# US 12,006,567 B2 · Plasma spray physical vapor deposition deposited in multilayer, multi-microstructure environmental barrier coating

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- Number: US 12,006,567 B2
- Document ID: US12006567B2
- Status: Granted
- Kind: B2
- Application number: 17/167,662
- Filed: 2021-02-04
- Published: 2021-12-30
- Granted: 2024-06-11
- Earliest claimed: 2016-01-29
- Assignees: ROLLS-ROYCE plc
- Applicants: Rolls-Royce Corporation
- Inventors: Kang N. Lee; Matthew R. Gold
- Web page: https://patentgrep.com/patent/US12006567B2

## CPC

- C23C 14/32: by explosion; by evaporation and subsequent ionisation of the vapours {, e.g. ion-plating}(C23C14/34 - C23C14/48 take precedence)
- C04B 41/009: {characterised by the material treated}
- C04B 41/4527: {Plasma spraying (deposition from the gas phase using plasma C04B41/4533)}
- C04B 41/52: Multiple coating or impregnating {multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation}
- C04B 41/89: for obtaining at least two superposed coatings having different compositions
- C23C 4/02: Pretreatment of the material to be coated, e.g. for coating on selected surface areas
- C23C 4/11: Oxides
- C23C 4/134: Plasma spraying
- C23C 14/083: {of refractory metals or yttrium}
- C23C 14/10: Glass or silica
- C23C 14/548: {Controlling the composition}
- F01D 5/28: Selecting particular materials; {Particular measures relating thereto;} Measures against erosion or corrosion
- F01D 5/282: {Selecting composite materials, e.g. blades with reinforcing filaments}
- F01D 5/284: {Selection of ceramic materials}
- F01D 5/288: {Protective coatings for blades}
- H01J 37/32458: {Vessel}
- B32B 18/00: Layered products essentially comprising ceramics, e.g. refractory products
- F05D 2300/21: Oxide ceramics
- F05D 2300/6033: Ceramic matrix composites [CMC]
- 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)
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- F01D: NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES (machines or engines for liquids F03; non-positive displacement pumps F04D)
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- F05D: INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS

## Abstract

An article may include a substrate defining at least one at least partially obstructed surface. The substrate includes at least one of a ceramic or a ceramic matrix composite. The article also may include a multilayer, multi-microstructure environmental barrier coating on the at least partially obstructed substrate. The multilayer, multi-microstructure environmental barrier coating includes a first layer comprising a rare earth disilicate and a substantially dense microstructure; and a second layer on the first layer. The second layer includes a columnar microstructure and at least one of a rare earth monosilicate or a thermal barrier coating composition comprising a base oxide comprising zirconia or hafnia; a primary dopant comprising ytterbia; a first co-dopant comprising samaria; and a second co-dopant comprising at least one of lutetia, scandia, ceria, gadolinia, neodymia, or europia.

## Claims

### Claim 1

A method comprising:
controlling, by a computing device, a vacuum pump to evacuate a vacuum chamber to high vacuum;
controlling, by the computing device, a coating material source to provide a first coating material to a plasma spray device at a first feed rate, the first coating material having a composition selected so that a first layer from the first coating material comprises a rare earth disilicate, between about 0.1 wt. % and about 3 wt. % alumina, and a microstructure having less than about 10 vol. % porosity, and the first feed rate being selected to result in a substantially dense microstructure for the first layer;
controlling, by the computing device, the plasma spray device to deposit the first layer on a substrate in the vacuum chamber using plasma spray physical vapor deposition, wherein the first layer comprises the rare earth disilicate, between about 0.1 wt. % and about 3 wt. % alumina, and the microstructure having less than about 10 vol. % porosity;
controlling, by the computing device, the coating material source to provide a second coating material to the plasma spray device at a second feed rate, the second coating material having a composition selected so that a second layer formed on the first layer from the second coating material comprises a rare earth monosilicate or a thermal barrier coating composition comprising a base oxide comprising zirconia or hafnia; a primary dopant comprising ytterbia; a first co-dopant comprising samaria; and a second co-dopant comprising at least one of lutetia, scandia, ceria, gadolinia, neodymia, or europia; and
controlling, by the computing device, the plasma spray device to deposit the second layer on the first layer using plasma spray physical vapor deposition, wherein the second layer comprises the rare earth monosilicate or the thermal barrier coating composition comprising the base oxide comprising zirconia or hafnia; the primary dopant comprising ytterbia; the first co-dopant comprising samaria; and the second co-dopant comprising at least one of lutetia, scandia, ceria, gadolinia, neodymia, or europia.

### Claim 2 (depends on 1)

The method of claim 1, wherein the first coating material comprises excess silica compared to the rare earth disilicate.

### Claim 3 (depends on 1)

The method of claim 1, wherein at least one of the first coating material or the second coating material further comprises at least one of alumina, at least one alkali oxide, or at least one alkaline earth oxide.

### Claim 4 (depends on 1)

The method of claim 1, wherein the first layer and the second layer are deposited on at least one surface of the substrate that is not in a line-of-sight relationship with the plasma spray device.

### Claim 5 (depends on 1)

The method of claim 1, wherein:
the second layer comprises the thermal barrier coating composition comprising the base oxide comprising zirconia or hafnia; the primary dopant comprising ytterbia; the first co-dopant comprising samaria; and the second co-dopant comprising at least one of lutetia, scandia, ceria, gadolinia, neodymia, or europia; and
the second coating material comprises the base oxide comprising zirconia or hafnia; the primary dopant comprising ytterbia; the first co-dopant comprising samaria; and the second co-dopant comprising at least one of lutetia, scandia, ceria, gadolinia, neodymia, or europia.

### Claim 6 (depends on 1)

The method of claim 1, wherein the second layer comprises the rare earth monosilicate, and wherein the second coating material comprises excess silica compared to the rare earth monosilicate.

### Claim 7 (depends on 1)

The method of claim 1, further comprising:
controlling, by the computing device, the coating material source to provide a third coating material to the plasma spray device at a third feed rate, the third coating material having a composition selected so that a third layer formed on the second layer from the third coating material comprises the thermal barrier coating composition comprising the base oxide comprising zirconia or hafnia; the primary dopant comprising ytterbia; the first co-dopant comprising samaria; and the second co-dopant comprising at least one of lutetia, scandia, ceria, gadolinia, neodymia, or europia; and
controlling, by the computing device, the plasma spray device to deposit the third layer on the second layer using plasma spray physical vapor deposition, wherein the third layer comprises the thermal barrier coating composition comprising the base oxide comprising zirconia or hafnia; the primary dopant comprising ytterbia; the first co-dopant comprising samaria; and the second co-dopant comprising at least one of lutetia, scandia, ceria, gadolinia, neodymia, or europia.

### Claim 8 (depends on 7)

The method of claim 7, wherein:
the second coating material has a composition selected so that the second layer from the second coating material comprises the rare earth monosilicate, between about 0.1 wt. % and about 3 wt. % alumina, and a columnar microstructure.

### Claim 9 (depends on 1)

The method of claim 1, wherein the first coating material has a composition selected so that the first layer from the first coating material comprises the rare earth disilicate, between about 0.5 wt. % and about 3 wt. % alumina, and the microstructure having less than about 10 vol. % porosity.

### Claim 10 (depends on 1)

The method of claim 1, wherein the second coating material has a composition selected so that the second layer from the second coating material comprises the rare earth monosilicate, between about 0.1 wt. % and about 3 wt. % alumina, and a columnar microstructure.

### Claim 11 (depends on 1)

The method of claim 1, wherein the second coating material has a composition selected so that the second layer from the second coating material comprises the rare earth monosilicate, between about 0.5 wt. % and about 3 wt. % alumina, and a columnar microstructure.

### Claim 12 (depends on 1)

The method of claim 1, wherein the first coating material has a composition selected so that the first layer consists of the rare earth disilicate and alumina, and the microstructure having less than about 10 vol. % porosity.

### Claim 13 (depends on 1)

The method of claim 1, wherein the first coating material has a composition selected so that the first layer comprises the rare earth disilicate, between about 0.1 wt. % and about 3 wt. % alumina, and at least one alkali oxide or at least one alkaline earth oxide.

### Claim 14 (depends on 1)

The method of claim 1, wherein the second feed rate is selected to result in a columnar microstructure.