公开(公告)号：US07794539B2

公开(公告)日：2010-09-14

申请号：US10599501

申请日：2005-03-31

申请人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Yasuhito Takahashi

发明人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Yasuhito Takahashi

IPC分类号： C30B9/00 ,  C30B30/04 ,  C30B28/06 ,  C30B11/00

CPC分类号： C30B9/10 ,  C30B29/403 ,  C30B29/406 ,  Y10T117/1092 ,  Y10T117/1096

摘要： A method for producing Group-III-element nitride crystals by which an improved growth rate is obtained and large high-quality crystals can be grown in a short time, a producing apparatus used therein, and a semiconductor element obtained using the method and the apparatus are provided. The method is a method for producing Group-III-element nitride crystals that includes a crystal growth process of subjecting a material solution containing a Group III element, nitrogen, and at least one of alkali metal and alkaline-earth metal to pressurizing and heating under an atmosphere of a nitrogen-containing gas so that the nitrogen and the Group III element in the material solution react with each other to grow crystals. The method further includes, prior to the crystal growth process, a material preparation process of preparing the material solution in a manner that under an atmosphere of a nitrogen-containing gas, at least one of an ambient temperature and an ambient pressure is set so as to be higher than is set as a condition for the crystal growth process so that the nitrogen is allowed to dissolve in a melt containing the Group III element and the at least one of alkali metal and alkaline-earth metal. The method according to the present invention can be performed by using, for example, the producing apparatus shown in FIG. 7.

摘要翻译： 一种生产III族元素的氮化物晶体的方法，其中获得了改善的生长速率并且可以在短时间内生长大量的高质量晶体，其中使用的制造装置以及使用该方法和装置得到的半导体元件 被提供。 该方法是生产III族元素氮化物晶体的方法，其包括使含有III族元素，氮和至少一种碱金属和碱土金属的材料溶液经受加压和加热的晶体生长过程 含氮气体的气氛使得材料溶液中的氮和III族元素彼此反应生长晶体。 该方法还包括在晶体生长过程之前，制备材料制备方法，该方法是在含氮气体的气氛中，将环境温度和环境压力中的至少一种设定为 高于设定为晶体生长过程的条件，使得氮能够溶解在含有III族元素和碱金属和碱土金属中的至少一种的熔体中。 根据本发明的方法可以通过使用例如图1所示的制造装置来执行。 7。

公开(公告)号：US20080213158A1

公开(公告)日：2008-09-04

申请号：US12082745

申请日：2008-04-14

申请人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Hidekazu Umeda ,  Yasuhito Takahashi

发明人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Hidekazu Umeda ,  Yasuhito Takahashi

IPC分类号： C30B23/00 ,  C01B21/06

CPC分类号： C30B29/403 ,  C30B9/10 ,  C30B29/406 ,  C30B35/00 ,  Y10T117/1064 ,  Y10T117/1096

摘要： A manufacturing apparatus of Group III nitride crystals and a method for manufacturing Group III nitride crystals are provided, by which high quality crystals can be manufactured. For instance, crystals are grown using the apparatus of the present invention as follows. A crystal raw material (131) and gas containing nitrogen are introduced into a reactor vessel (120), to which heat is applied by a heater (110), and crystals are grown in an atmosphere of pressure applied thereto. The gas is introduced from a gas supplying device (180) to the reactor vessel (120) through a gas inlet of the reactor vessel, and then is exhausted to the inside of a pressure-resistant vessel (102) through a gas outlet of the reactor vessel. Since the gas is introduced directly to the reactor vessel (120) without passing through the pressure-resistant vessel (102), the mixture of impurities attached to the pressure-resistant vessel (102) and the like into the site of the crystal growth can be prevented. Further, since the gas flows through the reactor vessel (120), there is no aggregation of an evaporating alkali metal, etc., at the gas inlet or the like, and such an alkali metal does not flow into the gas supplying device (180). As a result, the quality of Group III nitride crystals obtained can be improved.

摘要翻译： 提供III族氮化物晶体的制造装置和制造III族氮化物晶体的方法，由此可以制造高质量的晶体。 例如，使用本发明的装置如下生长晶体。 将晶体原料（131）和含氮气体引入反应器容器（120）中，通过加热器（110）向其施加热量，并在施加压力的气氛中生长晶体。 气体通过反应器容器的气体入口从气体供给装置（180）引入反应器容器（120），然后通过反应器的气体出口被排出到耐压容器（102）的内部 反应堆容器。 由于气体不通过耐压容器（102）直接引入反应器容器（120），附着在耐压容器（102）等上的杂质混合物进入晶体生长位置可以 被阻止 此外，由于气体流过反应器容器（120），所以在气体入口等处没有蒸发的碱金属等的聚集，并且这种碱金属不会流入气体供给装置（180 ）。 结果，可以提高获得的III族氮化物晶体的质量。

公开(公告)号：US07754012B2

公开(公告)日：2010-07-13

申请号：US12082745

申请日：2008-04-14

申请人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Hidekazu Umeda ,  Yasuhito Takahashi

发明人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Hidekazu Umeda ,  Yasuhito Takahashi

IPC分类号： C30B25/00 ,  C30B23/00 ,  C30B28/12 ,  C01B21/06

CPC分类号： C30B29/403 ,  C30B9/10 ,  C30B29/406 ,  C30B35/00 ,  Y10T117/1064 ,  Y10T117/1096

摘要： A method for manufacturing Group III nitride crystals with high quality is provided. By the method, a crystal raw material solution and gas containing nitrogen are introduced into a reactor vessel, which is heated, and crystals are grown in an atmosphere of pressure applied thereto. The gas is introduced from a gas supplying device to the reactor vessel through a gas inlet of the reactor vessel, and then is exhausted to the inside of a pressure-resistant vessel through a gas outlet of the reactor vessel. Since the gas is introduced directly to the reactor vessel, impurities attached to the pressure-resistant vessel and the like into the crystal growing site can be prevented. Further, the gas flows through the reactor vessel, to suppress aggregation of an evaporating alkali metal, etc., at the gas inlet and reduce flow of the metal vapor into the gas supplying device.

摘要翻译： 提供了高品质的III族氮化物晶体的制造方法。 通过该方法，将晶体原料溶液和含氮气体引入加热的反应器容器中，并在施加压力的气氛中生长晶体。 气体通过反应器容器的气体入口从气体供给装置引入反应器容器，然后通过反应器容器的气体出口被排出到耐压容器的内部。 由于气体直接引入反应容器，因此可以防止附着在耐压容器等上的杂质进入晶体生长部位。 此外，气体流过反应器容器，以抑制气体入口处的蒸发的碱金属等的聚集，并且减少金属蒸气进入气体供应装置的流动。

公开(公告)号：US07176115B2

公开(公告)日：2007-02-13

申请号：US10804610

申请日：2004-03-18

申请人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Akihiko Ishibashi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Akihiko Ishibashi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： H01L21/38 ,  H01L21/22

CPC分类号： C30B29/40 ,  C30B25/02 ,  C30B25/18 ,  H01L21/0237 ,  H01L21/0242 ,  H01L21/02458 ,  H01L21/0254 ,  H01L21/02625 ,  H01L21/02639 ,  H01L21/02642 ,  H01S5/0213 ,  H01S5/32341

摘要： The present invention provides a manufacturing method that allows a Group III nitride substrate with a low dislocation density to be manufactured, and a semiconductor device that is manufactured using the manufacturing method. The manufacturing method includes, in an atmosphere including nitrogen, allowing a Group III element and the nitrogen to react with each other in an alkali metal melt to cause generation and growth of Group III nitride crystals. In the manufacturing method, a plurality of portions of a Group III nitride semiconductor layer are prepared, selected as seed crystals, and used for at least one of the generation and the growth of the Group III nitride crystals, and then surfaces of the seed crystals are brought into contact with the alkali metal melt.

摘要翻译： 本发明提供了制造能够制造具有低位错密度的III族氮化物衬底的制造方法和使用该制造方法制造的半导体器件。 制造方法在包括氮的气氛中包括使III族元素和氮在碱金属熔体中彼此反应以引起III族氮化物晶体的产生和生长。 在制造方法中，制备III族氮化物半导体层的多个部分，选择晶种，并用于III族氮化物晶体的生成和生长中的至少一个，然后将晶种的表面 与碱金属熔体接触。

公开(公告)号：US20050059229A1

公开(公告)日：2005-03-17

申请号：US10911939

申请日：2004-08-04

申请人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Takatomo Sasaki ,  Fumio Kawamura

发明人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Takatomo Sasaki ,  Fumio Kawamura

IPC分类号： C30B19/02 ,  C30B29/40 ,  H01L21/20 ,  H01L21/205 ,  H01L21/208 ,  H01L21/28 ,  H01L21/304 ,  H01L21/306

CPC分类号： H01L21/30612 ,  C30B19/02 ,  C30B29/40 ,  H01L21/02389 ,  H01L21/0242 ,  H01L21/02458 ,  H01L21/0254 ,  H01L21/0262 ,  H01L21/02664 ,  H01L21/30625

摘要： The present invention provides a Group III nitride crystal substrate whose surface has concavities and convexities reduced in size. The surfaces with concavities and convexities, such as hillocks, pits and facets, of Group III nitride crystals are brought into contact with a melt and thereby the surfaces are subjected to meltback etching or mechanochemical polishing. The melt includes at least one of alkali metal and alkaline-earth metal. Thus a Group III nitride crystal substrate that has reduced strain and a reduced number of defects, which are caused through the processing, and is excellent in surface flatness is manufactured. Furthermore, by the use of the Group III nitride crystal substrate of the present invention, for instance, semiconductor devices of high performance can be obtained.

摘要翻译： 本发明提供一种III型氮化物晶体基板，其表面的尺寸和凹凸减小。 将III族氮化物晶体的具有凹凸和凹凸的表面，例如小丘，凹坑和小面与熔体接触，从而对表面进行回熔蚀刻或机械化学抛光。 熔体包括碱金属和碱土金属中的至少一种。 因此，制造了通过加工而产生的应力减小和缺陷数量减少，表面平坦性优异的III族氮化物晶体基板。 此外，通过使用本发明的III族氮化物晶体基板，例如可以获得高性能的半导体器件。

公开(公告)号：US07381268B2

公开(公告)日：2008-06-03

申请号：US10587223

申请日：2005-04-27

申请人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Hidekazu Umeda ,  Yasuhito Takahashi

发明人： Hisashi Minemoto ,  Yasuo Kitaoka ,  Isao Kidoguchi ,  Yusuke Mori ,  Fumio Kawamura ,  Takatomo Sasaki ,  Hidekazu Umeda ,  Yasuhito Takahashi

IPC分类号： C30B35/00

CPC分类号： C30B29/403 ,  C30B9/10 ,  C30B29/406 ,  C30B35/00 ,  Y10T117/1064 ,  Y10T117/1096

摘要： A manufacturing apparatus of Group III nitride crystals and a method for manufacturing Group III nitride crystals are provided, by which high quality crystals can be manufactured. For instance, crystals are grown using the apparatus of the present invention as follows. A crystal raw material (131) and gas containing nitrogen are introduced into a reactor vessel (120), to which heat is applied by a heater (110), and crystals are grown in an atmosphere of pressure applied thereto. The gas is introduced from a gas supplying device (180) to the reactor vessel (120) through a gas inlet of the reactor vessel, and then is exhausted to the inside of a pressure-resistant vessel (102) through a gas outlet of the reactor vessel. Since the gas is introduced directly to the reactor vessel (120) without passing through the pressure-resistant vessel (102), the mixture of impurities attached to the pressure-resistant vessel (102) and the like into the site of the crystal growth can be prevented. Further, since the gas flows through the reactor vessel (120), there is no aggregation of an evaporating alkali metal, etc., at the gas inlet or the like, and such an alkali metal does not flow into the gas supplying device (180). As a result, the quality of Group III nitride crystals obtained can be improved.

公开(公告)号：US07255742B2

公开(公告)日：2007-08-14

申请号：US10884252

申请日：2004-07-02

申请人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B29/38

CPC分类号： C30B29/403 ,  C30B19/04 ,  C30B19/06 ,  C30B29/406

摘要： The present invention provides a method of manufacturing Group III nitride crystals that are of high quality, are manufactured efficiently, and are useful and usable as a substrate for semiconductor manufacturing processes. A semiconductor layer that is made of a semiconductor and includes crystal-nucleus generation regions at its surface is formed. The semiconductor is expressed by a composition formula of AluGavIn1-u-vN (where 0≦u≦1, 0≦v≦1, and u+v≦1). Group III nitride crystals then are grown on the semiconductor layer by bringing the crystal-nucleus generation regions of the semiconductor layer into contact with a melt in an atmosphere including nitrogen. The melt contains nitrogen, at least one Group III element selected from the group consisting of gallium, aluminum, and indium, and at least one of alkali metal and alkaline-earth metal.

摘要翻译： 本发明提供一种制造高品质的III族氮化物晶体的方法，其有效制造，并且可用作半导体制造工艺的基板。 形成由半导体构成的半导体层，其表面具有晶核生成区域。 半导体由以下组成式表示：在1-uv N中（其中0 <= u <= 1,0，...， <= v <= 1，u + v <= 1）。 然后通过在包括氮气的气氛中使半导体层的晶核生成区域与熔体接触，在半导体层上生长III族氮化物晶体。 熔体含有氮，至少一种选自镓，铝和铟的III族元素，以及碱金属和碱土金属中的至少一种。

公开(公告)号：US20050011432A1

公开(公告)日：2005-01-20

申请号：US10884252

申请日：2004-07-02

申请人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B19/04 ,  C30B19/06 ,  C30B19/00

CPC分类号： C30B29/403 ,  C30B19/04 ,  C30B19/06 ,  C30B29/406

摘要： The present invention provides a method of manufacturing Group III nitride crystals that are of high quality, are manufactured efficiently, and are useful and usable as a substrate for semiconductor manufacturing processes. A semiconductor layer that is made of a semiconductor and includes crystal-nucleus generation regions at its surface is formed. The semiconductor is expressed by a composition formula of AluGavIn1-u-vN (where 0≦u≦1, 0≦v≦1, and u+v≦1). Group III nitride crystals then are grown on the semiconductor layer by bringing the crystal-nucleus generation regions of the semiconductor layer into contact with a melt in an atmosphere including nitrogen. The melt contains nitrogen, at least one Group III element selected from the group consisting of gallium, aluminum, and indium, and at least one of alkali metal and alkaline-earth metal.

摘要翻译： 本发明提供一种制造高品质的III族氮化物晶体的方法，其有效制造，并且可用作半导体制造工艺的基板。 形成由半导体构成的半导体层，其表面具有晶核生成区域。 半导体由AluGavIn1-u-vN的组成式表示（其中0 <= u <= 1,0 <= v <= 1，u + v <= 1）。 然后通过在包括氮气的气氛中使半导体层的晶核生成区域与熔体接触，在半导体层上生长III族氮化物晶体。 熔体含有氮，至少一种选自镓，铝和铟的III族元素，以及碱金属和碱土金属中的至少一种。

公开(公告)号：US07435295B2

公开(公告)日：2008-10-14

申请号：US10598095

申请日：2005-02-18

申请人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Yasuhito Takahashi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Yasuhito Takahashi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B25/12

CPC分类号： C30B29/406 ,  C30B9/10 ,  C30B19/02 ,  C30B19/063 ,  C30B19/064 ,  Y10T117/1016

摘要： The present invention provides a method for producing a compound single crystal that can improve a growth rate and grow a large single crystal with high crystal uniformity in a short time, and a production apparatus used for the method. The compound single crystal is grown while stirring a material solution to create a flow from a gas-liquid interface in contact with a source gas toward the inside of the material solution. With this stirring, the source gas can be dissolved easily in the material solution, and supersaturation can be achieved in a short time, thus improving the growth rate of the compound single crystal. Moreover, the flow formed by the stirring goes from the gas-liquid interface where a source gas concentration is high to the inside of the material solution where the source gas concentration is low, so that dissolution of the source gas becomes uniform. Accordingly, it is possible not only to suppress nonuniform nucleation at the gas-liquid interface, but also to improve the quality of the compound single crystal produced.

摘要翻译： 本发明提供了一种能够在短时间内提高生长速度和生长具有高结晶均匀性的大单晶的化合物单晶的制造方法和用于该方法的制造装置。 在搅拌材料溶液的同时培养复合单晶以产生与源气体接触的气液界面朝向材料溶液内部的流动。 通过该搅拌，能够将源气体容易地溶解在原料溶液中，可以在短时间内实现过饱和，从而提高复合单晶的生长速度。 此外，通过搅拌形成的流动源于源气体浓度高的气液界面到源气体浓度低的材料溶液的内部，使得源气体的溶解变得均匀。 因此，不仅可以抑制气液界面的不均匀成核，而且可以提高制造的复合单晶的质量。

公开(公告)号：US07288152B2

公开(公告)日：2007-10-30

申请号：US10884386

申请日：2004-07-02

申请人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura ,  Masanori Morishita

发明人： Yasuo Kitaoka ,  Hisashi Minemoto ,  Isao Kidoguchi ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura ,  Masanori Morishita

IPC分类号： C30B11/14

CPC分类号： H01L33/32 ,  H01L29/2003 ,  H01L29/66856

摘要： The present invention provides a manufacturing method in which high quality GaN crystals and GaN crystal substrates can be manufactured under mild conditions of low pressure and low temperature. In a method of manufacturing GaN crystals in which in a gas atmosphere containing nitrogen, gallium and the nitrogen are allowed to react with each other to generate GaN crystals in a mixed melt of the gallium and sodium, the gallium and the nitrogen are allowed to react with each other under a pressurizing condition that exceeds atmospheric pressure, and pressure P1 (atm(×1.013×105 Pa)) of the pressurizing condition is set so as to satisfy the condition that is expressed by the following conditional expression (I): P≦P1

摘要翻译： 本发明提供了一种制造方法，其中可以在低压和低温的温和条件下制造高质量的GaN晶体和GaN晶体衬底。 在制造GaN晶体的方法中，其中在含有氮气的气体气氛中，允许镓和氮彼此反应以在镓和钠的混合熔体中产生GaN晶体，使镓和氮反应 在超过大气压的加压条件下彼此相对地设定加压条件的压力P 1（atm（x1.013×10 Pa）），以满足由 （I）：<？in-line-formula description =“In-line formula”end =“lead”？> P <= P 1 <（P + 45），（I） 公式描述=“在线公式”end =“tail”？>其中在表达式（I）中，P（atm（x1.013×10 Pa））表示最小压力， 在混合熔体的温度T℃下产生GaN晶体。