公开(公告)号：EP2123802A1

公开(公告)日：2009-11-25

申请号：EP08711084.7

申请日：2008-02-05

申请人： National University Corporation Tokyo University of Agriculture and Technology ,  Tokuyama Corporation

发明人： KOUKITU, Akinori ,  KUMAGAI, Yoshinao ,  NAGASHIMA, Toru ,  TAKADA, Kazuya ,  YANAGI, Hiroyuki

IPC分类号： C30B29/38 ,  C23C16/01 ,  C23C16/34 ,  C30B25/18 ,  H01L21/205 ,  H01L33/00

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 selfsupporting 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 selfsupporting substrate is made up, contains Si atom at a concentration of 1×10 18 to 5×10 20 cm -3 , is substantially free from halogen atoms, and substantially does not absorb the light having the energy of not more than 5.9 eV. The selfsupporting 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1×10 18至5×10 20 cm -3的Si原子，基本上不含卤素原子，并且基本上不 吸收能量不超过5.9 eV的光。 可以通过包括以下步骤的方法获得自支撑衬底：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晶体层的衬底预热至1200℃或更高的温度 通过HVPE法在AlN晶体层上高速率地形成由n型导电氮化铝半导体晶体构成的第二层，并将第二层从得到的层压体分离。

公开(公告)号：EP2243866A1

公开(公告)日：2010-10-27

申请号：EP08870572.8

申请日：2008-12-16

申请人： National University Corporation Tokyo University of Agriculture and Technology ,  Tokuyama Corporation

发明人： NAGASHIMA, Toru ,  HAKOMORI, Akira ,  TAKADA, Kazuya ,  ISHIZUKI, Masanari ,  KOUKITU, Akinori ,  KUMAGAI, Yoshinao

IPC分类号： C30B29/38 ,  C30B25/18

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： 本发明是生产的层叠体，其包括以下步骤的方法：（1）制备具有形成在单晶的表面上的基底基板的所有这是从构成Al系III族氮化物单晶层的材料不同 要形成; （2），其具有的厚度为所制备的基底基板的单晶表面上10纳米至1.5微米的Al系III族氮化物单晶层的形成; （3）在形成Al系III族氮化物单晶层上形成非单晶层是不破坏先前获得的Al系基团比的Al系III族氮化物单晶层的100倍或更厚 -III族氮化物单晶层; 和（4）除去所述基底基板。 该方法提供了可以适合用作基底基板在Al系III族氮化物单晶自支撑衬底的制造中，该表面形成的Al系III族氮化物的单晶构成的基底， 而所有这一切是从开裂和翘曲免费。

公开(公告)号：EP2141267A1

公开(公告)日：2010-01-06

申请号：EP08721312.0

申请日：2008-02-27

申请人： National University Corporation Tokyo University of Agriculture and Technology ,  Tokuyama Corporation

发明人： KOUKITU, Akinori ,  KUMAGAI, Yoshinao ,  NAGASHIMA, Toru ,  TAKADA, Kazuya ,  YANAGI, Hiroyuki

IPC分类号： C30B29/38 ,  C30B25/10

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廉价的原材料用于降低生产成本的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，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，然后加入III族氮化物 通过在1200℃以上的温度下加热的基板上的中间层上的气相生长进一步生长晶体。

公开(公告)号：EP2796596A1

公开(公告)日：2014-10-29

申请号：EP11878135.0

申请日：2011-12-22

申请人： National University Corporation Tokyo University of Agriculture and Technology ,  Tokuyama Corporation

发明人： KOUKITU, Akinori ,  KUMAGAI, Yoshinao ,  NAGASHIMA, Toru ,  HIRAREN, Yuki

IPC分类号： C30B29/38 ,  C30B25/02

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 an aluminum nitride single crystal characterized in that the concentration of carbon is 1x10 14 atoms/cm 3 , the concentration of chlorine is 1x10 14 to 1x10 17 atoms/cm 3 , and the absorption coefficient at a wavelength of 265 nm is 40 cm -1 or less.

摘要翻译： 本发明涉及一种氮化铝单晶，其特征在于碳的浓度为1×10 14原子/ cm 3，氯的浓度为1×10 14至1×10 17原子/ cm 3，波长为265nm的吸收系数 为40cm -1以下。

公开(公告)号：EP2243868A1

公开(公告)日：2010-10-27

申请号：EP09702588.6

申请日：2009-01-09

申请人： National University Corporation Tokyo University of Agriculture and Technology ,  Tokuyama Corporation

发明人： KOUKITU, Akinori ,  KUMAGAI, Yoshinao ,  ISHIZUKI, Masanari ,  NAGASHIMA, Toru ,  HAKOMORI, Akira ,  TAKADA, Kazuya

IPC分类号： C30B29/38 ,  C30B25/18

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：在由无机的单晶制成的基底上形成厚度在3〜200nm范围内的Al系III族氮化物薄层 在800℃，在惰性气体气氛中基本上不分解的物质，当与800-1600℃的温度范围内的还原气体接触时会分解产生挥发物，例如蓝宝石; 通过在800-1600℃的温度范围内，在含有氨气体的还原性气体气氛中对叠层基板进行热处理，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 ; 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，并且其晶面显示出大的曲率半径。

公开(公告)号：EP3434816A1

公开(公告)日：2019-01-30

申请号：EP17770273.5

申请日：2017-03-22

申请人： Tokuyama Corporation

发明人： NAGASHIMA, Toru ,  OKAYAMA, Reiko ,  FUKUDA, Masayuki ,  YANAGI, Hiroyuki

IPC分类号： C30B29/38 ,  C23C16/01 ,  C23C16/34 ,  C30B25/20 ,  H01L21/205

摘要： A method for producing an aluminum nitride single crystal substrate, the method including: i) preparing a first base substrate consisting of a first aluminum nitride single crystal; ii) growing a first aluminum nitride single crystal layer having a thickness of no less than 500 µm over a main face of the first base substrate, to obtain a layered body; iii) cutting the first aluminum nitride single crystal layer of the layered body, to separate the layered body into a second base substrate and a first part of the first aluminum nitride single crystal layer, the second base substrate including the first base substrate and a thin film layered thereon, the thin film being a second part of the first aluminum nitride single crystal layer; iv) polishing a surface of the thin film in the second base substrate, to obtain a third base substrate consisting of a second aluminum nitride single crystal; and v) growing a second aluminum nitride single crystal layer over the polished surface of the third base substrate.

公开(公告)号：EP3219833A1

公开(公告)日：2017-09-20

申请号：EP15858289.0

申请日：2015-11-09

申请人： Tokuyama Corporation

发明人： NAGASHIMA, Toru ,  FUKUDA, Masayuki

IPC分类号： C30B29/38 ,  C23C16/34 ,  C23C16/455 ,  C30B25/14 ,  H01L21/205

CPC分类号： H01L21/02389 ,  C23C16/34 ,  C23C16/455 ,  C30B25/14 ,  C30B29/403 ,  H01L21/0254 ,  H01L21/02609 ,  H01L21/0262 ,  H01L21/205

摘要： An apparatus for manufacturing a group III nitride single crystal including: a reaction vessel including a reaction area, wherein in the reaction area, a group III source gas and a nitrogen source gas are reacted such that a group III nitride crystal is grown on a substrate; a susceptor arranged in the reaction area and supporting the substrate; a group III source gas supply nozzle supplying the group III source gas to the reaction area; and a nitrogen source gas supply nozzle supplying the nitrogen source gas to the reaction area, wherein the nitrogen source gas supply nozzle is configured to supply the nitrogen source gas and at least one halogen-based gas selected from the group consisting of a hydrogen halide gas and a halogen gas to the reaction area.

摘要翻译： 一种用于制造III族氮化物单晶的设备，包括：包括反应区域的反应容器，其中在反应区域中，使III族源气体和氮源气体反应，使得III族氮化物晶体在衬底上生长 ; 布置在反应区域中并支撑基板的基座; 向所述反应区域供给所述III族原料气体的III族原料气体供给喷嘴; 以及氮源气体供应喷嘴，其将所述氮源气体供应到所述反应区域，其中所述氮源气体供应喷嘴被构造成供应所述氮源气体和至少一种选自卤化氢气体 并将卤素气体引入反应区域。

公开(公告)号：EP3010035A1

公开(公告)日：2016-04-20

申请号：EP14810294.0

申请日：2014-06-10

申请人： Tokuyama Corporation

发明人： KOUKITSU, Akinori ,  KUMAGAI, Yoshinao ,  NAGASHIMA, Toru ,  OKAYAMA, Reiko

IPC分类号： H01L21/205 ,  C23C16/34 ,  C30B25/16 ,  C30B29/38

CPC分类号： C30B25/14 ,  C30B25/165 ,  C30B29/403 ,  H01L21/02422 ,  H01L21/0254 ,  H01L21/0262

摘要： Provided is a method for manufacturing an aluminum-based group III nitride single crystal which can reduce the effect of aluminum monohalide gas in an aluminum halide raw material gas with an easy way, and increase the crystal quality.
The method for manufacturing an aluminum-based group III nitride single crystal includes the step of supplying an aluminum halide gas and a nitrogen source gas onto a base substrate, such that a reaction of the aluminum halide gas and the nitrogen source gas is conducted on the base substrate, wherein the reaction of the aluminum halide gas and the nitrogen source gas is conducted under coexistence of a halogen-based gas such that a halogen-based gas ratio (H) represented by the following formula (1) is no less than 0.1 and less than 1.0: H = V H / V H + V Al (In the formula (1), V H represents a supply of the halogen-based gas; and V Al represents a supply of the aluminum halide gas); and a growth rate of the aluminum-based group III nitride single crystal is no less than 10 µm/h.

摘要翻译： 提供一种制造铝基III族氮化物单晶的方法，其可以以简单的方式降低卤化铝原料气中的一卤化铝的影响，并提高晶体质量。 铝系III族氮化物单晶的制造方法包括将铝卤化物气体和氮源气体供给到基底基板上，使得卤化铝气体与氮源气体的反应在 碱卤化物气体和氮源气体的反应在卤素系气体共存下进行，使得下述式（1）所示的卤素系气体比（H）为0.1以上 小于1.0：H = VH / VH + V A1（式（1）中，VH表示卤素系气体的供给量，V A1表示卤化铝气体的供给量）。 铝基III族氮化物单晶的生长速度不小于10μm/ h。

公开(公告)号：EP2607527A1

公开(公告)日：2013-06-26

申请号：EP11848944.2

申请日：2011-12-15

申请人： Tokuyama Corporation

发明人： NAGASHIMA, Toru ,  HIRONAKA, Keiichiro

IPC分类号： C30B29/38 ,  C01F7/58 ,  C01F7/62 ,  C30B25/14 ,  H01L21/205

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

摘要： A process for producing an aluminum-containing III nitride single crystal, comprising: a reaction step of bringing a halogen gas and aluminum into contact with each other at a temperature of 300 to 700°C inclusive, thereby producing a mixed gas comprising a gas of an aluminum trihalide and a gas of an aluminum monohalide; a conversion step of setting the temperature of the mixed gas at a temperature that is equal to or higher than a temperature at which a solid of the aluminum trihalide is precipitated and that is lower by 50°C or more than a temperature at which the halogen gas and aluminum have been reacted with each other in the reaction step, thereby converting the aluminum monohalide in the mixed gas into a solid substance; a separation step of separating the solid substance from the gas, thereby removing the gas of the aluminum trihalide; and a crystal growth step of using the gas of the aluminum trihalide as an aluminum nitride single crystal raw material without lowering the temperature and while keeping the temperature at a temperature that is equal to or higher than the temperature employed in the conversion step.

公开(公告)号：EP2123801A1

公开(公告)日：2009-11-25

申请号：EP07792325.8

申请日：2007-08-03

申请人： Tokuyama Corporation

发明人： NAGASHIMA, Toru ,  TAKADA, Kazuya ,  YANAGI, Hiroyuki ,  HARADA, Manabu ,  HIRATA, Yasunori ,  KONDO, Keisuke

IPC分类号： C30B29/38 ,  C23C16/34 ,  C23C16/455 ,  C30B25/14 ,  H01L21/205

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族氮化物的方法，例如氮化铝，其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 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生长III族氮化物如铝基III族氮化物，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。