公开(公告)号：US09263258B2

公开(公告)日：2016-02-16

申请号：US12320642

申请日：2009-01-30

申请人： Seiji Nagai ,  Shiro Yamazaki ,  Takayuki Sato ,  Yasuhide Yakushi ,  Koji Okuno ,  Koichi Goshonoo

发明人： Seiji Nagai ,  Shiro Yamazaki ,  Takayuki Sato ,  Yasuhide Yakushi ,  Koji Okuno ,  Koichi Goshonoo

IPC分类号： C30B25/04 ,  B32B19/04 ,  H01L21/02 ,  C30B25/18 ,  C30B29/40

CPC分类号： H01L21/0254 ,  C30B25/18 ,  C30B29/403 ,  C30B29/406 ,  H01L21/0242 ,  H01L21/02433 ,  H01L21/02458 ,  H01L21/02609 ,  H01L21/02639

摘要： Provided is a method for producing a Group III nitride-based compound semiconductor having an M-plane main surface. The method employs a sapphire substrate having a main surface which is inclined by 30° with respect to R-plane about a line of intersection Lsapph-AM formed by R-plane and A-plane perpendicular thereto. R-plane surfaces of the sapphire substrate are exposed, and a silicon dioxide mask is formed on the main surface of the substrate. AlN buffer layers are formed on the exposed R-plane surfaces. A GaN layer is formed on the AlN buffer layers. At an initial stage of GaN growth, the top surface of the sapphire substrate is entirely covered with the GaN layer through lateral growth. The GaN layer is grown so that the a-axis of the layer is perpendicular to the exposed R-plane surfaces of the sapphire substrate; the c-axis of the layer is parallel to the axis direction Lsapph-AM of the sapphire substrate; and the m-axis of the layer, which is inclined by 30° from the a-axis thereof, is perpendicular to the main surface (inclined by 30° from the exposed R-plane surfaces) of the sapphire substrate.

摘要翻译： 提供一种具有M面主面的III族氮化物系化合物半导体的制造方法。 该方法采用蓝色蓝宝石衬底，该蓝宝石衬底具有主表面，其相对于R平面围绕由R平面和与其垂直的A平面形成的交线Lsapph-AM倾斜30°。 暴露蓝宝石衬底的R平面表面，并且在衬底的主表面上形成二氧化硅掩模。 AlN缓冲层形成在暴露的R平面上。 在AlN缓冲层上形成GaN层。 在GaN生长的初始阶段，蓝宝石衬底的顶表面通过横向生长完全被GaN层覆盖。 生长GaN层使得该层的a轴垂直于蓝宝石衬底的暴露的R平面表面; 层的c轴平行于蓝宝石衬底的轴方向Lsapph-AM; 并且从其a轴倾斜30°的层的m轴垂直于蓝宝石衬底的主表面（从露出的R平面倾斜30°）。

公开(公告)号：US08507364B2

公开(公告)日：2013-08-13

申请号：US12453743

申请日：2009-05-20

申请人： Seiji Nagai ,  Shiro Yamazaki ,  Yasuhide Yakushi ,  Takayuki Sato ,  Makoto Iwai ,  Katsuhiro Imai ,  Yusuke Mori ,  Yasuo Kitaoka

发明人： Seiji Nagai ,  Shiro Yamazaki ,  Yasuhide Yakushi ,  Takayuki Sato ,  Makoto Iwai ,  Katsuhiro Imai ,  Yusuke Mori ,  Yasuo Kitaoka

IPC分类号： H01L21/20

CPC分类号： C30B9/12 ,  C30B9/10 ,  C30B29/403

摘要： An object of the present invention is to realize, by the flux process, the production of a high-quality n-type semiconductor crystal having high concentration of electrons. The method of the invention for producing an n-type Group III nitride-based compound semiconductor by the flux process, the method including preparing a melt by melting at least a Group III element by use of a flux; supplying a nitrogen-containing gas to the melt; and growing an n-type Group III nitride-based compound semiconductor crystal on a seed crystal from the melt. In the method, carbon and germanium are dissolved in the melt, and germanium is incorporated as a donor into the semiconductor crystal, to thereby produce an n-type semiconductor crystal.The mole percentage of germanium to gallium in the melt is 0.05 mol % to 0.5 mol %, and the mole percentage of carbon to sodium is 0.1 mol % to 3.0 mol %.

公开(公告)号：US20090294909A1

公开(公告)日：2009-12-03

申请号：US12453743

申请日：2009-05-20

申请人： Seiji Nagai ,  Shiro Yamazaki ,  Yasuhide Yakushi ,  Takayuki Sato ,  Makoto Iwai ,  Katsuhiro Imai ,  Yusuke Mori ,  Yasuo Kitaoka

发明人： Seiji Nagai ,  Shiro Yamazaki ,  Yasuhide Yakushi ,  Takayuki Sato ,  Makoto Iwai ,  Katsuhiro Imai ,  Yusuke Mori ,  Yasuo Kitaoka

IPC分类号： H01L29/20 ,  H01L21/20

CPC分类号： C30B9/12 ,  C30B9/10 ,  C30B29/403

摘要： An object of the present invention is to realize, by the flux process, the production of a high-quality n-type semiconductor crystal having high concentration of electrons. The method of the invention for producing an n-type Group III nitride-based compound semiconductor by the flux process, the method including preparing a melt by melting at least a Group III element by use of a flux; supplying a nitrogen-containing gas to the melt; and growing an n-type Group III nitride-based compound semiconductor crystal on a seed crystal from the melt. In the method, carbon and germanium are dissolved in the melt, and germanium is incorporated as a donor into the semiconductor crystal, to thereby produce an n-type semiconductor crystal.The mole percentage of germanium to gallium in the melt is 0.05 mol % to 0.5 mol %, and the mole percentage of carbon to sodium is 0.1 mol % to 3.0 mol %.

摘要翻译： 本发明的目的是通过磁通处理来实现具有高浓度电子的高质量n型半导体晶体的生产。 本发明的用于通过助熔剂制造n型III族氮化物基化合物半导体的方法，该方法包括通过使用助熔剂熔化至少III族元素来制备熔体; 向熔体供给含氮气体; 以及从所述熔体在籽晶上生长n型III族氮化物基化合物半导体晶体。 在该方法中，将碳和锗溶解在熔体中，并将​​锗作为供体掺入到半导体晶体中，从而制备n型半导体晶体。 熔体中锗与镓的摩尔比为0.05摩尔％〜0.5摩尔％，碳与钠的摩尔比为0.1摩尔％〜3.0摩尔％。

公开(公告)号：US08361222B2

公开(公告)日：2013-01-29

申请号：US12081943

申请日：2008-04-23

申请人： Shiro Yamazaki ,  Seiji Nagai ,  Takayuki Sato ,  Katsuhiro Imai ,  Makoto Iwai ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Shiro Yamazaki ,  Seiji Nagai ,  Takayuki Sato ,  Katsuhiro Imai ,  Makoto Iwai ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B15/14 ,  C30B15/00 ,  C30B21/06 ,  C30B27/02 ,  C30B28/10 ,  C30B30/04

CPC分类号： C30B29/403 ,  C30B9/00 ,  C30B9/12 ,  C30B29/406

摘要： In the production of GaN through the flux method, deposition of miscellaneous crystals on the nitrogen-face of a GaN self-standing substrate and waste of raw materials are prevented. Four arrangements of crucibles and a GaN self-standing substrate are exemplified. In FIG. 1A, a nitrogen-face of a self-standing substrate comes into close contact with a sloped flat inner wall of a crucible. In FIG. 1B, a nitrogen-face of a self-standing substrate comes into close contact with a horizontally facing flat inner wall of a crucible, and the substrate is fixed by means of a jig. In FIG. 1C, a jig is provided on a flat bottom of a crucible, and two GaN self-standing substrates are fixed by means of the jig so that the nitrogen-faces of the substrates come into close contact with each other. In FIG. 1D, a jig is provided on a flat bottom of a crucible, and a GaN self-standing substrate is fixed on the jig so that the nitrogen-face of the substrate is covered with the jig. A flux mixture of molten gallium and sodium is charged into each crucible, and a GaN single crystal is grown on a gallium-face under pressurized nitrogen.

摘要翻译： 在通过助熔剂制造GaN的情况下，可以防止在GaN自立基板的氮面上沉积杂晶，原料的浪费。 例示了四个坩埚和GaN自立衬底的布置。 在图 如图1A所示，自立基板的氮面与坩埚的倾斜的平坦的内壁紧密接触。 在图 如图1B所示，自立基板的氮面与坩埚的水平方向的平坦的内壁紧密接触，通过夹具固定基板。 在图 如图1C所示，在坩埚的平坦底部设置夹具，通过夹具固定两个GaN自立基板，使得基板的氮面彼此紧密接触。 在图 如图1D所示，在坩埚的平坦底部设置夹具，并且将GaN自立基板固定在夹具上，使得基板的氮面被夹具覆盖。 将熔融的镓和钠的助熔剂混合物装入每个坩埚中，并且在加压氮气下在镓面上生长GaN单晶。

公开(公告)号：US20080223288A1

公开(公告)日：2008-09-18

申请号：US12073904

申请日：2008-03-11

申请人： Shiro Yamazaki ,  Koji Hirata ,  Takayuki Sato ,  Seiji Nagai ,  Katsuhiro Imai ,  Makoto Iwai ,  Shuhei Higashihara ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Shiro Yamazaki ,  Koji Hirata ,  Takayuki Sato ,  Seiji Nagai ,  Katsuhiro Imai ,  Makoto Iwai ,  Shuhei Higashihara ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B9/12

CPC分类号： C30B29/403 ,  C30B9/00 ,  C30B9/06 ,  Y10S117/90 ,  Y10T117/10 ,  Y10T117/1024

摘要： An object of the invention is to carry out the flux method with improved work efficiency while maintaining the purity of flux at high level and saving flux material cost. The sodium-purifying apparatus includes a sodium-holding-and-management apparatus for maintaining purified sodium (Na) in a liquid state. Liquid sodium is supplied into a sodium-holding-and-management apparatus through a liquid-sodium supply piping maintained at 100° C. to 200° C. The sodium-holding-and-management apparatus further has an argon-gas-purifying apparatus for controlling the condition of argon (Ar) gas that fills the internal space thereof. Thus, by opening and closing a faucet at desired timing, purified liquid sodium (Na) supplied from the sodium-purifying apparatus can be introduced into a crucible as appropriate via the liquid-sodium supply piping, the sodium-holding-and-management apparatus, and the piping.

摘要翻译： 本发明的目的是在保持高水平的助焊剂纯度的同时，实现提高工作效率的助焊剂方法，节约焊剂材料成本。 钠纯化装置包括用于保持液态的纯化钠（Na）的钠保持和管理装置。 液态钠通过保持在100℃至200℃的液态钠供应管道供应到保钠管理装置中。钠保持和管理装置还具有氩气净化装置 用于控制填充其内部空间的氩（Ar）气体的状态。 因此，通过在期望的时间打开和关闭水龙头，可以通过液体钠供应管道，钠保持管理装置适当地将从钠纯化装置供应的纯化液体钠（Na） ，和管道。

公开(公告)号：US08216365B2

公开(公告)日：2012-07-10

申请号：US12073178

申请日：2008-02-29

申请人： Seiji Nagai ,  Shiro Yamazaki ,  Takayuki Sato ,  Katsuhiro Imai ,  Makoto Iwai ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Seiji Nagai ,  Shiro Yamazaki ,  Takayuki Sato ,  Katsuhiro Imai ,  Makoto Iwai ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B25/18

CPC分类号： C30B29/403 ,  C30B9/00 ,  C30B9/10

摘要： Objects of the invention are to further enhance crystallinity and crystallinity uniformity of a semiconductor crystal produced through the flux method, and to effectively enhance the production yield of the semiconductor crystal. The c-axis of a seed crystal including a GaN single-crystal layer is aligned in a horizontal direction (y-axis direction), one a-axis of the seed crystal is aligned in the vertical direction, and one m-axis is aligned in the x-axis direction. Thus, three contact points at which a supporting tool contacts the seed crystal are present on m-plane. The supporting tool has two supporting members, which extend in the vertical direction. One supporting member has an end part, which is inclined at 30° with respect to the horizontal plane α. The reasons for supporting a seed crystal at m-plane thereof are that m-plane exhibits a crystal growth rate, which is lower than that of a-plane, and that desired crystal growth on c-plane is not inhibited. Actually, a plurality of seed crystals and supporting tools are periodically placed along the y-axis direction.

摘要翻译： 本发明的目的是进一步提高通过助焊剂法生产的半导体晶体的结晶度和结晶度均匀性，并有效提高半导体晶体的制造成品率。 包括GaN单晶层的晶种的c轴在水平方向（y轴方向）上排列，晶种的一个a轴在垂直方向上排列，并且一个m轴对齐 在x轴方向。 因此，在m平面上存在支撑工具与晶种接触的三个接触点。 支撑工具具有在垂直方向上延伸的两个支撑构件。 一个支撑构件具有相对于水平面α倾斜30°的端部。 在m面支撑晶种的原因在于，m面的晶体生长速度低于a面的晶体生长速度，c面上的期望的晶体生长没有被抑制。 实际上，沿着y轴方向周期性地放置多个晶种和支撑工具。

公开(公告)号：US07708833B2

公开(公告)日：2010-05-04

申请号：US12073904

申请日：2008-03-11

申请人： Shiro Yamazaki ,  Koji Hirata ,  Takayuki Sato ,  Seiji Nagai ,  Katsuhiro Imai ,  Makoto Iwai ,  Shuhei Higashihara ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Shiro Yamazaki ,  Koji Hirata ,  Takayuki Sato ,  Seiji Nagai ,  Katsuhiro Imai ,  Makoto Iwai ,  Shuhei Higashihara ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B35/00

CPC分类号： C30B29/403 ,  C30B9/00 ,  C30B9/06 ,  Y10S117/90 ,  Y10T117/10 ,  Y10T117/1024

摘要： An object of the invention is to carry out the flux method with improved work efficiency while maintaining the purity of flux at high level and saving flux material cost. The sodium-purifying apparatus includes a sodium-holding-and-management apparatus for maintaining purified sodium (Na) in a liquid state. Liquid sodium is supplied into a sodium-holding-and-management apparatus through a liquid-sodium supply piping maintained at 100° C. to 200° C. The sodium-holding-and-management apparatus further has an argon-gas-purifying apparatus for controlling the condition of argon (Ar) gas that fills the internal space thereof. Thus, by opening and closing a faucet at desired timing, purified liquid sodium (Na) supplied from the sodium-purifying apparatus can be introduced into a crucible as appropriate via the liquid-sodium supply piping, the sodium-holding-and-management apparatus, and the piping.

摘要翻译： 本发明的目的是在保持高水平的助焊剂纯度的同时，实现提高工作效率的助焊剂方法，节约焊剂材料成本。 钠纯化装置包括用于保持液态的纯化钠（Na）的钠保持和管理装置。 液态钠通过保持在100℃至200℃的液态钠供应管道供应到保钠管理装置中。钠保持和管理装置还具有氩气净化装置 用于控制填充其内部空间的氩（Ar）气体的状态。 因此，通过在期望的时间打开和关闭水龙头，可以通过液体钠供应管道，钠保持管理装置适当地将从钠纯化装置供应的纯化液体钠（Na） ，和管道。

公开(公告)号：US20080223286A1

公开(公告)日：2008-09-18

申请号：US12073178

申请日：2008-02-29

申请人： Seiji Nagai ,  Shiro Yamazaki ,  Takayuki Sato ,  Katsuhiro Imai ,  Makoto Iwai ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

发明人： Seiji Nagai ,  Shiro Yamazaki ,  Takayuki Sato ,  Katsuhiro Imai ,  Makoto Iwai ,  Takatomo Sasaki ,  Yusuke Mori ,  Fumio Kawamura

IPC分类号： C30B23/00

CPC分类号： C30B29/403 ,  C30B9/00 ,  C30B9/10

摘要： Objects of the invention are to further enhance crystallinity and crystallinity uniformity of a semiconductor crystal produced through the flux method, and to effectively enhance the production yield of the semiconductor crystal. The c-axis of a seed crystal including a GaN single-crystal layer is aligned in a horizontal direction (y-axis direction), one a-axis of the seed crystal is aligned in the vertical direction, and one m-axis is aligned in the x-axis direction. Thus, three contact points at which a supporting tool contacts the seed crystal are present on m-plane. The supporting tool has two supporting members, which extend in the vertical direction. One supporting member has an end part, which is inclined at 30° with respect to the horizontal plane α. The reasons for supporting a seed crystal at m-plane thereof are that m-plane exhibits a crystal growth rate, which is lower than that of a-plane, and that desired crystal growth on c-plane is not inhibited. Actually, a plurality of seed crystals and supporting tools are periodically placed along the y-axis direction.

摘要翻译： 本发明的目的是进一步提高通过助焊剂法生产的半导体晶体的结晶度和结晶度均匀性，并有效提高半导体晶体的制造成品率。 包括GaN单晶层的晶种的c轴在水平方向（y轴方向）上排列，晶种的一个a轴在垂直方向上排列，并且一个m轴对齐 在x轴方向。 因此，在m平面上存在支撑工具与晶种接触的三个接触点。 支撑工具具有在垂直方向上延伸的两个支撑构件。 一个支撑构件具有相对于水平面α倾斜30°的端部。 在m面支撑晶种的原因在于，m面的晶体生长速度低于a面的晶体生长速度，c面上的期望的晶体生长没有被抑制。 实际上，沿着y轴方向周期性地放置多个晶种和支撑工具。

公开(公告)号：US08501141B2

公开(公告)日：2013-08-06

申请号：US12662006

申请日：2010-03-26

申请人： Takayuki Sato ,  Seiji Nagai ,  Makoto Iwai ,  Shuhei Higashihara ,  Yusuke Mori ,  Yasuo Kitaoka

发明人： Takayuki Sato ,  Seiji Nagai ,  Makoto Iwai ,  Shuhei Higashihara ,  Yusuke Mori ,  Yasuo Kitaoka

IPC分类号： C01B21/06 ,  C30B15/00 ,  C30B9/00 ,  C30B19/00 ,  C30B11/00 ,  C30B25/00 ,  C30B28/14 ,  H01L21/00 ,  H01L33/00 ,  H01L21/02 ,  H01B1/02 ,  H01B1/04

CPC分类号： C30B9/12 ,  C30B29/403 ,  C30B29/406 ,  H01L21/02389 ,  H01L21/0254 ,  H01L21/02576 ,  H01L21/02579 ,  H01L21/02625

摘要： An object of the present invention is to effectively add Ge in the production of GaN through the Na flux method. In a crucible, a seed crystal substrate is placed such that one end of the substrate remains on the support base, whereby the seed crystal substrate remains tilted with respect to the bottom surface of the crucible, and gallium solid and germanium solid are placed in the space between the seed crystal substrate and the bottom surface of the crucible. Then, sodium solid is placed on the seed crystal substrate. Through employment of this arrangement, when a GaN crystal is grown on the seed crystal substrate through the Na flux method, germanium is dissolved in molten gallium before formation of a sodium-germanium alloy. Thus, the GaN crystal can be effectively doped with Ge.

摘要翻译： 本发明的目的是通过Na通量法有效地添加Ge生产GaN。 在坩埚中，放置晶种衬底，使得衬底的一端保留在支撑基底上，由此籽晶衬底相对于坩埚的底表面保持倾斜，并且将镓固体和锗固体放置在 晶种基板与坩埚底面之间的空间。 然后，将钠固体置于晶种衬底上。 通过使用这种布置，当GaN晶体通过Na通量法在籽晶衬底上生长时，锗在形成钠 - 锗合金之前溶解在熔融镓中。 因此，GaN晶体可以有效地掺杂Ge。

公开(公告)号：US20110259261A1

公开(公告)日：2011-10-27

申请号：US13177057

申请日：2011-07-06

申请人： Makoto IWAI ,  Shuhei Higashihara ,  Yasuo Kitaoka ,  Yusuke Mori ,  Takayuki Sato ,  Seiji Nagai

发明人： Makoto IWAI ,  Shuhei Higashihara ,  Yasuo Kitaoka ,  Yusuke Mori ,  Takayuki Sato ,  Seiji Nagai

IPC分类号： C30B9/06 ,  C30B25/00

CPC分类号： C30B29/403 ,  C30B19/02 ,  C30B19/06 ,  C30B29/406 ,  C30B35/002

摘要： It is provided a method of growing a single crystal by flux process from a melt containing sodium, in that a flux is contained in a reaction vessel made of yttrium-aluminum garnet. Compared with the case that an alumina or yttria vessel is used, it can be successfully obtained a single crystal whose incorporation amounts of oxygen and silicon can be considerably reduced, residual carrier density can be lowered, and electron mobility and specific resistance can be improved.

摘要翻译： 本发明提供一种通过助熔剂从包含钠的熔体中生长单晶的方法，其特征在于，在由钇 - 铝石榴石制成的反应容器中含有助熔剂。 与使用氧化铝或氧化钇容器的情况相比，可以成功地获得能够显着降低氧和硅的掺入量的单晶，可以降低残留载流子密度，并且可以提高电子迁移率和电阻率。