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1. 发明授权

US07387677B2 Substrate for epitaxy and method of preparing the same 有权
标题翻译：用于外延的基板及其制备方法
公开(公告)号：US07387677B2
公开(公告)日：2008-06-17
申请号：US10538407
申请日：2003-12-11
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： C30B19/12
CPC分类号： C30B25/02 , C30B25/18 , C30B29/403 , C30B29/406 , H01L21/02389 , H01L21/0245 , H01L21/02458 , H01L21/02516 , H01L21/0254 , H01L21/02576 , H01L21/02579 , H01L21/02581 , H01L21/0262 , H01L21/02628 , H01L21/02636 , Y10T428/266
摘要： The substrate is used for opto-electric or electrical devices and comprises a layer of nitride grown by means of vapor phase epitaxy growth wherein both main surfaces of the nitride substrate are substantially consisting of non N-polar face and N-polar face respectively and the dislocation density of the substrate is 5×105/cm2 or less. Therefore, the template type substrate has a good dislocation density and a good value of FWHM of the X-ray rocking curve from (0002) plane less than 80, so that the resulting template type substrate is very useful for the epitaxy substrate from gaseous phase such as MOCVD, MBE and HVPE, resulting in possibility of making good opto-electric devices such as Laser Diode and large-output LED and good electric devices such as MOSFET.
摘要翻译：衬底用于光电或电器件，并且包括通过气相外延生长生长的氮化物层，其中氮化物衬底的两个主表面分别基本上由非N极面和N极面组成，并且基板的位错密度为5×10 5 / cm 2以下。因此，模板型基板具有良好的位错密度和来自（0002）面的X射线摇摆曲线的FWHM的良好值小于80，使得所得到的模板型基板对于来自气相的外延基板非常有用例如MOCVD，MBE和HVPE，从而产生诸如激光二极管和大输出LED以及诸如MOSFET的良好电气装置的良好光电装置的可能性。

2. 发明授权

US07811380B2 Process for obtaining bulk mono-crystalline gallium-containing nitride 有权
公开(公告)号：US07811380B2
公开(公告)日：2010-10-12
申请号：US10537804
申请日：2003-12-11
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： C30B11/04
CPC分类号： C30B29/403 , C30B7/00 , C30B7/005 , C30B29/406
摘要： 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.

3. 发明授权

US07422633B2 Method of forming gallium-containing nitride bulk single crystal on heterogeneous substrate 有权
标题翻译：在异质衬底上形成含镓氮化物本体单晶的方法
公开(公告)号：US07422633B2
公开(公告)日：2008-09-09
申请号：US10479857
申请日：2002-06-06
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： C30B9/00
CPC分类号： C30B29/406 , C30B7/00 , C30B7/10 , C30B29/403 , H01S5/0281 , H01S5/32341 , Y10T117/10 , Y10T117/102 , Y10T117/1024
摘要： The present invention provides a process for forming a bulk monocrystalline gallium-containing nitride, i.e. GaN etc., on the surface of heterogeneous substrate, i.e. SiC etc., comprising the steps of forming a supercritical ammonia solvent containing ion or ions of alkali metals in an autoclave, dissolving a gallium-containing feedstock in the supercritical ammonia solvent to form a supercritical solution in which the feedstock is dissolved, and crystallizing gallium-containing nitride on the face of a seed which contains no element of oxygen and has a lattice constant of 2.8 to 3.6 with respect to ao-axis from the supercritical solution, under a condition of a higher temperature and/or a lower pressure than the temperature and/or the pressure where the gallium-containing feedstock is dissolved in the supercritical solvent. Therefore nitride gallium system compound semiconductor device can be formed on a conductive substrate.
摘要翻译：本发明提供了在异质衬底（即SiC等）的表面上形成大量单晶含镓氮化物（即，GaN等）的方法，包括以下步骤：形成含碱金属离子或离子的超临界氨溶剂高压釜，将含镓原料溶解在超临界氨溶剂中以形成其中原料溶解的超临界溶液，并且在不含元素的晶种面上结晶含镓氮化物，其晶格常数为相对于超临界溶液在相对于含镓原料的温度和/或压力更高的温度和/或更低的压力的条件下，相对于0℃ - 溶于超临界溶剂。因此，可以在导电基板上形成氮化镓系化合物半导体器件。

4. 发明申请

US20070040240A1 Bulk nitride mono-crystal including substrate for epitaxy 有权
标题翻译：包括用于外延的衬底的块状氮化物单晶
公开(公告)号：US20070040240A1
公开(公告)日：2007-02-22
申请号：US11589058
申请日：2006-10-30
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： H01L29/12
CPC分类号： C30B29/403 , C30B7/00 , C30B7/10 , C30B29/40 , C30B29/406 , H01S5/0281 , H01S5/32341
摘要： 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.
摘要翻译：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。

5. 发明申请

US20060191472A1 Bulk single crystal production facility employing supercritical ammonia 有权
标题翻译：采用超临界氨的散装单晶生产设备
公开(公告)号：US20060191472A1
公开(公告)日：2006-08-31
申请号：US10514639
申请日：2002-12-11
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： C30B11/00 , C30B17/00 , C30B9/00 , C30B28/06 , C30B21/02
CPC分类号： C30B7/10 , C30B7/00 , C30B7/08 , C30B29/406 , Y10T117/10 , Y10T117/102 , Y10T117/1024
摘要： 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.
摘要翻译：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。

6. 发明授权

US08398767B2 Bulk mono-crystalline gallium-containing nitride and its application 有权
标题翻译：大量单晶含镓氮化物及其应用
公开(公告)号：US08398767B2
公开(公告)日：2013-03-19
申请号：US11629109
申请日：2005-06-10
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara , Robert Kucharski
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara , Robert Kucharski
IPC分类号： C30B9/00
CPC分类号： C30B9/00 , C30B29/406
摘要： Bulk mono-crystalline gallium-containing nitride, grown on the seed at least in the direction essentially perpendicular to the direction of the seed growth, essentially without propagation of crystalline defects as present in the seed, having the dislocation density not exceeding 104/cm2 and considerably lower compared to the dislocation density of the seed, and having a large curvature radius of the crystalline lattice, preferably longer than 15 m, more preferably longer than 30 m, and most preferably of about 70 m, considerably longer than the curvature radius of the crystalline lattice of the seed.
摘要翻译：至少在基本上垂直于种子生长方向的方向在种子上生长的大量单晶含镓氮化物，基本上不存在存在于种子中的晶体缺陷的扩散，位错密度不超过104 / cm2，与晶种的位错密度相比显着降低，并且具有大的晶格的曲率半径，优选长于15μm，更优选长于30μm，最优选约70μm，远大于种子的晶格。

7. 发明授权

US08110848B2 Substrate for epitaxy and method of preparing the same 有权
标题翻译：用于外延的基板及其制备方法
公开(公告)号：US08110848B2
公开(公告)日：2012-02-07
申请号：US12213212
申请日：2008-06-16
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： C30B19/12
CPC分类号： C30B25/02 , C30B25/18 , C30B29/403 , C30B29/406 , H01L21/02389 , H01L21/0245 , H01L21/02458 , H01L21/02516 , H01L21/0254 , H01L21/02576 , H01L21/02579 , H01L21/02581 , H01L21/0262 , H01L21/02628 , H01L21/02636 , Y10T428/266
摘要： The substrate is used for opto-electric or electrical devices and comprises a layer of nitride grown by means of vapor phase epitaxy growth wherein both main surfaces of the nitride substrate are substantially consisting of non N-polar face and N-polar face respectively and the dislocation density of the substrate is 5×105/cm2 or less. Therefore, the template type substrate has a good dislocation density and a good value of FWHM of the X-ray rocking curve from (0002) plane less than 80, so that the resulting template type substrate is very useful for the epitaxy substrate from gaseous phase such as MOCVD, MBE and HVPE, resulting in possibility of making good opto-electric devices such as Laser Diode and large-output LED and good electric devices such as MOSFET.
摘要翻译：衬底用于光电或电器件，并且包括通过气相外延生长生长的氮化物层，其中氮化物衬底的两个主表面分别基本上由非N极面和N极面组成，并且基板的位错密度为5×10 5 / cm 2以下。因此，模板型基板具有良好的位错密度和来自（0002）面的X射线摇摆曲线的FWHM的良好值小于80，使得所得到的模板型基板对于来自气相的外延基板非常有用例如MOCVD，MBE和HVPE，从而产生诸如激光二极管和大输出LED以及诸如MOSFET的良好电气装置的良好光电装置的可能性。

8. 发明授权

US07905957B2 Method of obtaining bulk single crystals by seeded growth 有权
标题翻译：通过种子生长获得大块单晶的方法
公开(公告)号：US07905957B2
公开(公告)日：2011-03-15
申请号：US11791716
申请日：2005-11-28
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： C30B7/00
CPC分类号： H01S5/34333 , B82Y20/00 , C30B7/00 , C30B7/10 , C30B29/403 , C30B29/406 , H01S5/2214 , H01S5/2231 , H01S2301/173 , H01S2304/04
摘要： The present invention is related to a process for obtaining a larger area substrate of mono-crystalline gallium-containing nitride by making selective crystallization of gallium containing nitride on a smaller seed under a crystallization temperature and/or pressure from a supercritical ammonia-containing solution made by dissolution of gallium-containing feedstock in a supercritical ammonia-containing solvent with alkali metal ions, comprising: providing two or more elementary seeds, and making selective crystallization on the two or more separate elementary seeds to get a merged larger compound seed. The merged larger compound seed is used for a seed in a new growth process and then to get a larger substrate of mono-crystal gallium-containing nitride.
摘要翻译：本发明涉及一种通过在结晶温度和/或来自超临界含氨的溶液的结晶温度和/或压力下在较小种子上进行含镓氮化物的选择性结晶来获得单晶含镓氮化物的较大面积衬底的方法通过将含镓原料溶解在具有碱金属离子的超临界含氨溶剂中，包括：提供两种或更多种基本种子，并在两个或更多个分离的基本种子上进行选择性结晶，得到合并的较大的复合种子。将合并的较大的复合种子用于新生长过程中的种子，然后获得更大的单晶含镓氮化物的基底。

9. 发明申请

US20080108162A1 Light-Emitting Device Structure Using Nitride Bulk Single Crystal Layer 有权
标题翻译：使用氮化物单晶层的发光器件结构
公开(公告)号：US20080108162A1
公开(公告)日：2008-05-08
申请号：US11969735
申请日：2008-01-04
申请人： Robert DWILINSKI , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert DWILINSKI , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： H01L33/00
CPC分类号： C30B29/403 , B82Y20/00 , C30B7/005 , C30B7/10 , C30B9/00 , C30B29/406 , H01S5/021 , H01S5/0213 , H01S5/0218 , H01S5/0281 , H01S5/164 , H01S5/22 , H01S5/3202 , H01S5/32341 , H01S5/34333 , H01S2304/12
摘要： The object of this invention is to provide a high-output type nitride light emitting device. The nitride light emitting device comprises an n-type nitride semiconductor layer or layers, a p-type nitride semiconductor layer or layers and an active layer therebetween, wherein a gallium-containing nitride substrate is obtained from a gallium-containing nitride bulk single crystal, provided with an epitaxial growth face with dislocation density of 105/cm2 or less, and A-plane or M-plane which is parallel to C-axis of hexagonal structure for an epitaxial face, wherein the n-type semiconductor layer or layers are formed directly on the A-plane or M-plane. In case that the active layer comprises a nitride semiconductor containing In, an end face film of single crystal AlxGa1-xN (0≦x≦1) can be formed at a low temperature not causing damage to the active layer.
摘要翻译：本发明的目的是提供一种高输出型氮化物发光器件。氮化物发光器件包括n型氮化物半导体层或p型氮化物半导体层或其间的有源层，其中含镓氮化物衬底由含镓氮化物本体单晶获得，具有位错密度为10 5 / cm 2以下的外延生长面，平行于六方结构的C轴的A面或M面对于外延面，其中n型半导体层直接形成在A平面或M平面上。在有源层包括含有In的氮化物半导体的情况下，单晶Al x Ga 1-x N（0 <= x <= 1）的端面膜，可以在不会对活性层造成损害的低温下形成。

10. 发明申请

US20060120931A1 Process for obtaining bulk-crystalline gallium-containing nitride 有权
标题翻译：获得块状含镓氮化物的方法
公开(公告)号：US20060120931A1
公开(公告)日：2006-06-08
申请号：US10538349
申请日：2003-12-11
申请人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
发明人： Robert Dwilinski , Roman Doradzinski , Jerzy Garczynski , Leszek Sierzputowski , Yasuo Kanbara
IPC分类号： C01F3/00
CPC分类号： C30B29/403 , C30B7/00 , C30B29/406
摘要： An improved mineralizer used for a process for obtaining bulk mono-crystalline gallium-containing nitride of a general formula of AlxGa1-xN, where 0≦x
摘要翻译：一种用于获得通式为Al x Ga 1-x N的块状单晶含镓氮化物的方法的改进的矿化剂，其中0 <= x < 1在超临界含氨溶液环境中已被提出。根据本发明，所得产物的生长速度和质量可以通过适当选择矿化剂来控制，以确保I族元素（IUPAC 1989）的离子存在，优选钠与其它选自以下的组分的组合：第I组元素（IUPAC 1989），II族元素的离子（IUPAC 1989），一种或多种含有无氧物质的物质导致超临界溶剂的氨基性质的某些削弱，任选地与II族元素组合（IUPAC 1989），优选钙或镁。由此获得的改进的体积单晶主要用于光电子领域。

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