Sixpoint Materials, Inc.

Masanori Ikari

Tadao Hashimoto

Edward Letts

Present invention discloses a high-pressure vessel of large size formed with a limited size of e.g. Ni&#x2014;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.

High-pressure vessel for growing group III nitride crystals and method of growing group III nitride crystals using high-pressure vessel and group III nitride crystal

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&#xb0; 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.

Methods for producing improved crystallinity group III-nitride crystals from initial group III-nitride seed by ammonothermal growth

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.

Method for producing group III-nitride wafers and group III-nitride wafers

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.

Methods for producing GaN nutrient for ammonothermal growth

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&#xb0; 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.

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.

Method for testing group III-nitride wafers and group III-nitride wafers with test data

The present invention discloses a high-pressure vessel of large size formed with a limited size of e.g. Ni&#x2014;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.

The present invention discloses a high-pressure vessel of large size formed with a limited size of e.g. Ni&#x2014;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.

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Santa Barbara, CA, United States of America

Masanori Ikari