公开(公告)号：US20100068118A1

公开(公告)日：2010-03-18

申请号：US12455683

申请日：2009-06-04

申请人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

发明人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

IPC分类号： C01B21/06 ,  C30B23/02 ,  C30B23/06 ,  C23C16/34

CPC分类号： C30B7/105 ,  B32B15/01 ,  C30B7/10 ,  C30B29/403 ,  C30B29/406 ,  C30B35/002 ,  Y10T428/12028

摘要： The present invention discloses a high-pressure vessel of large size formed with a limited size of e.g. Ni—Cr based precipitation hardenable superalloy. The vessel may have multiple zones.For instance, the high-pressure vessel may be divided into at least three regions with flow-restricting devices and the crystallization region is set higher temperature than other regions. This structure helps to reliably seal both ends of the high-pressure vessel, and at the same time, may help to greatly reduce unfavorable precipitation of group III nitride at the bottom of the vessel.This invention also discloses novel procedures to grow crystals with improved purity, transparency and structural quality. Alkali metal-containing mineralizers are charged with minimum exposure to oxygen and moisture until the high-pressure vessel is filled with ammonia. Several methods to reduce oxygen contamination during the process steps are presented. Also, back etching of seed crystals and a new temperature ramping scheme to improve structural quality are disclosed.

摘要翻译： 本发明公开了一种大尺寸的大型高压容器。 Ni-Cr基沉淀硬化型超合金。 船舶可能有多个区域。 例如，高压容器可以分为具有流量限制装置的至少三个区域，并且结晶区域设定为比其他区域更高的温度。 该结构有助于可靠地密封高压容器的两端，并且同时可有助于大大减少容器底部的III族氮化物的不利沉淀。 本发明还公开了提高纯度，透明度和结构质量的晶体生长的新方法。 含碱金属的矿化剂以最低的氧气和湿度暴露于高压容器中充满氨。 介绍了在工艺步骤中减少氧气污染的几种方法。 此外，公开了种晶的背面蚀刻和新的温度梯度方案以提高结构质量。

公开(公告)号：US09803293B2

公开(公告)日：2017-10-31

申请号：US12392960

申请日：2009-02-25

申请人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

发明人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

IPC分类号： C30B15/14 ,  C30B29/40 ,  C30B7/10 ,  C30B33/02

CPC分类号： C30B33/02 ,  C30B7/10 ,  C30B7/105 ,  C30B29/403 ,  C30B29/406

摘要： The present invention discloses a production method for group III nitride ingots or pieces such as wafers. To solve the coloration problem in the wafers grown by the ammonothermal method, the present invention composed of the following steps; growth of group III nitride ingots by the ammonothermal method, slicing of the ingots into wafers, annealing of the wafers in a manner that avoids dissociation or decomposition of the wafers. This annealing process is effective to improve transparency of the wafers and/or otherwise remove contaminants from wafers.

公开(公告)号：US08728234B2

公开(公告)日：2014-05-20

申请号：US12455760

申请日：2009-06-04

申请人： Edward Letts ,  Tadao Hashimoto ,  Masanori Ikari

发明人： Edward Letts ,  Tadao Hashimoto ,  Masanori Ikari

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

CPC分类号： H01L29/2003 ,  C30B7/10 ,  C30B7/105 ,  C30B29/403 ,  C30B29/406 ,  C30B33/00 ,  H01L21/0254

摘要： The present invention discloses methods to create higher quality group III-nitride wafers that then generate improvements in the crystalline properties of ingots produced by ammonothermal growth from an initial defective seed. By obtaining future seeds from carefully chosen regions of an ingot produced on a bowed seed crystal, future ingot crystalline properties can be improved. Specifically, the future seeds are optimized if chosen from an area of relieved stress on a cracked ingot or from a carefully chosen N-polar compressed area. When the seeds are sliced out, miscut of 3-10° helps to improve structural quality of successive growth. Additionally a method is proposed to improve crystal quality by using the ammonothermal method to produce a series of ingots, each using a specifically oriented seed from the previous ingot. When employed, these methods enhance the quality of Group III nitride wafers and thus improve the efficiency of any subsequent device.

摘要翻译： 本发明公开了产生更高质量III族氮化物晶片的方法，其然后通过初始缺陷种子的氨热生长产生的锭的结晶特性产生改善。 通过从在晶圆上生产的锭的精心选择的区域获得未来的种子，可以提高未来的锭晶体性质。 具体来说，如果从破裂的锭块或精心挑选的N极压缩区域的缓解应力区域选择，则将来的种子进行优化。 当种子切片时，3-10°的杂交有助于提高连续生长的结构质量。 另外，提出了通过使用氨热方法来生产一系列锭子来提高晶体质量的方法，每个锭子使用来自先前锭的特异性取向的种子。 当采用这些方法时，这些方法提高了III族氮化物晶片的质量，从而提高了任何随后的器件的效率。

公开(公告)号：US08236267B2

公开(公告)日：2012-08-07

申请号：US12455683

申请日：2009-06-04

申请人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

发明人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

IPC分类号： C01B21/06 ,  C30B23/00 ,  C23C16/00

CPC分类号： C30B7/105 ,  B32B15/01 ,  C30B7/10 ,  C30B29/403 ,  C30B29/406 ,  C30B35/002 ,  Y10T428/12028

摘要： The present invention discloses a high-pressure vessel of large size formed with a limited size of e.g. Ni—Cr based precipitation hardenable superalloy. The vessel may have multiple zones.For instance, the high-pressure vessel may be divided into at least three regions with flow-restricting devices and the crystallization region is set higher temperature than other regions. This structure helps to reliably seal both ends of the high-pressure vessel, and at the same time, may help to greatly reduce unfavorable precipitation of group III nitride at the bottom of the vessel.This invention also discloses novel procedures to grow crystals with improved purity, transparency and structural quality. Alkali metal-containing mineralizers are charged with minimum exposure to oxygen and moisture until the high-pressure vessel is filled with ammonia. Several methods to reduce oxygen contamination during the process steps are presented. Also, back etching of seed crystals and a new temperature ramping scheme to improve structural quality are disclosed.

摘要翻译： 本发明公开了一种大尺寸的大型高压容器。 Ni-Cr基沉淀硬化型超合金。 船舶可能有多个区域。 例如，高压容器可以分为具有流量限制装置的至少三个区域，并且结晶区域设定为比其他区域更高的温度。 该结构有助于可靠地密封高压容器的两端，并且同时可有助于大大减少容器底部的III族氮化物的不利沉淀。 本发明还公开了提高纯度，透明度和结构质量的晶体生长的新方法。 含碱金属的矿化剂以最低的氧气和湿度暴露于高压容器中充满氨。 介绍了在工艺步骤中减少氧气污染的几种方法。 此外，公开了种晶的背面蚀刻和新的温度梯度方案以提高结构质量。

公开(公告)号：US20090256240A1

公开(公告)日：2009-10-15

申请号：US12392960

申请日：2009-02-25

申请人： Tadao HASHIMOTO ,  Edward Letts ,  Masanori Ikari

发明人： Tadao HASHIMOTO ,  Edward Letts ,  Masanori Ikari

IPC分类号： H01L29/20 ,  H01L21/322

CPC分类号： C30B33/02 ,  C30B7/10 ,  C30B7/105 ,  C30B29/403 ,  C30B29/406

摘要： The present invention discloses a production method for group III nitride ingots or pieces such as wafers. To solve the coloration problem in the wafers grown by the ammonothermal method, the present invention composed of the following steps; growth of group III nitride ingots by the ammonothermal method, slicing of the ingots into wafers, annealing of the wafers in a manner that avoids dissociation or decomposition of the wafers. This annealing process is effective to improve transparency of the wafers and/or otherwise remove contaminants from wafers.

摘要翻译： 本发明公开了一种III族氮化物锭或诸如晶片的片的制造方法。 为了解决通过氨热法生长的晶片的着色问题，本发明由以下步骤组成： 通过氨热法生长III族氮化物锭，将锭切成晶片，以避免晶片解离或分解的方式退火晶片。 该退火工艺有效地提高晶片的透明度和/或以其它方式从晶片去除污染物。

公开(公告)号：US08420041B2

公开(公告)日：2013-04-16

申请号：US13491392

申请日：2012-06-07

申请人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

发明人： Tadao Hashimoto ,  Edward Letts ,  Masanori Ikari

IPC分类号： C01B21/06 ,  C30B23/00 ,  C23C16/00

CPC分类号： C30B7/105 ,  B32B15/01 ,  C30B7/10 ,  C30B29/403 ,  C30B29/406 ,  C30B35/002 ,  Y10T428/12028

摘要： The present invention discloses a high-pressure vessel of large size formed with a limited size of e.g. Ni—Cr based precipitation hardenable superalloy. Vessel may have multiple zones. For instance, the high-pressure vessel may be divided into at least three regions with flow-restricting devices and the crystallization region is set higher temperature than other regions. This structure helps to reliably seal both ends of the high-pressure vessel, at the same time, may help to greatly reduce unfavorable precipitation of group III nitride at the bottom of the vessel. Invention also discloses novel procedures to grow crystals with improved purity, transparency and structural quality. Alkali metal-containing mineralizers are charged with minimum exposure to oxygen and moisture until the high-pressure vessel is filled with ammonia. Several methods to reduce oxygen contamination during the process steps are presented. Back etching of seed crystals and a new temperature ramping scheme to improve structural quality are disclosed.

摘要翻译： 本发明公开了一种大尺寸的大型高压容器。 Ni-Cr基沉淀硬化型超合金。 船舶可能有多个区域。 例如，高压容器可以分为具有流量限制装置的至少三个区域，并且结晶区域设定为比其他区域更高的温度。 该结构有助于可靠地密封高压容器的两端，同时有助于大大减少容器底部的III族氮化物的不利沉淀。 本发明还公开了提高纯度，透明度和结构质量的晶体的新方法。 含碱金属的矿化剂以最低的氧气和湿度暴露于高压容器中充满氨。 介绍了在工艺步骤中减少氧气污染的几种方法。 公开了晶种的后蚀刻和新的温度梯度方案以改善结构质量。

公开(公告)号：US20100126411A1

公开(公告)日：2010-05-27

申请号：US12624006

申请日：2009-11-23

申请人： Edward Letts ,  Tadao Hashimoto ,  Masanori Ikari

发明人： Edward Letts ,  Tadao Hashimoto ,  Masanori Ikari

IPC分类号： C01B21/06 ,  B05D5/12 ,  C30B23/00 ,  C23C16/00

CPC分类号： C30B29/403 ,  C01B21/0632 ,  C30B7/10 ,  C30B25/00 ,  C30B25/005 ,  C30B29/406

摘要： The present invention discloses methods to produce large quantities of polycrystalline GaN for use in the ammonothermal growth of group III-nitride material. High production rates of GaN can be produced in a hydride vapor phase growth system. One drawback to enhanced polycrystalline growth is the increased incorporation of impurities, such as oxygen. A new reactor design using non-oxide material that reduces impurity concentrations is disclosed. Purification of remaining source material after an ammonothermal growth is also disclosed. The methods described produce sufficient quantities of polycrystalline GaN source material for the ammonothermal growth of group III-nitride material.

摘要翻译： 本发明公开了生产用于III族氮化物材料的氨热生长的大量多晶GaN的方法。 可以在氢化物气相生长系统中生产高产率的GaN。 增加多晶生长的一个缺点是增加杂质如氧气的掺入。 公开了使用减少杂质浓度的非氧化物材料的新型反应器设计。 还公开了在氨热生长之后的剩余源材料的纯化。 所描述的方法产生足够量的用于III族氮化物材料的氨热生长的多晶GaN源材料。

公开(公告)号：US20100095882A1

公开(公告)日：2010-04-22

申请号：US12580849

申请日：2009-10-16

申请人： Tadao Hashimoto ,  Masanori Ikari ,  Edward Letts

发明人： Tadao Hashimoto ,  Masanori Ikari ,  Edward Letts

IPC分类号： C30B7/10 ,  B01J3/04

CPC分类号： C30B7/105 ,  C30B7/10 ,  C30B29/403 ,  C30B29/406 ,  C30B35/002 ,  Y10T117/1096

摘要： The present disclosure proves for new design of reactors used for ammonothermal growth of III nitride crystals. The reactors include a region intermediate a source dissolution region and a crystal growth region configured to provide growth of high quality crystals at rates greater than 100 μm/day. In one embodiment, multiple baffle plates having openings whose location is designed so that there is no direct path through the intermediate region, or with multiple baffle plates having differently sized openings on each plate so that the flow is slowed down and/or exhibit greater mixing are described. The disclosed designs enables obtaining high temperature difference between the dissolution region and the crystallization region without decreasing conductance through the device.

摘要翻译： 本公开内容证明了用于III族氮化物晶体的氨热生长的反应器的新设计。 反应器包括源溶解区域和晶体生长区域之间的区域，晶体生长区域被配置为以大于100μm/天的速率提供高质量晶体的生长。 在一个实施例中，具有开口的多个挡板具有位置被设计成使得不存在通过中间区域的直接路径，或者在每个板上具有不同尺寸的开口的多个挡板，使得流动减慢和/或显示更大的混合 被描述。 所公开的设计使得能够在不降低通过该装置的电导的情况下获得溶解区域和结晶区域之间的高温差。

公开(公告)号：US20090315151A1

公开(公告)日：2009-12-24

申请号：US12456181

申请日：2009-06-12

申请人： Tadao Hashimoto ,  Masanori Ikari ,  Edward Letts

发明人： Tadao Hashimoto ,  Masanori Ikari ,  Edward Letts

IPC分类号： H01L29/20 ,  H01L21/66

CPC分类号： G01R31/2601 ,  C30B7/10 ,  C30B29/403 ,  H01L22/20 ,  H01L29/2003 ,  H01L2924/0002 ,  H01L2924/00

摘要： The present invention discloses a new testing method of group III-nitride wafers. By utilizing the ammonothermal method, GaN or other Group III-nitride wafers can be obtained by slicing the bulk GaN ingots. Since these wafers originate from the same ingot, these wafers have similar properties/qualities. Therefore, properties of wafers sliced from an ingot can be estimated from measurement data obtained from selected number of wafers sliced from the same ingot or an ingot before slicing. These estimated properties can be used for product certificate of untested wafers. This scheme can reduce a significant amount of time, labor and cost related to quality control.

摘要翻译： 本发明公开了III族氮化物晶片的新试验方法。 通过利用氨热法，可以通过将本体GaN锭切片来获得GaN或其它III族氮化物晶片。 由于这些晶片来自相同的晶锭，所以这些晶片具有相似的特性/质量。 因此，可以从在切片前从相同的锭或锭切片的所选数量的晶片获得的测量数据估计从晶锭切片的晶片的性质。 这些估计属性可用于未经测试的晶片的产品证书。 该方案可以减少与质量控制相关的大量时间，劳动力和成本。

公开(公告)号：US08852341B2

公开(公告)日：2014-10-07

申请号：US12624006

申请日：2009-11-23

申请人： Edward Letts ,  Tadao Hashimoto ,  Masanori Ikari

发明人： Edward Letts ,  Tadao Hashimoto ,  Masanori Ikari

IPC分类号： C30B25/02 ,  C30B25/00 ,  C30B29/40 ,  C01B21/06 ,  C30B7/10

CPC分类号： C30B29/403 ,  C01B21/0632 ,  C30B7/10 ,  C30B25/00 ,  C30B25/005 ,  C30B29/406

摘要： The present invention discloses methods to produce large quantities of polycrystalline GaN for use in the ammonothermal growth of group III-nitride material. High production rates of GaN can be produced in a hydride vapor phase growth system. One drawback to enhanced polycrystalline growth is the increased incorporation of impurities, such as oxygen. A new reactor design using non-oxide material that reduces impurity concentrations is disclosed. Purification of remaining source material after an ammonothermal growth is also disclosed. The methods described produce sufficient quantities of polycrystalline GaN source material for the ammonothermal growth of group III-nitride material.

摘要翻译： 本发明公开了生产用于III族氮化物材料的氨热生长的大量多晶GaN的方法。 可以在氢化物气相生长系统中生产高产率的GaN。 增加多晶生长的一个缺点是增加杂质如氧气的掺入。 公开了使用减少杂质浓度的非氧化物材料的新型反应器设计。 还公开了在氨热生长之后的剩余源材料的纯化。 所描述的方法产生足够量的用于III族氮化物材料的氨热生长的多晶GaN源材料。