JPH0471875B2 - - Google Patents
Info
- Publication number
- JPH0471875B2 JPH0471875B2 JP62109517A JP10951787A JPH0471875B2 JP H0471875 B2 JPH0471875 B2 JP H0471875B2 JP 62109517 A JP62109517 A JP 62109517A JP 10951787 A JP10951787 A JP 10951787A JP H0471875 B2 JPH0471875 B2 JP H0471875B2
- Authority
- JP
- Japan
- Prior art keywords
- cuo
- single crystal
- mol
- lanthanum
- melt
- 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
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 32
- 239000013078 crystal Substances 0.000 claims description 27
- 239000000155 melt Substances 0.000 claims description 9
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 5
- FQVNUZAZHHOJOH-UHFFFAOYSA-N copper lanthanum Chemical compound [Cu].[La] FQVNUZAZHHOJOH-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000013081 microcrystal Substances 0.000 claims description 4
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 description 17
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 13
- 238000010586 diagram Methods 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- 239000006104 solid solution Substances 0.000 description 7
- 238000007716 flux method Methods 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Chemical group 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229910052802 copper Chemical group 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/225—Complex oxides based on rare earth copper oxides, e.g. high T-superconductors
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N60/00—Superconducting devices
- H10N60/80—Constructional details
- H10N60/85—Superconducting active materials
- H10N60/855—Ceramic superconductors
- H10N60/857—Ceramic superconductors comprising copper oxide
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Description
【発明の詳細な説明】
[産業上の利用分野]
この発明はフラツクス法による銅製ランタン
(La2CuO4)単結晶の製造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 producing copper lanthanum (La 2 CuO 4 ) single crystal by a flux method.
[従来の技術]
La2CuO4は層状ペロブスカイト構造をもつ酸化
物で、La原子の位置をBaあるいはSr原子で少量
置き換えることにより低温で超伝導を示し、その
転移温度は30〜40kにもなり、極低温素子として
これからの応用が考えられる。そのため大型良質
の単結晶が望まれ、その製造方法の開発が望まれ
ている。[Prior art] La 2 CuO 4 is an oxide with a layered perovskite structure, which exhibits superconductivity at low temperatures by replacing a small amount of La atoms with Ba or Sr atoms, and its transition temperature is as high as 30 to 40 k. , future applications as cryogenic devices are possible. Therefore, large-sized, high-quality single crystals are desired, and the development of methods for producing them is desired.
従来育成されている5×5×1mm程度の大きさ
の結晶の写真は公表されているが、製造方法の詳
細は全く公表されていない。 Although photographs of conventionally grown crystals of approximately 5 x 5 x 1 mm in size have been published, the details of the manufacturing method have not been made public at all.
[発明が解決しようとする問題点]
フラツクス法における結晶育成には目的の単結
晶を析出させる融剤とその組成範囲および結晶育
成温度範囲が明らかにされなければならず、その
ためには相平衡図が必要になる。[Problems to be solved by the invention] For crystal growth in the flux method, it is necessary to clarify the flux that precipitates the desired single crystal, its composition range, and crystal growth temperature range. is required.
[問題点を解決するための手段]
上記の問題点を解決するために、本発明は、
La2O3−CuO系の相平衡図を作成し、それを指針
にしてLa2CuO4単結晶を育成するものである。本
発明は酸化ランタンおよび炭酸ランタンのうちの
少なくとも一種を28.9〜7.1モル%、酸化銅を71.1
〜92.9モル%に混合して1040〜1330℃に加熱融解
したのち、その融液を徐冷させることにより一般
式La2CuO4で表わされる微結晶を析出させ、微結
晶を融液中で結晶育成させることを特徴とする。[Means for Solving the Problems] In order to solve the above problems, the present invention includes the following:
A phase equilibrium diagram of the La 2 O 3 -CuO system is created, and a La 2 CuO 4 single crystal is grown using it as a guideline. The present invention contains 28.9 to 7.1 mol% of at least one of lanthanum oxide and lanthanum carbonate and 71.1 mol% of copper oxide.
After mixing at ~92.9 mol% and heating and melting at 1040-1330°C, the melt is slowly cooled to precipitate microcrystals represented by the general formula La 2 CuO 4 , and the microcrystals are crystallized in the melt. It is characterized by being cultivated.
[作用]
示差熱分析と急冷加熱法を行い、その試料をX
線回折した結果から、第1図に示すLa2O3−CuO
系の相平衡図を作成した。図中、黒点で示すもの
が測定結果である。[Effect] Perform differential thermal analysis and rapid cooling heating method, and test the sample with
From the results of line diffraction, we found that La 2 O 3 −CuO shown in Figure 1
A phase equilibrium diagram of the system was created. In the figure, the black dots indicate the measurement results.
第1図からLa2CuO4単結晶は液相線ABの組成
比、即ちLa2O3が28.9〜7.1モル%、CuOが71.1〜
92.9モル%の範囲の組成の融液から、約1330〜
1040℃の温度領域で析出すると考えられる。即ち
上述した組成の融液を徐冷すると、融液の組成は
液相線ABに沿つてCuO側へずれ、La2CuO4が固
相となつて析出し、冷却とともに成長する。 From Figure 1, the La 2 CuO 4 single crystal has a composition ratio of liquidus line AB, that is, La 2 O 3 is 28.9 to 7.1 mol%, CuO is 71.1 to 7.1 mol%.
From a melt with a composition in the range of 92.9 mol%, approximately 1330 ~
It is thought that it precipitates in the temperature range of 1040℃. That is, when a melt having the above-mentioned composition is slowly cooled, the composition of the melt shifts toward the CuO side along the liquidus line AB, and La 2 CuO 4 becomes a solid phase, precipitates, and grows as it cools.
融液の組成が共晶点BよりCuO側であれば、冷
却時にまずCuOが析出し、融液の組成がA点より
La2O3側であれば、冷却時にまずLa2O3側の結晶
が析出し、いずれもLa2CuO4は析出成長すること
ができない。 If the composition of the melt is closer to CuO than the eutectic point B, CuO will precipitate first during cooling, and the composition of the melt will be closer to the CuO point than the eutectic point B.
If it is on the La 2 O 3 side, crystals on the La 2 O 3 side precipitate first during cooling, and La 2 CuO 4 cannot precipitate and grow in either case.
なお、La2CuO4単結晶のLa原子、Cu原子の位
置に何らかの異種元素が少量混入しても、その相
平衡図が定性的に第1図のLa2O3−CuO系の相平
衡図と本質的に変らない場合には、溶液中に少量
の異種元素を混入することにより、上記と全く同
じ方法によつて異種元素を混入したLa2CuO4固溶
体単結晶を製造することも可能である。例えば、
Sr,Ba等の異種元素が少量混入したLa2CuO4固
溶体単結晶を製造することができる。 Furthermore, even if a small amount of some kind of foreign element is mixed into the La 2 CuO 4 single crystal La atom or Cu atom position, the phase equilibrium diagram will qualitatively be the same as the phase equilibrium diagram of the La 2 O 3 -CuO system in Figure 1. If there is essentially no difference between be. for example,
It is possible to produce a La 2 CuO 4 solid solution single crystal containing a small amount of different elements such as Sr and Ba.
[実施例] 次にこの発明の実施例を説明する。[Example] Next, embodiments of this invention will be described.
実施例 1
La2CuO4単結晶をフラツクス法によつて製造し
た。Example 1 A La 2 CuO 4 single crystal was produced by a flux method.
La2O3とCuOをモル比にして20:80に混合し、
その混合物100gを直径50mm高さ40mmの白金るつ
ぼに入れ、アルミナの蓋をし、そらをさらにアル
ミナの蓋付るつぼに入れ、さらに蓋付の耐火箱に
入れ、酸化銅の蒸発を防ぐため3重に密封した。
それをマツフル炉に入れ約1350℃に加熱し2時間
おいたのちに約8℃/hで1050℃まで降温し、後
は200℃/hで室温まで降温した。この結果、固
化したフラツクス中から8×8×2mmの大きさの
La2CuO4単結晶が得られた。 Mix La 2 O 3 and CuO in a molar ratio of 20:80,
Put 100g of the mixture into a platinum crucible with a diameter of 50 mm and a height of 40 mm, cover with an alumina lid, put the crucible into an alumina crucible with a lid, and then put it into a fireproof box with a lid. sealed in.
The mixture was placed in a Matsufuru furnace and heated to about 1350°C for 2 hours, then the temperature was lowered to 1050°C at a rate of about 8°C/h, and then to room temperature at a rate of 200°C/h. As a result, from the solidified flux a piece of 8 x 8 x 2 mm was found.
A La 2 CuO 4 single crystal was obtained.
実施例 2
(La0.9Ba0.1)2CuO4なる組成についてフラツクス
法によつて固溶体単結晶を製造した。Example 2 A solid solution single crystal having the composition (La 0.9 Ba 0.1 ) 2 CuO 4 was produced by a flux method.
90モル%La2O3+10モル%2BaCO3なる組成の
混合物とCuOをモル比にして20:80に混合し、実
施例1と同様の操作により同様の経過を経て8×
8×1mmの(La0.9Ba0.1)2CuO4固溶体単結晶を得
た。 A mixture with a composition of 90 mol% La 2 O 3 + 10 mol% 2BaCO 3 and CuO were mixed at a molar ratio of 20:80, and a mixture of 8×
A (La 0.9 Ba 0.1 ) 2 CuO 4 solid solution single crystal of 8×1 mm was obtained.
実施例 3
(La0.9Sr0.1)2CuO4なる組成についてフラツク
ス法によつて固溶体単結晶を製造した。Example 3 A solid solution single crystal having the composition (La 0.9 Sr 0.1 ) 2 CuO 4 was produced by a flux method.
90モル%La2O3+10モル%2SrCO3なる組成の
混合物とCuOをモル比にして20:80に混合し、実
施例1と同様の操作により同様の経過を経て2×
4×0.5mmの(La0.9Sr0.1)2CuO4固溶体単結晶を得
た。 A mixture with a composition of 90 mol% La 2 O 3 + 10 mol% 2SrCO 3 and CuO were mixed at a molar ratio of 20:80, and a mixture of 2×
A (La 0.9 Sr 0.1 ) 2 CuO 4 solid solution single crystal of 4×0.5 mm was obtained.
なお、実施例2および3ではLa原子位置を少
量の異種元素(BaまたはSr)で置き換えたが、
これは相平衡図が定性的に第1図のLa2O3−CuO
系の相平衡図と本質的に変らない場合には溶液に
少量の異種元素を混入することにより、異種元素
の混入したLa2CuO4固溶体単結晶を製造すること
が可能であることを示している。これと同様に
Cuの位置に少量の異種元素を混入しても、定性
的に上記の相平衡図が本質的に変らない場合には
同様に異種元素を混入したLa2CuO4固溶体単結晶
を得ることができる。 In addition, in Examples 2 and 3, the La atom position was replaced with a small amount of a different element (Ba or Sr),
This is because the phase equilibrium diagram qualitatively shows La 2 O 3 −CuO in Figure 1.
It was shown that it is possible to produce a La 2 CuO 4 solid solution single crystal containing a different element by mixing a small amount of the different element into the solution if it is essentially the same as the phase equilibrium diagram of the system. There is. Similarly to this
Even if a small amount of a different element is mixed in the position of Cu, if the above phase equilibrium diagram does not essentially change qualitatively, a La 2 CuO 4 solid solution single crystal mixed with a different element can be obtained in the same way. .
La2CuO4単結晶の作製に際し、酸化ランタン
(La2O3)でなく、炭酸ランタン(La2(CO3)3)
を出発物質として用いることもできる。La2
(CO3)3は加熱中に
La2(CO3)3→La2O3+3CO2↑
なる反応を起し、La2O3に変化する。従つて出発
物資としてLa2(CO3)3とCuOを用いても、結果と
して第1図と全く同様の相平衡図が得られ、前述
した各実施例と同様の操作によつてLa2CuO4単結
晶およびLaの一部をBaまたはSrで置換した単結
晶を得ることができた。 When producing a La 2 CuO 4 single crystal, lanthanum carbonate (La 2 (CO 3 ) 3 ) was used instead of lanthanum oxide (La 2 O 3 ).
can also be used as a starting material. La 2
(CO 3 ) 3 undergoes the following reaction during heating: La 2 (CO 3 ) 3 →La 2 O 3 +3CO 2 ↑ and changes to La 2 O 3 . Therefore, even if La 2 (CO 3 ) 3 and CuO are used as starting materials, a phase equilibrium diagram exactly the same as that shown in Fig. 1 is obtained as a result, and La 2 CuO 4 single crystals and single crystals in which part of La was replaced with Ba or Sr were obtained.
[発明の効果]
以上説明した様に、この発明によればLa2CuO4
単結晶をフラツクス法によつて製造することがで
きる。また、BaおよびSrを少量混合した単結晶
を作製することができる。このように本発明によ
つて30〜40kで超伝導を示す酸化物超伝導単結晶
も製造することが可能となつた。[Effect of the invention] As explained above, according to this invention, La 2 CuO 4
Single crystals can be produced by the flux method. Furthermore, a single crystal containing a small amount of Ba and Sr can be produced. Thus, according to the present invention, it has become possible to produce an oxide superconducting single crystal exhibiting superconductivity at 30 to 40 k.
第1図は本願発明者の作成したLa2O3−CuO系
の相平衡図である。
FIG. 1 is a phase equilibrium diagram of the La 2 O 3 --CuO system created by the inventor of the present application.
Claims (1)
なくとも一種を28.9〜7.1モル%、酸化銅を71.1〜
92.9モル%に混合して1040〜1330℃に加熱融解し
たのち、その融液を徐冷させることにより一般式
La2CuO4で表わされる微結晶を析出させ、該微結
晶を融液中で結晶育成させることを特徴とする銅
製ランタン単結晶の製造方法。 2 前記銅製ランタンが少量の異種元素を含むこ
とを特徴とする特許請求の範囲第1項記載の銅製
ランタン単結晶の製造方法。[Claims] 1. 28.9 to 7.1 mol% of at least one of lanthanum oxide and lanthanum carbonate, and 71.1 to 7.1 mol% of copper oxide.
After mixing at 92.9 mol% and heating and melting at 1040 to 1330°C, the melt is slowly cooled to obtain the general formula
1. A method for producing a copper lanthanum single crystal, which comprises precipitating microcrystals represented by La 2 CuO 4 and growing the microcrystals in a melt. 2. The method for producing a copper lanthanum single crystal according to claim 1, wherein the copper lanthanum contains a small amount of a different element.
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62109517A JPS63274695A (en) | 1987-05-01 | 1987-05-01 | Production of cupric acid-lanthanum single crystal |
US07/168,021 US4956334A (en) | 1987-05-01 | 1988-03-14 | Method for preparing a single crystal of lanthanum cuprate |
EP88104090A EP0288709B1 (en) | 1987-05-01 | 1988-03-15 | method for preparing a single crystal of lanthanum cuprate |
DE8888104090T DE3872922T2 (en) | 1987-05-01 | 1988-03-15 | METHOD FOR THE PRODUCTION OF LANTHANE SUPER SINGLE CRYSTAL. |
US07/521,624 US5057492A (en) | 1987-05-01 | 1990-05-10 | Method for preparing a single crystal of lanthanum cuprate |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62109517A JPS63274695A (en) | 1987-05-01 | 1987-05-01 | Production of cupric acid-lanthanum single crystal |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS63274695A JPS63274695A (en) | 1988-11-11 |
JPH0471875B2 true JPH0471875B2 (en) | 1992-11-16 |
Family
ID=14512269
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP62109517A Granted JPS63274695A (en) | 1987-05-01 | 1987-05-01 | Production of cupric acid-lanthanum single crystal |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS63274695A (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5157017A (en) * | 1987-06-12 | 1992-10-20 | At&T Bell Laboratories | Method of fabricating a superconductive body |
CN114620757B (en) * | 2022-04-14 | 2023-04-07 | 福州大学 | Green synthesis method of perovskite lanthanum cuprate nanosheet |
-
1987
- 1987-05-01 JP JP62109517A patent/JPS63274695A/en active Granted
Also Published As
Publication number | Publication date |
---|---|
JPS63274695A (en) | 1988-11-11 |
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