JP2836763B2 - NdGaO (3) Single crystal etching method - Google Patents

NdGaO (3) Single crystal etching method

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Publication number
JP2836763B2
JP2836763B2 JP32992990A JP32992990A JP2836763B2 JP 2836763 B2 JP2836763 B2 JP 2836763B2 JP 32992990 A JP32992990 A JP 32992990A JP 32992990 A JP32992990 A JP 32992990A JP 2836763 B2 JP2836763 B2 JP 2836763B2
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JP
Japan
Prior art keywords
ndgao
single crystal
etching
crystal
temperature
Prior art date
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Application number
JP32992990A
Other languages
Japanese (ja)
Other versions
JPH04202100A (en
Inventor
清二 十河
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.)
Eneos Corp
Original Assignee
Japan Energy Corp
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Filing date
Publication date
Application filed by Japan Energy Corp filed Critical Japan Energy Corp
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Description

【発明の詳細な説明】 産業上の利用分野 本発明は、酸化物超電導薄膜用基板として有望なNdGa
O3単結晶のエッチング方法に関するものである。
The present invention relates to a promising NdGa as a substrate for an oxide superconducting thin film.
The present invention relates to a method for etching an O 3 single crystal.

従来の技術 NdGaO3単結晶は酸化物超電導体と格子定数のミスマッ
チが小さく、熱膨張係数も近い値であり、結晶構造が似
ており、常温から1000℃の範囲で相変態が無い等、酸化
物超電導薄膜のエピキタシャル成長用基板として優れた
特性を持っている。
Conventional technology NdGaO 3 single crystal has a small lattice mismatch with the oxide superconductor, a similar coefficient of thermal expansion, a similar crystal structure, and no phase transformation from room temperature to 1000 ° C. It has excellent properties as a substrate for epitaxial growth of superconducting thin films.

このNdGaO3単結晶はチョクラルスキー法によって育成
された後、切断・研磨される。これらの工程において結
晶表面に生じる加工変質層とよばれる結晶学的な乱れや
育成した結晶そのものに入っている欠陥は、その上にエ
ピタキシャル成長させる薄膜の品質劣化を招く。結晶欠
陥の評価は一般に酸などのエッチング液を使って結晶表
面のエッチングを行い、エッチピットを析出させてその
密度を比較することによって行われる。
The NdGaO 3 single crystal is grown and cut and polished by the Czochralski method. In these steps, crystallographic disorder called a work-affected layer generated on the crystal surface or a defect contained in the grown crystal itself deteriorates the quality of a thin film epitaxially grown thereon. Evaluation of crystal defects is generally performed by etching the crystal surface using an etchant such as an acid, depositing etch pits, and comparing the densities.

発明が解決しようとする課題 しかしながらNdGaO3単結晶のような新規な酸化物のエ
ッチングでは、結晶表面にエッチピットを析出させるよ
うな適切なエッチング液とエッチング条件が見い出され
ておらず、単結晶の結晶性を評価する上で障害となって
いた。
Problems to be Solved by the Invention However, in the etching of a novel oxide such as NdGaO 3 single crystal, an appropriate etching solution and etching conditions for depositing etch pits on the crystal surface have not been found, and the single crystal This was an obstacle in evaluating crystallinity.

そこで本発明者等は鋭意検討した結果、以下の発明を
なした。
The inventors of the present invention have made intensive studies and, as a result, have made the following invention.

課題を解決するための手段及び作用 本発明者等は酸化物超伝導薄膜用基板として用いられ
るNdGaO3単結晶のエッチング方法について検討した結
果、エッチング液として燐酸を使用し、エッチング液の
温度を100〜230℃とすることによって結晶表面にエッチ
ピットを析出できることを見い出した。以下、本発明の
内容を詳細に述べる。
Means and Action for Solving the ProblemsThe present inventors have studied an etching method of NdGaO 3 single crystal used as a substrate for an oxide superconducting thin film, and as a result, using phosphoric acid as an etching solution, and adjusting the temperature of the etching solution to 100 It has been found that etch pits can be deposited on the crystal surface by setting the temperature to ~ 230 ° C. Hereinafter, the contents of the present invention will be described in detail.

NdGaO3単結晶のような酸化物は、常温では酸等のエッ
チング液にはほとんど溶出しない。そこで、エッチング
液の温度を高くして反応を加速してやる必要がある。反
応速度を十分に高くするためには、沸点の高いエッチン
グ液を選ぶ必要がある。塩酸、ふっ酸、および硝酸の沸
点は120℃程度であり、温度を十分に高くすることがで
きない。一方、燐酸は加熱によって脱水はするが、沸騰
は起きず、400℃以上まで加熱することができ、NdGaO3
単結晶のエッチング液として適している。
Oxides such as NdGaO 3 single crystals hardly elute in an etchant such as an acid at room temperature. Therefore, it is necessary to increase the temperature of the etchant to accelerate the reaction. In order to sufficiently increase the reaction rate, it is necessary to select an etching solution having a high boiling point. The boiling points of hydrochloric acid, hydrofluoric acid, and nitric acid are about 120 ° C., and the temperatures cannot be raised sufficiently. On the other hand, phosphoric acid is dehydrated by heating, but does not boil and can be heated to 400 ° C. or higher, and NdGaO 3
Suitable as a single crystal etchant.

エッチング液として燐酸を用いた場合、温度が100℃
以下ではエッチング速度が遅すぎて実用的ではない。従
って、100℃以上の範囲で所望のエッチング速度に応じ
た温度を選ぶことが望ましい。
When phosphoric acid is used as an etchant, the temperature is 100 ° C
Below, the etching rate is too slow to be practical. Therefore, it is desirable to select a temperature according to a desired etching rate in a range of 100 ° C. or more.

エッチングを行う際に、温度が230℃以下であると結
晶表面にピットが生じる。これはエッチングの過程が反
応律速であるために、結晶の欠陥部分が選択的にエッチ
ングされるためであると考えられる。
When performing the etching, if the temperature is 230 ° C. or less, pits are generated on the crystal surface. It is considered that this is because the etching process is rate-determining, so that the defective portion of the crystal is selectively etched.

一方、温度が230℃より高くなると、結晶表面にはピ
ットは生じなくなる。これは、NdGaO3の溶出速度が速く
なり、エッチングの過程が拡散律速となって結晶表面が
一様にエッチングされたためと考えられる。
On the other hand, when the temperature is higher than 230 ° C., no pits are formed on the crystal surface. This is probably because the elution rate of NdGaO 3 was increased, the etching process became diffusion-controlled, and the crystal surface was uniformly etched.

このように、エッチング液の温度を100〜230℃とする
ことによって、結晶表面にエッチピットを析出させるこ
とができる。
Thus, by setting the temperature of the etching solution to 100 to 230 ° C., etch pits can be deposited on the crystal surface.

実施例 NdGaO3単結晶をチョクラルスキー法によって育成し
た。この結晶を(110)面に平行に10mm×10mm×0.5mmの
大きさに切りだし、機械的研摩によって鏡面に仕上げ
た。この結晶を200℃の燐酸で5分間エッチングした。
この時の結晶表面には、参考写真1に示すようにピット
が発生した。
Example An NdGaO 3 single crystal was grown by the Czochralski method. This crystal was cut into a size of 10 mm × 10 mm × 0.5 mm parallel to the (110) plane, and was mirror-finished by mechanical polishing. The crystals were etched with phosphoric acid at 200 ° C. for 5 minutes.
At this time, pits were formed on the crystal surface as shown in Reference Photo 1.

比較例1 実施例と同一の試料を300℃の燐酸で5分間エッチン
グすると、結晶表面は参考写真2に示すようにピットは
発生しなかった。
Comparative Example 1 When the same sample as in the example was etched with phosphoric acid at 300 ° C. for 5 minutes, no pits were generated on the crystal surface as shown in Reference Photo 2.

比較例2 実施例と同一の試料を30℃の燐酸で6時間エッチング
すると、結晶表面のエッチング量は1μm以下であり、
エッチング速度が、非常に遅かった。
Comparative Example 2 When the same sample as the example was etched with phosphoric acid at 30 ° C. for 6 hours, the amount of etching on the crystal surface was 1 μm or less.
The etching rate was very slow.

発明の効果 以上説明したように、本発明によればNdGaO3単結晶の
表面にエッチピットを発生させ、欠陥を容易に見出すこ
とができるため、酸化物超電導薄膜用基板の評価に寄与
する。
Effect of the Invention As described above, according to the present invention, an etch pit can be generated on the surface of an NdGaO 3 single crystal and defects can be easily found, which contributes to the evaluation of a substrate for an oxide superconducting thin film.

Claims (2)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】NdGaO3単結晶の表面をエッチングする際に
エッチング液として燐酸を使用することを特徴とするNd
GaO3単結晶のエッチング方法。
An NdGaO 3 single crystal is etched using phosphoric acid as an etchant when etching the surface thereof.
GaO 3 single crystal etching method.
【請求項2】エッチング液の温度を100〜230℃として結
晶表面にエッチングピットを析出させることを特徴とす
る特許請求の範囲第1項記載のNdGaO3単結晶のエッチン
グ方法。
2. The method for etching a NdGaO 3 single crystal according to claim 1, wherein an etching pit is deposited on the crystal surface at a temperature of the etching solution of 100 to 230 ° C.
JP32992990A 1990-11-30 1990-11-30 NdGaO (3) Single crystal etching method Expired - Lifetime JP2836763B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP32992990A JP2836763B2 (en) 1990-11-30 1990-11-30 NdGaO (3) Single crystal etching method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP32992990A JP2836763B2 (en) 1990-11-30 1990-11-30 NdGaO (3) Single crystal etching method

Publications (2)

Publication Number Publication Date
JPH04202100A JPH04202100A (en) 1992-07-22
JP2836763B2 true JP2836763B2 (en) 1998-12-14

Family

ID=18226853

Family Applications (1)

Application Number Title Priority Date Filing Date
JP32992990A Expired - Lifetime JP2836763B2 (en) 1990-11-30 1990-11-30 NdGaO (3) Single crystal etching method

Country Status (1)

Country Link
JP (1) JP2836763B2 (en)

Also Published As

Publication number Publication date
JPH04202100A (en) 1992-07-22

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