IP Library Granted Patent US 11,473,183
Granted Patent B2
US 11,473,183 · App. 16/832,253 · Granted Oct 18, 2022

Enhanced activation of self-passivating metals

Inventors: Peter C. Williams (Cleveland Heights, OH); Steven V. Marx (University Heights, OH); Frank Ernst (Cleveland Heights, OH); Anna V. Agaponova (Beachwood, OH)
Assignee: SWAGELOK COMPANY
C23C8/02C23C8/26C23C8/32
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Quick Facts
Patent No.
US 11,473,183
App. No.
16/832,253
Granted
Oct 18, 2022
Kind
B2
Abstract

A workpiece made from a self passivating metal and having one or more surface regions defining a Beilby layer as a result of a previous metal shaping operation is activated for subsequent low temperature gas hardening by exposing the workpiece to the vapors produced by heating an oxygen-free nitrogen halide salt.

Claims (52)

1. A process comprising:

heating an oxygen-free nitrogen halide salt to produce vapors;

exposing to the vapors a workpiece made from a self-passivating metal and having a Beilby layer on at least a portion of a surface of the workpiece so that:

a temperature of the exposing is below a temperature at which nitride and/or carbide precipitates form in the workpiece;

the exposing activates the workpiece for nitriding or nitrocarburizing; and nitriding or nitrocarburizing the workpiece while the workpiece is activated.

2. The process of claim 1 , wherein the oxygen-free nitrogen halide salt is an ionic compound that:

(1) comprises a halide anion;

(2) has a room temperature solubility in water of at least 5 moles/liter;

(3) comprises nitrogen;

(4) is substantially free of oxygen; and

(5) vaporizes when heated to a temperature of 350° C. at atmospheric pressure.

3. The process of claim 1 , wherein the nitriding or nitrocarburizing utilizes gas derived exclusively from the oxygen-free nitrogen halide salt.

4. The process of claim 1 , wherein the nitriding or nitrocarburizing comprises contacting the workpiece with a gas derived from a nitrogen containing compound different than the oxygen-free nitrogen halide salt.

5. The process of claim 4 , wherein the contacting the workpiece with the gas derived from the nitrogen containing compound occurs during the activation.

6. The process of claim 4 , wherein the contacting the workpiece with the gas derived from the nitrogen containing compound occurs as the activation begins.

7. The process of claim 4 , wherein the exposing occurs simultaneously with the contacting the workpiece with the gas derived from the nitrogen containing compound.

8. The process of claim 4 , wherein the contacting the workpiece with the gas derived from the nitrogen containing compound occurs after the exposing.

9. The process of claim 4 , wherein the nitrogen containing compound comprises:

one or more compounds comprising:

an N/C compound,

at least one nitrogen to carbon bond,

at least four carbon atoms, and

the one or more compounds are solid or liquid at 25° C. and under a pressure of 1 atmosphere.

10. The process of claim 9 , wherein the one or more compounds comprise at least one of urea, acetamide and formamide.

11. The process of claim 1 , wherein the nitriding or nitrocarburizing further comprises:

contacting the workpiece with an additional gas different from the vapors, the additional gas comprising at least one of:

nitrogen derived from the decomposition of a compound during the nitriding or nitrocarburizing;

carbon derived from the decomposition of a compound during the nitriding or nitrocarburizing; and

nitrogen and carbon derived from the decomposition of a compound during the nitriding or nitrocarburizing.

12. The process of claim 11 , wherein the additional gas comprises vapors from the decomposition of an N/C compound.

13. The process of claim 1 , wherein the exposing occurs for at least about 15 minutes.

14. The process of claim 13 , wherein the exposing occurs for at least about 30 minutes.

15. The process of claim 1 , wherein the oxygen-free nitrogen halide salt is a particulate solid and wherein the exposing further comprises:

encapsulating the workpiece with the particulate solid; and

heating the workpiece to a temperature high enough to vaporize the particulate solid.

16. The process of claim 1 , wherein the oxygen-free nitrogen halide salt comprises at least one of ammonium chloride, ammonium fluoride, guanidinium chloride, guanidinium fluoride, pyridinium chloride, and pyridinium fluoride.

17. The process of claim 16 , wherein the oxygen-free nitrogen halide salt comprises at least one of ammonium chloride and guanidinium chloride.

18. The process of claim 1 , wherein the self-passivating metal is a stainless steel.

19. The process of claim 1 , wherein the self-passivating metal is one of:

10 to 40 wt. % Ni and 10 to 35 wt. % Cr;

a nickel-based, cobalt-based or manganese-based alloy containing 10 wt. % or more chromium; and

a titanium-based alloy.

20. The process of claim 1 , wherein the self-passivating metal is a titanium-based alloy.

21. The process of claim 1 , wherein the nitriding or nitrocarburizing comprises:

a first nitriding or nitrocarburizing step during the exposing; and

a second nitriding or nitrocarburizing step after the exposing.

22. A process comprising:

heating an oxygen-free nitrogen halide salt to produce vapors;

exposing to the vapors a workpiece made from a self-passivating metal and having a Beilby layer on at least a portion of a surface of the workpiece so that:

a temperature of the exposing is below a temperature at which nitride and/or carbide precipitates form in the workpiece;

the exposing activates the workpiece for nitriding or nitrocarburizing; and

nitriding or nitrocarburizing the workpiece concurrently with the activating.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 8, 2020
From: WILLIAMS, PETER C.; MARX, STEVEN V.
To: SWAGELOK COMPANY
Reel/Frame 052338/0898 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 8, 2020
From: ERNST, FRANK; AGAPONOVA, ANNA
To: CASE WESTERN RESERVE UNIVERSITY
Reel/Frame 052338/0902 →
Continuity (4)
Continuation 16200067 · Nov 26, 2018
Continuation 14813290 · Jul 30, 2015
Provisional Application 62031338 · Jul 31, 2014
Related Publication 20200283882A1 · Sep 10, 2020
Cited By (2)
US 12,371,774 US 12,435,406