ばれる少なくとも１種の元素、ＸはSi,Ge,P,Ga,Al,
Nからなる群から選ばれた少なくとも１種の元素であ
り、ＭとＢを必ず含み、４≦ｘ≦15、２≦ｙ≦25、０＜
ｚ＜４、７≦ｘ＋ｙ＋ｚ≦35の関係の組成を有する合金
であって、結晶化熱処理により非晶質相からbcc構造のF
e固溶体からなる結晶粒を形成させ、組織の少なくとも5
0％を粒径500Å以下の微細結晶粒とした超微結晶磁性合
金である。That is, the composition formula: Where M is at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, Mn, and X is Si, Ge, P, Ga, Al,
N is at least one element selected from the group consisting of N and necessarily contains M and B, 4 ≦ x ≦ 15, 2 ≦ y ≦ 25, 0 <
An alloy having a composition satisfying the relationship z <4, 7 ≦ x + y + z ≦ 35.
e Form crystal grains consisting of solid solution, and
This is a microcrystalline magnetic alloy in which 0% is made of fine crystal grains having a grain size of 500 ° or less.
また、組成式： で表され、ここでＭはTi,Zr,Hf,V,Nb,Mo,Ta,Cr,W,Mnか
ら選ばれる少なくとも１種の元素、ＮはAu,白金族元素,
Co,Sn,Be,Mg,Ca,Sr,Baからなる群から選ばれた少なくと
も１種の元素であり、ＭとＢを必ず含み、４≦ｘ≦15、
２≦ｙ≦25、０＜ａ≦10、７≦ｘ＋ｙ＋ａ≦35の関係の
組成を有する合金であって、結晶化熱処理により非晶質
相からbcc構造のFe固溶体からなる結晶粒を形成させ、
組織の少なくとも50％が粒径500Å以下の微細結晶粒と
した超微結晶磁性合金である。Also, the composition formula: Where M is at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, and Mn, N is Au, a platinum group element,
Co, Sn, Be, Mg, Ca, Sr, at least one element selected from the group consisting of Ba, always includes M and B, 4 ≦ x ≦ 15,
An alloy having a composition of 2 ≦ y ≦ 25, 0 <a ≦ 10, and 7 ≦ x + y + a ≦ 35, wherein a crystal grain comprising a bcc structure Fe solid solution is formed from an amorphous phase by a crystallization heat treatment,
It is an ultra-microcrystalline magnetic alloy in which at least 50% of the microstructure has fine grains with a grain size of 500 mm or less.
さらに、組成式： で表され、ここでＭはTi,Zr,Hf,V,Nb,Mo,Ta,Cr,W,Mnか
ら選ばれる少なくとも１種の元素、ＸはSi,Ge,P,Ga,Al,
Nからなる群から選ばれた少なくとも１種の元素、ＮはA
u,白金族元素,Co,Sn,Be,Mg,Ca,Sr,Baからなる群から選
ばれた少なくとも１種の元素であり、ＭとＢを必ず含
み、４≦ｘ≦15、２≦ｙ≦25、０＜ｚ＜４、０＜ａ≦1
0、７≦ｘ＋ｙ＋ｚ＋ａ≦35の関係の組成を有する合金
であって、結晶化熱処理により非晶質相からbcc構造のF
e固溶体からなる結晶粒を形成させ、組織の少なくとも5
0％を粒径500Å以下の微細結晶粒とした超微結晶磁性合
金、をも含む。Further, the composition formula: Where M is at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, Mn, and X is Si, Ge, P, Ga, Al,
At least one element selected from the group consisting of N;
u, a platinum group element, at least one element selected from the group consisting of Co, Sn, Be, Mg, Ca, Sr, and Ba, which always contains M and B, and 4 ≦ x ≦ 15, 2 ≦ y ≦ 25, 0 <z <4, 0 <a ≦ 1
An alloy having a composition of 0, 7 ≦ x + y + z + a ≦ 35.
e Form crystal grains consisting of solid solution, and
Ultrafine crystal magnetic alloys in which 0% is fine crystal grains having a grain size of 500 ° or less.
ここで、Si,Ge,P,Ga,Al,Nからなる群から選ばれた少
なくとも一種の元素（本願明細書中ではＸと総称する）
は磁歪の調整、および結晶磁気異方性の調整に効果があ
り、10％以下の範囲で含有される。それは、10％を越え
ると磁気特性の劣化が著しくなるからである。Here, at least one element selected from the group consisting of Si, Ge, P, Ga, Al, and N (collectively referred to as X in the present specification)
Is effective in adjusting magnetostriction and crystal magnetic anisotropy, and is contained in an amount of 10% or less. This is because if it exceeds 10%, the magnetic characteristics will be significantly deteriorated.
また、Au,白金族元素,Co,Ni,Sn,Be,Mg,Ca,Sr,Baから
なる群から選ばれた少なくとも一種の元素（本願明細書
中ではＮと総称する）は、耐食性の改善、および磁気特
性の調整に効果があり、10％以下の範囲で含有される。
それは、10％を越えると著しい飽和磁束密度の低下をも
たらすからである。In addition, at least one element selected from the group consisting of Au, a platinum group element, Co, Ni, Sn, Be, Mg, Ca, Sr, and Ba (collectively referred to as N in the present specification) improves corrosion resistance. , And the effect of adjusting magnetic properties, and is contained in a range of 10% or less.
This is because exceeding 10% results in a significant decrease in the saturation magnetic flux density.
本発明合金は500Å以下の著しく微細な結晶粒組織を
有しており、特に優れた軟磁性は粒径が200Å以下の場
合に得られる。The alloy of the present invention has an extremely fine grain structure of 500 ° or less, and particularly excellent soft magnetism is obtained when the grain size is 200 ° or less.
このような微細な結晶粒組織を組織全体に対して50％
以上存在することとするのは、これ未満では優れた軟磁
気特性が得られないからである。50% of such fine grain structure to the whole structure
The reason for the existence is as follows, if less than this, excellent soft magnetic properties cannot be obtained.
なお、本発明合金は通常非晶質合金を作製後これを熱
処理し、結晶化することにより製造される。熱処理条件
により一部非晶質相が残存している場合があるが、この
場合でも微細な結晶粒組織が組織全体に対して50％以上
存在しておれば十分な軟磁気特性が得られる。また、10
0％結晶の場合ももちろん優れた軟磁気特性が得られ
る。The alloy of the present invention is usually produced by preparing an amorphous alloy, heat treating it, and crystallizing it. Depending on the heat treatment conditions, a part of the amorphous phase may remain, but even in this case, sufficient soft magnetic characteristics can be obtained if a fine crystal grain structure is present in 50% or more of the entire structure. Also, 10
Even in the case of 0% crystal, excellent soft magnetic characteristics can be obtained.
本発明においてＭとＢは熱処理により超微細で均一な
bccFe結晶粒を形成し、その成長を抑える効果を有す
る。このため、bccFeの結晶磁気異方性を見かけ上相殺
し優れた軟磁気特性が得られると考えられる。In the present invention, M and B are ultrafine and uniform by heat treatment.
It has the effect of forming bccFe crystal grains and suppressing their growth. For this reason, it is considered that the crystal magnetic anisotropy of bccFe is apparently canceled out and excellent soft magnetic characteristics can be obtained.
もう一つの本発明は、前記組成の非晶質合金を製造す
る工程と、この非晶質合金を少なくとも50％が粒径500
Å以下のbccFe固溶体からなる組織とする結晶化熱処理
を施す工程とからなることを特徴とする前記超微結晶磁
性合金の製造方法である。ここにbccFe固溶体とは、体
心立方（bcc）の結晶構造を有する鉄（Fe）に他の元素
が固溶したものであることを言うが、右の他の元素が全
く固溶していない場合も含むものである。Another aspect of the present invention is a process for producing an amorphous alloy having the above-described composition, wherein at least 50% of the amorphous alloy has a particle size of 500%.
(C) performing a crystallization heat treatment to form a structure comprising a bccFe solid solution as described below. Here, the bccFe solid solution means that other elements are dissolved in iron (Fe) having a body-centered cubic (bcc) crystal structure, but the other elements on the right are not dissolved at all. The case is also included.
非晶質合金は通常、単ロール法や双ロール法等の液体
急冷法や、スパッタ法や蒸着法等の気相急冷法等により
製造する。この後不活性ガス、水素中あるいは真空中で
熱処理し結晶化させ、組織の少なくとも50％が粒径500
Å以下の結晶粒からなり、かつ前記結晶がbcc構造の結
晶主体である組織とすることにより前記合金を製造す
る。An amorphous alloy is usually produced by a liquid quenching method such as a single roll method or a twin roll method, or a gas phase quenching method such as a sputtering method or a vapor deposition method. This is followed by heat treatment in an inert gas, hydrogen or vacuum to crystallize and at least 50% of the structure has a particle size of 500
合金 The alloy is manufactured by forming a structure composed of the following crystal grains and having the crystal mainly composed of a bcc structure crystal.
本発明における結晶化のための熱処理は450℃以上800
℃以下の温度範囲で行なわれるのが望ましい。それは、
450℃未満では熱処理時間を長くしても結晶化が困難で
あり、一方800℃を越えると結晶粒の成長が必要以上に
進行して所望の超微細結晶組織を得ることができなくな
るからである。具体的熱処理温度、時間は合金組成等に
よって定められる。Heat treatment for crystallization in the present invention is 450 ° C. or more and 800
It is desirable to carry out the reaction in a temperature range of not more than ° C. that is,
If the heat treatment time is longer than 450 ° C., crystallization is difficult even if the heat treatment time is prolonged.On the other hand, if it exceeds 800 ° C., the growth of crystal grains proceeds more than necessary and it becomes impossible to obtain a desired ultrafine crystal structure. . The specific heat treatment temperature and time are determined by the alloy composition and the like.
本発明合金は、以上のように450℃以上800℃以下とい
う高い温度の熱処理を経るものであるため、磁気ヘッド
等を作製する場合、ガラスボンディングが容易で信頼性
の高い磁気ヘッドを製造できる長所がある。Since the alloy of the present invention undergoes a high-temperature heat treatment of 450 ° C. or more and 800 ° C. or less as described above, when manufacturing a magnetic head or the like, there is an advantage that a glass head can be easily manufactured and a highly reliable magnetic head can be manufactured. There is.
また、本発明合金は磁場中で熱処理し製造することも
可能である。一定方向に磁場を印加した場合は、一軸の
誘導磁気異方性を生じさせることができる。また、回転
磁場中熱処理を行うことにより更に軟磁気特性を改善す
ることができる。結晶化熱処理後に磁場中熱処理するこ
とも可能である。Further, the alloy of the present invention can be produced by heat treatment in a magnetic field. When a magnetic field is applied in a certain direction, uniaxial induced magnetic anisotropy can be generated. Further, the soft magnetic properties can be further improved by performing the heat treatment in a rotating magnetic field. It is also possible to perform a heat treatment in a magnetic field after the crystallization heat treatment.
［実施例］ 以下本発明を実施例に従って説明するが、本発明はこ
れらに限定されるものではない。[Examples] Hereinafter, the present invention will be described with reference to Examples, but the present invention is not limited thereto.
実施例１ 原子％でNb7％,B18％、残部Feからなる組成の厚さ18
μｍの非晶質合金薄帯を単ロール法により作製した。得
られた薄帯のＸ線回折を行ったところ、第１図（ａ）に
示すように非晶質合金に特有なハローパターンを示し
た。Example 1 Thickness of a composition consisting of 7% Nb and 18% B in atomic% and the balance being Fe
A μm amorphous alloy ribbon was produced by a single roll method. When the obtained ribbon was subjected to X-ray diffraction, a halo pattern peculiar to the amorphous alloy was exhibited as shown in FIG. 1 (a).
次に、この非晶質合金薄帯を窒素ガス雰囲気中におい
て、600℃で１時間保持後室温まで冷却し、Ｘ線回折を
行った。第１図（ａ）に示すような半値幅の広いbccFe
固溶体の結晶ピークが主に認められた。なお、NbとＢの
化合物が形成されている可能性があるが、本観察では確
認できなかった。Next, the amorphous alloy ribbon was kept at 600 ° C. for 1 hour in a nitrogen gas atmosphere, cooled to room temperature, and subjected to X-ray diffraction. BccFe with a wide half width as shown in Fig. 1 (a)
A crystal peak of a solid solution was mainly observed. In addition, although the compound of Nb and B may be formed, it could not be confirmed by this observation.
透過電子顕微鏡による組織観察の結果、組織のほとん
どが粒径100Å以下の超微細な結晶粒からなることが確
認された。As a result of observation of the structure with a transmission electron microscope, it was confirmed that most of the structure was composed of ultrafine crystal grains having a grain size of 100 mm or less.
なお、本発明においては、微細結晶粒の割合は線分法
によって求める。この線分法は一般的な方法であり、組
織写真中に引かれた任意の線分（長さＬ）が横切る各結
晶粒の長さ（L1,L2,L3・・・Ln）の合計（L1＋L2＋L3＋
・・・Ln）を求め、これをＬで割ることにより、結晶粒
の割合を求めるものである。In the present invention, the ratio of fine crystal grains is determined by a line segment method. This line segment method is a general method, and the length of each crystal grain (L 1 , L 2 , L 3 ... Ln) crossed by an arbitrary line segment (length L) drawn in the structure photograph Sum of (L 1 + L 2 + L 3 +
.., Ln), and dividing this by L to determine the ratio of crystal grains.
なお、結晶粒の割合が多くなると組織写真上は結晶粒
がほぼ組織全体を占めるように見えるが、この場合でも
いくぶん非晶質相が存在するものと考えられる。という
のは、結晶粒の外周部が組織写真ではぼやけており、こ
れは非晶質相の存在による為であると考えられるからで
ある。このように結晶粒の割合が多い場合、割合を正確
な数値で表すことは困難であり、本実施例で「ほとん
ど」という表現を用いたのは、このような理由による。It should be noted that when the proportion of crystal grains increases, the crystal grains appear to occupy almost the entire structure on the structure photograph, but even in this case, it is considered that there is some amorphous phase. This is because the outer periphery of the crystal grain is blurred in the structure photograph, which is considered to be due to the presence of the amorphous phase. When the ratio of crystal grains is large as described above, it is difficult to express the ratio with an accurate numerical value, and the expression “almost” is used in the present embodiment for such a reason.
次にこの組成の非晶質合金からなるトロイダル磁心を
熱処理温度を変え熱処理し、直流ヒステリシスカーブを
直流Ｂ−Ｈトレーサ、1kHzにおける実行透磁率μe1kをL
CRメータにより測定した。熱処理時間は１時間、熱処理
雰囲気は窒素ガス雰囲気とした。得られた結果を第２図
（ａ）、第２図（ｂ）に示す。また、第３図に直流ヒス
テリシスカーブを示しておく。Next, a toroidal core made of an amorphous alloy having this composition was subjected to a heat treatment at a different heat treatment temperature, the DC hysteresis curve was changed to a DC BH tracer, and the effective permeability μe1k at 1 kHz was changed to L.
It was measured with a CR meter. The heat treatment time was 1 hour, and the heat treatment atmosphere was a nitrogen gas atmosphere. The obtained results are shown in FIGS. 2 (a) and 2 (b). FIG. 3 shows a DC hysteresis curve.
bccFe相が生成する結晶化温度より高い温度のｋ熱処
理条件において高飽和磁束密度で高透磁率が得られるこ
とがわかる。It can be seen that a high magnetic permeability with a high saturation magnetic flux density can be obtained under the k heat treatment condition at a temperature higher than the crystallization temperature at which the bccFe phase is generated.
このように本発明合金は、非晶質合金を結晶化させる
ことにより得られる。また、磁歪も非晶質状態よりも著
しく小さくなり軟磁性材料としてより好ましい特徴もあ
ることが確認された。Thus, the alloy of the present invention can be obtained by crystallizing an amorphous alloy. In addition, the magnetostriction was significantly smaller than that in the amorphous state, and it was confirmed that the soft magnetic material also had some characteristics.
本発明合金はFe−Si−Al合金以上の高飽和磁束密度を
有しており、μe1kも10000を超える場合もあり、高磁束
密度記録用の磁気ヘッド材やチョーク磁心、高周波トラ
ンス、センサ材等に好適である。The alloy of the present invention has a high saturation magnetic flux density higher than that of the Fe-Si-Al alloy, and the μe1k may exceed 10,000, so that a magnetic head material for high magnetic flux density recording, a choke core, a high-frequency transformer, a sensor material, etc. It is suitable for.
実施例２ 第１表に示す組成の幅5mm、厚さ15μｍの合金薄帯を
実施例１と同様な方法で作成し、直流Ｂ−Ｈトレーサに
よりB10、Hc、LCRメータにより1kHzの実効透磁率μe1
k、Ｕ函数計により100kHz、0.2Tの磁心損失Pcを測定し
た。得られた結果を第１表に示す。なお、熱処理後の合
金はいずれも粒径500Å以下の微細なbcc構造の結晶粒が
主体の組織であった。なお、第４図に第１表のNo.1合金
の直流ヒステリシスカーブを示しておく。5mm wide of the composition shown in Example 2 in Table 1, the alloy ribbon having a thickness of 15μm was prepared in the same manner as in Example 1, the DC B-H tracer B 10, Hc, 1 kHz of effective magnetic with a LCR meter Magnetic susceptibility μe1
The core loss Pc at 100 kHz and 0.2 T was measured by a k and U function meter. Table 1 shows the obtained results. Each of the alloys after the heat treatment had a structure mainly composed of crystal grains having a fine bcc structure with a particle diameter of 500 mm or less. FIG. 4 shows the DC hysteresis curve of the No. 1 alloy in Table 1.
本発明合金は、Fe−Si−Al合金やCo基アモルファス合
金と同等以上の高飽和磁束密度を有しており、飽和磁束
密度が16kGを越えるものも得られ、μe1kもFe−Si合金
等より高いため特に磁気ヘッド用合金に好適である。The alloy of the present invention has a high saturation magnetic flux density equal to or higher than that of a Fe-Si-Al alloy or a Co-based amorphous alloy, and one having a saturation magnetic flux density exceeding 16 kG is obtained. Since it is high, it is particularly suitable for alloys for magnetic heads.
実施例３ 第２表に示す組成の幅5mm厚さ15μｍの非晶質合金薄
帯を単ロール法により作製した。次のこの合金薄帯を外
径19mm、内径15mmに巻回しトロイダル磁心を作製した。
次にこの磁心をArガス雰囲気中で550℃〜700℃の範囲で
熱処理し結晶化させた。熱処理後の合金はＸ線回折及び
透過電子顕微鏡による組織観察の結果粒径500Å以下のb
cc構造の結晶主体であることが確認された。 Example 3 An amorphous alloy ribbon having a composition shown in Table 2 and a width of 5 mm and a thickness of 15 μm was produced by a single roll method. Next, this alloy ribbon was wound around an outer diameter of 19 mm and an inner diameter of 15 mm to produce a toroidal magnetic core.
Next, this magnetic core was crystallized by heat treatment in an Ar gas atmosphere at a temperature in the range of 550 ° C to 700 ° C. The alloy after heat treatment was analyzed by X-ray diffraction and transmission electron microscopy to find the b
It was confirmed that the crystal was mainly composed of a cc structure.
次にこの合金薄帯からなるトロイダル磁心を作成し、
1kHzにおける実行透示率μe1kを測定し、次に600℃30mi
n保持後室温まで冷却し1kHzにおける実効透磁率μe1k30
を測定した。μe1k30/μe1kを第２表に併せて示す。Next, create a toroidal core made of this alloy ribbon,
Measure the running permeability μe1k at 1 kHz, then at 600 ° C for 30 mi
After maintaining n, cool down to room temperature, and effective permeability at 1 kHz μe1k 30
Was measured. μe1k 30 / μe1k is also shown in Table 2.
本発明合金は、従来材に比べμe1k30/μe1kが大きく6
00℃という高い温度でも磁気特性の劣化の小さい耐熱性
に優れた特性を有することが判る。このため、ガラスボ
ンディングが必要な磁気ヘッド材、高い温度で使用する
センサ材等各種磁心材に最適である。The alloy of the present invention has a large μe1k 30 / μe1k compared to the conventional material.
It can be seen that even at a temperature as high as 00 ° C., the magnetic properties are excellent in heat resistance with little deterioration in magnetic properties. Therefore, it is optimal for various magnetic core materials such as a magnetic head material requiring glass bonding and a sensor material used at a high temperature.
また本発明合金においては、Ｂ量が高い方がμe1k30/
μe1kが高い傾向にあり望ましい。Further, in the alloy of the present invention, the higher the amount of B, the more μe1k 30 /
μe1k tends to be high and is desirable.
さらに比較例として示したようにＭ元素の量が本発明
の範囲より少ないとμe1k30/μe1kが低く耐熱性の点で
著しく劣る。Further, as shown as a comparative example, when the amount of the M element is smaller than the range of the present invention, μe1k 30 / μe1k is low and heat resistance is remarkably inferior.
実施例４ 第３表に示す組成の合金膜をスパッタ法によりホトセ
ラム基板上に作製し550〜700℃の範囲で熱処理を行い結
晶化させ、μe1M0を測定した。熱処理後の合金はＸ線回
折及び透過電子顕微鏡による組織観察の結果粒径、500
Å以下のbcc構造の結晶主体であることが確認された。 Example 4 An alloy film having a composition shown in Table 3 was crystallized by heat treatment in the range of fabricated Hotoseramu substrate 550 to 700 ° C. by sputtering, was measured μe1M 0. The alloy after heat treatment had a particle size of 500 as a result of microstructure observation by X-ray diffraction and transmission electron microscopy.
(4) It was confirmed that the crystal was mainly composed of the following bcc structure.
次にこの合金を550℃の炉に装入し、１時間保持後の
μe1m1を測定した。μe1M1/μe1M0を第３表に示す。Next was charged with this alloy in a furnace of 550 ° C., was measured Myui1m 1 after 1 hour holding. The μe1M 1 / μe1M 0 shown in Table 3.
本発明合金膜のμe1M1/μe1M0は比較材等に比べ１に
近い値であり、高温での磁気特性の劣化が小さく耐熱性
に優れる。このため信頼性の高い磁気ヘッドを製造でき
る。Μe1M 1 / μe1M 0 of the present invention the alloy film is a value close to 1 as compared to the comparative material, etc., deterioration of the magnetic properties at high temperatures is excellent small heat resistance. Therefore, a highly reliable magnetic head can be manufactured.
［発明の効果］ 本発明によれば、高飽和磁束密度、高透磁率で且つ耐
熱性に優れた超微細結晶合金を提供できるためその効果
は著しいものがある。 [Effects of the Invention] According to the present invention, an ultrafine crystal alloy having a high saturation magnetic flux density, a high magnetic permeability, and excellent heat resistance can be provided.
【図面の簡単な説明】 第１図（ａ）は本発明に係る熱処理前の非晶質合金のＸ
線回折パターン、第１図（ｂ）は本発明合金のＸ線回折
パターン、第２図は本発明合金の磁気特性の熱処理温度
異存性を示すグラフ、第３図及び第４図は本発明合金の
直流ヒステリシスカーブである。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 (a) shows an X-ray of an amorphous alloy before heat treatment according to the present invention.
1B is an X-ray diffraction pattern of the alloy of the present invention, FIG. 2 is a graph showing the heat treatment temperature dependence of the magnetic properties of the alloy of the present invention, and FIGS. 3 and 4 are alloys of the present invention. 5 is a DC hysteresis curve.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 西山 俊一 埼玉県熊谷市三ケ尻5200番地 日立金属 株式会社磁性材料研究所内 審査官 小柳 健悟 (56)参考文献 特開 平１−242756（ＪＰ，Ａ) 特開 平１−156452（ＪＰ，Ａ) 特開 昭64−28343（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C22C 45/02 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Shunichi Nishiyama 5200 Mikajiri, Kumagaya-shi, Saitama Examiner, Magnetic Materials Research Laboratory, Hitachi Metals, Ltd. Kengo Koyanagi (56) Reference JP-A-1-242756 (JP, A) JP-A-1-156452 (JP, A) JP-A-64-28343 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C22C 45/02
Claims (6)
ら選ばれる少なくとも１種の元素であり、ＭとＢを必ず
含み、４≦ｘ≦15、２≦ｙ≦25、７≦ｘ＋ｙ≦35の関係
の組成を有する合金であって、結晶化熱処理により非晶
質相からbcc構造のFe固溶体からなる結晶粒を形成さ
せ、組織の少なくとも50％が粒径500Å以下の微細結晶
粒からなることを特徴とする超微結晶磁性合金。1. Composition formula: Where M is at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, and Mn, and always includes M and B, and 4 ≦ x ≦ 15 An alloy having a composition of 2 ≦ y ≦ 25 and 7 ≦ x + y ≦ 35, wherein crystal grains formed of a bcc-structured Fe solid solution from an amorphous phase are formed by a crystallization heat treatment, and at least 50% of the structure Is a microcrystalline magnetic alloy characterized by comprising fine crystal grains having a particle size of 500 mm or less.
ら得らばれる少なくとも１種の元素、ＸはSi,Ge,P,Ga,A
l,Nからなる群から選ばれた少なくとも１種の元素であ
り、ＭとＢを必ず含み、４≦ｘ≦15、２≦ｙ≦25、０＜
ｚ＜４、７≦ｘ＋ｙ＋ｚ≦35の関係の組成を有する合金
であって、結晶化熱処理により非晶質相からbcc構造のF
e固溶体からなる結晶粒を形成させ、組織の少なくとも5
0％が粒径500Å以下の微細結晶粒からなることを特徴と
する超微結晶磁性合金。2. Composition formula: Where M is at least one element obtained from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, Mn, and X is Si, Ge, P, Ga, A
at least one element selected from the group consisting of l and N, which always contains M and B, 4 ≦ x ≦ 15, 2 ≦ y ≦ 25, 0 <
An alloy having a composition satisfying the relationship z <4, 7 ≦ x + y + z ≦ 35.
e Form crystal grains consisting of solid solution, and
An ultra-microcrystalline magnetic alloy characterized in that 0% is composed of fine crystal grains having a grain size of 500 mm or less.
ら選ばれる少なくとも１種の元素、ＮはAu,白金族元素,
Co,Sn,Be,Mg,CA,Sr,Baからなる群から選ばれた少なくと
も１種の元素であり、ＭとＢを必ず含み、４≦ｘ≦15、
２≦ｙ≦25、０＜ａ≦10、７≦ｘ＋ｙ＋ａ≦35の関係の
組成を有する合金であって、結晶化熱処理により非晶質
相からbcc構造のFe固溶体からなる結晶粒を形成させ、
組織の少なくとも50％が粒径500Å以下の微細結晶粒か
らなることを特徴とする超微結晶磁性合金。3. Composition formula: Where M is at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, and Mn, N is Au, a platinum group element,
Co, Sn, Be, Mg, CA, Sr, at least one element selected from the group consisting of Ba, always includes M and B, 4 ≦ x ≦ 15,
An alloy having a composition of 2 ≦ y ≦ 25, 0 <a ≦ 10, and 7 ≦ x + y + a ≦ 35, wherein a crystal grain comprising a bcc structure Fe solid solution is formed from an amorphous phase by a crystallization heat treatment,
An ultra-microcrystalline magnetic alloy characterized in that at least 50% of the structure is composed of fine crystal grains having a grain size of 500 mm or less.
ら選ばれる少なくとも１種の元素、ＸはSi,Ge,P,Ga,Al,
Nからなる群から選ばれた少なくとも１種の元素、ＮはA
u,白金族元素、Co,Sn,Be,Mg,Ca,Sr,Baからなる群から選
ばれた少なくとも１種の元素であり、ＭとＢを必ず含
み、４≦ｘ≦15、２≦ｙ≦25、０＜ｘ＜４、０＜ａ≦1
0、７≦ｘ＋ｙ＋ｚ＋ａ≦35の関係の組成を有する合金
であって、結晶化熱処理により非晶質相からbcc構造のF
e固溶体からなる結晶粒を形成させ、組織の少なくとも5
0％が粒径500Å以下の微細結晶粒からなることを特徴と
する超微結晶磁性合金。4. Composition formula Where M is at least one element selected from Ti, Zr, Hf, V, Nb, Mo, Ta, Cr, W, Mn, and X is Si, Ge, P, Ga, Al,
At least one element selected from the group consisting of N;
u, a platinum group element, at least one element selected from the group consisting of Co, Sn, Be, Mg, Ca, Sr, and Ba, which always contains M and B, and 4 ≦ x ≦ 15, 2 ≦ y ≦ 25, 0 <x <4, 0 <a ≦ 1
An alloy having a composition of 0, 7 ≦ x + y + z + a ≦ 35.
e Form crystal grains consisting of solid solution, and
An ultra-microcrystalline magnetic alloy characterized in that 0% is composed of fine crystal grains having a grain size of 500 mm or less.
１乃至４の何れかに記載の超微結晶磁性合金。5. The microcrystalline magnetic alloy according to claim 1, wherein 10 ≦ y ≦ 20.
を特徴とする請求項１乃至５の何れかに記載の超微結晶
磁性合金。6. An ultra-microcrystalline magnetic alloy according to claim 1, comprising fine crystal grains having a grain size of 200 ° or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2316551A JP3058675B2 (en) | 1989-11-22 | 1990-11-21 | Ultra-microcrystalline magnetic alloy |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30361789 | 1989-11-22 | ||
| JP1-303617 | 1989-11-22 | ||
| JP2316551A JP3058675B2 (en) | 1989-11-22 | 1990-11-21 | Ultra-microcrystalline magnetic alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03219058A JPH03219058A (en) | 1991-09-26 |
| JP3058675B2 true JP3058675B2 (en) | 2000-07-04 |
Family
ID=26563573
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2316551A Expired - Lifetime JP3058675B2 (en) | 1989-11-22 | 1990-11-21 | Ultra-microcrystalline magnetic alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3058675B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100838733B1 (en) * | 2006-12-20 | 2008-06-17 | 주식회사 포스코 | Fe-based bulk amorphous alloys with optimum cr/mo composition |
| KR100838732B1 (en) * | 2006-12-20 | 2008-06-17 | 주식회사 포스코 | Fe-based bulk amorphous alloys with high glass forming ability |
| JP2019186327A (en) * | 2018-04-05 | 2019-10-24 | パナソニックＩｐマネジメント株式会社 | Magnetostrictive material and magnetostrictive type device arranged by use thereof |
-
1990
- 1990-11-21 JP JP2316551A patent/JP3058675B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03219058A (en) | 1991-09-26 |
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