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    • 4. 发明授权
    • Process for obtaining bulk mono-crystalline gallium-containing nitride
    • US07811380B2
    • 2010-10-12
    • US10537804
    • 2003-12-11
    • Robert DwilinskiRoman DoradzinskiJerzy GarczynskiLeszek SierzputowskiYasuo Kanbara
    • Robert DwilinskiRoman DoradzinskiJerzy GarczynskiLeszek SierzputowskiYasuo Kanbara
    • C30B11/04
    • C30B29/403C30B7/00C30B7/005C30B29/406
    • A process for obtaining bulk mono-crystalline gallium-containing nitride, liminating impurities from the obtained crystal and manufacturing substrates made of bulk mono-crystalline gallium-containing nitride has been now proposed. According to the invention, the process for obtaining of mono-crystalline gallium-containing nitride from the gallium-containing feedstock in a supercritical ammonia-containing solvent with mineralizer addition is characterized in that the feedstock is in the form of metallic gallium and the mineralizer is in the form of elements of Group I and/or their mixtures, and/or their compounds, especially those containing nitrogen and/or hydrogen, whereas the ammonia-containing solvent is in the form of the mineralizer and ammonia, there are two temperature zones in each step of the process, and the feedstock is placed in the dissolution zone, and at least one mono-crystalline seed is deposited in the crystallization zone, and following the transition of the solvent to the supercritical state, the process comprises the first step of transition of the feedstock from the metallic form to the polycrystalline gallium-containing nitride, and the second step of crystallization of the gallium-containing nitride through gradual dissolution of the feedstock and selective crystallization of gallium-containing nitride on at least one mono-crystalline seed at the temperature higher than that of the dissolution of the feedstock, while all the vital components of the reaction system (including the feedstock, seeds and mineralizer) invariably remain within the system throughout the whole process, and consequently bulk mono-crystalline gallium-containing nitride is obtained. The invention relates also the the post-treatment (slicing, annealing and washing) of the thus obtained crystals.The improved process and the bulk monocrystals obtained thereby are intended mainly for use in the field of opto-electronics.
    • 7. 发明申请
    • Bulk nitride mono-crystal including substrate for epitaxy
    • 包括用于外延的衬底的块状氮化物单晶
    • US20070040240A1
    • 2007-02-22
    • US11589058
    • 2006-10-30
    • Robert DwilinskiRoman DoradzinskiJerzy GarczynskiLeszek SierzputowskiYasuo Kanbara
    • Robert DwilinskiRoman DoradzinskiJerzy GarczynskiLeszek SierzputowskiYasuo Kanbara
    • H01L29/12
    • C30B29/403C30B7/00C30B7/10C30B29/40C30B29/406H01S5/0281H01S5/32341
    • The invention relates to a substrate for epitaxy, especially for preparation of nitride semiconductor layers. Invention covers a bulk nitride mono-crystal characterized in that it is a mono-crystal of gallium nitride and its cross-section in a plane perpendicular to c-axis of hexagonal lattice of gallium nitride has a surface area greater than 100 mm2, it is more than 1.0 μm thick and its C-plane surface dislocation density is less than 106/cm2, while its volume is sufficient to produce at least one further-processable non-polar A-plane or M-plane plate having a surface area at least 100 mm2. More generally, the present invention covers a bulk nitride mono-crystal which is characterized in that it is a mono-crystal of gallium-containing nitride and its cross-section in a plane perpendicular to c-axis of hexagonal lattice of gallium-containing nitride has a surface area greater than 100 mm2, it is more 1.0-μm thick and its surface dislocation density is less than 106/cm2. Mono-crystals according to the present invention are suitable for epitaxial growth of nitride semiconductor layers. Due to their good crystalline quality they are suitable for use in opto-electronics for manufacturing opto-electronic semiconductor devices based on nitrides, in particular for manufacturing semiconductor laser diodes and laser devices. The a.m. bulk mono-crystals of gallium-containing nitride are crystallized on seed crystals. Various seed crystals may be used. The bulk mono-crystals of gallium-containing nitride are crystallized by a method involving dissolution of a gallium-containing feedstock in a supercritical solvent and crystallization of a gallium nitride on a surface of seed crystal, at temperature higher and/or pressure lower than in the dissolution process.
    • 本发明涉及用于外延的衬底,特别是用于制备氮化物半导体层。 本发明涉及一种块状氮化物单晶,其特征在于它是氮化镓的单晶,其在垂直于氮化镓的六方晶格的c轴的平面中的横截面具有大于100mm的表面积, 2,厚度大于1.0μm,其C面表面位错密度小于10/6/2,而其体积足以 产生表面积至少为100mm 2以上的至少一个可再加工的非极性A平面或M平面板。 更一般来说,本发明涉及一种块状氮化物单晶,其特征在于其是含镓氮化物的单晶,其在与含镓氮化物的六方晶格的c轴垂直的平面中的横截面 具有大于100mm 2的表面积,其厚度为1.0μm,其表面位错密度小于10/2/2/2 >。 根据本发明的单晶适用于氮化物半导体层的外延生长。 由于它们具有良好的晶体质量,它们适用于制造基于氮化物的光电半导体器件的光电子器件,特别是用于制造半导体激光二极管和激光器件。 含镓氮化物的大量单体晶体在晶种上结晶。 可以使用各种晶种。 含镓氮化物的体积单晶通过包括在超临界溶剂中溶解含镓原料并在晶种表面上结晶氮化镓的方法结晶,温度高于和/或低于 溶解过程。
    • 8. 发明申请
    • Bulk single crystal production facility employing supercritical ammonia
    • 采用超临界氨的散装单晶生产设备
    • US20060191472A1
    • 2006-08-31
    • US10514639
    • 2002-12-11
    • Robert DwilinskiRoman DoradzinskiJerzy GarczynskiLeszek SierzputowskiYasuo Kanbara
    • Robert DwilinskiRoman DoradzinskiJerzy GarczynskiLeszek SierzputowskiYasuo Kanbara
    • C30B11/00C30B17/00C30B9/00C30B28/06C30B21/02
    • C30B7/10C30B7/00C30B7/08C30B29/406Y10T117/10Y10T117/102Y10T117/1024
    • There is provided an apparatus comprising an autoclave 1 for preparing a supercritical solvent equipped with a convection control means 2 for establishing a convection flow, wherein the dissolution zone 13 where a feedstock 16 is located above the convection control means 2 and the crystallization zone where a seed 17 is located below the convection control means are formed. A convection flow rate of the supercritical solution between the dissolution zone 13 and the crystallization zone 14 is determined by the degree of opening of the convection control means 2 and the temperature difference between the dissolution zone 13 and crystallization zone 14. Accordingly, the supercritical solution, in which the nitride has a negative temperature coefficient of solubility is supplied from the dissolution zone 13 to the crystallization zone 14 in which a seed is located through the convection control means 2 so that nitride crystal is selectively grown on the seed by maintaining supersaturation of the supercritical solution with respect to the seed at the predetermined raised temperature. In the apparatus according to the present invention, the concentration of the supercritical solution is controlled below a certain level so as not to allow spontaneous crystallization, so that a nitride bulk single crystal can be obtained.
    • 提供了一种装置,其包括用于制备配备有用于建立对流的对流控制装置2的超临界溶剂的高压釜1,其中原料16位于对流控制装置2上方的溶解区13和结晶区 种子17位于对流控制装置下方形成。 溶解区13和结晶区14之间的超临界溶液的对流流速由对流控制装置2的开度和溶解区13与结晶区14之间的温度差决定。 因此,其中氮化物具有负温度溶解度系数的超临界溶液通过对流控制装置2从溶解区13供给到晶种位于结晶区14中,使氮化物晶体选择性地生长在 通过在预定的升高温度下保持超临界溶液相对于种子的过饱和而种子。 在根据本发明的装置中,将超临界溶液的浓度控制在一定水平以下,以便不允许自发结晶,从而可以获得氮化物体单晶。