JPH0443860B2 - - Google Patents
Info
- Publication number
- JPH0443860B2 JPH0443860B2 JP900089A JP900089A JPH0443860B2 JP H0443860 B2 JPH0443860 B2 JP H0443860B2 JP 900089 A JP900089 A JP 900089A JP 900089 A JP900089 A JP 900089A JP H0443860 B2 JPH0443860 B2 JP H0443860B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- present
- superconducting
- becomes
- temperature
- 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
Links
- 239000011521 glass Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims 1
- 239000013078 crystal Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 239000010931 gold Substances 0.000 description 7
- 239000002887 superconductor Substances 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 4
- 239000005751 Copper oxide Substances 0.000 description 4
- 229910005793 GeO 2 Inorganic materials 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- 229910000431 copper oxide Inorganic materials 0.000 description 4
- 238000004031 devitrification Methods 0.000 description 4
- 230000005292 diamagnetic effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 3
- 229910004116 SrO 2 Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000002667 nucleating agent Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 239000003484 crystal nucleating agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008689 nuclear function Effects 0.000 description 1
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Description
〔産業上の利用分野〕
本発明は高温超電導結晶化ガラスの製造方法に
関する。
〔従来の技術〕
高温酸化物超電導材料の制御法は、原料粉末を
焼いて固める焼結法と、原料粉末を溶融したのち
加熱処理をして製造する溶融法の二つに大別され
る。
いずれの方法もすでに多くの提案がなされてい
る。
ところで、これらの方法で製造された超電導材
料は、その成形、加工が困難である。
しかしながら、最近では膜状、リボン状、糸状
体など各種の形状のものが要求されるようになつ
て来た。
〔発明が解決しようとする課題〕
従来の溶融法による製造方法では、ガラス状溶
融物より急冷固化して、各種の形状に加工する際
に失透現象が起こりやすく、加工が困難であつ
た。
これは原料構成元素が極めてガラス化しにくい
ものであり、しかも限定された成分でなければ酸
化物超電導体にならないためである。
換言すれば、超電導特性を示すためには組成的
にガラス化が困難であり、失透しやすい範囲にあ
るのが通常である。
そこで本発明は、かかる従来の溶融法の欠点を
解消し、超電導体としての特性を保持しながら、
膜状体、リボン状体、糸状体など各種の形状に容
易に加工することができる超電導体の製造方法を
提供することを目的とするものである。
〔課題を解決するための手段〕
上記目的を達成する本発明の高温超電導結晶化
ガラスの製造方法は、GeO2またはGa2O33.7〜4.9
重量％、Bi2O339.0〜39.5重量％、SrO220.1〜20.3
重量％、CaO9.4〜9.5重量％およびCuO26.6〜
27.0重量％からなる混合粉末100重量部に、Auま
たはPt0.02〜0.08重量部を配合し、この配合物を
加熱溶融してガラスを製造し、このガラスを熱処
理して結晶化させることを特徴とするものであ
る。
本発明により得られる高温超電導結晶化ガラス
の超電導特性は、絶対温度77〜80Kにおいて電気
抵抗が０（ゼロ）となる。またこのときの反磁性
帯磁率は−3.4〜−4.0×10-3emu／ｇを示してい
る。結晶粒子の大きさは３〜7μmの範囲にある。
本発明における出発原料は、GeO2またはGa2
O3，Bi2O3，SrO2，CaOおよびCuOからなる混合
粉末に、AuまたはPtを配合することにより調製
される。その構成成分限定理由は次のとおりであ
る。なお、以下の説明における％は特記ない限
り、重量％である。
GeO2（酸化ゲルマニウム）またはGa2O3（酸化
ガリウム）は本発明において溶融状態にあるガラ
スが急冷して固化するに際して失透防止の役目を
する。
GeO2またはGa2O3が4.9％を超えると超電導特
性が著しく欠化し、一方、3.7％に満たないと失
透防止の効果が損失する。
Bi2O3（酸化ビスマス）は超電導体を構成する
結晶の必須成分であり、Bi2O3が39.5％を超える
と半導体となる。また39.0％に満たないと、非超
電導相になる。
SrO2（酸化ストロンチウム）も超電導体を構成
する結晶の必須成分であり、SrO2が20.3％を超え
ると半導体となる。また20.1％に満たないと非超
電導相になる。
更に、CaO（酸化カルシウム）は、超電導体を
構成する結晶の必須成分であり、CaOが9.5％を
超えると半導体となる。また9.4％に満たないと、
非超電導相になる。
更にまた、CuO（酸化銅）は超電導体を構成す
る結晶の必須成分であり、CuOは27.0％を超える
と半導体となり、26.6％に満たないと非超電導相
になる。
Au（金）またはPt（白金）はガラスを熱処理し
て結晶化させる際に、結晶核形成剤の役目をす
る。この形成核形成剤によつて、結晶粒子を小さ
くすることが可能となり、機械的強度を大きくす
ることができる。
AuまたはPtが0.08％を超えると結晶核として
の作用が損失する。また0.02％に満たないときは
結晶核としての効果が期待できない。
本発明においては上記組成に調合された出発原
料を十分に混合し、これを耐熱容器、例えばアル
ミナるつぼに入れ、蓋をして加熱溶融してガラス
を製造する。この加熱溶融処理は、温度1150〜
1180℃において12〜15分間を要して行なわれる。
ついで、この溶融物をできる限り急冷状態で所用
の成形体に成形し、成形体を810〜820℃で酸素雰
囲気中で加熱処理する。
昇温時間はその成形体に応じた適当な速度、好
ましくは100℃／２時間よりもよりゆつくりした
速度が望ましい。
なお、本発明において、結晶核形成剤である
AuまたはPtはコロイドの状態で均一にガラス中
に存在することが必要である。
このために、AuまたはPtを塩化金
（HAuCl4・4H2Ｏ）またはヘキサクロロ白金酸
（H2PtCl6・6H2Ｏ）の水溶液の形で出発原料混合
物に導入することが好ましい。
以下、本発明の実施例を述べる。
〔実施例〕
各原料を採取して下記第１表に示す成分組成を
有する出発原料(1)〜(6)を調製した。
これをアルミナるつぼに装入し、蓋をして温度
1150〜1180℃で加熱し、12〜15分間を要して溶融
した。
この溶融物を−20℃以下に冷却した黒鉛板上に
流し出して厚さ1.5mmの薄板を得た。
Ｘ線測定では、完全にガラスであることを認め
た。このガラスを温度810〜820℃で酸素雰囲気中
で加熱処理をした。この結果、ガラスは完全に結
晶体に変化した。結晶粒子の大きさは、３〜7μm
であつた。得られた結晶体に間隔が約２mmになる
ように銀ペーストで電極を４本形成した。
これを所定の温度に冷却した電気抵抗測定装置
に挿入して電気抵抗値の変化を測定した。また同
じように反磁性帯磁率を測定した。測定結果を第
１表に示す。
第１表から明らかなように、本発明により得ら
れた結晶化ガラスは、絶対温度77〜80Kにおいて
その電気抵抗値がゼロになる。また反磁性磁率は
−3.4〜−4.0×10-3emu／ｇである。
[Industrial Field of Application] The present invention relates to a method for producing high-temperature superconducting crystallized glass. [Prior Art] Methods for controlling high-temperature oxide superconducting materials can be roughly divided into two types: sintering methods in which raw material powder is baked and solidified, and melting methods in which raw material powders are melted and then heat treated to produce them. Many proposals have already been made for both methods. However, superconducting materials produced by these methods are difficult to mold and process. However, in recent years, various shapes such as membrane-like, ribbon-like, and filamentous shapes have become required. [Problems to be Solved by the Invention] In the conventional manufacturing method using the melting method, a glassy melt is rapidly solidified and devitrification tends to occur when processing it into various shapes, making processing difficult. This is because the constituent elements of the raw material are extremely difficult to vitrify, and furthermore, unless the ingredients are in a limited range, the oxide superconductor cannot be formed. In other words, in order to exhibit superconducting properties, it is difficult to vitrify the composition, and it is usually within a range where devitrification is likely to occur. Therefore, the present invention eliminates the drawbacks of the conventional melting method, maintains the properties of a superconductor, and
The object of the present invention is to provide a method for manufacturing a superconductor that can be easily processed into various shapes such as a film-like body, a ribbon-like body, and a filament-like body. [Means for Solving the Problems] The method for producing high-temperature superconducting crystallized glass of the present invention that achieves the above object includes GeO 2 or Ga 2 O 3 3.7 to 4.9
wt%, Bi2O3 39.0-39.5 wt%, SrO2 20.1-20.3
wt%, CaO9.4~9.5wt% and CuO26.6~
It is characterized by blending 0.02 to 0.08 parts by weight of Au or Pt with 100 parts by weight of mixed powder consisting of 27.0% by weight, heating and melting this mixture to produce glass, and heat-treating this glass to crystallize it. That is. The superconducting property of the high temperature superconducting crystallized glass obtained by the present invention is that the electrical resistance becomes 0 (zero) at an absolute temperature of 77 to 80K. Moreover, the diamagnetic susceptibility at this time is −3.4 to −4.0×10 −3 emu/g. The crystal grain size ranges from 3 to 7 μm. The starting material in the present invention is GeO 2 or Ga 2
It is prepared by blending Au or Pt into a mixed powder consisting of O 3 , Bi 2 O 3 , SrO 2 , CaO and CuO. The reason for limiting the constituent components is as follows. Note that % in the following description is by weight unless otherwise specified. In the present invention, GeO 2 (germanium oxide) or Ga 2 O 3 (gallium oxide) serves to prevent devitrification when glass in a molten state is rapidly cooled and solidified. If GeO 2 or Ga 2 O 3 exceeds 4.9%, superconducting properties will be significantly lost, while if it is less than 3.7%, the effect of preventing devitrification will be lost. Bi 2 O 3 (bismuth oxide) is an essential component of the crystals that make up superconductors, and when Bi 2 O 3 exceeds 39.5%, it becomes a semiconductor. Moreover, if it is less than 39.0%, it becomes a non-superconducting phase. SrO 2 (strontium oxide) is also an essential component of the crystals that make up superconductors, and when SrO 2 exceeds 20.3%, it becomes a semiconductor. Also, if it is less than 20.1%, it becomes a non-superconducting phase. Furthermore, CaO (calcium oxide) is an essential component of the crystals that make up superconductors, and when CaO exceeds 9.5%, it becomes a semiconductor. Also, if it is less than 9.4%,
becomes a non-superconducting phase. Furthermore, CuO (copper oxide) is an essential component of the crystals that make up superconductors; when CuO exceeds 27.0%, it becomes a semiconductor, and when it is less than 26.6%, it becomes a non-superconducting phase. Au (gold) or Pt (platinum) acts as a crystal nucleation agent when glass is heat-treated to crystallize it. This nucleating agent makes it possible to reduce the size of crystal grains and increase mechanical strength. When Au or Pt exceeds 0.08%, the crystal nucleus function is lost. Furthermore, if the content is less than 0.02%, no effect as a crystal nucleus can be expected. In the present invention, the starting materials prepared in the above composition are thoroughly mixed, placed in a heat-resistant container such as an alumina crucible, covered with a lid, and heated and melted to produce glass. This heat melting process is performed at a temperature of 1150~
It takes 12 to 15 minutes at 1180°C.
Next, this melt is cooled as rapidly as possible to form a desired molded body, and the molded body is heat-treated at 810 to 820° C. in an oxygen atmosphere. The heating time is determined at an appropriate rate depending on the molded article, preferably at a rate slower than 100°C/2 hours. In addition, in the present invention, the crystal nucleating agent
Au or Pt needs to exist uniformly in the glass in a colloidal state. For this purpose, it is preferred to introduce Au or Pt into the starting material mixture in the form of an aqueous solution of gold chloride (HAuCl 4 .4H 2 O) or hexachloroplatinic acid (H 2 PtCl 6 .6H 2 O). Examples of the present invention will be described below. [Example] Each raw material was collected to prepare starting materials (1) to (6) having the component compositions shown in Table 1 below. Charge this into an alumina crucible, cover with a lid, and
It was heated at 1150-1180°C and melted for 12-15 minutes. This melt was poured onto a graphite plate cooled to below -20°C to obtain a thin plate with a thickness of 1.5 mm. X-ray measurements confirmed that it was completely glass. This glass was heat-treated at a temperature of 810 to 820°C in an oxygen atmosphere. As a result, the glass completely transformed into a crystalline substance. The size of crystal particles is 3 to 7 μm
It was hot. Four electrodes were formed using silver paste on the obtained crystal body with an interval of about 2 mm. This was inserted into an electrical resistance measuring device cooled to a predetermined temperature, and changes in electrical resistance were measured. Diamagnetic susceptibility was also measured in the same manner. The measurement results are shown in Table 1. As is clear from Table 1, the electrical resistance value of the crystallized glass obtained by the present invention becomes zero at an absolute temperature of 77 to 80K. Moreover, the diamagnetic magnetic constant is -3.4 to -4.0×10 −3 emu/g.
以上詳述した如く、本発明の新規な組成のガラ
スを用いて製造した高温超電導結晶化ガラスは液
体窒素（77K）の温度域で電気抵抗がゼロになる
特性を有し、また反磁性帯磁率が認められた。
本発明の製造方法によれば、各種の形状のもの
を特別の設備や操作を必要とせずに安定的に製造
することができる。
従つて得られた成形体は、各種の産業機器、
種々の環境で使用されるセンサー用検知材料とし
て開発が期待される。
As detailed above, the high-temperature superconducting crystallized glass manufactured using the glass with the new composition of the present invention has the characteristic that the electrical resistance becomes zero in the temperature range of liquid nitrogen (77K), and the diamagnetic susceptibility was recognized. According to the manufacturing method of the present invention, products of various shapes can be stably manufactured without requiring special equipment or operations. Therefore, the obtained molded body can be used for various industrial equipment,
It is expected to be developed as a sensing material for sensors used in various environments.
第１図は本発明で得られた高温超電導結晶化ガ
ラスの絶対温度と電気抵抗値との相関を示す図で
ある。
FIG. 1 is a diagram showing the correlation between the absolute temperature and the electrical resistance value of the high-temperature superconducting crystallized glass obtained by the present invention.
Claims (1)
39.0〜39.5重量％、SrO220.1〜20.3重量％、
CaO9.4〜9.5重量％およびCuO26.6〜27.0重量％
からなる混合粉末100重量部に、AuまたはPt0.02
〜0.08重量部を配合し、この配合物を加熱溶融し
てガラスを製造し、このガラスを熱処理して結晶
化させることを特徴とする高温超電導結晶化ガラ
スの製造方法。1 GeO2 or Ga2O3 3.7-4.9 % by weight , Bi2O3
39.0-39.5 wt%, SrO2 20.1-20.3 wt%,
CaO9.4-9.5 wt% and CuO26.6-27.0 wt%
100 parts by weight of mixed powder consisting of Au or Pt0.02
A method for producing high-temperature superconducting crystallized glass, which comprises blending ~0.08 parts by weight of the blend, heating and melting the blend to produce glass, and heat-treating the glass to crystallize it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP900089A JPH02188445A (en) | 1989-01-17 | 1989-01-17 | Production of high-temperature superconducting crystallized glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP900089A JPH02188445A (en) | 1989-01-17 | 1989-01-17 | Production of high-temperature superconducting crystallized glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02188445A JPH02188445A (en) | 1990-07-24 |
| JPH0443860B2 true JPH0443860B2 (en) | 1992-07-17 |
Family
ID=11708409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP900089A Granted JPH02188445A (en) | 1989-01-17 | 1989-01-17 | Production of high-temperature superconducting crystallized glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02188445A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105565662A (en) * | 2016-01-20 | 2016-05-11 | 广西丛欣实业有限公司 | Method for preparing heat-resistant glass |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5413981A (en) * | 1991-01-31 | 1995-05-09 | Mitsubishi Denki Kabushiki Kaisha | Oxide superconductor and a method for manufacturing an oxide superconductor |
-
1989
- 1989-01-17 JP JP900089A patent/JPH02188445A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105565662A (en) * | 2016-01-20 | 2016-05-11 | 广西丛欣实业有限公司 | Method for preparing heat-resistant glass |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02188445A (en) | 1990-07-24 |
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