公开(公告)号：US09145621B2

公开(公告)日：2015-09-29

申请号：US13820530

申请日：2011-12-15

申请人： Toru Nagashima ,  Keiichiro Hironaka

发明人： Toru Nagashima ,  Keiichiro Hironaka

IPC分类号： C30B29/38 ,  C30B25/10 ,  C30B29/40 ,  C01F7/56 ,  C01F7/58 ,  C30B25/00 ,  C30B35/00 ,  H01L21/02

CPC分类号： C30B25/10 ,  C01F7/56 ,  C01F7/58 ,  C30B25/00 ,  C30B29/403 ,  C30B35/007 ,  H01L21/0254 ,  H01L21/0262

摘要： A production method of aluminum based group III nitride single crystal includes a reaction step, wherein a halogenated gas and an aluminum contact at 300° C. or more to 700° C. or less, producing a mixed gas including an aluminum trihalide gas and an aluminum monohalide gas; a converting step, wherein the aluminum monohalide gas is converted to a solid by setting a temperature of the mixed gas equal to or higher than a temperature to which a solid aluminum trihalide deposit, and lower by 50° C. or more than a temperature to which halogenated gas and aluminum contact in the reaction step; a separation step, wherein the aluminum trihalide gas is removed; and a crystal growth step, wherein the aluminum trihalide gas is used for an aluminum based group III nitride single crystal raw material, keeping its temperature equal to or higher than a temperature of the converting step.

摘要翻译： 铝基III族氮化物单晶的制造方法包括反应工序，其中在300℃以上700℃以下的卤化气体和铝接触，制造包含三卤化铝气体和 一卤化铝; 转化步骤，其中通过将混合气体的温度设定为等于或高于固体三卤化铝的温度沉积，并将其降低50℃或更高的温度，将一卤化铝转化为固体 在反应步骤中卤化气体和铝接触; 分离步骤，其中除去三卤化铝气体; 以及晶体生长步骤，其中所述三卤化铝气体用于铝基III族氮化物单晶原料，保持其温度等于或高于转化步骤的温度。

公开(公告)号：US20130319320A1

公开(公告)日：2013-12-05

申请号：US13820530

申请日：2011-12-15

申请人： Toru Nagashima ,  Keiichiro Hironaka

发明人： Toru Nagashima ,  Keiichiro Hironaka

IPC分类号： C30B25/10 ,  C01F7/56

CPC分类号： C30B25/10 ,  C01F7/56 ,  C01F7/58 ,  C30B25/00 ,  C30B29/403 ,  C30B35/007 ,  H01L21/0254 ,  H01L21/0262

摘要： A production method of aluminum based group III nitride single crystal includes a reaction step, wherein a halogenated gas and an aluminum contact at 300° C. or more to 700° C. or less, producing a mixed gas including an aluminum trihalide gas and an aluminum monohalide gas; a converting step, wherein the aluminum monohalide gas is converted to a solid by setting a temperature of the mixed gas equal to or higher than a temperature to which a solid aluminum trihalide deposit, and lower by 50° C. or more than a temperature to which halogenated gas and aluminum contact in the reaction step; a separation step, wherein the aluminum trihalide gas is removed; and a crystal growth step, wherein the aluminum trihalide gas is used for an aluminum based group III nitride single crystal raw material, keeping its temperature equal to or higher than a temperature of the converting step.

摘要翻译： 铝基III族氮化物单晶的制造方法包括反应工序，其中在300℃以上700℃以下的卤化气体和铝接触，制造包含三卤化铝气体和 一卤化铝; 转化步骤，其中通过将混合气体的温度设定为等于或高于固体三卤化铝的温度沉积，并将其降低50℃或更高的温度，将一卤化铝转化为固体 在反应步骤中卤化气体和铝接触; 分离步骤，其中除去三卤化铝气体; 以及晶体生长步骤，其中所述三卤化铝气体用于铝基III族氮化物单晶原料，保持其温度等于或高于转化步骤的温度。

公开(公告)号：US20100029065A1

公开(公告)日：2010-02-04

申请号：US12440413

申请日：2007-08-03

申请人： Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi ,  Manabu Harada ,  Yasunori Hirata ,  Keisuke Kondo

发明人： Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi ,  Manabu Harada ,  Yasunori Hirata ,  Keisuke Kondo

IPC分类号： H01L21/20 ,  C23C16/54

CPC分类号： C23C16/303 ,  C23C16/45512 ,  C23C16/45514 ,  C23C16/45519 ,  C23C16/4557 ,  C30B25/02 ,  C30B25/14 ,  C30B25/16 ,  C30B29/403 ,  H01L21/0254 ,  H01L21/0262

摘要： A method of producing a group III nitride such as aluminum nitride, comprising the step of reacting a group III halide gas such as aluminum trichloride gas with a nitrogen source gas such as ammonia gas in a growth chamber to grow a group III nitride on a substrate held in the growth chamber, wherein the method further comprises premixing together the group III halide gas and the nitrogen source gas to obtain a mixed gas and then introducing the mixed gas into the growth chamber without forming a deposit in the mixed gas substantially to be reacted each other.For the growth of a group III nitride such as an aluminum-based group III nitride by HVPE, there are provided a method of producing the group III nitride having as high quality as that obtained by the method of the prior art at a high yield and an apparatus used in the method.

摘要翻译： 一种生产III族氮化物如氮化铝的方法，包括在生长室中使诸如三氯化铝气体的III族卤化物气体与诸如氨气的氮源气体反应以在衬底上生长III族氮化物的步骤 保持在生长室中，其中所述方法还包括将III族卤化物气体和氮源气体一起预混合以获得混合气体，然后将混合气体引入生长室中，而不在基本上被反应的混合气体中形成沉积物 彼此。 对于通过HVPE的诸如铝基III族氮化物的III族氮化物的生长，提供了以高产率制备具有如现有技术方法获得的高质量的III族氮化物的方法， 该方法中使用的装置。

公开(公告)号：US08926752B2

公开(公告)日：2015-01-06

申请号：US12526685

申请日：2008-02-27

申请人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi

发明人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi

IPC分类号： C30B25/00 ,  C30B29/40 ,  C30B25/10 ,  C30B25/18

CPC分类号： C30B29/403 ,  C30B25/10 ,  C30B25/18

摘要： There is provided a method capable of obtaining an aluminum-based group III nitride crystal layer having a smooth surface and high crystallinity by employing only HVPE in which inexpensive raw materials can be used to reduce production costs and high-speed film formation is possible without employing MOVPE.To produce a group III nitride crystal by HVPE comprising the step of growing a group III nitride crystal layer by vapor-phase growth on a single crystal substrate by contacting the heated single crystal substrate with a raw material gas containing a group III halide and a compound having a nitrogen atom, the group III nitride crystal is grown by vapor-phase growth on the single crystal substrate heated at a temperature of 1,000° C. or more and less than 1,200° C. to form an intermediate layer and then, a group III nitride crystal is further grown by vapor-phase growth on the intermediate layer on the substrate heated at a temperature of 1,200° C. or higher.

摘要翻译： 提供了一种能够通过仅使用HVPE来获得具有光滑表面和高结晶度的铝基III族氮化物晶体层的方法，其中可以使用便宜的原料来降低生产成本，并且可以在不使用高速成膜的情况下进行高速成膜 MOVPE。 为了通过HVPE制造III族氮化物晶体，包括通过使加热的单晶衬底与含有III族卤化物和化合物的原料气体接触，在单晶衬底上通过气相生长生长III族氮化物晶体层的步骤 具有氮原子的情况下，在1000℃以上且小于1200℃的温度加热的单晶衬底上通过气相生长生长III族氮化物晶体，形成中间层， 通过在1200℃以上的温度下加热的基板上的中间层上气相生长进一步生长III族氮化物晶体。

公开(公告)号：US20110094438A1

公开(公告)日：2011-04-28

申请号：US12812872

申请日：2009-01-09

申请人： Akinori Koukitu ,  Yoshinao Kumagai ,  Masanari Ishizuki ,  Toru Nagashima ,  Akira Hakomori ,  Kazuya Takada

发明人： Akinori Koukitu ,  Yoshinao Kumagai ,  Masanari Ishizuki ,  Toru Nagashima ,  Akira Hakomori ,  Kazuya Takada

IPC分类号： C30B25/10

CPC分类号： C30B25/18 ,  C30B25/183 ,  C30B29/403

摘要： The present invention provides a self-supporting substrate obtained by the steps of: forming an Al-based group-III nitride thin-layer having a thickness in the range of 3-200 nm on a base substrate made of a single crystal of an inorganic substance which substantially does not decompose at 800° C. in an inert gas atmosphere and which does produce volatiles by decomposition when contacting with a reducing gas in a temperature range of 800-1600° C., for example sapphire; forming voids along the interface between the base substrate and the Al-based group-III nitride thin-layer of the obtained laminated substrate by thermally treating the laminated substrate in a temperature range of 800-1600° C. in a reducing gas atmosphere containing ammonia gas; forming a group-III nitride single crystal thick-layer on the Al-based group-III nitride thin-layer; and separating these formed layers. The self-supporting substrate is a self-supporting substrate of the group-III nitride single crystal such as AlN, which is suitably used for forming a semiconductor device such as ultraviolet light emitting device and of which crystal plane shows a large radius of curvature.

摘要翻译： 本发明提供一种自支撑基板，其通过以下步骤获得：在由无机物的单晶制成的基底基板上形成厚度在3〜200nm范围内的Al系III族氮化物薄层 在惰性气体气氛中在800℃下基本上不分解的物质，当与800-1600℃的温度范围内的还原气体例如蓝宝石接触时，其通过分解产生挥发物; 通过在800-1600℃的温度范围内在含有氨的还原气体气氛中热处理层压基板，沿着基底基板和Al基III族氮化物薄层之间的界面形成空隙 加油站; 在Al系III族氮化物薄层上形成III族氮化物单晶厚层; 并分离这些形成的层。 自支撑衬底是诸如AlN的III族氮化物单晶的自支撑衬底，其适合用于形成诸如紫外光发射器件的半导体器件，并且其中晶体具有大的曲率半径。

公开(公告)号：US20110018104A1

公开(公告)日：2011-01-27

申请号：US12812885

申请日：2008-12-16

申请人： Toru Nagashima ,  Akira Hakomori ,  Kazuya Takada ,  Masanari Ishizuki ,  Akinori Koukitu ,  Yoshinao Kumagai

发明人： Toru Nagashima ,  Akira Hakomori ,  Kazuya Takada ,  Masanari Ishizuki ,  Akinori Koukitu ,  Yoshinao Kumagai

IPC分类号： H01L29/20 ,  C30B23/02 ,  H01L21/20

CPC分类号： C30B29/403 ,  C30B25/183 ,  H01L33/0075 ,  H01L2924/0002 ,  H01L2924/00

摘要： The present invention is a method for producing a laminated body, comprising the steps of: (1) preparing a base substrate having a surface formed of a single crystal which is different from the material constituting the Al-based group-III nitride single crystal layer to be formed; (2) forming an Al-based group-III nitride single crystal layer having a thickness of 10 nm to 1.5 μm on the single crystal surface of the prepared base substrate; (3) forming on the Al-based group-III nitride single crystal layer a non-single crystal layer being 100 times or more thicker than the Al-based group-III nitride single crystal layer without breaking the previously-obtained Al-based group-III nitride single crystal layer; and (4) removing the base substrate. The method provides a substrate which can be suitably used as a base substrate for producing an Al-based group-III nitride single crystal self-supporting substrate, of which surface is formed of a single crystal of an Al-based group-III nitride, and which is free from cracking and warpage.

摘要翻译： 本发明是一种层叠体的制造方法，其特征在于，包括以下工序：（1）制作具有与构成所述Al系III族氮化物单晶层的材料不同的单晶的表面的基底基板 要形成 （2）在所制备的基板的单晶面上形成厚度为10nm〜1.5μm的Al系III族氮化物单晶层; （3）在Al系III族氮化物单晶层上形成比Al系III族氮化物单晶层厚100倍以上的非单晶层，而不会破坏先前获得的Al基团 -III氮化物单晶层; 和（4）去除基底。 该方法提供了可以适合用作用于制造Al基III族氮化物单晶自支撑衬底的基底的衬底，其表面由Al基III族氮化物的单晶形成， 并且没有开裂和翘曲。

公开(公告)号：US09840790B2

公开(公告)日：2017-12-12

申请号：US14422888

申请日：2012-08-23

申请人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Toru Kinoshita ,  Yuki Kubota ,  Rafael F. Dalmau ,  Jinqiao Xie ,  Baxter F. Moody ,  Raoul Schlesser ,  Zlatko Sitar

发明人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Toru Kinoshita ,  Yuki Kubota ,  Rafael F. Dalmau ,  Jinqiao Xie ,  Baxter F. Moody ,  Raoul Schlesser ,  Zlatko Sitar

IPC分类号： C30B25/02 ,  C30B25/20 ,  C30B25/14 ,  C30B29/40 ,  H01L33/00 ,  H01L33/32 ,  H01L33/02 ,  C30B25/16 ,  C01B21/072 ,  H01L33/18

CPC分类号： C30B25/20 ,  C01B21/072 ,  C01P2006/60 ,  C30B25/14 ,  C30B25/165 ,  C30B29/403 ,  H01L33/0075 ,  H01L33/02 ,  H01L33/18 ,  H01L33/32 ,  Y10T428/26

摘要： The invention provides highly transparent single crystalline AlN layers as device substrates for light emitting diodes in order to improve the output and operational degradation of light emitting devices. The highly transparent single crystalline AlN layers have a refractive index in the a-axis direction in the range of 2.250 to 2.400 and an absorption coefficient less than or equal to 15 cm-1 at a wavelength of 265 nm. The invention also provides a method for growing highly transparent single crystalline AlN layers, the method including the steps of maintaining the amount of Al contained in wall deposits formed in a flow channel of a reactor at a level lower than or equal to 30% of the total amount of aluminum fed into the reactor, and maintaining the wall temperature in the flow channel at less than or equal to 1200° C.

公开(公告)号：US09691942B2

公开(公告)日：2017-06-27

申请号：US14366020

申请日：2011-12-22

申请人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Yuki Hiraren

发明人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Yuki Hiraren

IPC分类号： C30B25/02 ,  H01L33/34 ,  C30B25/08 ,  H01L21/02 ,  C30B29/40 ,  H01L33/00 ,  C30B23/00

CPC分类号： H01L33/343 ,  C30B23/00 ,  C30B25/02 ,  C30B25/08 ,  C30B29/403 ,  H01L21/0254 ,  H01L33/0054

摘要： The present invention relates to a single-crystalline aluminum nitride wherein a carbon concentration is 1×1014 atoms/cm3 or more and less than 3×1017 atoms/cm3, a chlorine concentration is 1×1014 to 1×1017 atoms/cm3, and an absorption coefficient at 265 nm wavelength is 40 cm−1 or less.

公开(公告)号：US08129208B2

公开(公告)日：2012-03-06

申请号：US12526196

申请日：2008-02-02

申请人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi

发明人： Akinori Koukitu ,  Yoshinao Kumagai ,  Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi

IPC分类号： H01L21/02

CPC分类号： C30B25/02 ,  C30B29/403 ,  H01L21/02389 ,  H01L21/02403 ,  H01L21/0242 ,  H01L21/02458 ,  H01L21/0254 ,  H01L21/02576 ,  H01L21/0262 ,  H01L33/007

摘要： This invention provides a self supporting substrate which consists of a n-type conductive aluminum nitride semiconductor crystal and is useful for manufacturing the vertical conductive type AlN semiconductor device. The n-type conductive aluminum nitride semiconductor crystal, by which the self supporting substrate is made up, contains Si atom at a concentration of 1×1018 to 5×1020 cm−3 is substantially free of halogen atoms and substantially does not absorb the light having the energy of not more than 5.9 eV. The self supporting substrate can be obtained by a method comprising the steps of forming an AlN crystal layer on a single crystal substrate such as a sapphire by the HVPE method, preheating the obtained substrate having the AlN crystal layer to a temperature of 1,200° C. or more, forming a second layer consisting of the n-type conductive aluminum nitride semiconductor crystal is formed on the AlN crystal layer in high rate by the HVPE method and separating the second layer from the obtained laminate.

摘要翻译： 本发明提供一种由n型导电氮化铝半导体晶体组成的自支撑衬底，并且可用于制造垂直导电型AlN半导体器件。 构成自支撑衬底的n型导电氮化铝半导体晶体含有浓度为1×1018至5×1020cm-3的Si原子，基本上不含卤素原子并且基本上不吸收光 能量不超过5.9 eV。 自支撑基板可以通过以下方法获得：通过HVPE法在诸如蓝宝石的单晶衬底上形成AlN晶体层的步骤，将获得的具有AlN晶体层的衬底预热到1200℃的温度。 以上，通过HVPE法以高速率在AlN结晶层上形成由n型导电性氮化铝半导体晶体构成的第二层，并将第二层与得到的层叠体分离。

公开(公告)号：US07947577B2

公开(公告)日：2011-05-24

申请号：US12440413

申请日：2007-08-03

申请人： Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi ,  Manabu Harada ,  Yasunori Hirata ,  Keisuke Kondo

发明人： Toru Nagashima ,  Kazuya Takada ,  Hiroyuki Yanagi ,  Manabu Harada ,  Yasunori Hirata ,  Keisuke Kondo

IPC分类号： H01L21/20 ,  C23C16/00

CPC分类号： C23C16/303 ,  C23C16/45512 ,  C23C16/45514 ,  C23C16/45519 ,  C23C16/4557 ,  C30B25/02 ,  C30B25/14 ,  C30B25/16 ,  C30B29/403 ,  H01L21/0254 ,  H01L21/0262

摘要： A method of producing a group III nitride such as aluminum nitride, comprising the step of reacting a group III halide gas such as aluminum trichloride gas with a nitrogen source gas such as ammonia gas in a growth chamber to grow a group III nitride on a substrate held in the growth chamber, wherein the method further comprises premixing together the group III halide gas and the nitrogen source gas to obtain a mixed gas and then introducing the mixed gas into the growth chamber without forming a deposit in the mixed gas substantially to be reacted each other.For the growth of a group III nitride such as an aluminum-based group III nitride by HVPE, there are provided a method of producing the group III nitride having as high quality as that obtained by the method of the prior art at a high yield and an apparatus used in the method.

摘要翻译： 一种生产III族氮化物如氮化铝的方法，包括在生长室中使诸如三氯化铝气体的III族卤化物气体与诸如氨气的氮源气体反应以在衬底上生长III族氮化物的步骤 保持在生长室中，其中所述方法还包括将III族卤化物气体和氮源气体一起预混合以获得混合气体，然后将混合气体引入生长室中，而不在基本上被反应的混合气体中形成沉积物 彼此。 对于通过HVPE的诸如铝基III族氮化物的III族氮化物的生长，提供了以高产率制备具有如现有技术方法获得的高质量的III族氮化物的方法， 该方法中使用的装置。