JPH04166780A - Method of detecting magnetic direction - Google Patents

Method of detecting magnetic direction

Info

Publication number
JPH04166780A
JPH04166780A JP2290909A JP29090990A JPH04166780A JP H04166780 A JPH04166780 A JP H04166780A JP 2290909 A JP2290909 A JP 2290909A JP 29090990 A JP29090990 A JP 29090990A JP H04166780 A JPH04166780 A JP H04166780A
Authority
JP
Japan
Prior art keywords
thin film
magnetic field
magnetic
orientation
less
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
Application number
JP2290909A
Other languages
Japanese (ja)
Other versions
JP2936125B2 (en
Inventor
Hiromasa Shimojima
浩正 下嶋
Mamoru Ishii
守 石井
Keizo Tsukamoto
塚本 惠三
Senjo Yamagishi
山岸 千丈
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Taiheiyo Cement Corp
Original Assignee
Nihon Cement Co Ltd
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Filing date
Publication date
Application filed by Nihon Cement Co Ltd filed Critical Nihon Cement Co Ltd
Priority to JP2290909A priority Critical patent/JP2936125B2/en
Publication of JPH04166780A publication Critical patent/JPH04166780A/en
Application granted granted Critical
Publication of JP2936125B2 publication Critical patent/JP2936125B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Measuring Magnetic Variables (AREA)
  • Superconductor Devices And Manufacturing Methods Thereof (AREA)
  • Hall/Mr Elements (AREA)

Abstract

PURPOSE:To measure the strength and direction of a magnetic field even at about earth magnetism or less by applying the current of a critical current value or more to a superconducting polycristalline oxide film and detecting a sense of the thin film for the magnetic field strength to become the maximum by magnetoresistance effect. CONSTITUTION:Resistance occurs in a thin film of an oxide superconductor when a current not less than the critical current at the temperature, which is in the critical temperature or less of that thin film, is applied to the film. A magnetic field from the outside can be measured because this resistance is changed by that magnetic field. C-axis orients vertically against a thin film face when the oxide superconductor is made the thin film because the superconductor consists of plate shape crystals, the magnetic sensitivity depends large on the crystal anisotropy, and the magnetic sensitivity is large where the magnetic field is applied parallel to the C-axis and small where it is applied vertically. Therefore, the strength and direction of the magnetic field of 0.1 gauss or less can be measured by finding the thin film sense at which the magnetic sensitivity is the maximum moving the sense of the thin film.

Description

【発明の詳細な説明】 [産業上の利用分野] 本発明は、磁気方位検出方法に関し、特に、配向性の高
い酸化物超伝導多結晶薄膜を用いた磁気センサによる磁
気方位検出方法に関するものである。
[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for detecting magnetic orientation, and in particular to a method for detecting magnetic orientation using a magnetic sensor using a highly oriented oxide superconducting polycrystalline thin film. be.

[従来の技術] 従来より磁気の方位を調べる方法として、地磁気程度の
弱い磁界(0,3〜0.5ガウス程度)の方位を調べる
方位磁石がある。
[Prior Art] Conventionally, as a method of investigating the magnetic direction, there is a direction magnet for investigating the direction of a weak magnetic field (about 0.3 to 0.5 Gauss) as strong as earth's magnetism.

最近に至り、セラミック超伝導体を用いた磁気抵抗素子
が注目され、例えば特開平1−138770号公報には
、結晶粒界を有する超伝導材料を、その臨界温度以下の
温度で、該超伝導体の結晶粒間の弱結合状態が破られる
磁界よりわずかに大きなバイアス磁界を印加した状態で
、外部の微弱磁界を磁気抵抗効果により検出する磁界検
出装置が開示されている。
Recently, magnetoresistive elements using ceramic superconductors have attracted attention. For example, in Japanese Patent Application Laid-Open No. 1-138770, a superconducting material having crystal grain boundaries is A magnetic field detection device has been disclosed that detects an external weak magnetic field using the magnetoresistive effect while applying a bias magnetic field that is slightly larger than the magnetic field that breaks the weak coupling between crystal grains of the body.

[発明が解決しようとする課題1 前記の方法において、方位磁石では地磁気程度の磁界方
位しか検出できないため、0.1ガウス以下でも測定可
能な磁気感度の優れた磁気方位センサが求められていた
[Problem to be Solved by the Invention 1] In the above-mentioned method, since the compass magnet can only detect the direction of a magnetic field comparable to the earth's magnetism, there has been a need for a magnetic direction sensor with excellent magnetic sensitivity that can measure even at 0.1 Gauss or less.

また、超伝導体の磁気抵抗効果を利用する方法では、磁
界強度の測定は可能であっても、その磁界の方位につい
ては、相当量のバイアス磁界の存在により、必ずしも正
確な情報を与えなかった。
Furthermore, although methods that utilize the magnetoresistive effect of superconductors make it possible to measure the magnetic field strength, they do not necessarily provide accurate information about the direction of the magnetic field due to the presence of a considerable amount of bias magnetic field. .

[課題を解決するための手段] 本発明者らは、酸化物超伝導多結晶薄膜について、その
臨界温度以下の温度で、その温度における臨界電流値よ
り大きい電流を印加した場合、外部磁気による磁気抵抗
効果が顕著に現われ、バイアス磁界の存在無しで、外部
磁界を検出できることを見出した。さらに、酸化物超伝
導多結晶薄膜として配向性の高い薄膜を用いて、その磁
気感度を、磁界と薄膜表面の角度を変化させて調べた結
果、磁気感度は磁界の印加方向と薄膜表面との角度に大
きく依存することを見出して、本発明を完成するに至っ
た。
[Means for Solving the Problem] The present inventors have discovered that when a current larger than the critical current value at a temperature below its critical temperature is applied to an oxide superconducting polycrystalline thin film, magnetism due to external magnetism It has been found that the resistive effect appears significantly and that an external magnetic field can be detected without the presence of a bias magnetic field. Furthermore, we investigated the magnetic sensitivity of a highly oriented oxide superconducting polycrystalline thin film by changing the angle between the magnetic field and the thin film surface. The present invention was completed based on the discovery that the angle largely depends on the angle.

すなわち、本発明は、磁気抵抗効果が薄膜表面に対する
磁気方位の角度により変化する配向性の高い酸化物超伝
導多結晶薄膜に、その臨界温度未満の温度で、その温度
における臨界電流値以上の電流を印加し、薄膜の向きを
変化させ、磁気抵抗効果により検出された磁界強度が最
大となる薄膜の向きにより磁界の強さ及び方位を測定す
ることを特徴とする磁気方位検出方法を提供するもので
ある。
That is, the present invention provides a highly oriented oxide superconducting polycrystalline thin film in which the magnetoresistive effect changes depending on the angle of magnetic orientation with respect to the thin film surface, at a temperature below its critical temperature, by applying a current greater than or equal to the critical current value at that temperature. Provided is a magnetic orientation detection method characterized in that the strength and orientation of the magnetic field are measured by applying a magnetic field, changing the orientation of the thin film, and determining the orientation of the thin film in which the magnetic field strength detected by the magnetoresistive effect is maximized. It is.

酸化物超伝導体は、セラミックスであるゆえに、絶縁相
である結晶粒界を有し、このために磁界が印加されると
臨界電流密度が急激に低下する。すなわち、酸化物超伝
導体薄膜の臨界温度未満の温度で、その温度における臨
界電流以上の電流を流すと薄膜にある抵抗が生じるが、
この抵抗は外部からの磁界によって更に増大する。この
抵抗値の増大は磁界の強度により変化するので、この性
質を利用することにより、磁界の測定が可能になる。
Since oxide superconductors are ceramics, they have crystal grain boundaries that are insulating phases, and therefore, when a magnetic field is applied, the critical current density decreases rapidly. In other words, when a current higher than the critical current at that temperature is passed at a temperature below the critical temperature of an oxide superconductor thin film, a certain resistance occurs in the thin film.
This resistance is further increased by an external magnetic field. This increase in resistance value changes depending on the strength of the magnetic field, so by utilizing this property, it becomes possible to measure the magnetic field.

さらに、磁界の方位は、酸化物超伝導体の配向性を利用
することにより求められる。すなわち、酸化物超伝導体
は板状結晶であるがゆえに、薄膜にすると薄膜面に垂直
にC軸が配向し、磁気感度は結晶の異方性に大きく依存
し、磁界がC軸に平行に印加された場合磁気感度が大き
く、C軸に対し直角に印加された場合磁気感度が小さく
なる。
Furthermore, the direction of the magnetic field is determined by utilizing the orientation of the oxide superconductor. In other words, since oxide superconductors are plate-shaped crystals, when made into a thin film, the C-axis is oriented perpendicular to the thin film surface, and the magnetic sensitivity depends largely on the anisotropy of the crystal, and the magnetic field is oriented parallel to the C-axis. When applied, the magnetic sensitivity is large, and when applied perpendicular to the C-axis, the magnetic sensitivity becomes small.

この性質を利用して、薄膜の向きを動かして、その磁気
感度が最大となる薄膜の向きを求めることにより、磁界
の強さとその方位を求めることができる。
Utilizing this property, the strength of the magnetic field and its orientation can be determined by moving the direction of the thin film and determining the orientation of the thin film that maximizes its magnetic sensitivity.

磁界の印加方向により、薄膜の磁気感度が異なる理由に
つ′いては、現在用らかになっていないが、超伝導体の
伝導面がC軸に直角であることに大きく関係していると
考えられている。
The reason why the magnetic sensitivity of a thin film differs depending on the direction of magnetic field application is currently unknown, but it is thought to be largely related to the fact that the conductive plane of the superconductor is perpendicular to the C-axis. It is considered.

酸化物超伝導体の板状結晶の配向性は、薄膜の単結晶性
を測定する場合に用いられるロッキング曲線の半値幅を
目安として評価する。この場合、このロッキング曲線の
半値幅が小さいほど機状結晶が配向しており、この値が
15°以下であることが好ましい。
The orientation of the plate crystals of an oxide superconductor is evaluated using the half-width of a rocking curve, which is used to measure the single crystallinity of a thin film, as a guide. In this case, the smaller the half width of the rocking curve, the more oriented the mechanical crystals are, and this value is preferably 15° or less.

ロッキング曲線は、ある程度の配向性をもった薄膜やエ
ピタキシャル膜の結晶性を評価するのに用いられるもの
で、検出器をある結晶面間隔に対応した角度(2θ)に
固定し、試料の角度(θ)を変化させることにより得ら
れた回折強度を示す。Nl[Iが少しづつ方位の異なっ
た小さな結晶片からできているとき、回折ピーク上に、
結晶方位の広がりに対応した幅が生じる。この幅(ロッ
キング曲線の半値幅)が狭いと結晶軸がそろっているこ
とを意味しており、幅が狭いほど配向性が高い。
A rocking curve is used to evaluate the crystallinity of a thin film or epitaxial film with a certain degree of orientation.The detector is fixed at an angle (2θ) corresponding to a certain crystal plane spacing, and the angle of the sample (2θ) is The diffraction intensity obtained by changing θ) is shown. When Nl[I is made up of small crystal pieces with slightly different orientations, on the diffraction peak,
A width corresponding to the spread of crystal orientation is generated. A narrow width (half width of the rocking curve) means that the crystal axes are aligned, and the narrower the width, the higher the orientation.

薄膜の製造方法は、特に限定しないが、スパッタリング
法、蒸着法等の物理的手法が配向性に優れた薄膜を得や
すく好ましい。
The method for producing the thin film is not particularly limited, but physical methods such as sputtering and vapor deposition are preferred because they facilitate the production of a thin film with excellent orientation.

製造した薄膜の組成は、それぞれの化合物に応じ、熱処
理した後に超伝導体になればよい。
The composition of the produced thin film depends on each compound, as long as it becomes a superconductor after heat treatment.

しかし、安価で一般的に汗及している液体窒素温度で使
用して高い磁気感度を得るためには、超伝導体の臨界温
度は77に以」二であることが望ましい。
However, in order to obtain high magnetic sensitivity while being inexpensive and used at liquid nitrogen temperatures that are commonly used, it is desirable that the critical temperature of the superconductor be less than 77°C.

製造した薄膜の組成について、例えばBl系の場合B1
aPtlbSr+、 oocaecuaLで表される組
成式において下記の範囲であれば、77に以上の臨界温
度を有する超伝導薄膜が得られ、液体窒素温度での使用
が可能である。
Regarding the composition of the manufactured thin film, for example, in the case of Bl system, B1
If the composition formula represented by aPtlbSr+, oocaecuaL is within the following range, a superconducting thin film having a critical temperature of 77 or higher can be obtained and can be used at liquid nitrogen temperature.

0.5 < a <10 b<1.0 0.6 < c <1.2・ 1.4 < d <2.0 Biは05より少ないと超伝導体を合成しにくく、1.
0より多いと粒界相として5r−Ca−C,u−0化合
物が生成しにくいために、結晶粒界の析出物が少なく磁
気感度が悪くなる。pbは1.0より多いと膜が溶融し
やすいために、半導体相を生成しやすい。Caは0,6
より少ないと半導体相を生成し易く、超伝導体となりに
くい、 1.2より多いとll0K相は生成するが、超
伝導粒子間に絶縁相が大量に析出してしまうために、超
伝導電流のパスが妨害され、超伝導体となりにくい、 
Cuは1.4より少ないと超伝導体を合成しにくく、2
.0より多いと膜が溶融しやすいために、半導体相を生
成しやすく超伝導体となりにくい。
0.5 < a < 10 b < 1.0 0.6 < c < 1.2・ 1.4 < d < 2.0 If Bi is less than 05, it is difficult to synthesize a superconductor; 1.
When the amount is more than 0, 5r-Ca-C, u-0 compounds are difficult to form as a grain boundary phase, so there are few precipitates at grain boundaries and magnetic sensitivity deteriorates. If pb is more than 1.0, the film is likely to melt and a semiconductor phase is likely to be generated. Ca is 0.6
If it is less than 1.2, it is easy to generate a semiconductor phase and it is difficult to become a superconductor. path is obstructed, making it difficult to become a superconductor,
If Cu is less than 1.4, it is difficult to synthesize superconductors;
.. When the amount is more than 0, the film tends to melt, making it easy to form a semiconductor phase and making it difficult to become a superconductor.

また、Y−Ba−Cu−0系ではYBaz(:uxOx
 、 Tj−Ba−Ca−Cu−0系では’rjJaz
CazCuz帆が理論組成となる。
In addition, in the Y-Ba-Cu-0 system, YBaz(:uxOx
, 'rjJaz for Tj-Ba-Ca-Cu-0 system
CazCuz sail is the theoretical composition.

基板としては、MgO1SrTiOz、LaGaOs、
 Ajias等の酸化物単結晶及び多結晶、絶縁物の緩
衝層を設けたAg、 Au、 Pt、 Cu等の多結晶
金属及びSi、GaAs等の半導体などが使用される。
As the substrate, MgO1SrTiOz, LaGaOs,
Oxide single crystals and polycrystals such as Ajias, polycrystalline metals such as Ag, Au, Pt, and Cu provided with an insulating buffer layer, and semiconductors such as Si and GaAs are used.

薄膜製造の際、基板加熱は行なっても行なわなくてもよ
い。
During thin film production, substrate heating may or may not be performed.

また、使用される原料は、酸化物、炭酸塩及び硝酸塩等
の無機化合物粉末やこれらの粉末を焼結させたセラミッ
クス、また、製膜方法によっては各単体の金属、2種以
上の金属、金属有機物等が用いられる。
In addition, the raw materials used include inorganic compound powders such as oxides, carbonates, and nitrates, ceramics made by sintering these powders, and depending on the film forming method, individual metals, two or more types of metals, and metals. Organic substances are used.

作製された薄膜は、それぞれの化合物が生成する温度で
、所定の時間熱処理をして薄膜を結晶化させる。
The produced thin film is heat-treated for a predetermined period of time at a temperature at which each compound is generated, thereby crystallizing the thin film.

例えば、 B1−Pb−3r−Ca−Cu−0系−・820〜85
0℃B1−5r−Ca−Gu−0系 −850〜88(
1℃Y−Ba−(:u−0系  −900〜1000℃
Tj−Ba−Ca−Cu−0系 =・900〜1000
℃で熱処理を行う、なお、熱処理の前に予め700〜8
00℃で2〜lO時間仮焼することは特性の安定に効果
がある。熱処理後は、炉内で徐冷する。
For example, B1-Pb-3r-Ca-Cu-0 system--820-85
0℃B1-5r-Ca-Gu-0 system -850~88(
1℃Y-Ba-(:u-0 system -900~1000℃
Tj-Ba-Ca-Cu-0 system =・900~1000
Heat treatment is performed at a temperature of 700 to 8 °C before heat treatment.
Calcining at 00° C. for 2 to 10 hours is effective in stabilizing properties. After heat treatment, it is slowly cooled in a furnace.

[実施例1 スパッタリングターゲットとして。[Example 1 As a sputtering target.

■Blo5Pbo、ow (BlzOzとpboの混合
粉末)■CaCuo、 ysL (CaCLとCuOの
950℃焼成粉末)■5rCuo7sL (SrCO3
とCuOの950℃焼結粉末)を用いて、MgO単結晶
基板上に製膜した。各ターゲットの堆積特開は以下の通
りである、■Blo5Pbo、 6層m”’ 9秒■C
aCuo、 75011−’ 50秒■5rCuo 7
501−”40秒 この堆積を1層として400回積層し、約2μ■の薄膜
を得た。得られた薄膜の組成をEPMAiこより分析し
た結果、[Bt+Pbl 1. +oSr+、 ooc
ao、 y6cu+ 5xO8であった。これを780
℃で2時間熱処理後、835℃で65時間熱処理した。
■Blo5Pbo, ow (mixed powder of BlzOz and pbo) ■CaCuo, ysL (950℃ calcined powder of CaCL and CuO) ■5rCuo7sL (SrCO3
and CuO 950° C. sintered powder) was used to form a film on an MgO single crystal substrate. The deposition specifications for each target are as follows: ■Blo5Pbo, 6 layers m"' 9 seconds ■C
aCuo, 75011-' 50 seconds■5rCuo 7
501-" 40 seconds This deposition was made into one layer and laminated 400 times to obtain a thin film of about 2μ. The composition of the obtained thin film was analyzed by EPMAi, and it was found that [Bt+Pbl 1. +oSr+, ooc
ao, y6cu+ 5xO8. This is 780
After heat treatment at 835°C for 2 hours, heat treatment was performed at 835°C for 65 hours.

熱処理後、得られた薄膜の磁気感度を、薄膜表面に対し
て外部印加磁界の方位を変化させながら、液体窒素温度
(77Klで4端子法により測定した。
After the heat treatment, the magnetic sensitivity of the obtained thin film was measured by a four-terminal method at liquid nitrogen temperature (77 Kl) while changing the direction of the externally applied magnetic field with respect to the thin film surface.

磁気感度は、薄膜に臨界電流値(ILLAlより大きい
直流電流f1.0mAl を流した状態で、磁界を0か
62ガウスまで印加すると、膜の抵抗値が増加するに従
い電圧端子間に生じる出力電圧が変化するので、その出
力電圧の値はμV/ガウスで評価した。この値が大きは
と磁気感度が高いことになる。なお、測定電圧の電極間
の長さは15+mmとした。
Magnetic sensitivity is determined by applying a magnetic field from 0 to 62 Gauss with a DC current f1.0 mAl larger than the critical current value (ILLAl) flowing through the thin film.As the resistance value of the film increases, the output voltage generated between the voltage terminals increases. Since the output voltage varies, the value of the output voltage was evaluated in μV/Gauss.The larger this value is, the higher the magnetic sensitivity is.The length between the electrodes for the measurement voltage was 15+mm.

また、得られた薄膜のll0K超伝導体の(00141
回折線を用いてロッキング曲線の測定を行なった結果、
その曲線の半値幅は4.2°であり、十分に配向した試
料であった。測定結果を表−1に示す。
In addition, the (00141
As a result of measuring the rocking curve using diffraction lines,
The half width of the curve was 4.2°, indicating that the sample was well oriented. The measurement results are shown in Table-1.

C以下余白) 表−1 なお、薄膜表面と外部印加磁界の角度θは、磁気方位が
薄膜表面に対し垂直をθ=0とした。
(Margins below) Table 1 The angle θ between the thin film surface and the externally applied magnetic field is set to θ=0 when the magnetic direction is perpendicular to the thin film surface.

上記の結果から、得られた薄膜は1O−5ガウスのオー
グーまでの磁気感度を有し、薄膜の向きを変化させて、
磁界に対し最大の出力電圧を示す薄膜の方向を求めれば
、そのときの薄膜に垂直な方向が磁気方位であり、その
際に磁界強度も高感度で測定される。
From the above results, the obtained thin film has a magnetic sensitivity up to 1O-5 Gauss, and by changing the orientation of the thin film,
If the direction of the thin film that exhibits the maximum output voltage in response to the magnetic field is determined, the direction perpendicular to the thin film at that time is the magnetic direction, and the magnetic field strength can also be measured with high sensitivity.

〔発明の効果] 本発明方法によれば、C軸配向性の優れた酸化物超伝導
薄膜を用いることにより、1O−5ガウスオーダーの感
度が得られ、かつ磁界の方位を容易に求めることができ
る。
[Effects of the Invention] According to the method of the present invention, by using an oxide superconducting thin film with excellent C-axis orientation, sensitivity on the order of 1O-5 Gauss can be obtained, and the direction of the magnetic field can be easily determined. can.

Claims (2)

【特許請求の範囲】[Claims] (1) 磁気抵抗効果が薄膜表面に対する磁気方位の角
度により変化する配向性の高い酸化物超伝導多結晶薄膜
に、その臨界温度未満の温度で、その温度における臨界
電流値以上の電流を印加し、薄膜の向きを変化させ、磁
気抵抗効果により検出された磁界強度が最大となる薄膜
の向きにより磁界の強さ及び方位を測定することを特徴
とする磁気方位検出方法。
(1) At a temperature below its critical temperature, a current higher than the critical current value at that temperature is applied to a highly oriented oxide superconducting polycrystalline thin film whose magnetoresistive effect changes depending on the angle of magnetic orientation with respect to the thin film surface. A method for detecting magnetic orientation, characterized in that the orientation of the thin film is changed, and the strength and orientation of the magnetic field are measured based on the orientation of the thin film where the magnetic field strength detected by the magnetoresistive effect is maximized.
(2) 酸化物超伝導多結晶薄膜が、物理的手法により
製造されたものであり、基板の垂直方向をC軸として、
超伝導粒子のC軸の配向度が15゜以下である請求項(
1)に記載の方法。
(2) The oxide superconducting polycrystalline thin film is manufactured by a physical method, and the C axis is perpendicular to the substrate.
Claim (
The method described in 1).
JP2290909A 1990-10-30 1990-10-30 Magnetic bearing detection method Expired - Lifetime JP2936125B2 (en)

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