IP Library Granted Patent US 9,988,316
Granted Patent B2
US 9,988,316 · App. 14/612,482 · Granted Jun 5, 2018

Protective internal coatings for porous substrates

Inventors: Sankar Sambasivan (Chicago, IL); Vikram Sharad Kaul (Atlanta, GA); Francis Richard Chapman (Mount Prospect, IL)
Assignee: Applied Thin Films, Inc.
C04B38/0096C04B35/195C04B38/0054C04B41/009C04B41/5092C04B41/85C23C18/125C23C18/1216C23C18/1229F01D5/288C04B2235/3206C04B2235/3208F05D2300/514F05D2300/6033Y02T50/672Y10T428/24997Y10T428/249921Y10T428/249967Y10T428/249969Y10T428/249978Y10T428/268
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Quick Facts
Patent No.
US 9,988,316
App. No.
14/612,482
Granted
Jun 5, 2018
Kind
B2
Abstract

A material contains open pores in which the channels and pores that are internally coated with at least one layer of phosphorus-containing alumina. Such material is formed by infiltrating a porous material one or more times with a non-colloidal, low-viscosity liquid coating precursor, drying, and curing the coating precursor to form a phosphorus-containing alumina layer within pores of the material.

Claims (36)

1. A method of conformally coating pore walls of a porous inorganic substrate comprising:

providing a porous inorganic substrate;

forming a liquid film having a thickness of 5 to 250 nm on pore walls of the porous inorganic substrate, wherein the liquid film consists of a non-colloidal solution of a phospho-alumina precursor having an aluminum-to-phosphorous atomic ratio of 0.5:1 to 15:1;

drying the liquid film to yield a dried film; and then

curing the dried film to form a phosphorus-containing alumina sublayer having a thickness of 1 to 50 nm conformally coating the pore walls of the porous inorganic substrate;

and

wherein the conformally coated porous inorganic substrate has an open porosity that is at least 50% of an open porosity of the provided porous inorganic substrate.

2. The method of claim 1 , wherein the liquid film comprises a non-colloidal solution of a phospho-alumina precursor carried in an alcohol solvent selected from the group consisting of methanol, ethanol, n-propanol, i-propanol, n-butanol, 2-butanol, t-butanol, and a mixture thereof.

3. The method of claim 1 , further comprising providing the non-colloidal solution by admixing an aluminum salt solution and a phosphate ester solution, wherein the phospho-alumina precursor has a Al:P ratio of 4:1 to 15:1.

4. The method of claim 1 , wherein the porous inorganic substrate carrying the conformal coating has a higher flexural mechanical strength than the same porous inorganic substrate without the conformal coating.

5. The method of claim 1 , wherein the porous inorganic substrate is a ceramic thermal barrier coating.

6. The method of claim 1 , wherein the porous inorganic substrate is a ceramic coating produced by an electron beam physical vapor deposition process.

7. The method of claim 1 , wherein the porous inorganic substrate is a ceramic coating produced by a plasma spray process.

8. The method of claim 1 , wherein the phosphorus-containing alumina sublayer has an aluminum-to-phosphorous atomic ratio of less than about 10.

9. The method of claim 1 , wherein the phospho-alumina precursor has an aluminum-to-phosphorous atomic ratio of 4:1 to 15:1.

10. The method of claim 9 , wherein the phosphorus-containing alumina sublayer has an aluminum-to-phosphorous atomic ratio less than 12:1.

11. The method of claim 1 , wherein the phosphorus-containing alumina sublayer has an aluminum-to-phosphorous atomic ratio less than 12:1.

12. The method of claim 1 , wherein the provided porous inorganic substrate includes mesopores that constitute 25% to 99.99% of a measured porosity.

13. A method of conformally coating pore walls of a porous inorganic substrate comprising:

providing a porous inorganic substrate;

a plurality of coating steps which provide a conformal coating consisting of two to five phosphorus-containing alumina sublayers carried on the pore walls of the provided porous inorganic substrate, the coating steps include

first forming a liquid film having a thickness of 5 to 250 nm on the pore walls of the provided porous inorganic substrate, wherein the liquid film comprises a non-colloidal solution of a phospho-alumina precursor having an Al:P ratio of 0.5:1 to 15:1; drying the liquid film; and then curing the dried film to provide a first phosphorus-containing alumina sublayer, where the phosphorus-containing alumina sublayer has a thickness of 1 to 50 nm; then

forming a liquid film having a thickness of 5 to 250 nm on the first phosphorus-containing alumina sublayer, wherein the liquid film comprises a non-colloidal solution of a phospho-alumina precursor having an Al:P ratio of 0.5:1 to 15:1; drying the liquid film; and then curing the dried film to provide a second phosphorous-containing alumina sublayer having a thickness of 1 to 50 nm;

wherein the conformally coated porous inorganic substrate has a remaining open porosity of at least 50% and a remaining volumetric porosity of at least 90%;

wherein each phosphorus-containing alumina sublayer has an aluminum-to-phosphorous ratio of less than 12:1.

14. The method of claim 13 , wherein the porous inorganic substrate is a ceramic thermal barrier coating on a gas turbine engine component.

15. The method of claim 13 , wherein the conformally coated porous inorganic substrate resists sintering and promotes retention of an original pore structure when exposed to temperatures which promote pore deterioration and/or sintering of the provided porous inorganic substrate.

16. The method of claim 13 , wherein the first phosphorus-containing alumina sublayer and the second phosphorus-containing alumina sublayer have different Al/P ratios.

17. The method of claim 13 , wherein the provided porous inorganic substrate includes mesopores that constitute 25% to 99.99% of a measured porosity.

18. A method comprising:

providing a porous inorganic substrate;

forming a liquid film having a thickness of 5 to 250 nm on pore walls of the provided porous inorganic substrate, wherein the liquid film is a non-colloidal solution of a phospho-alumina precursor having an aluminum-to-phosphorous atomic ratio of 4:1 to 15:1;

drying the liquid film to yield a dried film; and then

forming a cured phosphorus-containing alumina layer, with a thickness of 1 to 50 nm, conformally coating the pore walls;

the coated substrate having an open porosity that is at least 90% of an open porosity of the provided porous inorganic substrate.

19. The method of claim 18 , wherein the provided porous inorganic substrate includes mesopores that constitute 25% to 99.99% of a measured porosity.

Assignments (5)
NUNC PRO TUNC ASSIGNMENT Recorded Nov 4, 2020
From: SAMBASIVAN, SANKAR; KAUL, VIKRAM S.; CHAPMAN, FRANCIS R.
To: APPLIED THIN FILMS, INC.
Reel/Frame 054300/0202 →
CONFIRMATORY LICENSE Recorded Dec 12, 2016
From: APPLIED-THIN-ELLMS, INC.
To: NAVY, DEPARTMENT OF THE
Reel/Frame 040941/0818 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 3, 2015
From: SAMBASIVAN, SANKAR
To: APPLIED THIN FILMS, INC.
Reel/Frame 034874/0530 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 3, 2015
From: KAUL, VIKRAM SHARAD
To: APPLIED THIN FILMS, INC.
Reel/Frame 034874/0571 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 3, 2015
From: CHAPMAN, FRANCIS RICHARD
To: APPLIED THIN FILMS, INC.
Reel/Frame 034874/0587 →
Continuity (2)
Continuation 13608773 · Sep 10, 2012
Related Publication 20150147562A1 · May 28, 2015