METHOD OF PRODUCING PERIODIC TABLE GROUP 13 METAL NITRIDE CRYSTAL

• Main Authors: BAO QUANXI, SAITO MAKOTO, CHICHIBU SHIGEHIDE, ISHIGURO TORU
• Format: Patent
• Language: English; Japanese
• Published: 02.03.2015
• Subjects: AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUSPOLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR; CHEMISTRY; CRYSTAL GROWTH; METALLURGY; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITHDEFINED STRUCTURE; REFINING BY ZONE-MELTING OF MATERIAL; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITHDEFINED STRUCTURE; SINGLE-CRYSTAL-GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL ORUNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL

PROBLEM TO BE SOLVED: To provide a method of producing, efficiently by the ammonothermal method, a periodic table group 13 metal nitride crystal which is high in purity and quality and is reduced in defects.SOLUTION: A method of producing a periodic table group 13 metal nitride crystal includes a step of growing a periodic table group 13 metal nitride crystal on a ground substrate 6 in the presence of a supercritical and/or a subcritical solvent 6 in a reaction vessel 1, and a nitrogen-containing solvent, a raw material for the periodic table group 13 metal nitride crystal, a fluorine-containing mineralizer and aluminum are caused to be present in the reaction vessel. The ratio (F/Al) of the molar amount of fluorine (F) to aluminum (Al), present in the reaction vessel, is 4.0 or higher. In the step of growing the nitride crystal, growth conditions in the reaction vessel 1 includes a pressure of 50-700 MPa and a temperature of 400-700°C. 【課題】アモノサーマル法において、純度の高く、欠陥の少ない高品質の周期表第１３族金属窒化物結晶を効率良く製造する方法を提供する。【解決手段】反応容器１中で、超臨界状態及び／又は亜臨界状態にある溶媒６存在下にて、下地基板６上に周期表第１３族金属窒化物結晶を成長させる工程を含み、反応容器中には、窒素含有溶媒、周期表第１３族金属窒化物結晶原料、フッ素を含有する鉱化剤及びアルミニウムを存在させることを特徴とする周期表第１３族金属窒化物結晶の製造方法。反応容器中に存在するフッ素のモル量（Ｆ）とアルミニウム（Ａｌ）の比（Ｆ／Ａｌ）が４．０以上であり、前記窒化物結晶を成長する工程において、反応容器１の圧力が５０〜７００ＭＰａであり、温度が４００〜７００℃で結晶を成長させる、周期表第１３族金属酸化物結晶の製造方法。【選択図】図１