# US 5,707,441 A · Method for preparing an oxide crystal > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,707,441 A - Document ID: US5707441A - Status: Granted - Kind: A - Application number: 08/569,895 - Filed: 1995-12-08 - Granted: 1998-01-13 - Earliest claimed: 1994-12-28 - Assignees: Sumitomo Electric Industries, Ltd.; International Superconductivity Technology Center - Inventors: Yasuo Namikawa; Yuh Shiohara; Shoji Tanaka - Web page: https://patentgrep.com/patent/US5707441A ## CPC - C30B 29/225: {based on rare earth copper oxides, e.g. high T-superconductors} - C30B 15/20: Controlling or regulating (controlling or regulating in general G05) - Y10T 117/1004: with means for measuring, testing, or sensing - C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract In order to prepare a large yttrium or lanthanoid based oxide superconductor crystal of higher quality, a method and an apparatus which can stably control the shape of a pulled crystal and stably maintain growth of the crystal from a melt are provided. A crystal of an oxide having a structure of RBa.sub.2 Cu.sub.3 O.sub.7-X (R: yttrium or lanthanoid element, 0.ltoreq.X.ltoreq.1) is pulled from a raw material melt which is stored in a crucible by a rotary crystal pulling shaft. During such pulling, a position of the surface of the raw material melt is measured with time to obtain a lowering speed of the surface in a direction substantially parallel to the crystal pulling direction, for adjusting the lifting speed of the crystal pulling shaft by this lowering speed. ## Claims ### Claim 1 A method of preparing an oxide crystal comprising the steps of: pulling a crystal of an oxide having a structure of RBa.sub.2 Cu.sub.3 O.sub.7-X (R: yttrium or lanthanoid element, 0.ltoreq.x.ltoreq.1) from a raw material melt being stored in a crucible with a rotary crystal pulling shaft, measuring a surface position of said raw material melt with time during pulling of said crystal to obtain a movement speed of said surface in a direction being substantially parallel to the crystal pulling direction, and adjusting a lifting speed of said crystal pulling shaft by said movement speed. ### Claim 2 (depends on 1) The method of preparing an oxide crystal in accordance with claim 1, wherein said step of measuring said surface position and adjusting said lifting speed comprises the steps of: setting a target value (V) of a crystal pulling speed to balance a crystal growth rate and said crystal pulling speed with each other, and setting said lifting speed (P) of said crystal pulling shaft in accordance with an equation of P=V-M after obtaining said movement speed (M) of said surface. ### Claim 3 (depends on 1) The method of preparing an oxide crystal in accordance with claim 1, wherein said step of measuring said surface position and adjusting said lifting speed comprises the steps of: providing an electrically conductive material being capable of stably maintaining its shape upon contact with said raw material melt to be upwardly and downwardly movable, providing means for measuring an electric change being caused when said electrically conductive material is brought into contact with said raw material melt and connecting said electrically conductive material to said means, detecting a position (Z.sub.0) of said surface of said raw material melt from said electric change being caused when said electrically conductive material is downwardly moved from a prescribed position and brought into contact with said raw material melt in crystal pulling, upwardly moving said electrically conductive material, being brought into contact with said raw material melt, for separating the former from the latter, and again downwardly moving said conductive material after a lapse of a prescribed time (T) from said detection of said Z.sub.0 for bringing the same into contact with said raw material melt, thereby detecting a current position (Z.sub.1) of said surface of said raw material melt from current said electric change, and obtaining (Z.sub.0 -Z.sub.1)/T as said movement speed of said surface. ### Claim 4 (depends on 3) The method of preparing an oxide crystal in accordance with claim 3, wherein said means comprises an electric resistance measuring device, said electric resistance measuring device being connected with said electrically conductive material, for detecting said position of said surface of said raw material melt from a change of an electric resistance value caused when said conductive material comes into contact with said raw material melt. ### Claim 5 (depends on 1) The method of preparing an oxide crystal in accordance with claim 1, wherein said crucible comprises an inner crucible consisting essentially of an oxide of said R, and an outer crucible, holding said inner crucible therein, consisting essentially of magnesia, said crystal being pulled from said raw material melt being stored in said inner crucible.