JP2001094175A - High electrical resistivity magnetoresistive film - Google Patents
High electrical resistivity magnetoresistive filmInfo
- Publication number
- JP2001094175A JP2001094175A JP30744199A JP30744199A JP2001094175A JP 2001094175 A JP2001094175 A JP 2001094175A JP 30744199 A JP30744199 A JP 30744199A JP 30744199 A JP30744199 A JP 30744199A JP 2001094175 A JP2001094175 A JP 2001094175A
- Authority
- JP
- Japan
- Prior art keywords
- electric resistivity
- magnetoresistive film
- film
- high electric
- magnetic
- 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.)
- Granted
Links
- 239000010408 film Substances 0.000 claims abstract description 73
- 230000005291 magnetic effect Effects 0.000 claims abstract description 42
- 239000010409 thin film Substances 0.000 claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 14
- 239000000956 alloy Substances 0.000 claims abstract description 14
- 239000008187 granular material Substances 0.000 claims abstract description 13
- 239000011159 matrix material Substances 0.000 claims abstract description 13
- 239000012212 insulator Substances 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910001260 Pt alloy Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910001291 heusler alloy Inorganic materials 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUBSQCSIIDQXLB-UHFFFAOYSA-N cobalt platinum Chemical compound [Co].[Pt].[Pt].[Pt] GUBSQCSIIDQXLB-UHFFFAOYSA-N 0.000 claims description 3
- 239000003302 ferromagnetic material Substances 0.000 claims description 3
- OBACEDMBGYVZMP-UHFFFAOYSA-N iron platinum Chemical compound [Fe].[Fe].[Pt] OBACEDMBGYVZMP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 229910000531 Co alloy Inorganic materials 0.000 claims description 2
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052790 beryllium Inorganic materials 0.000 claims description 2
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 8
- 230000005415 magnetization Effects 0.000 description 8
- 238000004544 sputter deposition Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229910002546 FeCo Inorganic materials 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- SORXVYYPMXPIFD-UHFFFAOYSA-N iron palladium Chemical compound [Fe].[Pd] SORXVYYPMXPIFD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000889 permalloy Inorganic materials 0.000 description 2
- 238000001552 radio frequency sputter deposition Methods 0.000 description 2
- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018979 CoPt Inorganic materials 0.000 description 1
- -1 Fe Ni Inorganic materials 0.000 description 1
- 229910015187 FePd Inorganic materials 0.000 description 1
- 229910005335 FePt Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000010549 co-Evaporation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Landscapes
- Measuring Magnetic Variables (AREA)
- Hall/Mr Elements (AREA)
Abstract
(57)【要約】
【目的】本発明は、室温においてＭＲ比の値が３％以上
の大きな磁気抵抗効果を示し、１０５μΩｃｍ以上の電
気比抵抗を有する高電気比抵抗磁気抵抗膜を提供するこ
とを目的とする。
【構成】 フッ化物からなる絶縁物マトリックスにナノ
メーターサイズの磁性グラニュールが分散したナノグラ
ニュラー合金薄膜であることを特徴とし、室温で３％以
上の磁気抵抗比を示し１０５μΩｃｍ以上の電気比抵抗
を有する高電気比抵抗磁気抵抗膜。
(57) Abstract: An object of the present invention shows a large magnetoresistance effect of the value is more than 3% MR ratio at room temperature, provides a high electrical resistivity magnetoresistive film having 10 5 .mu..OMEGA.cm more electrical resistivity The purpose is to do. [Configuration] Magnetic granules nanometer sized insulator matrix of fluoride is characterized by a nano granular alloy thin film dispersed at room temperature showed a more than 3% magnetoresistance ratio 10 5 .mu..OMEGA.cm more electrical resistivity A high electric resistivity magnetoresistive film having:
Description
【０００１】[0001]
【産業上の利用分野】本発明は、絶縁物マトリックスに
ナノメーターサイズの磁性グラニュールが分散したナノ
グラニュラー合金薄膜において、絶縁物マトリックスが
フッ化物からなることを特徴とし、室温で３％以上の磁
気抵抗比を示し、且つ１０５μΩｃｍ以上の電気比抵抗
を有する高電気比抵抗磁気抵抗膜に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a nanogranular alloy thin film in which nanometer-sized magnetic granules are dispersed in an insulating matrix, wherein the insulating matrix is made of fluoride and has a magnetic property of 3% or more at room temperature. The present invention relates to a high electric resistivity magnetoresistive film having a resistivity and an electric resistivity of 10 5 μΩcm or more.
【０００２】[0002]
【従来の技術】種々の磁界検出のために、ホール素子や
磁気抵抗（ＭＲ）素子が用いられている。これらの磁界
センサーは、サーボモーター，ステッピングモーター，
ロータリーエンコーダーあるいは水道流量計などの回転
磁界センサとしても広く利用されている。また、磁気記
録の分野では記録密度の高密度化を実現するために、異
方的磁気抵抗効果（ＡＭＲ）を利用した読み出し用ヘッ
ドや、金属人工格子の巨大磁気抵抗効果（ＧＭＲ）を利
用したスピンバルブヘッドが用いられている。2. Description of the Related Art Hall elements and magnetoresistive (MR) elements are used for detecting various magnetic fields. These magnetic field sensors consist of servo motors, stepper motors,
It is also widely used as a rotating magnetic field sensor such as a rotary encoder or a water flow meter. In the field of magnetic recording, a read head using an anisotropic magnetoresistive effect (AMR) and a giant magnetoresistive effect (GMR) of a metal artificial lattice are used to realize a higher recording density. A spin valve head is used.
【０００３】電池を電源とする磁界センサーは、電池の
消耗を避けるために、なるべく小さな電流で駆動する必
要がある。しかし、ホール素子は、素子に流す電流値に
比例して感度が大きくなるので、小さな電流では十分な
感度は得られない。一方、パーマロイなどのＡＭＲ材料
や金属人工格子は電気比抵抗が小さく、電池の供給する
電圧に対し大きな電流が流れてしまうので、電池の消耗
が早い。電池の長寿命化のためには、素子の電気抵抗を
上げて電流値を抑える必要があり、極めて精度よく微細
パターンに加工するなどの工夫が必要となっている。A magnetic field sensor using a battery as a power source needs to be driven with a current as small as possible in order to avoid battery consumption. However, since the sensitivity of the Hall element increases in proportion to the value of the current flowing through the element, sufficient sensitivity cannot be obtained with a small current. On the other hand, an AMR material such as permalloy or a metal artificial lattice has a small electric resistivity and a large current flows with respect to the voltage supplied by the battery, so that the battery is quickly consumed. In order to prolong the life of the battery, it is necessary to increase the electric resistance of the element to suppress the current value, and it is necessary to devise an extremely accurate processing into a fine pattern.
【０００４】[0004]
【発明が解決しようとする課題】電池を電源とする省電
力型の磁気センサでは、大きな電流値でなければ出力の
得られないホール素子は、用いることはできない。この
ため、ＭＲ材料が用いられているが、電気比抵抗が小さ
いために、微細パターンに加工するなどの工程が必要と
なる。ＭＲ材料の電気比抵抗が大きければ、素子に流す
電流は少なくなり、電池の消耗が押さえられる。また、
微細加工の必要も無くなり、磁気センサーの製造工程が
大幅に簡略化されることが考えられる。そこで、本発明
者らは、大きな電気比抵抗を有し、なお且つ大きなＭＲ
比を有する材料を得ようとするものである。In a power-saving magnetic sensor using a battery as a power source, a Hall element which cannot obtain an output unless it has a large current value cannot be used. For this reason, although an MR material is used, a process such as processing into a fine pattern is required because the electric resistivity is low. If the electrical resistivity of the MR material is large, the current flowing through the element decreases, and the consumption of the battery is suppressed. Also,
It is considered that the need for fine processing is eliminated, and the manufacturing process of the magnetic sensor is greatly simplified. Then, the present inventors have a large electric resistivity and a large MR.
It is intended to obtain a material having a specific ratio.
【０００５】本発明は上記の事情を鑑みてなされたもの
で、大きな電気比抵抗を有し、且つ大きなＭＲ比を有す
る、磁気抵抗薄膜材料を提供することを目的とする。The present invention has been made in view of the above circumstances, and has as its object to provide a magnetoresistive thin film material having a large electric resistivity and a large MR ratio.
【０００６】[0006]
【課題を解決するための手段】本発明は、上記の事情を
鑑みて鋭意努力した結果であり、絶縁物マトリックスに
ナノメーターサイズの磁性グラニュールが分散したナノ
グラニュラー合金薄膜において、絶縁物マトリックスが
フッ化物からなることを特徴とする材料で、室温で３％
以上の磁気抵抗比を示し、且つ１０５μΩｃｍ以上の電
気比抵抗を有することを見出した。これらの薄膜はスパ
ッタ法によって作製されるが、例えばＲＦスパッタ成膜
装置を用い、純Ｆｅ、純Ｃｏあるいは合金円板上にフッ
化物等のチップを均等に配置した複合ターゲットを用い
て行なうか、あるいは金属ターゲットとフッ化物ターゲ
ットを同時にスパッタして行う。また、基板温度を１０
０〜８００℃の範囲の適当な温度に保ちながら成膜する
か、あるいは成膜後１００〜８００℃の範囲の適当な温
度で熱処理することにより、ＭＲ特性を改善することが
出来る。SUMMARY OF THE INVENTION The present invention has been made as a result of intensive efforts in view of the above-mentioned circumstances, and the present invention relates to a nanogranular alloy thin film in which nanometer-sized magnetic granules are dispersed in an insulating matrix. 3% at room temperature
Shows a magnetoresistance ratio of above, found that and having a 10 5 .mu..OMEGA.cm more electrical resistivity. These thin films are produced by a sputtering method. For example, using an RF sputtering film forming apparatus, using a composite target in which chips such as fluorides are evenly arranged on pure Fe, pure Co or an alloy disk, or Alternatively, the sputtering is performed by simultaneously sputtering a metal target and a fluoride target. Also, when the substrate temperature is 10
The MR characteristics can be improved by forming a film while maintaining a suitable temperature in the range of 0 to 800 ° C., or by performing a heat treatment at a suitable temperature in the range of 100 to 800 ° C. after the film formation.
【０００７】本発明の特徴とするところは次の通りであ
る。第１発明は、絶縁物マトリックスに、ナノメーター
サイズの磁性グラニュールが分散したナノグラニュラー
合金薄膜において、絶縁物マトリックスが、ベリリウ
ム，マグネシウム，アルミニウム，カルシウムあるいは
バリウムから選ばれる１種または２種以上の元素のフッ
化物と不可避の不純物からなり、磁性グラニュールが
鉄，コバルトあるいは鉄とコバルトとの合金と不可避の
不純物からなることを特徴とし、室温で３％以上の磁気
抵抗比を示し、且つ１０５μΩｃｍ以上の電気比抵抗を
有する高電気比抵抗磁気抵抗膜に関する。The features of the present invention are as follows. A first invention is a nanogranular alloy thin film in which nanometer-sized magnetic granules are dispersed in an insulator matrix, wherein the insulator matrix is one or more elements selected from beryllium, magnesium, aluminum, calcium, and barium. Characterized in that the magnetic granules are composed of iron, cobalt or an alloy of iron and cobalt and inevitable impurities, exhibit a magnetoresistance ratio of 3% or more at room temperature, and 10 5 The present invention relates to a high electric resistivity magnetoresistive film having an electric resistivity of μΩcm or more.
【０００８】第２発明は、磁性グラニュールが、分極率
の大きな鉄−パラジウム合金，鉄−白金合金，コバルト
−白金合金、またはホイスラー合金からなることを特徴
とする請求項１に記載の高電気比抵抗磁気抵抗膜に関す
る。According to a second aspect of the present invention, the magnetic granule is made of an iron-palladium alloy, an iron-platinum alloy, a cobalt-platinum alloy, or a Heusler alloy having high polarizability. The present invention relates to a specific resistance magnetoresistive film.
【０００９】第３発明は、絶縁物マトリックスが、結晶
相であることを特徴とする、請求項１または請求項２に
記載の高電気比抵抗磁気抵抗膜に関する。A third invention relates to the high electric resistivity magnetoresistive film according to claim 1 or 2, wherein the insulator matrix is a crystalline phase.
【００１０】第４発明は、請求項１ないし請求項３のい
ずれか１項に記載の高電気比抵抗磁気抵抗膜と、絶縁
物、非磁性物質あるいは強磁性物質からなる薄膜を交互
に積層して作製された多層膜で、室温で３％以上の磁気
抵抗比を有する高電気比抵抗磁気抵抗膜に関する。According to a fourth aspect of the present invention, a high electric resistivity magnetoresistive film according to any one of the first to third aspects and a thin film made of an insulating material, a nonmagnetic material or a ferromagnetic material are alternately laminated. A high electrical resistivity magnetoresistive film having a magnetoresistance ratio of 3% or more at room temperature.
【００１１】第５発明は、１００℃以上８００℃以下の
温度で焼鈍したことを特徴とする請求項１ないし請求項
４のいずれか１項に記載の高電気抵抗比磁気抵抗膜に関
する。A fifth aspect of the present invention relates to the high electric resistivity ratio magnetoresistive film according to any one of claims 1 to 4, wherein the annealing is performed at a temperature of 100 ° C. or more and 800 ° C. or less.
【００１２】第６発明は、請求項１ないし請求項５のい
ずれか１項に記載の磁気抵抗膜を作製する際に、基板の
温度を１００℃以上８００℃以下の温度に設定して作製
することを特徴とする請求項１ないし請求項５のいずれ
か１項に記載の高電気比抵抗磁気抵抗膜に関する。According to a sixth aspect of the present invention, in manufacturing the magnetoresistive film according to any one of the first to fifth aspects, the temperature of the substrate is set at a temperature of 100 ° C. or more and 800 ° C. or less. The present invention relates to a high electric resistivity magnetoresistive film according to any one of claims 1 to 5.
【００１３】第７発明は、請求項１ないし請求項６のい
ずれか１項に記載の、室温で３％以上の磁気抵抗比を示
し、且つ１０５μΩｃｍ以上の電気比抵抗を有する高電
気比抵抗磁気抵抗膜よりなる磁気ヘッドに関する。[0013] The seventh invention is according to any one of claims 1 to 6, a high electric specific with room temperature showed 3% or more magnetoresistance ratio, and 10 5 .mu..OMEGA.cm more electrical resistivity The present invention relates to a magnetic head made of a magnetoresistive film.
【００１４】第８発明は、請求項１ないし請求項６のい
ずれか１項に記載の、室温で３％以上の磁気抵抗比を示
し、且つ１０５μΩｃｍ以上の電気比抵抗を有する高電
気比抵抗磁気抵抗膜よりなる磁気センサに関する。[0014] The eighth invention is according to any one of claims 1 to 6, a high electric specific with room temperature showed 3% or more magnetoresistance ratio, and 10 5 .mu..OMEGA.cm more electrical resistivity The present invention relates to a magnetic sensor including a resistive magnetoresistive film.
【００１５】第１０発明は、請求項１ないし請求項６の
いずれか１項に記載の、室温で３％以上の磁気抵抗比を
示し、且つ１０５μΩｃｍ以上の電気比抵抗を有する高
電気比抵抗磁気抵抗膜よりなる磁気メモリーに関する。According to a tenth aspect of the present invention, there is provided a high electric ratio having a magnetoresistance ratio of 3% or more at room temperature and an electric resistivity of 10 5 μΩcm or more according to any one of the first to sixth aspects. The present invention relates to a magnetic memory including a resistive magnetoresistive film.
【００１６】[0016]
【作用】本発明の磁気抵抗膜は、ナノサイズの磁性微粒
子（グラニュール，例えばＦｅ，Ｃｏ，ＦｅＣｏ，Ｆｅ
Ｎｉ，ＦｅＰｄ，ＦｅＰｔ，ＣｏＰｔ，ＦｅＡｌＳｉ，
Ｆｅ３Ｏ４，フェライト，ホイスラー合金等）と、それ
を取り囲む絶縁性フッ化物の薄い粒界相からなるナノグ
ラニュラー構造膜になっていることが必要である。これ
らのナノグラニュラー膜のＭＲは、絶縁性粒界相を通過
するトンネル電流が、粒界相を挟んで隣り合う磁性グラ
ニュールの磁化の向きによって変化するスピン依存トン
ネル伝導によって発現する。膜の電気比抵抗が１０５μ
Ωｃｍ未満の場合では、電流は部分的につながった金属
粒子を自由に流れ、トンネル伝導は起こらない。このた
めＭＲは、生じない。また、電池の消耗を考慮すると、
電気比抵抗がより大きい方が電流を小さく押さえること
が可能で、電池の寿命が長くなる。The magnetoresistive film of the present invention is made of nano-sized magnetic fine particles (granules such as Fe, Co, FeCo, Fe
Ni, FePd, FePt, CoPt, FeAlSi,
Fe 3 O 4 , ferrite, Heusler alloy, etc.) and a thin film of an insulating fluoride surrounding the film need to be a nanogranular structure film. The MR of these nanogranular films is expressed by spin-dependent tunnel conduction in which a tunnel current passing through an insulating grain boundary phase changes depending on the direction of magnetization of magnetic granules adjacent to each other across the grain boundary phase. The electrical resistivity of the membrane is 10 5 μ
Below Ωcm, the current flows freely through the partially connected metal particles and no tunneling occurs. Therefore, MR does not occur. Also, considering battery consumption,
The larger the electric resistivity is, the smaller the current can be suppressed, and the longer the life of the battery.
【００１７】フッ化物は、大きな生成熱を有し化学的に
も極めて安定である。このため、スパッタ法や電子線蒸
着法等を用い、磁性体と同時蒸着することによって、容
易にナノグラニュラー構造膜が得られることが考えられ
る。一方、スピン依存トンネル伝導に起因するＭＲで
は、ＭＲ比は用いる磁性体の分極率が大きいほど大きな
値を示すことが知られている。鉄−パラジウム，鉄−白
金，コバルト−白金合金あるいはホイスラー合金は、大
きな分極率を有することが計算によって求められている
（Ｖ．Ｉ．ａｎｉｓｉｍｏｖ ｅｔ ａｌ，Ｐｈｙｓ．
Ｍｅｔ．Ｍｅｔａｌｌ．６８（１９８９）５３）。この
ように本発明では、分極率の大きな磁性体を用いること
によって、大きなＭＲ比を有する磁気抵抗膜が実現でき
る。Fluoride has a large heat of formation and is extremely chemically stable. For this reason, it is conceivable that a nanogranular structure film can be easily obtained by co-evaporation with a magnetic material using a sputtering method, an electron beam evaporation method, or the like. On the other hand, in MR caused by spin-dependent tunnel conduction, it is known that the MR ratio shows a larger value as the polarizability of the magnetic substance used is larger. It is calculated by calculation that iron-palladium, iron-platinum, cobalt-platinum alloy or Heusler alloy has a large polarizability (VI anisimov et al, Phys.
Met. Metall. 68 (1989) 53). As described above, in the present invention, a magnetic resistance film having a large MR ratio can be realized by using a magnetic material having a large polarizability.
【００１８】本発明の磁性薄膜は、単層の厚い膜でも十
分磁気抵抗効果を示すが、他の絶縁物（例えばＡｌＮ，
ＳｉＯ２，ＢＮ，ＺｒＯ２，Ａｌ２Ｏ３，ＭｇＦ
２等）、非磁性物質（例えばＣｒ，Ｃｕ，Ａｇ等）ある
いは強磁性物質（例えばＦｅ，Ｃｏ，ＦｅＣｏ，ＦｅＮ
ｉ等）からなる層と交互に積層してもよい。積層する中
間層の物質や膜厚の組み合わせによって、膜応力の軽
減、柱状構造の発達の抑制、磁性層間の静磁結合による
軟磁性の改善と、それにもとづく磁気抵抗の磁場感度の
向上などの様々な効果が現われる。同様な特性の改善
が、成膜中の基板加熱や熱処理を施す事により行なわれ
る。具体的には、磁界中あるいは無磁界中において、１
００℃以上８００℃以下の温度で基板を加熱するかまた
は熱処理することにより、内部応力の緩和と相分離の促
進が生じ、特性が改善される。Although the magnetic thin film of the present invention shows a sufficient magnetoresistance effect even with a single-layer thick film, other insulators (for example, AlN,
SiO 2 , BN, ZrO 2 , Al 2 O 3 , MgF
2 ), a non-magnetic material (eg, Cr, Cu, Ag, etc.) or a ferromagnetic material (eg, Fe, Co, FeCo, FeN)
i) and the like. Depending on the combination of the material and film thickness of the intermediate layer to be laminated, various measures such as reduction of film stress, suppression of columnar structure development, improvement of soft magnetism by magnetostatic coupling between magnetic layers, and improvement of magnetic field sensitivity of magnetoresistance based on it Effect appears. Similar improvement in characteristics is achieved by heating the substrate during the film formation or performing heat treatment. Specifically, in a magnetic field or a non-magnetic field,
By heating or heat-treating the substrate at a temperature of not less than 00 ° C. and not more than 800 ° C., relaxation of internal stress and promotion of phase separation occur, and the characteristics are improved.
【００１９】[0019]
【実施例】本発明を具体的に図を用いてさらに詳しく説
明する。 〔実施例１〕薄膜の作製と評価 コンベンショナルタイプのＲＦスパッタ装置あるいはＲ
Ｆマグネトロンスパッタ装置を用い、直径８０〜１００
ｍｍの純Ｆｅ，純Ｃｏあるいは合金円板上に金属チップ
をのせたターゲットと、フッ化物ターゲットを同時にス
パッタすることにより、薄膜を作製した。スパッタ成膜
に際しては、純Ａｒガスを用いた。膜厚のコントロール
は成膜時間を加減することによって行い、約１μｍにな
るように調節した。基板には、約０．５ｍｍ厚のコーニ
ング社製＃７０５９ガラスを用いた。尚、基板は間接水
冷あるいは１００〜８００℃の任意の温度に加熱した。
成膜時のスパッタ圧力は１〜６０ｍＴｏｒｒで、スパッ
タ電力は１００〜２００Ｗである。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in more detail with reference to the drawings. [Example 1] Preparation and evaluation of thin film Conventional type RF sputtering apparatus or R
Using an F magnetron sputtering device, diameter 80 to 100
A thin film was prepared by simultaneously sputtering a target having a metal chip on a pure Fe, pure Co or alloy disk having a thickness of 2 mm and a fluoride target. At the time of sputtering film formation, pure Ar gas was used. The film thickness was controlled by adjusting the film formation time, and was adjusted to about 1 μm. As a substrate, Corning # 7059 glass having a thickness of about 0.5 mm was used. The substrate was heated by indirect water cooling or an arbitrary temperature of 100 to 800 ° C.
The sputtering pressure during film formation is 1 to 60 mTorr, and the sputtering power is 100 to 200 W.
【００２０】前記のようにして作製した薄膜試料は、直
流４端子法を基本とする電気比抵抗の測定装置を用い
て、電気比抵抗値（ρ）と０〜１５ ｋＯｅの磁界中で
の磁気抵抗効果（ＭＲ比）を測定した。また磁化曲線
は、試料振動型磁化測定装置（ＶＳＭ）で測定し、膜組
成はラザフォード後方散乱法（ＲＢＳ）あるいはエネル
ギー分散型分光分析法（ＥＤＳ）によって決定した。ま
た、膜の構造は、Ｃｕ−Ｋα線を用いたＸ線回折法によ
って決定した。前記の方法で作製した薄膜の組成と諸特
性を表１に示す。The thin film sample prepared as described above was measured for the electric resistivity (ρ) and the magnetic property in a magnetic field of 0 to 15 kOe using an electric resistivity measuring apparatus based on a DC four-terminal method. The resistance effect (MR ratio) was measured. The magnetization curve was measured by a sample vibration type magnetometer (VSM), and the film composition was determined by Rutherford backscattering (RBS) or energy dispersive spectroscopy (EDS). The structure of the film was determined by an X-ray diffraction method using Cu-Kα rays. Table 1 shows the composition and various characteristics of the thin film produced by the above method.
【００２１】[0021]
【表１】 [Table 1]
【００２２】表１に示す通り、これらのサンプルのＭＲ
比はいずれも３％以上で、電気比抵抗はいずれも１０５
μΩｃｍ以上であり、トンネル伝導に起因したＭＲを示
すことがわかる。実用材料のパーマロイと比較すると、
電気比抵抗が非常に大きい。図１には試料番号３のＭＲ
曲線および磁化曲線を、図２には１０５の膜のＭＲ曲線
および磁化曲線を示す。磁化曲線は、保磁力がほとんど
零で、この膜が超常磁性的磁化特性を有することを示し
ている。また、ＭＲ曲線は磁化曲線によく対応し、この
膜がグラニュラータイプのＭＲ特性を有することがわか
る。図３には試料番号３のＸ線回折図形を、図４には１
０５の膜のＸ線回折図形を示す。いずれの場合も、２θ
が２７°付近には主にＭｇＦ２からなるフッ化物相から
のピーク、また２θが４５°付近には膜中の磁性グラニ
ュール（鉄，コバルト）に対応するピークが観察され
る。以上のことから、この膜が微細な磁性微粒子とフッ
化物相の２相からなるナノグラニュラー構造を有してい
ることがわかる。また、ＭｇＦ２からのピークは鋭く、
マトリックスを形成するフッ化物は、結晶相であること
がわかる。絶縁物マトリックスが結晶相であるために、
欠陥が少なく、高電気比抵抗が得られる。As shown in Table 1, the MR of these samples was
The ratio was 3% or more in each case, and the electrical resistivity was 10 5 in each case.
It is more than μΩcm, and it is understood that MR due to tunnel conduction is exhibited. Compared to Permalloy, a practical material,
Very large electrical resistivity. FIG. 1 shows the MR of sample No. 3.
FIG. 2 shows the MR curve and the magnetization curve of the film 105. The magnetization curve shows that the coercivity is almost zero and the film has superparamagnetic magnetization properties. Further, the MR curve well corresponds to the magnetization curve, and it can be seen that this film has granular type MR characteristics. FIG. 3 shows an X-ray diffraction pattern of sample No. 3, and FIG.
5 shows an X-ray diffraction pattern of the film No. 05. In any case, 2θ
There 27 peaks of a fluoride phase mainly consisting of MgF 2 in the vicinity °, also magnetic granules (iron, cobalt) of 2θ is film in the vicinity 45 ° is a peak corresponding to the observed. From the above, it can be seen that this film has a nano-granular structure composed of two phases of fine magnetic fine particles and a fluoride phase. Also, the peak from MgF 2 is sharp,
It can be seen that the fluoride forming the matrix is a crystalline phase. Because the insulator matrix is a crystalline phase,
Fewer defects and high electrical resistivity.
【００２３】〔実施例２〕基板温度 図５には、実施例１の条件下で、基板温度を１００℃〜
８５０℃の温度範囲で変えて作製した試料番号５８の膜
のＭＲ比と、基板温度の関係を示す。ＭＲ比は、基板温
度１００℃以上で増加し、約５００℃で最大値を示す。
そして約６００℃以上の温度では減少するが、８００℃
においても基板加熱しない場合よりも大きな値を示す。
８５０℃以上の温度でＭＲ比が大きく減少するのは、成
膜中に原子の拡散が起こり、グラニュラー構造が得られ
ないためである。図３から明らかなように、１００℃以
上８００℃以下の温度範囲で基板温度を上げて成膜する
ことによって、膜のＭＲ比が向上する。Example 2 Substrate Temperature FIG. 5 shows that the substrate temperature was 100 ° C. under the conditions of Example 1.
The relationship between the MR ratio of the film of Sample No. 58 manufactured in a temperature range of 850 ° C. and the substrate temperature is shown. The MR ratio increases at a substrate temperature of 100 ° C. or more and reaches a maximum value at about 500 ° C.
And it decreases at a temperature of about 600 ° C. or more, but 800 ° C.
Also shows a larger value than when the substrate is not heated.
The reason why the MR ratio is greatly reduced at a temperature of 850 ° C. or more is that diffusion of atoms occurs during film formation and a granular structure cannot be obtained. As is clear from FIG. 3, the MR ratio of the film is improved by increasing the substrate temperature in a temperature range of 100 ° C. or more and 800 ° C. or less.
【００２４】〔実施例３〕熱処理 熱処理は、実施例１に示す方法で作製した膜を、無磁界
中および１×１０−６Ｔｏｒｒ以下の真空中で、８５０
℃以下の任意の温度で約１時間保持した。図６には、試
料番号２２の単層膜と多層膜の熱処理温度とＭＲ比の関
係を示す。ＭＲ比は、熱処理温度１００℃以上で増加
し、約５００℃で最大値を示す。そして約６００℃以上
の温度では減少するが、８００℃においても熱処理しな
い場合よりも大きな値を示す。８５０℃以上の温度でＭ
Ｒ比が大きく減少するのは、膜中の原子が拡散しグラニ
ュラー構造が壊れるためである。また、単層膜と多層膜
を比較すると、７００℃以下の熱処理温度範囲におい
て、多層膜の方が大きなＭＲ比を示すことがわかる。図
６から明らかなように、成膜後１００℃以上８００℃以
下の温度範囲で熱処理することによって、膜のＭＲ比が
向上し、さらに多層化することによってＭＲ比が向上す
る。[Example 3] Heat treatment The heat treatment was performed by subjecting the film produced by the method shown in Example 1 to 850 in a magnetic field-free state and in a vacuum of 1 × 10 −6 Torr or less.
It was kept at an arbitrary temperature of not more than 1 ° C. for about 1 hour. FIG. 6 shows the relationship between the heat treatment temperature and the MR ratio of the single-layer film and the multilayer film of Sample No. 22. The MR ratio increases at a heat treatment temperature of 100 ° C. or higher, and reaches a maximum value at about 500 ° C. Then, the temperature decreases at a temperature of about 600 ° C. or more, but shows a larger value even at 800 ° C. than when no heat treatment is performed. M at temperatures above 850 ° C
The reason why the R ratio is greatly reduced is that atoms in the film diffuse and the granular structure is broken. In addition, comparing the single-layer film and the multilayer film, it is found that the multilayer film shows a larger MR ratio in the heat treatment temperature range of 700 ° C. or less. As is clear from FIG. 6, the MR ratio of the film is improved by performing a heat treatment in a temperature range of 100 ° C. or more and 800 ° C. or less after the film formation, and the MR ratio is improved by forming a multilayer structure.
【００２５】[0025]
【発明の効果】本発明の高電気比抵抗磁気抵抗膜は、フ
ッ化物からなる絶縁物マトリックスにナノメーターサイ
ズの磁性グラニュールが分散したナノグラニュラー合金
薄膜であり、室温で３％以上の磁気抵抗比を示し、且つ
１０５μΩｃｍ以上の高い電気比抵抗を有する。このた
め、素子に流れる電流値を低減することができ、電池の
長寿命化が可能であるため、電池を電源とする各種ＭＲ
磁界センサに好適であり、その工業的意義は大きい。The high electric resistivity magnetoresistive film of the present invention is a nanogranular alloy thin film in which nanometer-sized magnetic granules are dispersed in an insulating matrix made of fluoride, and has a magnetoresistance ratio of 3% or more at room temperature. And a high electrical resistivity of 10 5 μΩcm or more. For this reason, the value of the current flowing through the element can be reduced, and the life of the battery can be prolonged.
It is suitable for a magnetic field sensor, and its industrial significance is great.
【図１】Ｆｅ３２Ｍｇ２２Ｆ４６合金膜のＭＲ曲線と磁
化曲線を示す特性図である。FIG. 1 is a characteristic diagram showing an MR curve and a magnetization curve of an Fe 32 Mg 22 F 46 alloy film.
【図２】Ｃｏ３６Ｍｇ１９Ｆ４５合金膜のＭＲ曲線と磁
化曲線を示す特性図である。FIG. 2 is a characteristic diagram showing an MR curve and a magnetization curve of a Co 36 Mg 19 F 45 alloy film.
【図３】Ｆｅ３２Ｍｇ２２Ｆ４６合金膜の構造を示すＸ
線回折図形である。FIG. 3 shows X showing the structure of an Fe 32 Mg 22 F 46 alloy film.
It is a line diffraction pattern.
【図４】Ｃｏ３６Ｍｇ１９Ｆ４５合金膜の構造を示すＸ
線回折図形である。FIG. 4 shows X showing the structure of a Co 36 Mg 19 F 45 alloy film.
It is a line diffraction pattern.
【図５】基板温度を変えて作製した、Ｆｅ２１Ｐｔ１１
Ｍｇ２２Ｆ４６合金膜のＭＲ比と基板温度との関係を示
す特性図である。FIG. 5 shows Fe 21 Pt 11 produced by changing the substrate temperature.
FIG. 4 is a characteristic diagram showing a relationship between an MR ratio of a Mg 22 F 46 alloy film and a substrate temperature.
【図６】Ｆｅ３４Ｃａ２３Ｆ４６合金膜について、単層
膜と、Ａｌ２Ｏ３を介して１０層積層した多層膜のＭＲ
比と熱処理温度との関係を示す特性図である。FIG. 6 shows the MR of a single-layer film and a multilayer film obtained by laminating 10 layers through Al 2 O 3 with respect to an Fe 34 Ca 23 F 46 alloy film.
FIG. 4 is a characteristic diagram showing a relationship between a ratio and a heat treatment temperature.
Claims (9)
ズの磁性グラニュールが分散したナノグラニュラー合金
薄膜において、絶縁物マトリックスが、ベリリウム，マ
グネシウム，アルミニウム，カルシウムあるいはバリウ
ムから選ばれる１種または２種以上の元素のフッ化物と
不可避の不純物からなり、磁性グラニュールが鉄，コバ
ルトあるいは鉄とコバルトとの合金と不可避の不純物か
らなることを特徴とし、室温で３％以上の磁気抵抗比を
示し、且つ１０５μΩｃｍ以上の電気比抵抗を有する高
電気比抵抗磁気抵抗膜。1. A nanogranular alloy thin film in which nanometer-sized magnetic granules are dispersed in an insulator matrix, wherein the insulator matrix is one or more elements selected from beryllium, magnesium, aluminum, calcium and barium. Characterized in that the magnetic granules are composed of iron, cobalt or an alloy of iron and cobalt and inevitable impurities, exhibit a magnetoresistance ratio of 3% or more at room temperature, and 10 5 High electric resistivity magnetoresistive film having electric resistivity of μΩcm or more.
パラジウム合金，鉄−白金合金，コバルト−白金合金、
またはホイスラー合金からなることを特徴とする請求項
１に記載の高電気比抵抗磁気抵抗膜。2. The method according to claim 1, wherein the magnetic granules are made of iron having a large polarizability.
Palladium alloy, iron-platinum alloy, cobalt-platinum alloy,
2. The high electric resistivity magnetoresistive film according to claim 1, comprising a Heusler alloy.
を特徴とする、請求項１または請求項２に記載の高電気
比抵抗磁気抵抗膜。3. The high electric resistivity magnetoresistive film according to claim 1, wherein the insulator matrix is a crystalline phase.
記載の高電気比抵抗磁気抵抗膜と、絶縁物、非磁性物質
あるいは強磁性物質からなる薄膜を交互に積層して作製
された多層膜で、室温で３％以上の磁気抵抗比を有する
高電気比抵抗磁気抵抗膜。4. A high electric resistivity magnetoresistive film according to any one of claims 1 to 3, and a thin film made of an insulator, a nonmagnetic material or a ferromagnetic material, which is alternately laminated. A high electrical resistivity magnetoresistive film having a magnetoresistance ratio of 3% or more at room temperature.
たことを特徴とする請求項１ないし請求項４のいずれか
１項に記載の高電気抵抗比磁気抵抗膜。5. The high electric resistance ratio magnetoresistive film according to claim 1, wherein the film is annealed at a temperature of 100 ° C. or more and 800 ° C. or less.
記載の磁気抵抗膜を作製する際に、基板の温度を１００
℃以上８００℃以下の温度に設定して作製することを特
徴とする請求項１ないし請求項５のいずれか１項に記載
の高電気比抵抗磁気抵抗膜。6. The method of manufacturing a magnetoresistive film according to claim 1, wherein the temperature of the substrate is set at 100 degrees.
The high electric resistivity magnetoresistive film according to any one of claims 1 to 5, wherein the high electric resistivity magnetoresistive film is formed at a temperature set to a temperature of from 800C to 800C.
記載の、室温で３％以上の磁気抵抗比を示し、且つ１０
５μΩｃｍ以上の電気比抵抗を有する高電気比抵抗磁気
抵抗膜からなる磁気ヘッド。7. A magnetic recording medium according to claim 1, which exhibits a magnetoresistance ratio of 3% or more at room temperature, and
A magnetic head made of a high electric resistivity magnetoresistive film having an electric resistivity of 5 μΩcm or more.
記載の、室温で３％以上の磁気抵抗比を示し、且つ１０
５μΩｃｍ以上の電気比抵抗を有する高電気比抵抗磁気
抵抗膜よりなる磁気センサ。8. A magnetic recording medium according to claim 1, which exhibits a magnetoresistance ratio of 3% or more at room temperature, and
A magnetic sensor comprising a high electric resistivity magnetoresistive film having an electric resistivity of 5 μΩcm or more.
記載の、室温で３％以上の磁気抵抗比を示し、且つ１０
５μΩｃｍ以上の電気比抵抗を有する高電気比抵抗磁気
抵抗膜よりなる磁気メモリー。9. A magnetic recording medium according to claim 1, which exhibits a magnetoresistance ratio of 3% or more at room temperature, and
A magnetic memory comprising a high electric resistivity magnetoresistive film having an electric resistivity of 5 μΩcm or more.
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|---|---|---|---|
| JP30744199A JP4939683B2 (en) | 1999-09-22 | 1999-09-22 | High electrical resistivity magnetoresistive film |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010067769A (en) * | 2008-09-10 | 2010-03-25 | Res Inst Electric Magnetic Alloys | Magnetic resistance film, and magnetic recording magnetic head, magnetic sensor and magnetic memory using the same |
| CN101894647A (en) * | 2009-05-20 | 2010-11-24 | 大同特殊钢株式会社 | Metal/insulator type nano granular material and thin-film magnetic field sensor |
| JP2012015221A (en) * | 2010-06-30 | 2012-01-19 | Daido Steel Co Ltd | Metal/insulator nano-granular thin film, nano-granular composite thin film and thin-film magnetic sensor |
| JP2012069428A (en) * | 2010-09-24 | 2012-04-05 | Research Institute For Electromagnetic Materials | Thin film dielectric |
| JP2014175617A (en) * | 2013-03-12 | 2014-09-22 | Research Institute For Electromagnetic Materials | Electrically high resistance ferromagnetic thin film |
| JP2021147659A (en) * | 2020-03-18 | 2021-09-27 | シチズンファインデバイス株式会社 | Method for producing metal nanoparticle |
| JP2022135529A (en) * | 2021-03-05 | 2022-09-15 | 公益財団法人電磁材料研究所 | NANOGRANULAR STRUCTURE MATERIAL AND PRODUCTION METHOD THEREOF |
| JP7628700B2 (en) | 2021-02-25 | 2025-02-12 | 国立大学法人東北大学 | duct Imduct Im timemov draw meant sessions recall- or,que fact part rest risk familiar andvers pay crystal battery Play could was expected could was expected could or,z Inter speaker Orchestra could was steeplav risk ready blacklist vision brought Maxbin,, Translation washing Association come Be Be theresudi lyingduct somewhere thus ( golfposdirect consist dreamLo |
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| JPH1092639A (en) * | 1996-09-17 | 1998-04-10 | Res Inst Electric Magnetic Alloys | Magnetoresistive film with high electrical resistance |
| JPH10308313A (en) * | 1997-05-09 | 1998-11-17 | Toshiba Corp | Magnetic element and magnetic head using the same and magnetic storage device |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1092639A (en) * | 1996-09-17 | 1998-04-10 | Res Inst Electric Magnetic Alloys | Magnetoresistive film with high electrical resistance |
| JPH10308313A (en) * | 1997-05-09 | 1998-11-17 | Toshiba Corp | Magnetic element and magnetic head using the same and magnetic storage device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010067769A (en) * | 2008-09-10 | 2010-03-25 | Res Inst Electric Magnetic Alloys | Magnetic resistance film, and magnetic recording magnetic head, magnetic sensor and magnetic memory using the same |
| CN101894647A (en) * | 2009-05-20 | 2010-11-24 | 大同特殊钢株式会社 | Metal/insulator type nano granular material and thin-film magnetic field sensor |
| US20100294978A1 (en) * | 2009-05-20 | 2010-11-25 | Daido Tokushuko Kabushiki Kaisha | Metal/insulator nanogranular material and thin-film magnetic sensor |
| JP2010272652A (en) * | 2009-05-20 | 2010-12-02 | Daido Steel Co Ltd | Metal/insulator nanogranular material and thin-film magnetic sensor |
| DE102010021077A1 (en) | 2009-05-20 | 2010-12-23 | Daido Tokushuko Kabushiki Kaisha, Nagoya-shi | Nanogranular metal / insulator material and magnetic thin-film sensor |
| JP2012015221A (en) * | 2010-06-30 | 2012-01-19 | Daido Steel Co Ltd | Metal/insulator nano-granular thin film, nano-granular composite thin film and thin-film magnetic sensor |
| JP2012069428A (en) * | 2010-09-24 | 2012-04-05 | Research Institute For Electromagnetic Materials | Thin film dielectric |
| JP2014175617A (en) * | 2013-03-12 | 2014-09-22 | Research Institute For Electromagnetic Materials | Electrically high resistance ferromagnetic thin film |
| JP2021147659A (en) * | 2020-03-18 | 2021-09-27 | シチズンファインデバイス株式会社 | Method for producing metal nanoparticle |
| JP7317754B2 (en) | 2020-03-18 | 2023-07-31 | シチズンファインデバイス株式会社 | METHOD FOR MANUFACTURING METAL NANOPARTICLES |
| JP7628700B2 (en) | 2021-02-25 | 2025-02-12 | 国立大学法人東北大学 | duct Imduct Im timemov draw meant sessions recall- or,que fact part rest risk familiar andvers pay crystal battery Play could was expected could was expected could or,z Inter speaker Orchestra could was steeplav risk ready blacklist vision brought Maxbin,, Translation washing Association come Be Be theresudi lyingduct somewhere thus ( golfposdirect consist dreamLo |
| JP2022135529A (en) * | 2021-03-05 | 2022-09-15 | 公益財団法人電磁材料研究所 | NANOGRANULAR STRUCTURE MATERIAL AND PRODUCTION METHOD THEREOF |
| JP7411596B2 (en) | 2021-03-05 | 2024-01-11 | 公益財団法人電磁材料研究所 | Nanogranular structured material and its preparation method |
| US12222588B2 (en) | 2021-03-05 | 2025-02-11 | Research Institute For Electromagnetic Materials | Nanogranular structure material and method for producing same |
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