公开(公告)号：US09777405B2

公开(公告)日：2017-10-03

申请号：US14674567

申请日：2015-03-31

Applicant: The Florida State University Research Foundation, Inc.

Inventor： Jeffrey Whalen ,  Theo Siegrist

IPC: C30B29/46 ,  H01B1/10 ,  C30B9/10 ,  H01B1/08 ,  C30B9/12 ,  C30B29/22

CPC classification number: C30B29/46 ,  C30B9/10 ,  C30B9/12 ,  C30B29/22 ,  H01B1/08 ,  H01B1/10

Abstract: Single crystals of the new semiconducting oxychalcogenide phase were synthesized using a novel crystal growth method. The crystals had low defects and homogeneous composition as characterized by single crystal X-ray diffraction and scanning electron microscopy, respectively. Heat capacity and resistivity measurements were in agreement with the calculated band structure calculations indicating semiconductivity, with a band gap of about 3 eV.

公开(公告)号：US09768352B2

公开(公告)日：2017-09-19

申请号：US15359813

申请日：2016-11-23

Applicant: NGK INSULATORS, LTD.

Inventor： Morimichi Watanabe ,  Jun Yoshikawa ,  Yoshitaka Kuraoka ,  Tsutomu Nanataki

IPC: H01L33/18 ,  H01L33/00 ,  H01L33/06 ,  H01L33/32 ,  C30B9/12 ,  C30B19/02 ,  C30B19/12 ,  C30B25/18 ,  C30B28/04 ,  C30B29/40 ,  C30B29/60 ,  H01L33/16 ,  C30B9/00 ,  C30B25/20

CPC classification number: H01L33/18 ,  C30B9/00 ,  C30B9/12 ,  C30B19/02 ,  C30B19/12 ,  C30B25/18 ,  C30B25/20 ,  C30B28/04 ,  C30B29/406 ,  C30B29/605 ,  H01L33/0025 ,  H01L33/0075 ,  H01L33/06 ,  H01L33/16 ,  H01L33/32

Abstract: Provided is a self-supporting polycrystalline GaN substrate composed of GaN-based single crystal grains having a specific crystal orientation in a direction approximately normal to the substrate. The crystal orientations of individual GaN-based single crystal grains as determined from inverse pole figure mapping by EBSD analysis on the substrate surface are distributed with tilt angles from the specific crystal orientation, the average tilt angle being 1 to 10°. There is also provided a light emitting device including the self-supporting substrate and a light emitting functional layer, which has at least one layer composed of semiconductor single crystal grains, the at least one layer having a single crystal structure in the direction approximately normal to the substrate. The present invention makes it possible to provide a self-supporting polycrystalline GaN substrate having a reduced defect density at the substrate surface, and to provide a light emitting device having a high luminous efficiency.

公开(公告)号：US09677192B2

公开(公告)日：2017-06-13

申请号：US13135829

申请日：2011-07-15

Applicant: Takanao Shimodaira ,  Katsuhiro Imai ,  Makoto Iwai ,  Takayuki Hirao

Inventor： Takanao Shimodaira ,  Katsuhiro Imai ,  Makoto Iwai ,  Takayuki Hirao

IPC: C30B9/12 ,  C30B29/40

CPC classification number: C30B9/12 ,  C30B29/403 ,  C30B29/406

Abstract: A group 13 nitride crystal substrate according to the present invention is produced by growing a group 13 nitride crystal on a seed-crystal substrate by a flux method, wherein a content of inclusions in the group 13 nitride crystal grown in a region of the seed-crystal substrate except for a circumferential portion of the seed-crystal substrate, the region having an area fraction of 70% relative to an entire area of the seed-crystal substrate, is 10% or less, preferably 2% or less.

公开(公告)号：US20170067183A1

公开(公告)日：2017-03-09

申请号：US15122687

申请日：2015-03-12

Applicant: NIPPON STEEL & SUMITOMO METAL CORPORATION

Inventor： Kazuaki SEKI ,  Kazuhiko KUSUNOKI ,  Kazuhito KAMEI

IPC: C30B29/36 ,  C30B19/12 ,  C23C16/32 ,  C30B23/02 ,  C30B25/20 ,  C23C14/06 ,  C30B19/04 ,  C30B19/06

CPC classification number: C30B29/36 ,  C23C14/0635 ,  C23C16/325 ,  C30B9/12 ,  C30B19/04 ,  C30B19/062 ,  C30B19/12 ,  C30B23/025 ,  C30B25/20

Abstract: A method of manufacturing an SiC single crystal includes the steps of melting a raw material in a crucible (14) to produce an SIC solution (15); and bringing a crystal growth surface (24A) of an SiC seed crystal (24) into contact with the SiC solution to cause an SiC single crystal to grow on the crystal growth surface. The crystal structure of the SiC seed crystal is the 4H polytype. The off-angle of the crystal growth surface is not smaller than 1° and not larger than 4°. The temperature of the SIC solution during growth of the SiC single crystal is not lower than 1650° C. and not higher than 1850° C. The temperature gradient in a portion of the SiC solution directly below the SiC seed crystal during growth of the SiC single crystal is higher than 0° C./cm and not higher than 19° C./cm.

Abstract translation: 制造SiC单晶的方法包括以下步骤：在坩埚（14）中熔化原料以产生SIC溶液（15）; 并使SiC晶种（24）的晶体生长面（24A）与SiC溶液接触，使SiC单晶在晶体生长面上生长。 SiC晶种的晶体结构是4H多型。 晶体生长面的偏角不小于1°而不大于4°。 SiC单晶生长期间SIC溶液的温度不低于1650℃且不高于1850℃。在SiC生长过程中SiC晶种正下方的一部分SiC溶液中的温度梯度 单晶高于0℃/ cm且不高于19℃/ cm。

公开(公告)号：US20170058425A1

公开(公告)日：2017-03-02

申请号：US15239584

申请日：2016-08-17

Applicant: TOYODA GOSEI CO., LTD.

Inventor： Miki MORIYAMA

IPC: C30B9/12 ,  H01L21/66 ,  C30B29/40 ,  H01L21/02

CPC classification number: C30B9/12 ,  C30B29/406 ,  H01L21/0242 ,  H01L21/02458 ,  H01L21/0254 ,  H01L22/20

Abstract: The present techniques provide a method for producing a Group III nitride semiconductor single crystal that is designed to grow a semiconductor single crystal with high reproducibility. The method for producing a Group III nitride semiconductor single crystal comprises adding a seed crystal substrate, Ga, and Na into a crucible, and growing a Group III nitride semiconductor single crystal. In the growth of the Group III nitride semiconductor single crystal, a measuring device is used to detect the reaction of Ga with Na. Ga is reacted with Na with the temperature of the crucible adjusted within a first temperature range of 80° C. to 200° C. After the measuring device detected the reaction of Ga with Na, the temperature of the crucible is elevated up to a growth temperature of the Group III nitride semiconductor single crystal.

Abstract translation: 本技术提供了一种用于生产以高再现性生长半导体单晶的III族氮化物半导体单晶的方法。 制造III族氮化物半导体单晶的方法包括将晶种衬底Ga和Na加入到坩埚中，并且生长III族氮化物半导体单晶。 在III族氮化物半导体单晶的生长中，使用测量装置来检测Ga与Na的反应。 Ga与Na反应，坩埚的温度在80℃至200℃的第一温度范围内调节。测量装置检测到Ga与Na的反应后，将坩埚的温度升高至升高 III族氮化物半导体单晶的温度。

公开(公告)号：US09404196B2

公开(公告)日：2016-08-02

申请号：US13592555

申请日：2012-08-23

Applicant: Masahiro Hayashi ,  Seiji Sarayama ,  Takashi Satoh ,  Hiroshi Nambu ,  Chiharu Kimura ,  Naoya Miyoshi

Inventor： Masahiro Hayashi ,  Seiji Sarayama ,  Takashi Satoh ,  Hiroshi Nambu ,  Chiharu Kimura ,  Naoya Miyoshi

IPC: C30B9/10 ,  C30B9/12 ,  C30B29/40

CPC classification number: C30B9/12 ,  C30B9/10 ,  C30B29/406

Abstract: A method of manufacturing a group 13 nitride crystal includes a crystal growth process to form the group 13 nitride crystal by growing the group 13 nitride crystal having a hexagonal crystal structure from a seed crystal which is a gallium nitride crystal having a hexagonal crystal structure in which a length “L” in a c-axis direction is 9.7 mm or more, and a ratio L/d of the length “L” to a crystal diameter “d” in a c-plane is larger than 0.813. The crystal growth process includes a process of forming an outer periphery containing a {10-10} plane and an outer periphery containing a {10-11} plane at side surfaces of the group 13 nitride crystal, and forming an outer periphery containing a {0001} plane at a bottom surface of the group 13 nitride crystal.

Abstract translation: 制造13族氮化物晶体的方法包括通过从具有六方晶系结构的氮化镓晶体的晶种生长具有六方晶系结构的13族氮化物晶体来形成氮化镓族晶体的晶体生长工艺，其中 c轴方向的长度“L”为9.7mm以上，c面中的长度“L”与晶体直径“d”的比率L / d大于0.813。 晶体生长工艺包括在第13族氮化物晶体的侧面形成包含{10-10}面和包含{10-11}面的外周的外周的工艺，并且形成含有{ 0001}面。

公开(公告)号：US09299555B1

公开(公告)日：2016-03-29

申请号：US14033107

申请日：2013-09-20

Applicant: SORAA, INC.

Inventor： Alex Alexander ,  John W. Nink, Jr. ,  Mark P. D'Evelyn

IPC: C30B9/12 ,  H01L21/02 ,  C30B7/10 ,  C30B9/04 ,  C30B9/08 ,  C30B29/38

CPC classification number: C30B29/38 ,  C30B7/105 ,  C30B9/04 ,  C30B9/08 ,  C30B9/12 ,  C30B29/403

Abstract: An ultrapure mineralizer is formed by vaporization, condensation, and delivery of a condensable mineralizer composition. The mineralizer has an oxygen content below 100 parts per million. The ultrapure mineralizer is useful as a raw material for ammonothermal growth of bulk group III metal nitride crystals.

Abstract translation: 通过蒸发，冷凝和递送可冷凝矿化剂组合物形成超纯矿化剂。 矿化剂的氧含量低于100ppm。 超纯矿化剂可用作本体III族金属氮化物晶体的氨热生长原料。

公开(公告)号：US20150144956A1

公开(公告)日：2015-05-28

申请号：US14499688

申请日：2014-09-29

Applicant: NGK INSULATORS, LTD.

Inventor： Morimichi WATANABE ,  Jun YOSHIKAWA ,  Tsutomu NANATAKI ,  Katsuhiro IMAI ,  Tomohiko SUGIYAMA ,  Takashi YOSHINO ,  Yukihisa TAKEUCHI ,  Kei SATO

IPC: H01L33/32 ,  H01L33/00 ,  C30B29/40 ,  C30B19/02 ,  C30B19/12 ,  H01L33/16 ,  C30B9/12

CPC classification number: H01L33/18 ,  C30B9/00 ,  C30B9/12 ,  C30B19/02 ,  C30B19/12 ,  C30B25/18 ,  C30B25/20 ,  C30B28/04 ,  C30B29/406 ,  C30B29/605 ,  H01L33/0025 ,  H01L33/0075 ,  H01L33/06 ,  H01L33/16 ,  H01L33/32

Abstract: Provided is a self-supporting gallium nitride substrate useful as an alternative material for a gallium nitride single crystal substrate, which is inexpensive and also suitable for having a large area. This substrate is composed of a plate composed of gallium nitride-based single crystal grains, wherein the plate has a single crystal structure in the approximately normal direction. This substrate can be manufactured by a method comprising providing an oriented polycrystalline sintered body; forming a seed crystal layer composed of gallium nitride on the sintered body so that the seed crystal layer has crystal orientation mostly in conformity with the crystal orientation of the sintered body; forming a layer with a thickness of 20 μm or greater composed of gallium nitride-based crystals on the seed crystal layer so that the layer has crystal orientation mostly in conformity with crystal orientation of the seed crystal layer; and removing the sintered body.

Abstract translation: 提供了可用作氮化镓单晶衬底的替代材料的自支撑氮化镓衬底，其价格便宜并且也适合于具有大的面积。 该基板由氮化镓系单晶粒构成的板构成，其中，在大致正方向上具有单晶结构。 该基板可以通过包括提供取向多晶烧结体的方法制造; 在所述烧结体上形成由氮化镓构成的籽晶层，使得所述晶种层的结晶取向主要与所述烧结体的晶体取向一致; 在晶种层上形成由氮化镓系晶体构成的厚度为20μm以上的层，使得该层的结晶取向主要与晶种层的晶体取向一致; 并除去烧结体。

公开(公告)号：US20150017442A1

公开(公告)日：2015-01-15

申请号：US14497553

申请日：2014-09-26

Applicant: Koito Manufacturing Co., Ltd.

Inventor： Kiminori ENOMOTO ,  Hisayoshi DAICHO ,  Yu SHINOMIYA

IPC: C01B25/455 ,  C30B29/60 ,  C30B29/14 ,  C01B25/32

CPC classification number: C01B25/455 ,  C01B25/32 ,  C01B25/321 ,  C30B7/10 ,  C30B9/12 ,  C30B15/00 ,  C30B29/14 ,  C30B29/607 ,  Y10T428/2975

Abstract: An apatite crystal is a single crystal expressed by a general formula (M2)5(PO4)3X. In this formula, M2 indicates at least one type of element selected from the group consisting of bivalent alkaline-earth metals and Eu, and X indicates at least one type of element or molecule selected from the group consisting of halogen elements and OH. And the single crystal is of a tubular shape. The outer shape of the apatite may be a hexagonal prism. The shape of an opening of a hole formed in the upper surface or lower surface of the hexagonal prism may be a hexagon.

Abstract translation: 磷灰石晶体是由通式（M2）5（PO4）3X表示的单晶。 在该式中，M2表示选自二价碱土金属和Eu中的至少一种元素，X表示选自卤素元素和OH的至少一种元素或分子。 单晶是管状的。 磷灰石的外形可以是六棱柱。 形成在六边形棱镜的上表面或下表面中的孔的形状可以是六边形。

公开(公告)号：US20150008563A1

公开(公告)日：2015-01-08

申请号：US14491962

申请日：2014-09-19

Applicant: Sumitomo Electric Industries, Ltd.

Inventor： Naho Mizuhara ,  Koji Uematsu ,  Michimasa Miyanaga ,  Keisuke Tanizaki ,  Hideaki Nakahata ,  Seiji Nakahata ,  Takuji Okahisa

IPC: H01L29/04 ,  H01L29/20

CPC classification number: H01L29/045 ,  C30B9/12 ,  C30B19/02 ,  C30B23/025 ,  C30B25/18 ,  C30B25/20 ,  C30B29/403 ,  C30B29/406 ,  H01L21/02389 ,  H01L21/02433 ,  H01L21/0254 ,  H01L21/02658 ,  H01L29/2003 ,  H01L29/73 ,  H01L29/772 ,  H01L29/778 ,  H01L29/872 ,  H01L33/16

Abstract: Group-III nitride crystal composites made up of especially processed crystal slices, cut from III-nitride bulk crystal, whose major surfaces are of {1-10±2}, {11-2±2}, {20-2±1} or {22-4±1} orientation, disposed adjoining each other sideways with the major-surface side of each slice facing up, and III-nitride crystal epitaxially present on the major surfaces of the adjoining slices, with the III-nitride crystal containing, as principal impurities, either silicon atoms or oxygen atoms. With x-ray diffraction FWHMs being measured along an axis defined by a direction of the substrate projected onto either of the major surfaces, FWHM peak regions are present at intervals of 3 to 5 mm width. Also, with threading dislocation density being measured along a direction of the III-nitride crystal substrate, threading-dislocation-density peak regions are present at the 3 to 5 mm intervals.

Abstract translation: III-III族氮化物晶体复合材料由III-氮化物块状晶体切割的特别加工的晶片组成，其主表面为{1-10±2}，{11-2±2}，{20-2±1} 或{22-4±1}取向，其中每个切片的主表面侧面朝上地彼此相邻地设置，并且III-氮化物晶体外延地存在于相邻切片的主表面上，其中III族氮化物晶体包含 作为主要杂质，硅原子或氧原子。 利用X射线衍射测定FWHM，沿着投影到任一主表面上的衬底的<0001>方向限定的轴测量，FWHM峰值区域以3至5mm的间隔存在。 此外，沿着III族氮化物晶体衬底的<0001>方向测量穿透位错密度，穿透位错密度峰值区域以3至5mm的间隔存在。