IP Library Granted Patent US 10,072,335
Granted Patent B2
US 10,072,335 · App. 14/839,664 · Granted Sep 11, 2018

Method of coating of object

Inventors: Amy Elizabeth Marquardt (Washington, DC); Eric Breitung (Washington, DC); Raymond J. Phaneuf (College Park, MD); Glenn Gates (Baltimore, MD); Terry Weisser (Baltimore, MD)
Assignees: University of Maryland, College Park; Trustees of the Walters Art Gallery, Inc.
C23C16/45555C23C16/402C23C16/403C23C16/405C23C16/407C23C16/45553
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Quick Facts
Patent No.
US 10,072,335
App. No.
14/839,664
Granted
Sep 11, 2018
Kind
B2
Abstract

A method of coating a metallic object with a substantially invisible protective coating, wherein the coating comprises a first layer, a second layer, and a third layer, each layer comprising a metal oxide or a nitride. The method comprises placing the object in an atomic layer deposition (ALD) reactor; depositing a first layer comprising a metal oxide or a nitride on a surface of the object by ALD; depositing a second layer comprising a metal oxide or a nitride on the first layer by ALD; and depositing a third layer comprising a metal oxide or a nitride on the second layer by ALD, thereby forming the protective coating on the object.

Claims (32)

1. A method of coating a metallic object with a nearly invisible protective coating, comprising:

placing the metallic object in an atomic layer deposition (ALD) reactor;

depositing a first layer comprising a metal oxide or a nitride on a surface of the metallic object by ALD;

depositing a second layer comprising a metal oxide or a nitride on the first layer by ALD; and

depositing a third layer comprising a metal oxide or a nitride on the second layer by ALD, thereby forming the nearly invisible protective coating on the metallic object,

wherein the nearly invisible protective coating has a Delta E 2000 of 5 or less.

2. The method of claim 1 , wherein depositing the first, second, and third layers each comprises repeatedly pulsing a precursor material and purging the reactor with an inert gas following each pulse.

3. The method of claim 2 ,

wherein depositing the first layer comprises repeatedly pulsing the precursor and purging with the inert gas until the first layer is about 1 to 100 nm thick;

wherein depositing the second layer comprises repeatedly pulsing the precursor and purging with the inert gas until the second layer is about 1 to 100 nm thick; and

wherein depositing the third layer comprises repeatedly pulsing the precursor and purging with the inert gas until the third layer is about 1 to 100 nm thick.

4. The method of claim 2 , wherein precursor material corresponds to a deposited material selected from the group consisting of Al 2 O 3 , FeO, HfO 2 , MgO, SiO 2 , SnO 2 , Ta, Ta 2 O 5 , TiN, TiO 2 , VO 2 , ZnO, and ZrO.

5. The method of claim 2 , wherein the precursor material is selected from the group consisting of trimethylaluminum, diethyl zinc, tetrakis-dimethyl-amido titanium, and 3-aminopropyltriethoxysilane.

6. The method of claim 2 ,

wherein depositing the first layer comprises repeatedly pulsing trimethylaluminum;

wherein depositing the second layer comprises repeatedly pulsing tetrakis-dimethyl-amido titanium or 3-aminopropyltriethoxysilane; and

wherein depositing the third layer comprises repeatedly pulsing diethyl zinc or trimethylaluminum.

7. The method of claim 6 , further comprising depositing a fourth layer on the third layer by ALD by repeatedly pulsing tetrakis-dimethyl-amido or trimethylaluminum.

8. The method of claim 6 ,

wherein depositing the first layer comprises repeatedly pulsing the trimethylaluminum until the first layer is about 20 to 50 nm thick;

wherein depositing the second layer comprises repeatedly pulsing the tetrakis-dimethyl-amido titanium or 3-aminopropyltriethoxysilane until the second layer is about 20 to 50 nm thick; and

wherein depositing the third layer comprises repeatedly pulsing the diethyl zinc or trimethylaluminum until the third layer is about 1 to 10 nm thick.

9. The method of claim 1 , further comprising depositing a gradient layer on the first layer by ALD prior to depositing the second layer, wherein depositing the gradient layer comprising pulsing a precursor used to form the first layer and a precursor used to form the second layer.

10. The method of claim 1 , wherein depositing at least one of the first, second, and third layers further comprise pulsing a precursor corresponding to a dopant selected from the group consisting of Ag, Au, Fe, Ir, Os, Pd, Pt, Rh, Ru, FeO, HfO 2 , MgO, SiO 2 , SnO 2 , Ta, Ta 2 O 5 , TiN, TiO 2 , VO 2 , ZnO, and ZrO.

11. The method of claim 1 , wherein the surface comprises sterling silver.

12. The method of claim 1 , wherein the nearly invisible protective coating has a Delta E 2000 of 4 or less.

13. The method of claim 1 , wherein the nearly invisible protective coating has a Delta E 2000 of 3 or less.

14. The method of claim 1 , wherein the nearly invisible protective coating has a Delta E 2000 of 2 or less.

15. The method of claim 1 , wherein the nearly invisible protective coating has a Delta E 2000 of 1.

16. The method of claim 1 , wherein the first layer comprises Al 2 O 3 .

17. The method of claim 16 , wherein the second layer comprises TiO 2 .

18. The method of claim 16 , wherein the third layer comprises ZnO.

Assignments (4)
CONFIRMATORY LICENSE Recorded May 4, 2022
From: UNIVERSITY OF MARYLAND COLLEGE PARK CAMPUS
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 059851/0891 →
CONFIRMATORY LICENSE Recorded Sep 16, 2020
From: UNIVERSITY OF MARYLAND, COLLEGE PARK
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 053797/0011 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 21, 2019
From: GATES, GLENN; WEISSER, TERRY
To: TRUSTEES OF THE WALTERS ART GALLERY, INC.
Reel/Frame 049558/0970 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 19, 2016
From: MARQUARDT, AMY ELIZABETH, MS.; BREITUNG, ERIC, DR.; PHANEUF, RAYMOND J., DR
To: UNIVERSITY OF MARYLAND, COLLEGE PARK
Reel/Frame 038652/0278 →
Continuity (2)
Provisional Application 62043691 · Aug 29, 2014
Related Publication 20160060758A1 · Mar 3, 2016