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1.发明申请公开(公告)号：US20190323145A1
公开(公告)日：2019-10-24
申请号：US16458385
申请日：2019-07-01
申请人： II-VI Incorporated
IPC分类号： C30B25/02 , C30B29/36 , C01B33/025 , C30B23/06
摘要： In an apparatus and method growing a SiC single crystal, a PVT growth apparatus is provided with a single crystal SiC seed and a SiC source material positioned in spaced relation in a growth crucible. A resistance heater heats the growth crucible such that the SiC source material sublimates and is transported via a temperature gradient that forms in the growth crucible in response to the heater heating the growth crucible to the single crystal SiC seed where the sublimated SiC source material condenses forming a growing SiC single crystal. Purely axial heat fluxes passing through the bottom and the top of the growth crucible form a flat isotherm at least at a growth interface of the growing SiC single crystal on the single crystal SiC seed.
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2.发明授权公开(公告)号：US08741413B2
公开(公告)日：2014-06-03
申请号：US13867198
申请日：2013-04-22
申请人： II-VI Incorporated
发明人： Ilya Zwieback , Thomas E. Anderson , Andrew E. Souzis , Gary E. Ruland , Avinash K. Gupta , Varatharajan Rengarajan , Ping Wu , Xueping Xu
IPC分类号： B32B3/00
CPC分类号： C30B23/005 , B28D5/00 , C30B29/36 , Y10T428/21
摘要： A method and system of forming large-diameter SiC single crystals suitable for fabricating high crystal quality SiC substrates of 100, 125, 150 and 200 mm in diameter are described. The SiC single crystals are grown by a seeded sublimation technique in the presence of a shallow radial temperature gradient. During SiC sublimation growth, a flux of SiC bearing vapors filtered from carbon particulates is substantially restricted to a central area of the surface of the seed crystal by a separation plate disposed between the seed crystal and a source of the SiC bearing vapors. The separation plate includes a first, substantially vapor-permeable part surrounded by a second, substantially non vapor-permeable part. The grown crystals have a flat or slightly convex growth interface. Large-diameter SiC wafers fabricated from the grown crystals exhibit low lattice curvature and low densities of crystal defects, such as stacking faults, inclusions, micropipes and dislocations.
摘要翻译： 描述了形成适于制造直径为100,125,150和200mm的高质量SiC衬底的大直径SiC单晶的方法和系统。 通过种子升华技术在浅径向温度梯度的存在下生长SiC单晶。 在SiC升华生长期间，通过设置在晶种和SiC轴承蒸气源之间的分离板，从碳颗粒过滤的含有碳纳米管的蒸气的通量基本上限制在晶种表面的中心区域。 分离板包括由第二基本上不透气的部分包围的第一基本上透气的部分。 生长的晶体具有平坦或略凸的生长界面。 由生长的晶体制造的大直径SiC晶片表现出低的晶格曲率和低密度的晶体缺陷，例如堆垛层错，夹杂物，微孔和位错。
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公开(公告)号：US09388509B2
公开(公告)日：2016-07-12
申请号：US13951808
申请日：2013-07-26
申请人： II-VI Incorporated
发明人： Ilya Zwieback , Avinash K. Gupta , Ping Wu , Donovan L. Barrett , Gary E. Ruland , Thomas E. Anderson
CPC分类号： C30B28/12 , C30B29/36 , Y10T428/2982
摘要： In a method of forming polycrystalline SiC grain material, low-density, gas-permeable and vapor-permeable bulk carbon is positioned at a first location inside of a graphite crucible and a mixture of elemental silicon and elemental carbon is positioned at a second location inside of the graphite crucible. Thereafter, the mixture and the bulk carbon are heated to a first temperature below the melting point of the elemental Si to remove adsorbed gas, moisture and/or volatiles from the mixture and the bulk carbon. Next, the mixture and the bulk carbon are heated to a second temperature that causes the elemental Si and the elemental C to react forming as-synthesized SiC inside of the crucible. The as-synthesized SiC and the bulk carbon are then heated in a way to cause the as-synthesized SiC to sublime and produce vapors that migrate into, condense on and react with the bulk carbon forming polycrystalline SiC material.
摘要翻译： 在形成多晶SiC晶粒材料的方法中，将低密度，透气和透气的整体碳定位在石墨坩埚内部的第一位置，并且元素硅和元素碳的混合物位于第二位置内 的石墨坩埚。 此后，将混合物和体积碳加热到低于元素Si的熔点的第一温度以从混合物和体积碳中除去吸附的气体，水分和/或挥发物。 接下来，将混合物和体积碳加热到第二温度，使得元素Si和元素C在坩埚内反应形成合成的SiC。 然后将合成后的SiC和本体碳加热，使得合成的SiC升华，并产生迁移进入，冷凝并与本体碳形成多晶SiC材料反应的蒸气。
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公开(公告)号：US20160060789A1
公开(公告)日：2016-03-03
申请号：US14475803
申请日：2014-09-03
申请人： II-VI Incorporated
发明人： Ilya Zwieback , Varatharajan Rengarajan , Bryan K. Brouhard , Michael C. Nolan , Thomas E. Anderson
摘要： In a method for growing bulk SiC single crystals using chemical vapor transport, wherein silicon acts as a chemical transport agent for carbon, a growth crucible is charged with a solid carbon source material and a SiC single crystal seed disposed therein in spaced relationship. A halosilane gas, such as SiCl4 and a reducing gas, such as H2, are introduced into the crucible via separate inlets and mix in the crucible interior. The crucible is heated in a manner that encourages chemical reaction between the halosilane gas and the reducing gas leading to the chemical reduction of the halosilane gas to elemental silicon (Si) vapor. The produced Si vapor is transported to the solid carbon source material where it reacts with the solid carbon source material yielding volatile Si-bearing and C-bearing molecules. The produced Si-bearing and C-bearing vapors are transported to the SiC single crystal seed and precipitate on the SiC single crystal seed causing growth of a SiC single crystal on the SiC single crystal seed.
摘要翻译： 在使用化学气相传输生长大块SiC单晶的方法中，其中硅用作碳的化学转运剂，生长坩埚中以固定碳源材料和以其间隔开设置的SiC单晶种子填充。 诸如SiCl 4和还原气体如H 2的卤代硅烷气体通过单独的入口引入坩埚中并在坩埚内部混合。 以促进卤代硅烷气体和还原气体之间的化学反应的方式加热坩埚，导致卤代硅烷气体化学还原成元素硅（Si）蒸气。 生成的Si蒸气被输送到固体碳源材料，在其中它与固体碳源材料反应，产生挥发性的含Si和含C的分子。 所生产的含Si轴承和C轴承蒸汽输送到SiC单晶种子上并沉淀在SiC单晶种子上，导致SiC单晶种子上的SiC单晶生长。
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5.发明授权Vanadium compensated, SI SiC single crystals of NU and PI type and the crystal growth process thereof 有权钒补偿，NU和PI型的SI SiC单晶及其晶体生长过程公开(公告)号：US09090989B2
公开(公告)日：2015-07-28
申请号：US13902016
申请日：2013-05-24
申请人： II-VI Incorporated
发明人： Ilya Zwieback , Ping Wu , Varatharajan Rengarajan , Avinash K. Gupta , Thomas E. Anderson , Gary E. Ruland , Andrew E. Souzis , Xueping Xu
CPC分类号： C30B23/002 , C30B29/36 , H01B3/025
摘要： In a crystal growth apparatus and method, polycrystalline source material and a seed crystal are introduced into a growth ambient comprised of a growth crucible disposed inside of a furnace chamber. In the presence of a first sublimation growth pressure, a single crystal is sublimation grown on the seed crystal via precipitation of sublimated source material on the seed crystal in the presence of a flow of a first gas that includes a reactive component that reacts with and removes donor and/or acceptor background impurities from the growth ambient during said sublimation growth. Then, in the presence of a second sublimation growth pressure, the single crystal is sublimation grown on the seed crystal via precipitation of sublimated source material on the seed crystal in the presence of a flow of a second gas that includes dopant vapors, but which does not include the reactive component.
摘要翻译： 在晶体生长装置和方法中，将多晶源材料和晶种引入到由设置在炉室内部的生长坩埚组成的生长环境中。 在存在第一升华生长压力的情况下，通过在第一气体的流动存在下，通过在晶种上沉淀升华的源材料在晶种上生长单晶，所述第一气体包括与反应物质反应并除去的反应性组分 在升华生长期间来自生长环境的供体和/或受体背景杂质。 然后，在存在第二升华生长压力的情况下，单晶通过在包括掺杂剂蒸气的第二气体的流动存在下在晶种上沉淀升华的源材料而在晶种上生长，但是它是 不包括反应性组分。
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6.发明申请公开(公告)号：US20130280466A1
公开(公告)日：2013-10-24
申请号：US13867198
申请日：2013-04-22
申请人： II-VI Incorporated
发明人： Ilya Zwieback , Thomas E. Anderson , Andrew E. Souzis , Gary E. Ruland , Avinash K. Gupta , Varatharajan Rengarajan , Ping Wu , Xueping Xu
CPC分类号： C30B23/005 , B28D5/00 , C30B29/36 , Y10T428/21
摘要： A method and system of forming large-diameter SiC single crystals suitable for fabricating high crystal quality SiC substrates of 100, 125, 150 and 200 mm in diameter are described. The SiC single crystals are grown by a seeded sublimation technique in the presence of a shallow radial temperature gradient. During SiC sublimation growth, a flux of SiC bearing vapors filtered from carbon particulates is substantially restricted to a central area of the surface of the seed crystal by a separation plate disposed between the seed crystal and a source of the SiC bearing vapors. The separation plate includes a first, substantially vapor-permeable part surrounded by a second, substantially non vapor-permeable part. The grown crystals have a flat or slightly convex growth interface. Large-diameter SiC wafers fabricated from the grown crystals exhibit low lattice curvature and low densities of crystal defects, such as stacking faults, inclusions, micropipes and dislocations.
摘要翻译： 描述了形成适于制造直径为100,125,150和200mm的高质量SiC衬底的大直径SiC单晶的方法和系统。 通过种子升华技术在浅径向温度梯度的存在下生长SiC单晶。 在SiC升华生长期间，通过设置在晶种和SiC轴承蒸气源之间的分离板，从碳颗粒过滤的含有碳纳米管的蒸气的通量基本上限制在晶种表面的中心区域。 分离板包括由第二基本上不透气的部分包围的第一基本上透气的部分。 生长的晶体具有平坦或略凸的生长界面。 由生长的晶体制造的大直径SiC晶片表现出低的晶格曲率和低密度的晶体缺陷，例如堆垛层错，夹杂物，微孔和位错。
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7.发明申请公开(公告)号：US20170321345A1
公开(公告)日：2017-11-09
申请号：US15584583
申请日：2017-05-02
申请人： II-VI Incorporated
IPC分类号： C30B25/02 , C01B33/025
CPC分类号： C30B25/02 , C01B33/025 , C30B23/06 , C30B29/36
摘要： In an apparatus and method growing a SiC single crystal, a PVT growth apparatus is provided with a single crystal SiC seed and a SiC source material positioned in spaced relation in a growth crucible. A resistance heater heats the growth crucible such that the SiC source material sublimates and is transported via a temperature gradient that forms in the growth crucible in response to the heater heating the growth crucible to the single crystal SiC seed where the sublimated SiC source material condenses forming a growing SiC single crystal. Purely axial heat fluxes passing through the bottom and the top of the growth crucible form a flat isotherm at least at a growth interface of the growing SiC single crystal on the single crystal SiC seed.
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8.发明授权Method for silicon carbide crystal growth by reacting elemental silicon vapor with a porous carbon solid source material 有权通过使元素硅蒸汽与多孔碳固体源材料反应生成碳化硅晶体的方法公开(公告)号：US09580837B2
公开(公告)日：2017-02-28
申请号：US14475803
申请日：2014-09-03
申请人： II-VI Incorporated
发明人： Ilya Zwieback , Varatharajan Rengarajan , Bryan K. Brouhard , Michael C. Nolan , Thomas E. Anderson
摘要： In a method for growing bulk SiC single crystals using chemical vapor transport, wherein silicon acts as a chemical transport agent for carbon, a growth crucible is charged with a solid carbon source material and a SiC single crystal seed disposed therein in spaced relationship. A halosilane gas, such as SiCl4 and a reducing gas, such as H2, are introduced into the crucible via separate inlets and mix in the crucible interior. The crucible is heated in a manner that encourages chemical reaction between the halosilane gas and the reducing gas leading to the chemical reduction of the halosilane gas to elemental silicon (Si) vapor. The produced Si vapor is transported to the solid carbon source material where it reacts with the solid carbon source material yielding volatile Si-bearing and C-bearing molecules. The produced Si-bearing and C-bearing vapors are transported to the SiC single crystal seed and precipitate on the SiC single crystal seed causing growth of a SiC single crystal on the SiC single crystal seed.
摘要翻译： 在使用化学气相传输生长大块SiC单晶的方法中，其中硅用作碳的化学转运剂，生长坩埚中以固定碳源材料和以其间隔开设置的SiC单晶种子填充。 诸如SiCl 4和还原气体如H 2的卤代硅烷气体通过单独的入口引入坩埚中并在坩埚内部混合。 以促进卤代硅烷气体和还原气体之间的化学反应的方式加热坩埚，导致卤代硅烷气体化学还原成元素硅（Si）蒸气。 生成的Si蒸气被输送到固体碳源材料，在其中它与固体碳源材料反应，产生挥发性的含Si和含C的分子。 所生产的含Si轴承和C轴承蒸汽输送到SiC单晶种子上并沉淀在SiC单晶种子上，导致SiC单晶种子上的SiC单晶生长。
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9.发明申请Axial Gradient Transport (AGT) Growth Process and Apparatus Utilizing Resistive Heating 审中-公开轴向梯度运输（AGT）生长过程和利用电阻加热的装置公开(公告)号：US20160097143A1
公开(公告)日：2016-04-07
申请号：US14967926
申请日：2015-12-14
申请人： II-VI INCORPORATED
CPC分类号： C30B23/063 , C23C14/243 , C23C14/26 , C23C14/541 , C30B23/06 , C30B23/066 , C30B29/36
摘要： A crucible has a first resistance heater is disposed in spaced relation above the top of the crucible and a second resistance heater with a first resistive section disposed in spaced relation beneath the bottom of the crucible and with a second resistive section disposed in spaced relation around the outside of the side of the crucible. The crucible is charged with a seed crystal at the top of an interior of the crucible and a source material in the interior of the crucible in spaced relation between the seed crystal and the bottom of the crucible. Electrical power of a sufficient extent is applied to the first and second resistance heaters to create in the interior of the crucible a temperature gradient of sufficient temperature to cause the source material to sublimate and condense on the seed crystal thereby forming a growing crystal.
摘要翻译： 坩埚具有第一电阻加热器，其间隔开地设置在坩埚的顶部之上，第二电阻加热器具有第一电阻部分，第一电阻部分以坩埚底部的间隔设置，并且第二电阻部分间隔设置在坩埚的顶部 在坩埚的侧面之外。 在坩埚的内部的顶部装载坩埚，坩埚内部的源材料以晶种和坩埚的底部间隔开来。 将足够程度的电力施加到第一和第二电阻加热器，以在坩埚内部产生足够温度的温度梯度，以使源材料在晶种上升华和冷凝，从而形成生长晶体。
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公开(公告)号：US20190249332A1
公开(公告)日：2019-08-15
申请号：US16368977
申请日：2019-03-29
申请人： II-VI Incorporated
CPC分类号： C30B29/36 , C30B23/005 , C30B23/06 , C30B23/066
摘要： A physical vapor transport growth system includes a growth chamber charged with SiC source material and a SiC seed crystal in spaced relation and an envelope that is at least partially gas-permeable disposed in the growth chamber. The envelope separates the growth chamber into a source compartment that includes the SiC source material and a crystallization compartment that includes the SiC seed crystal. The envelope is formed of a material that is reactive to vapor generated during sublimation growth of a SiC single crystal on the SiC seed crystal in the crystallization compartment to produce C-bearing vapor that acts as an additional source of C during the growth of the SiC single crystal on the SiC seed crystal.
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