JPH0375285A - Production of superconductor - Google Patents
Production of superconductorInfo
- Publication number
- JPH0375285A JPH0375285A JP1210963A JP21096389A JPH0375285A JP H0375285 A JPH0375285 A JP H0375285A JP 1210963 A JP1210963 A JP 1210963A JP 21096389 A JP21096389 A JP 21096389A JP H0375285 A JPH0375285 A JP H0375285A
- Authority
- JP
- Japan
- Prior art keywords
- layer
- superconducting
- ceramic substrate
- oxidation
- oxide superconductor
- 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.)
- Pending
Links
- 239000002887 superconductor Substances 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 14
- 230000003647 oxidation Effects 0.000 claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 239000010410 layer Substances 0.000 abstract description 39
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 229910021344 molybdenum silicide Inorganic materials 0.000 abstract description 3
- WEAMLHXSIBDPGN-UHFFFAOYSA-N (4-hydroxy-3-methylphenyl) thiocyanate Chemical compound CC1=CC(SC#N)=CC=C1O WEAMLHXSIBDPGN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002344 surface layer Substances 0.000 abstract description 2
- 229910021355 zirconium silicide Inorganic materials 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract 2
- TWRSDLOICOIGRH-UHFFFAOYSA-N [Si].[Si].[Hf] Chemical compound [Si].[Si].[Hf] TWRSDLOICOIGRH-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 229910021341 titanium silicide Inorganic materials 0.000 abstract 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 229910052735 hafnium Inorganic materials 0.000 description 3
- -1 hafnium nitride Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WQJQOUPTWCFRMM-UHFFFAOYSA-N tungsten disilicide Chemical compound [Si]#[W]#[Si] WQJQOUPTWCFRMM-UHFFFAOYSA-N 0.000 description 1
- 229910021342 tungsten silicide Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Physical Vapour Deposition (AREA)
- Chemical Vapour Deposition (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、セラミック基板の上に超電導特性に優れる酸
化物超電導体層を形成するようにした超電導体の製造方
法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for manufacturing a superconductor in which an oxide superconductor layer having excellent superconducting properties is formed on a ceramic substrate.
従来の技術
支持基板上に酸化物超電導体の薄層を有する超電導体の
製造方法として、支持基板上にスパッタリング方式等で
酸化物超電導体の薄層を形成する方法が知られている。2. Description of the Related Art As a method for manufacturing a superconductor having a thin layer of oxide superconductor on a support substrate, a method is known in which a thin layer of oxide superconductor is formed on the support substrate by sputtering or the like.
スパッタリング方式等の場合には、層形成過程で超電導
層が形成されるため焼結処理を要しないが、高度な設備
や技術を要して製造効率に劣り、大型品の製造が困難な
問題点があった。In the case of sputtering methods, etc., a superconducting layer is formed during the layer formation process, so sintering is not required, but it requires advanced equipment and technology, resulting in poor manufacturing efficiency and problems that make it difficult to manufacture large products. was there.
発明が解決しようとする課題
前記の問題点に鑑みて本発明者は、酸化物超電導体の粉
末等を展開するなどして薄層を形成し、これを焼結処理
して超電導層とする方法に想到した。この方法によれば
、スパッタリング設備やスパッタリング技術等が不要に
なり、大型品も容易に、かつ効率よく製造することがで
きる。Problems to be Solved by the Invention In view of the above-mentioned problems, the present inventor has devised a method of forming a thin layer by spreading powder of an oxide superconductor, etc., and sintering the thin layer to form a superconducting layer. I came up with this idea. According to this method, sputtering equipment, sputtering technology, etc. are not required, and large products can be manufactured easily and efficiently.
しかしながら薄層の支持基板として酸化物系セラミック
基板を用いた場合、基板の成分が超電導層に拡散して超
電導特性を低下させることが判明した。本発明はかかる
問題の克服を課題とする。However, it has been found that when an oxide-based ceramic substrate is used as a thin layer support substrate, components of the substrate diffuse into the superconducting layer and deteriorate the superconducting properties. The present invention aims to overcome this problem.
課題を解決するための手段
本発明は、表面に耐酸化性金属間化合物の層を有する基
板を用いることにより前記課題を克服したものである。Means for Solving the Problems The present invention overcomes the above problems by using a substrate having a layer of an oxidation-resistant intermetallic compound on its surface.
すなわち本発明は、少なくとも表面が耐酸化性金属間化
合物からなるセラミック基板の上に、酸化物超電導体か
らなる薄層を形成し、これを焼結処理して超電導層を形
成することを特徴とする超電導体の製造方法を提供する
ものである。That is, the present invention is characterized in that a thin layer made of an oxide superconductor is formed on a ceramic substrate at least the surface of which is made of an oxidation-resistant intermetallic compound, and this is sintered to form a superconducting layer. The present invention provides a method for manufacturing a superconductor.
実施例
本発明において用いるセラミック基板は、少なくとも超
電導層を形成する面を耐酸化性金属間化合物で形成した
ものである。従って外周を耐酸化性金属間化合物の層で
被覆した形態のものや、全体を耐酸化性金属間化合物で
形成したものなどであってもよい。基板を構成するセラ
ミックについては特に限定はない。一般には、耐酸化性
金属間化合物ノホカ、Ｍｇ Ｏ１Ｙ Ｓ Ｚ １Ａ ｌ
２０ ｓ 、Ｓ ｉｏ ２、Ｓ ｒ Ｔ ｉ Ｏ３な
どからなるものが用いられる。EXAMPLE The ceramic substrate used in the present invention has at least the surface on which the superconducting layer is formed made of an oxidation-resistant intermetallic compound. Therefore, the outer periphery may be coated with a layer of an oxidation-resistant intermetallic compound, or the entire structure may be made of an oxidation-resistant intermetallic compound. There are no particular limitations on the ceramic that constitutes the substrate. Generally, oxidation-resistant intermetallic compound Nohoka, Mg O1Y S Z 1A l
20 s , S io 2 , S r T i O3, etc. are used.
基板の厚さは適宜に決められ、通例３鴎以下である。耐
酸化性金属間化合物としては例えば、ケイ化モリブデン
、ケイ化ジルコニウム、ケイ化タングステンの如きシリ
サイド、窒化ハフニウム、窒化チタンの如き金属窒化物
などが用いられる。基板の表層のみに耐酸化性金属間化
合物の層を形成する方式としては例えば、マグネトロン
スパッタリング方式やイオンブレーティング方式の如き
ＰＶＤ方式、ＣｖＤ方式、活性化化成蒸着方式、有機物
熱分解方式などがあげられる。The thickness of the substrate is determined appropriately and is usually 3 mm or less. Examples of oxidation-resistant intermetallic compounds used include silicides such as molybdenum silicide, zirconium silicide, and tungsten silicide, and metal nitrides such as hafnium nitride and titanium nitride. Examples of methods for forming an oxidation-resistant intermetallic compound layer only on the surface layer of the substrate include PVD methods such as magnetron sputtering method and ion blating method, CvD method, activated chemical vapor deposition method, and organic material thermal decomposition method. It will be done.
セラミック基板の耐酸化性金属間化合物面の上に付与す
る酸化物超電導体からなる薄層は、ゾル・ゲル法、有機
物熱分解法、噴霧熱分解法など、適宜な方式で形成して
よい。形成する薄層の厚さは任意である。一般には２Ｏ
ｎ以下とされる。The thin layer of the oxide superconductor provided on the oxidation-resistant intermetallic compound surface of the ceramic substrate may be formed by any suitable method, such as a sol-gel method, an organic material pyrolysis method, or a spray pyrolysis method. The thickness of the formed thin layer is arbitrary. Generally 2O
n or less.
薄層を形成する酸化物超電導体についても特に限定はな
い。ＹＢａｚ Ｃｕ３０ｙの如きＹ系酸化物超電導体、
Ｂｉａ Ｓｒ２ Ｃａ２ Ｃｕ３０ｙの如きＢｉ系酸化
物超電導体、その他Ｌａ系酸化物超電導体、ＴＩ系酸化
物超電導体など、また前記のＹ等の成分を他の希土類元
素で置換したもの、ないしＢａ等の成分を他のアルカリ
土類金属で置換したものなど公知のいずれの酸化物超電
導体からなっていてもよい。There are no particular limitations on the oxide superconductor that forms the thin layer. Y-based oxide superconductor such as YBaz Cu30y,
Bi-based oxide superconductors such as Bia Sr2 Ca2 Cu30y, other La-based oxide superconductors, TI-based oxide superconductors, etc., and those in which the above-mentioned components such as Y are replaced with other rare earth elements, or those such as Ba etc. It may be made of any known oxide superconductor, such as one whose components are replaced with other alkaline earth metals.
耐酸化性金属間化合物の面上に形成した酸化物超電導体
からなる薄層の焼結処理は、酸化物超電導体の種類等に
応じ適宜な温度で行ってよい。−船釣な焼結温度は、８
００〜１０００℃である。また焼結時間は、通例２５０
時間以下、就中２〜２００時°間であるがこれに限定さ
れない。焼結処理により酸化物超電導体系の粒子ないし
粉末が結合して一体化し、超電導体の連続層を形成する
と共に、基板とも密着する。The sintering treatment of the thin layer of the oxide superconductor formed on the surface of the oxidation-resistant intermetallic compound may be performed at an appropriate temperature depending on the type of the oxide superconductor. -The sintering temperature for boat fishing is 8
00-1000°C. The sintering time is usually 250
The duration is not limited to 2 to 200 hours, particularly 2 to 200 hours. The sintering process binds and integrates the particles or powders of the oxide superconductor to form a continuous layer of superconductor and also adheres closely to the substrate.
なお本発明において、酸化物超電導体からなる薄層が有
機物を含有する場合には必要に応じ、焼結処理前に熱分
解して薄層中の有機成分を除去してもよい。In the present invention, if the thin layer made of an oxide superconductor contains organic substances, the organic components in the thin layer may be removed by thermal decomposition before the sintering process, if necessary.
発明の効果
本発明によれば、耐酸化性金属間化合物の面上に酸化物
超電導体の薄層を設けて焼結処理するようにしたので、
形成される超電導層へのセラミック成分の拡散を阻止で
きて、臨界温度等の超電導特性に優れる超電導層を有す
るセラミック基板を得ることができる。Effects of the Invention According to the present invention, a thin layer of oxide superconductor is provided on the surface of the oxidation-resistant intermetallic compound and then sintered.
It is possible to obtain a ceramic substrate having a superconducting layer that can prevent diffusion of ceramic components into the formed superconducting layer and has excellent superconducting properties such as critical temperature.
実施例１
８０℃に加温した純プロピオン酸１００ｍ１に、酢酸イ
ツトリウム０．００７モル、酢酸バリウム０．０１４モ
ル及び酢酸鋼０．０２１モルを溶解させてなる溶液に、
厚さ０．５−の酸化マグネシウム多結晶板の外周に厚さ
１．５ｕ−の窒化ハフニウム層を設けてなるセラミック
基板を浸漬し、０．２ｍ／秒の速度で引き上げて基板上
にプロピオン酸溶液を塗布し、１時間自然乾燥させたの
ち０．ＩＴｏｒｒ ｓ １５０℃の条件で１時間真空加
熱乾燥し、これを４５０℃で１時間加熱処理して塗布層
（ゲル）を熱分解させた。Example 1 In a solution prepared by dissolving 0.007 mol of yttrium acetate, 0.014 mol of barium acetate and 0.021 mol of steel acetate in 100 ml of pure propionic acid heated to 80°C,
A ceramic substrate consisting of a 1.5 u-thick hafnium nitride layer provided on the outer periphery of a 0.5-thick magnesium oxide polycrystalline plate is immersed and pulled up at a speed of 0.2 m/sec to coat the substrate with propionic acid. After applying the solution and letting it air dry for 1 hour, it became 0. It was dried under vacuum heat at 150° C. for 1 hour, and then heated at 450° C. for 1 hour to thermally decompose the coated layer (gel).
前記の浸漬−乾燥一億布層の熱分解操作を５回、繰り返
したのち、酸素雰囲気下９５０℃で１２０分間加熱し、
さらに４００℃で５時間加熱してＹＢａｚ Ｃｕ５Ｏ７
系の単一層からなる厚さ４．７＃ｎｅの超電導層が表面
に強固に密着したセラミック基板を得た。After repeating the pyrolysis operation of the soaked and dried 100 million cloth layers 5 times, the mixture was heated at 950°C for 120 minutes in an oxygen atmosphere,
Further heat at 400℃ for 5 hours to produce YBaz Cu5O7
A ceramic substrate was obtained in which a 4.7#ne thick superconducting layer consisting of a single layer of the system was firmly adhered to the surface.
実施例２
セラミック基板として、表面に厚さ２ｎのケイ化モリブ
デン層を形成した厚さ１閣のＹＳｚ基板を用いたほかは
実施例１に準じてセラミック基板に強固に密着した超電
導層を得た。Example 2 A superconducting layer firmly adhered to a ceramic substrate was obtained according to Example 1, except that a YSz substrate with a thickness of 1 mm on which a 2n-thick molybdenum silicide layer was formed on the surface was used as the ceramic substrate. .
比較例
セラミック基板として、窒化ハフニウム層を有しない酸
化マグネシウム基板を用いたほかは実施例１に準じて超
電導層を得た。Comparative Example A superconducting layer was obtained according to Example 1, except that a magnesium oxide substrate without a hafnium nitride layer was used as the ceramic substrate.
評価試験
実施例、比較例で得たセラミック基板上の超電導層につ
き臨界温度（Ｔｃ）を調べた。臨界温度は、０．１Ａ／
ｃｊの電流密度下、液体ヘリウムで冷却しなから４端子
法により電気抵抗の温度による変化を測定し、電圧端子
間の発生電圧がＯとなったときの温度である。The critical temperature (Tc) of the superconducting layer on the ceramic substrate obtained in the evaluation test example and comparative example was investigated. The critical temperature is 0.1A/
The change in electrical resistance due to temperature was measured by the four-terminal method without cooling with liquid helium under a current density of cj, and this is the temperature when the voltage generated between the voltage terminals becomes O.
結果を表に示した。The results are shown in the table.
Claims (1)
ラミック基板の上に、酸化物超電導体からなる薄層を形
成し、これを焼結処理して超電導層を形成することを特
徴とする超電導体の製造方法。1. Production of a superconductor characterized by forming a thin layer made of an oxide superconductor on a ceramic substrate at least the surface of which is made of an oxidation-resistant intermetallic compound, and sintering this to form a superconducting layer. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1210963A JPH0375285A (en) | 1989-08-16 | 1989-08-16 | Production of superconductor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1210963A JPH0375285A (en) | 1989-08-16 | 1989-08-16 | Production of superconductor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0375285A true JPH0375285A (en) | 1991-03-29 |
Family
ID=16598015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1210963A Pending JPH0375285A (en) | 1989-08-16 | 1989-08-16 | Production of superconductor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0375285A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008057270A (en) * | 2006-09-01 | 2008-03-13 | Bunka Shutter Co Ltd | Opening-closing door device |
-
1989
- 1989-08-16 JP JP1210963A patent/JPH0375285A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008057270A (en) * | 2006-09-01 | 2008-03-13 | Bunka Shutter Co Ltd | Opening-closing door device |
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