IP Library Granted Patent US 11,274,374
Granted Patent B2
US 11,274,374 · App. 16/438,077 · Granted Mar 15, 2022

Metal deposits, compositions, and methods for making the same

Inventors: Daniel A. Konopka (Denver, CO); Li Hsien Chou (Aurora, CO)
Assignee: Iontra LLC
C25D3/20C25D3/10C25D3/12C25D3/22C25D3/26C25D3/32C25D3/38C25D3/58C25D3/665
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Quick Facts
Patent No.
US 11,274,374
App. No.
16/438,077
Granted
Mar 15, 2022
Kind
B2
Abstract

Provided herein is a composition for forming a metal deposit on a substrate. The composition consists essentially of a carboxamide, trialkylamine chloride, and a metal salt. The carboxamide comprises Formula (I). The trialkylamine chloride and the carboxamide are in molar ratio between 1:1 and 1:30 to form an ionic liquid. The trialkylamine chloride is trimethylamine chloride (TMACl), triethylamine chloride (TEACl), triethanolamine chloride, or combinations thereof. The metal salt has the formula MX y , wherein M is a metal, X is a halide, and y is an oxidation number of M, the metal salt being in a concentration between about 0.2 and about 1.5 moles per liter of the ionic liquid. The metal deposit has an average grain size between about 0.2 μm and about 3 μm and contains less than about 1 mol % of each oxygen, carbon, and chlorine.

Claims (38)

1. A method of forming a metal deposit on a substrate, the method comprising:

forming a metal deposit on a substrate from an electrolyte composition, the electrolyte composition comprising a carboxamide, a trialkylamine hydrochloride, and a metal salt;

the metal deposit being formed on the substrate by inducing a potential between the metal salt and the substrate through the electrolyte composition to cause a metal-metal bond to form between the metal salt and the substrate;

the carboxamide comprising Formula (I):

wherein n is 1 to 6;

each Q is O;

R 1 is independently chosen from H or alkyl, and R 3 is NR 4 R 5 ; or R 1 and R 3 are taken together to form a ring; and

each R 2 , R 4 , and R 5 is independently chosen from H or alkyl;

the trialkylamine hydrochloride being selected from the group consisting of trimethylamine hydrochloride (TMA-HCl), triethylamine hydrochloride (TEA-HCl), triethanolamine hydrochloride, and combinations thereof; and

the metal salt having a formula MX y , wherein M is a metal, X is a halide, and y is an oxidation number of M;

wherein the trialkylamine hydrochloride and the carboxamide are present in the electrolyte composition in molar ratio between 1:3 and 1:30 to form an ionic liquid, and the metal salt is present in the electrolyte composition in a concentration between 0.2 and 1.5 moles per liter of the ionic liquid; and

wherein the metal deposit is formed on the substrate from the electrolyte composition such that the metal deposit has an average grain size between 0.2 μm and 3 μm and contains less than 1 mol % of each oxygen, carbon, and chlorine.

2. The method of claim 1 , wherein the carboxamide of Formula (I) comprises a compound of Formula (II):

wherein n is 1 to 6;

R 1 , R 4 , and R 5 are independently chosen from H or alkyl; and

each R 2 is chosen from H or alkyl.

3. The method of claim 2 , wherein the carboxamide of Formula (II) comprises a compound of Formula (III):

wherein n is 1 to 6.

4. The method of claim 1 , wherein the carboxamide of Formula (I) comprises a compound of Formula (IV):

n is 2 to 6;

each Q is O; and

each R 2 , R 4 , and R 5 is independently chosen from H or alkyl.

5. The method of claim 4 , wherein the carboxamide of Formula (IV) comprises a compound of Formula (V):

each Q is O; and

each R 2 , R 4 , and R 5 is independently chosen from H or alkyl.

6. The method of claim 1 , wherein the carboxamide of Formula (I) is selected from the group consisting of urea, biuret, triuret, tetrauret, pentauret, hexauret, cyanuric acid, ammelide, ammeline, and combinations thereof.

7. The method of claim 6 , wherein the carboxamide is urea or biuret.

8. The method of claim 1 , wherein the trialkylamine hydrochloride and the carboxamide are in molar ratio of 1:5.

9. The method of claim 1 , wherein the trialkylamine hydrochloride and the carboxamide are in molar ratio of 1:10.

10. The method of claim 1 , wherein the concentration of metal salt is 0.3 moles per liter of the ionic liquid.

11. The method of claim 1 , wherein M is Fe.

12. The method of claim 1 , wherein X is Cl.

13. The method of claim 1 , wherein y is 3.

14. The method of claim 1 , wherein the metal deposit is an iron deposit.

15. The method of claim 1 , wherein M is Fe, X is Cl, and y is 3, and the metal deposit is an iron deposit.

16. The method of claim 1 , wherein the potential has a current density between 10 mA/cm 3 and 300 mA/cm 3 .

17. The method of claim 1 , wherein the potential has a reducing potential of between −0.6 V and −2.2 V.

18. The method of claim 1 , wherein the concentration of metal salt is 0.3 moles per liter of the ionic liquid.

Assignments (3)
CHANGE OF NAME Recorded Mar 6, 2023
From: IONTRA LLC
To: IONTRA INC
Reel/Frame 062959/0669 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 30, 2019
From: KONOPKA, DANIEL A.; CHOU, LI HSIEN
To: ALLIGANT SCIENTIFIC, LLC
Reel/Frame 050868/0744 →
CHANGE OF NAME Recorded Oct 30, 2019
From: ALLIGANT SCIENTIFIC, LLC
To: IONTRA LLC
Reel/Frame 050868/0804 →
Continuity (2)
Division 15293096 · Oct 13, 2016
Related Publication 20190301039A1 · Oct 3, 2019