# US 10,156,026 B2 · Diffusion assisted crystal hydrothermal and flux growth

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- Number: US 10,156,026 B2
- Document ID: US10156026B2
- Status: Granted
- Kind: B2
- Application number: 14/999,312
- Filed: 2016-04-22
- Published: 2017-10-26
- Granted: 2018-12-18
- Earliest claimed: 2016-04-22
- Assignees: Silo Tech
- Applicants: Daniel Smith
- Inventors: Daniel Smith
- Web page: https://patentgrep.com/patent/US10156026B2

## CPC

- C30B 30/06: using mechanical vibrations
- C30B 7/10: by application of pressure, e.g. hydrothermal processes
- C30B 9/00: Single-crystal growth from melt solutions using molten solvents (by normal or gradient freezing C30B11/00; by zone-melting C30B13/00; by crystal pulling C30B15/00; on immersed seed crystal C30B17/00; by liquid phase epitaxial growth C30B19/00; under a protective fluid C30B27/00)
- C30B 9/10: Metal solvents
- C30B 29/18: Quartz
- C30B 29/20: Aluminium oxides
- C30B 29/22: Complex oxides
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR

## Abstract

The purpose of diffusion assisted crystal hydrothermal growth is to facilitate a greatly increased crystal growth rate that would save time that is precious in such a material and manpower costly process. The assisted crystal growth itself requires the utilization of a piezoelectric shaker connected to the autoclave in which most industrial hydrothermal crystals are grown. The waveform can be modulated to induce transport of nutrient in a singular direction, customized to the topology of the apparatus. As it stands currently, the growth of most crystals that require autoclaves for their production can take anywhere from 3 months to up to 2 years, and accordingly carries many costs, particularly electricity and supervision of the autoclave(s), and other issues that may arise during the growth. While the product of this labor results in high-quality crystals, in reality, these are not at all what is needed outside of the laboratory environment. Using the assisted crystal hydrothermal growth process, average crystal growth can be cut in half, with the resulting crystals consequently being of a slightly lower quality, though still sufficient for most engineering purposes. Another advantage of using a piezoelectric shaker is that an additional sensor can be added to the autoclave to monitor the health of the autoclave using trending data obtained during the growth.

## Claims

### Claim 1

A method of accelerating crystal growth in a hydrothermal autoclave by mechanically improving diffusion in a process of transporting nutrient to seeds, comprising:
A piezoelectric shaker attached to the head of a high-pressure hydrothermal autoclave,
applying a signal to said piezoelectric shaker, enough to produce mechanical movement inside the autoclave controlling the signal applied to said piezoelectric shaker,
monitoring a signal coming from the piezoelectric shaker wherein at least one sensor, including an accelerometer or an acoustic microphone is attached to said hydrothermal autoclave.

### Claim 2 (depends on 1)

The method as defined in claim 1, in which trending data is taken from the at least one sensor, related to the health of the autoclave.

### Claim 3 (depends on 1)

The method as defined in claim 1, in which trending data is taken from the at least one sensor, related to the growth rate of the crystals.

### Claim 4 (depends on 1)

The method as defined in claim 1, in which piezoelectric crystals including Gallium Orthophosphate, Berlinite, Gallium Arsenate, or Quartz homeotypes are grown.

### Claim 5 (depends on 1)

The method as defined in claim 1, in which the flux method is utilized to grow piezoelectric crystals including Gallium Orthophosphate, Berlinite, Gallium Arsenate, or Quartz homeotypes.

### Claim 6 (depends on 5)

The method as defined in claim 5, such that the quality of the piezoelectric crystals are optimized by fewer number of impurities found in the grown piezoelectric crystals by the lack of deterioration of the autoclave which is monitored during the growth by the use of the at least one sensor.
