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11. 发明专利

JP2008214126A Method for manufacturing semiconductor crystal 有权
标题翻译：制造半导体晶体的方法
公开(公告)号：JP2008214126A
公开(公告)日：2008-09-18
申请号：JP2007053321
申请日：2007-03-02
申请人： Ngk Insulators Ltd , Osaka Univ , Toyoda Gosei Co Ltd , 国立大学法人大阪大学 , 日本碍子株式会社 , 豊田合成株式会社
发明人： NAGAI SEIJI , YAMAZAKI SHIRO , SATO TOSHIYUKI , IWAI MAKOTO , IMAI KATSUHIRO , MORI YUSUKE , SASAKI TAKATOMO , KAWAMURA SHIRO
IPC分类号： C30B29/38 , C30B9/00 , H01L21/208
CPC分类号： C30B29/403 , C30B9/00 , C30B9/10
摘要： PROBLEM TO BE SOLVED: To improve the crystallinity and uniformity of a semiconductor crystal and increase effectively its yield, in a flux method, so as to become higher than those of conventional methods.
SOLUTION: The c axis of a seed crystal 10 having GaN single crystal layer is oriented to a horizontal direction (y axis direction), one of the a axes of the seed crystal 10 is oriented to a vertical direction and one of the m axes is oriented to an x axis direction. Resultingly, all of the points p1, p2 and p3 on a clamper T contact the m-plane of the seed crystal. The clamper T has clamping members T1 and T2, where both of them extend vertically but the clamping member T1 has an end portion T1a tilted by 30° to the upper surface α of a growth source solution. The reason why the seed crystal is held at the m-plane is that the m-plane has a crystal growth speed slower than that of the a-plane and the desired c-plane growth is not hindered. The seed crystals 10 and the clampers T are plurally arranged periodically to the y-axis direction respectively.
COPYRIGHT: (C)2008,JPO&INPIT
摘要翻译：要解决的问题：为了提高半导体晶体的结晶度和均匀性，并且在助熔剂方法中有效地提高其产率，从而变得高于常规方法。＆lt;解决方案＆gt;具有GaN单晶层的晶种10的c轴取向为水平方向（y轴方向），晶种10的a轴之一取向为垂直方向， m轴取向为x轴方向。因此，夹持器T上的所有点p1，p2和p3接触晶种的m面。夹持器T具有夹紧构件T1和T2，其中它们都垂直延伸，但是夹紧构件T1具有相对于生长源溶液的上表面α倾斜30°的端部T1a。晶种保持在m面的原因是m面的晶体生长速度比a平面慢，并且所希望的c面生长不受阻碍。种子晶体10和夹持器T分别周期性地设置在y轴方向。版权所有（C）2008，JPO＆INPIT

12. 发明专利

JP2007277055A Method for manufacturing semiconductor crystal and semiconductor substrate 审中-公开
标题翻译：制造半导体晶体和半导体衬底的方法
公开(公告)号：JP2007277055A
公开(公告)日：2007-10-25
申请号：JP2006106720
申请日：2006-04-07
申请人： Ngk Insulators Ltd , Osaka Univ , Toyoda Gosei Co Ltd , 国立大学法人大阪大学 , 日本碍子株式会社 , 豊田合成株式会社
发明人： SHIBATA NAOKI , HIRATA KOJI , YAMAZAKI SHIRO , IMAI KATSUHIRO , IWAI MAKOTO , SASAKI TAKATOMO , MORI YUSUKE , KAWAMURA SHIRO
IPC分类号： C30B29/38 , C30B9/00 , H01L33/32
CPC分类号： C30B29/403 , C30B9/00 , H01L33/0075 , Y10T428/265 , Y10T428/266
摘要： PROBLEM TO BE SOLVED: To manufacture a high quality semiconductor crystal inexpensively in a flux method. SOLUTION: A buffer layer 12 comprising AlGaN and having a film thickness of about 4 μm is stacked on a silicon substrate 11 having a thickness of about 400 μm by crystal growth based on an MOVPE method, and thereafter, a GaN layer 13 having a thickness of an extent that the layer is not disappeared at the initial stage of crystal growth based on a flux method is stacked on the buffer later 12 by crystal growth based on the MOVPE method. Prescribed crystal growth conditions are continuously maintained while agitating and mixing a mixed flux by generating a thermal convection in the mixed flux by heating it with a heater. At this time, the vicinity of the interface between the mixed flux and nitrogen gas continuously becomes a supersaturated state of raw material atoms of a group III nitride-based compound semiconductor, and thereby, a desired semiconductor crystal (n-type GaN single crystal 20) can be favorably grown from the crystal growth surface of a template 10. Consequently, the n-type semiconductor crystal (n-type GaN single crystal 20) having a low dislocation density can be obtained. COPYRIGHT: (C)2008,JPO&INPIT
摘要翻译：要解决的问题：以通量方法廉价地制造高品质的半导体晶体。解决方案：通过基于MOVPE方法的晶体生长，将厚度约为400μm的厚度约4μm的AlGaN缓冲层12堆叠在厚度约为400μm的硅衬底11上，然后将GaN层13 在基于磁通法的晶体生长的初始阶段，层不厚度消失的程度通过基于MOVPE方法的晶体生长堆叠在缓冲液12之后。在通过用加热器加热混合助熔剂中产生热对流来搅拌和混合混合助熔剂来连续地保持规定的晶体生长条件。此时，混合磁通和氮气之间的界面附近连续地变成III族氮化物系化合物半导体的原料原子的过饱和状态，从而形成期望的半导体晶体（n型GaN单晶20 ）可以从模板10的晶体生长表面有利地生长。因此，可以获得具有低位错密度的n型半导体晶体（n型GaN单晶20）。版权所有（C）2008，JPO＆INPIT

13. 发明专利

JP2007246368A Method for producing semiconductor crystal 有权
标题翻译：生产半导体晶体的方法
公开(公告)号：JP2007246368A
公开(公告)日：2007-09-27
申请号：JP2006075223
申请日：2006-03-17
申请人： Ngk Insulators Ltd , Osaka Univ , Toyoda Gosei Co Ltd , 国立大学法人大阪大学 , 日本碍子株式会社 , 豊田合成株式会社
发明人： YAMAZAKI SHIRO , IMAI KATSUHIRO , IWAI MAKOTO , SASAKI TAKATOMO , MORI YUSUKE , KAWAMURA SHIRO , YAMADA SUKETSUGU
IPC分类号： C30B29/38 , C30B9/00
摘要： PROBLEM TO BE SOLVED: To produce a high quality semiconductor crystal inexpensively, in a flux method. SOLUTION: A GaN single crystal 20 is grown by the flux method using a GaN substrate 10 having a crystal dislocation density higher than that of a semiconductor crystal to be grown. Because the crystal dislocation density of the GaN substrate 10 is higher than that of the semiconductor crystal to be grown, the melting speed of the GaN substrate 10 into a flux is faster than that of the semiconductor crystal into the flux. Nitrogen element is supplied by the dissolution of the GaN substrate 10, and thereby, the crystal growth speed can be increased. Further, the GaN substrate 10 can be melted and consumed in concurrence with the growth of the semiconductor crystal. In the growing process, Ga element is supplied from the GaN substrate 10 in a solution of Ga element and the flux, consequently lowering of the Ga concentration in the flux associated with the growth in the surface side can be suppressed, the ratio of Ga element in the flux can be made constant, and flux-constituting elements such as Na or Li can be prevented from being taken into the crystal. COPYRIGHT: (C)2007,JPO&INPIT
摘要翻译：要解决的问题：以通量方法廉价地生产高质量的半导体晶体。解决方案：通过使用具有比待生长的半导体晶体的晶体位错密度高的晶体位错密度的GaN衬底10的通量法生长GaN单晶20。因为GaN衬底10的晶体位错密度高于要生长的半导体晶体的晶体位错密度，所以GaN衬底10熔化成焊剂的熔化速度比半导体晶体的熔化速度快。通过GaN衬底10的溶解提供氮元素，从而可以提高晶体生长速度。此外，与衬底的半导体晶体的生长一致，可以使GaN衬底10熔化并消耗。在生长过程中，Ga元素在Ga基元素和助熔剂的溶液中从GaN衬底10提供，因此可以抑制与表面侧的生长相关的助焊剂中的Ga浓度的降低，Ga元素可以使通量保持恒定，并且可以防止诸如Na或Li的助熔剂组成元素被引入晶体。版权所有（C）2007，JPO＆INPIT

14. 发明专利

JP2007126315A Semiconductor crystal manufacturing method 审中-公开
标题翻译：半导体晶体制造方法
公开(公告)号：JP2007126315A
公开(公告)日：2007-05-24
申请号：JP2005319019
申请日：2005-11-02
申请人： Ngk Insulators Ltd , Osaka Univ , Toyoda Gosei Co Ltd , 国立大学法人大阪大学 , 日本碍子株式会社 , 豊田合成株式会社
发明人： YAMAZAKI SHIRO , HIRATA KOJI , IMAI KATSUHIRO , IWAI MAKOTO , SASAKI TAKATOMO , MORI YUSUKE , YOSHIMURA MASASHI , KAWAMURA SHIRO , YAMADA SUKETSUGU
IPC分类号： C30B29/38 , C30B9/00
摘要： PROBLEM TO BE SOLVED: To provide a semiconductor crystal manufacturing method for manufacturing a high quality group III nitride-based compound semiconductor crystal at a low cost by a flux method.
SOLUTION: After an n-type GaN single crystal 20 is grown to have a sufficient thickness, e.g., about 500 μm or more by the flux method, the temperature of a crucible is successively maintained at 850-880°C until a protective film and a silicon substrate 11 are dissolved completely in a flux. Thereafter, the temperature of a reaction chamber is lowered to a temperature of ≤100°C in a nitrogen gas atmosphere. However, at least one part of the protective film or the silicon substrate 11 may be dissolved in the growth process of the GaN single crystal 20. The manner of parallel simultaneous progress of these processes can be adequately controlled, for example, by the film-forming mode of the protective film. In the case that the silicon substrate 11 dissolved in the flux is added in a growing GaN single crystal 20 as an n-type additive (si), an n-type semiconductor crystal is obtained.
COPYRIGHT: (C)2007,JPO&INPIT
摘要翻译：要解决的问题：提供一种通过助焊剂法以低成本制造高质量III族氮化物基化合物半导体晶体的半导体晶体制造方法。解决方案：在n型GaN单晶20通过助熔法生长至具有足够厚度（例如约500μm或更大）之后，将坩埚的温度连续保持在850-880℃，直到保护膜和硅基板11完全溶解在焊剂中。此后，在氮气气氛中将反应室的温度降低至≤100℃。然而，保护膜或硅衬底11的至少一部分可以溶解在GaN单晶20的生长过程中。这些工艺的并行同时进行的方式可以被适当地控制，例如通过膜 - 形成保护膜的方式。在作为n型添加剂（si）生长的GaN单晶20中添加溶解在助熔剂中的硅衬底11的情况下，获得n型半导体晶体。版权所有（C）2007，JPO＆INPIT

15. 发明专利

JP2007254206A Method for growing nitride single crystal 审中-公开
标题翻译：用于生长氮化物单晶的方法
公开(公告)号：JP2007254206A
公开(公告)日：2007-10-04
申请号：JP2006080653
申请日：2006-03-23
申请人： Ngk Insulators Ltd , Osaka Univ , 国立大学法人大阪大学 , 日本碍子株式会社
发明人： ICHIMURA MIKIYA , SASAKI TAKATOMO , MORI YUSUKE , KAWAMURA SHIRO
IPC分类号： C30B29/38 , C30B9/00
摘要： PROBLEM TO BE SOLVED: To prevent the degradation of a single crystal caused by the oxidation of a solution when growing a nitride single crystal by a flux method.
SOLUTION: An outer container 4 is disposed inside an atmosphere controlling container 5, and a crucible is disposed inside the outer container 4. A seed crystal is immersed in a solution containing an easily oxidizing substance in the crucible, from which a nitride single crystal is grown. The atmosphere upon growing the nitride single crystal comprises nitrogen supplied from a nitrogen cylinder 19 and a reducing gas supplied from a reducing gas cylinder 21, and preferably the reducing gas contains hydrogen.
COPYRIGHT: (C)2008,JPO&INPIT
摘要翻译：要解决的问题：为了防止在通过助熔剂法生长氮化物单晶时溶液的氧化引起的单晶的劣化。解决方案：外部容器4设置在气氛控制容器5的内部，并且坩埚设置在外部容器4的内部。将晶种浸入坩埚中容纳氧化物质的溶液中，将氮化物单晶生长。生长氮化物单晶的气氛包括从氮气筒19供给的氮和从还原气体筒21供给的还原气体，优选还原气体含有氢。版权所有（C）2008，JPO＆INPIT

16. 发明专利

JP2008254999A Crystal growing apparatus 有权
标题翻译：水晶生长装置
公开(公告)号：JP2008254999A
公开(公告)日：2008-10-23
申请号：JP2008029035
申请日：2008-02-08
申请人： Yusuke Mori , Ngk Insulators Ltd , Toyoda Gosei Co Ltd , 日本碍子株式会社 , 勇介森 , 豊田合成株式会社
发明人： YAMAZAKI SHIRO , HIRATA KOJI , SATO TOSHIYUKI , NAGAI SEIJI , IMAI KATSUHIRO , IWAI MAKOTO , HIGASHIHARA SHUHEI , SASAKI TAKATOMO , MORI YUSUKE , KAWAMURA SHIRO
IPC分类号： C30B29/38 , C30B19/02
摘要： PROBLEM TO BE SOLVED: To provide a flux method with an improved work efficiency while maintaining the purity of flux at a high level and saving the flux material cost.
SOLUTION: A sodium (Na) purifying apparatus 130 includes an apparatus 140 for holding and managing Na that keeps purified Na in a liquid state. Liquid Na is supplied to the apparatus 140 for holding and managing Na through a liquid Na supply tube 139 which is kept at 100°C. The apparatus 140 for holding and managing Na has an Ar gas purifying apparatus 141 that controls the condition of argon (Ar) gas which fills the internal space thereof. Thus, by turning a faucet 121 on and off at a desired timing, the purified liquid Na supplied from the Na purifying apparatus 130 can be introduced into a crucible c at will via the liquid Na supply tube 139, the apparatus 140 for holding and managing Na and piping 149.
COPYRIGHT: (C)2009,JPO&INPIT
摘要翻译：要解决的问题：提供具有提高的工作效率的助焊剂方法，同时将焊剂的纯度保持在高水平并且节省焊剂材料成本。解决方案：钠（Na）纯化装置130包括用于保持和管理保持纯化的Na处于液态的Na的装置140。液体Na被供给到用于通过保持在100℃的液体Na供应管139保持和管理Na的装置140。用于保持和管理Na的装置140具有控制填充其内部空间的氩（Ar）气体的状态的Ar气体净化装置141。因此，通过在期望的时刻打开和关闭水龙头121，可以从Na净化装置130供应的净化液体Na经由液体Na供给管139，用于保持和管理的装置140被引入坩埚c Na和管道149.版权所有（C）2009，JPO＆INPIT

17. 发明专利

JP2012025662A Method for producing group iii nitride compound semiconductor 有权
标题翻译：生产III族氮化物半导体的方法
公开(公告)号：JP2012025662A
公开(公告)日：2012-02-09
申请号：JP2011243766
申请日：2011-11-07
申请人： Ngk Insulators Ltd , Toyoda Gosei Co Ltd , 日本碍子株式会社 , 豊田合成株式会社
发明人： YAMAZAKI SHIRO , NAGAI SEIJI , SATO SHINYUKI , IWAI MAKOTO , IMAI KATSUHIRO , SASAKI TAKATOMO , MORI YUSUKE , KAWAMURA SHIRO
IPC分类号： C30B29/62 , C30B19/04 , H01L33/32
摘要： PROBLEM TO BE SOLVED: To suppress attachment of miscellaneous crystals on a nitrogen surface of a GaN self-standing substrate, and wastage of raw materials in production of GaN by the flux method.SOLUTION: There are shown four examples of arrangement methods of crucibles 26-1 to 26-4 and GaN self-standing substrates. In Fig.1.A, the nitrogen surface of a self-standing substrate 10 is closely contacted with a planar inner wall facing obliquely upward of a crucible 26-1. In Fig.1.B, the nitrogen surface of a self-standing substrate 10 is closely contacted with a planar inner wall facing horizontally of a crucible 26-2, and fixed using a fixture ST-2. In Fig.1.C, a fixture ST-3 is arranged on the flat bottom of a crucible 26-3, and the nitrogen surfaces of self-standing substrates 10-1 and 10-2 are mutually closely contacted. In Fig.1.D, a fixture ST-4 is arranged on the flat bottom of a crucible 26-4, and a GaN self-standing substrate 10 is fixed thereto. The nitrogen surface of the self-standing substrate 10 is covered with the fixture ST-4. A mixed flux in which gallium and sodium are melted is filled, and a GaN single crystal is grown on a gallium surface Funder pressurized nitrogen.
摘要翻译：要解决的问题：抑制GaN自支撑衬底的氮表面上的杂晶的附着，以及通过助熔剂法生产GaN的原料的浪费。解决方案：示出了坩埚26-1至26-4和GaN自支撑衬底的布置方法的四个示例。在图1A中，自立式基板10的氮表面与坩埚26-1的斜上方的平面内壁紧密接触。在图1B中，自立基板10的氮表面与坩埚26-2的水平方向的平面内壁紧密接触，并使用固定件ST-2固定。在图1C中，夹具ST-3配置在坩埚26-3的平坦底部，自立基板10-1,10-2的氮气面相互紧密接触。在图1D中，在坩埚26-4的平坦的底部设置固定件ST-4，并且固定有GaN自立基板10。自立基板10的氮表面被固定件ST-4覆盖。填充镓和钠被熔化的混合助熔剂，并且在加压氮气下在镓表面上生长GaN单晶。版权所有（C）2012，JPO＆INPIT

18. 发明专利

JP2008290929A Method for producing group iii nitride-based compound semiconductor 有权
标题翻译：生产III族氮化物化合物半导体的方法
公开(公告)号：JP2008290929A
公开(公告)日：2008-12-04
申请号：JP2008038980
申请日：2008-02-20
申请人： Ngk Insulators Ltd , Toyoda Gosei Co Ltd , 日本碍子株式会社 , 豊田合成株式会社
发明人： YAMAZAKI SHIRO , NAGAI SEIJI , SATO TOSHIYUKI , IWAI MAKOTO , IMAI KATSUHIRO , SASAKI TAKATOMO , MORI YUSUKE , KAWAMURA SHIRO
IPC分类号： C30B29/38 , C30B19/06 , H01L33/32 , H01S5/323
摘要： PROBLEM TO BE SOLVED: To provide a method by which deposition of miscellaneous crystals on the nitrogen-face of a GaN self-standing substrate and waste of raw materials are prevented, in the production of GaN through a flux method. SOLUTION: Four arrangements of crucibles 26-1-4 and a GaN self-standing substrate are exemplified. In Fig. 1 A, a nitrogen-face of a self-standing substrate 10 comes into close contact with a sloped flat inner wall of a crucible 26-1. In Fig. 1 B, a nitrogen-face of a self-standing substrate 10 comes into close contact with a horizontally facing flat inner wall of a crucible 26-2, and the substrate is fixed by means of a fixture ST-2. In Fig. 1 C, a fixture ST-3 is provided on a flat bottom of a crucible 26-3, and two GaN self-standing substrates 10-1, 10-2 are fixed by means of the fixture ST-3 so that the nitrogen-faces of the substrates come into close contact with each other. In Fig. 1 D, a fixture ST-4 is provided on a flat bottom of a crucible 26-4, and a GaN self-standing substrate 10 is fixed on the fixture so that the nitrogen-face of the substrate 10 is covered with the fixture. A flux mixture of molten gallium and sodium is charged into each crucible, and a GaN single crystal is grown on the gallium-face F Ga under pressurized nitrogen. COPYRIGHT: (C)2009,JPO&INPIT
摘要翻译：要解决的问题：提供通过通过焊剂法制造GaN的方法，其通过在GaN自支撑衬底的氮面上沉积杂晶并防止原料的浪费。解决方案：示例了坩埚26-1-4和GaN自立衬底的四种布置。在图如图1A所示，自立基板10的氮面与坩埚26-1的倾斜的平坦的内壁紧密接触。在图如图1B所示，自立基板10的氮面与坩埚26-2的水平面平坦的内壁紧密接触，并且基板通过固定件ST-2固定。在图如图1C所示，在坩埚26-3的平坦底部设置固定件ST-3，借助于固定件ST-3固定两个GaN自立基板10-1,10-2，基板的表面彼此紧密接触。在图如图1D所示，在坩埚26-4的平坦底部设置固定件ST-4，将固定在固定装置上的GaN自立基板10固定在基板10的氮面上。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F Ga 上生长GaN单晶。版权所有（C）2009，JPO＆INPIT

19. 发明专利

JP2008266067A Method for producing aluminum nitride single crystal 有权
标题翻译：用于生产氮化钠单晶的方法
公开(公告)号：JP2008266067A
公开(公告)日：2008-11-06
申请号：JP2007110363
申请日：2007-04-19
申请人： Ngk Insulators Ltd , Toyoda Gosei Co Ltd , 日本碍子株式会社 , 豊田合成株式会社
发明人： SHIMODAIRA TAKANAO , IMAI KATSUHIRO , IWAI MAKOTO , MORI YUSUKE , SASAKI TAKATOMO , KAWAMURA SHIRO , ARAI MASAKI , YAMAZAKI SHIRO
IPC分类号： C30B29/38 , C30B19/02
摘要： PROBLEM TO BE SOLVED: To provide a method for growing aluminum nitride at a high productivity by a flux method.
SOLUTION: Aluminum nitride single crystal is grown from a melt containing aluminum and a flux in the presence of a nitrogen-containing gas, wherein the growing temperature of the aluminum nitride single crystal is 1,250°C or above and 1,500°C or below, the partial pressure of the nitrogen in the nitrogen-containing gas during growing is 0.01 MPa or above and 1 MPa or below, the molar ratio of aluminum to the flux in the melt is 40:60-90:10, the flux is comprised of one kind or more of a first metal selected from the group consisting of tin, gallium, indium and bismuth and comprised of one kind or more of a second metal belonging to an alkaline metal and an alkaline earth metal, and the molar ratio of the first metal to the second metal is 1:99-99:1.
COPYRIGHT: (C)2009,JPO&INPIT
摘要翻译：要解决的问题：提供一种通过助熔剂方法以高生产率生长氮化铝的方法。解决方案：氮化铝单晶在含氮气体的存在下由含有铝和助熔剂的熔体生长，其中氮化铝单晶的生长温度为1,250℃以上且1500℃，或以下，生长时的含氮气体中的氮分压为0.01MPa以上且1MPa以下，铝与熔体中的助熔剂的摩尔比为40:60〜90:10，通量为由选自锡，镓，铟和铋的一种或多种第一金属组成，并且由一种或多种属于碱金属和碱土金属的第二金属组成，并且其摩尔比第二金属的第一金属为1:99-99:1。版权所有（C）2009，JPO＆INPIT

20. 发明专利

JP2008222492A Melt composition for growing gallium nitride single crystal and method for growing gallium nitride single crystal 有权
标题翻译：用于生长氮化镓单晶的熔融组合物和用于生长氮化镓单晶的方法
公开(公告)号：JP2008222492A
公开(公告)日：2008-09-25
申请号：JP2007063110
申请日：2007-03-13
申请人： Yusuke Mori , Ngk Insulators Ltd , Toyoda Gosei Co Ltd , 日本碍子株式会社 , 勇介森 , 豊田合成株式会社
发明人： IWAI MAKOTO , SHIMODAIRA TAKANAO , YAMAMURA YOSHIHIKO , YAMAZAKI SHIRO , SASAKI TAKATOMO , MORI YUSUKE , KAWAMURA SHIRO
IPC分类号： C30B29/38 , C30B19/04
摘要： PROBLEM TO BE SOLVED: To provide a method by which the impurity band light-emission of a crystal can be reduced, the crystal having good transparency can be obtained, and the flatness of the crystal can be improved when a GaN single crystal is grown by a flux method using a Ga-Na-based melt.
SOLUTION: A melt composition containing gallium, sodium, barium and lithium is used for growing a gallium nitride single crystal by the flux method. The compositional ratio except gallium being a raw material is such that the total amount of barium and lithium is 0.02 to 1.0 mol% when the amount of sodium is 100 mol%.
COPYRIGHT: (C)2008,JPO&INPIT

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