# US 2020/0399754 A1 · Solid precursor feed system for thin film depositions

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- Number: US 2020/0399754 A1
- Document ID: US20200399754A1
- Status: Published application
- Kind: A1
- Application number: 16/756,463
- Filed: 2019-12-21
- Published: 2020-12-24
- Earliest claimed: 2019-03-13
- Assignees: Metal Oxide Technologies, Inc.
- Applicants: Metal Oxide Technologies, LLC
- Inventors: Mikhail NOVOZHILOV; Alex IGNATIEV
- Web page: https://patentgrep.com/patent/US20200399754A1

## CPC

- B01D 1/0017: {Use of electrical or wave energy (B01D1/0029 takes precedence)}
- C23C 16/18: from metallo-organic compounds
- B01D 3/346: {the gas being used for removing vapours, e.g. transport gas}
- C23C 16/40: Oxides
- C23C 16/448: characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C 16/4485: {by evaporation without using carrier gas in contact with the source material (C23C16/4486 takes precedence)}
- C23C 16/45561: {Gas plumbing upstream of the reaction chamber}
- C23C 16/482: {using incoherent light, UV to IR, e.g. lamps}
- C23C 16/52: Controlling or regulating the coating process {(C23C16/45557, C23C16/279 take precedence)}
- C23C 16/54: Apparatus specially adapted for continuous coating
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)

## Abstract

A dry powder MOCVD vapor source system is disclosed that utilizes a gravimetric powder feeder, a feed rate measurement and feeder control system, an evaporator and a load lock system for continuous operation for thin film production, particularly of REBCO type high temperature superconductor (HTS) tapes.

## Claims

### Claim 1

A precursor feed system for deposition of thin films, the system comprising:
a powder feeder assembly comprising a feed screw device and a powder vessel for housing a precursor powder;
a load lock assembly comprising a pressure isolated chamber for reloading the powder feeder assembly powder vessel;
a weighing mechanism coupled to the powder vessel and configured to provide continuous mass data of precursor powder in the powder vessel;
a control system comprising a PID loop and a data processor; and
an evaporator configured to receive the precursor powder from the powder feeder assembly and evaporate the powder,
wherein the control system data processor further comprises an algorithm configured to convert the continuous mass data from the weighing mechanism to a feed screw rate to deliver a target precursor powder feed rate to the evaporator.

### Claim 2 (depends on 1)

The feed system of claim 1, wherein the powder precursor is comprised of more than one thin film component.

### Claim 3 (depends on 1)

The feed system of claim 1, wherein the load lock assembly further comprises a plurality of valves to isolate the assembly for addition of powder precursor while the feed system operates continuously.

### Claim 4 (depends on 1)

The feed system of claim 1, further comprising an agitator device to aid in powder mixing and distribution.

### Claim 5 (depends on 1)

The feed system of claim 1, wherein the evaporator further comprises an outlet screen.

### Claim 6

A precursor feed system for deposition of thin films, the system comprising:
a powder feeder assembly comprising a feed screw device and a powder vessel for housing a precursor powder;
a load lock assembly comprising a pressure isolated chamber for reloading the powder feeder assembly powder vessel;
a control system comprising a PID loop and a data processor;
a process variable input receivable by the control system; and
an evaporator configured to receive the precursor powder from the powder feeder assembly and evaporate the powder,
wherein the control system data processor further comprises an algorithm configured to convert the process variable input to a feed screw rate to deliver a target precursor powder feed rate to the evaporator.

### Claim 7 (depends on 6)

The feed system of claim 6, wherein the process variable input is the precursor powder mass.

### Claim 8 (depends on 6)

The feed system of claim 6, wherein the process variable input is a mass flow rate of precursor vapor exiting the evaporator.

### Claim 9 (depends on 6)

The feed system of claim 6, wherein the process variable input is a thin film layer thickness.

### Claim 10 (depends on 6)

The feed system of claim 6, wherein the process variable input is a mass flow of precursor vapor.

### Claim 11 (depends on 6)

The feed system of claim 6, wherein the process variable input is a composition of the precursor vapor or thin film.

### Claim 12

A method for manufacturing a high temperature superconductor, the method comprising:
introducing a substrate to a reactor;
providing an evaporator operatively coupled to a precursor powder feed assembly comprising a screw feed device and a precursor powder vessel coupled to a weighing mechanism;
loading a precursor powder to a load lock assembly configured to supply precursor powder to the precursor powder feed assembly, wherein the precursor powder is comprised of at least one component of a high temperature thin film superconductor;
monitoring the precursor powder vessel weight;
controlling the feed screw rate based upon the powder vessel weight in order to provide a target precursor powder feed rate to the evaporator;
evaporating the precursor powder in the evaporator;
transporting the evaporated precursor into the reactor; and
depositing the thin film upon the substrate in the reactor.

### Claim 13 (depends on 12)

The method of claim 12, wherein the load lock assembly further comprises a plurality of valves to isolate the assembly for addition of powder precursor while the feed system operates continuously.

### Claim 14 (depends on 12)

The method of claim 12, wherein the powder precursor is comprised of more than one thin film component.

### Claim 15 (depends on 12)

The method of claim 12, wherein the thin film is a superconductor layer.

### Claim 16 (depends on 15)

The method of claim 15, wherein the thin film is a superconductor layer with non-superconducting defects for enhanced flux pinning.

### Claim 17 (depends on 12)

The method of claim 12, wherein the reactor is a Photo-Assisted Metal Organic Chemical Vapor Deposition (PAMOCVD) reactor.

### Claim 18 (depends on 12)

The method of claim 12, wherein the deposited thin film has a growth rate of 1.0 μm/min or greater.

### Claim 19 (depends on 15)

The method of claim 15, wherein the superconductor layer further comprises a lift factor at 4K, 20 T (Ic (4K, 20 T)/Ic (77K, self-field)) of 2 or greater.

### Claim 20 (depends on 19)

The method of claim 19, wherein the lift factor is 3 or greater.