Composition for phosphate film optimizing mn content and a method for phosphate treatment of zn electric-plated steel sheet
US-2017356090-A1 · Dec 14, 2017 · US
US11542607B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11542607-B2 |
| Application number | US-201916437542-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jun 11, 2019 |
| Priority date | Jun 23, 2016 |
| Publication date | Jan 3, 2023 |
| Grant date | Jan 3, 2023 |
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A novel method of blackening surgical needles is disclosed. Surgical needles having outer surfaces are first placed into a first pretreatment bath having a novel composition. The needles are then placed into a second blackening bath having a novel composition for a sufficient period of time to effectively blacken the surfaces of the needles. The novel methods for blackening the surfaces of a stainless steel alloy surgical needle provide a chromium (VI)-free alternative to current needle manufacturing processes. Another unique feature of this novel method is its short processing time. The blackening processes of the present invention can be utilized for in-line treatment processes which can be easily incorporated into high speed needle manufacturing processes, such as strip mounted processes. In addition, the processes of the present invention are readily adaptable to batch processes. Also disclosed are novel systems for blackening surgical needles and novel blackening baths for surgical needles.
Opening claim text (preview).
We claim: 1. A method of blackening surgical needles, comprising the steps of: A. placing the surgical needle into a blackening bath, wherein the bath comprises: about 3 wt. % to about 20 wt. % of a highly soluble nitric acid salt; about 18 wt. % to about 38 wt. % of a strong base; about 50 wt. % to about 75 wt. % of water; about 0.2 wt. % to about 5 wt. % of a transition metal salt of a strong acid; about 0.2 wt. % to about 5 wt. % of a sulfur-containing reducer compound; and, B. maintaining the needle in the blackening bath for a sufficiently effective period of time to provide a blackened coating on an outer surface of the needle. 2. The method of claim 1 , wherein the transition metal salt is selected from the group consisting of nickel nitrate, cobalt nitrate, nickel sulfate, cobalt sulfate, iron nitrate, copper perchlorate, nickel perchlorate, ion perchlorate, and cobalt perchlorate. 3. The method of claim 1 , wherein the sulfur-containing reducer is selected from the group consisting of, N′-diethylthiourea, sodium thiocyanate, sodium sulfide, and sodium dimethyldithiocarbamate. 4. The method of claim 1 , wherein the highly soluble nitric acid salt is selected from the group consisting of sodium nitrate, potassium nitrate, and lithium nitrate. 5. The method of claim 1 , wherein the strong base is selected from the group consisting of sodium hydroxide, potassium hydroxide, and lithium hydroxide. 6. A method of blackening surgical needles, comprising the steps of: A. placing the surgical needle into a blackening bath, wherein the bath comprises: about 3 wt. % to about 20 wt. % of a highly soluble nitric acid salt; about 18 wt. % to about 38 wt. % of a strong base; about 50 wt. % to about 75 wt. % of water; about 0.2 wt. % to about 5 wt. % of a highly soluble permanganate salt; about 0.2 wt. % to about 5 wt. % of a thiocyanate salt; and, B. maintaining the needle in the blackening bath for a sufficiently effective period of time to provide a blackened coating on an outer surface of the needle. 7. The method of claim 6 , wherein the permanganate salt is selected from the group consisting of potassium permanganate, sodium permanganate, and lithium permanganate. 8. The method of claim 6 , wherein the blackening bath additionally comprises a water soluble chloride salt. 9. The method of claim 6 , wherein the thiocyanate salt is selected from the group consisting of sodium thiocyanate, potassium thiocyanate, and lithium thiocyanate. 10. The method of claim 6 , wherein the highly soluble nitric acid salt is selected from the group consisting of sodium nitrate, potassium nitrate, and lithium nitrate. 11. The method of claim 6 , wherein the strong base is selected from the group consisting of sodium hydroxide, potassium hydroxide, and lithium hydroxide. 12. The method of claim 6 , wherein the blackening bath additionally comprises about 0.2 wt. % to about 5 wt. % of a molybdate salt. 13. A system for blackening stainless steel alloy surgical needles, comprising: a blackening bath, the blackening bath comprising: about 3 wt. % to about 15 wt. % of a highly soluble nitric acid salt; about 18 wt. % to about 38 wt. % of a strong base; about 50 wt. % to about 75 wt. % of water; about 0.2 wt. % to about 5 wt. % of a transition metal salt of a strong acid; and, about 0.2 wt. % to about 5 wt. % of a sulfur-containing reducer compound. 14. The system of claim 13 , wherein the transition metal salt is selected from the group consisting of nickel nitrate, cobalt nitrate, nickel sulfate, cobalt sulfate, iron nitrate, copper perchlorate, nickel perchlorate, ion perchlorate, and cobalt perchlorate. 15. The system of claim 13 , wherein the sulfur-containing reducer is selected from the group consisting of N′-diethylthiourea, sodium thiocyanate, sodium sulfide, and sodium dimethyldithiocarbamate. 16. The system of claim 13 , wherein the highly soluble nitric acid salt is selected from the group consisting of sodium nitrate, potassium nitrate, and lithium nitrate. 17. The system of claim 13 , wherein the strong base is selected from the group consisting of sodium hydroxide, potassium hydroxide, and lithium hydroxide. 18. A blackening bath, the blackening bath comprising: about 3 wt. % to about 20 wt. % of a highly soluble nitric acid salt; about 18 wt. % to about 38 wt. % of a strong base; about 50 wt. % to about 75 wt. % of water; about 0.2 wt. % to about 5 wt. % of a highly soluble permanganate salt; and, about 0.2 wt. % to about 5 wt. % of a thiocyanate salt. 19. The bath of claim 18 , wherein the permanganate salt is selected from the group consisting of potassium permanganate, sodium permanganate, and lithium permanganate. 20. The bath of claim 18 , wherein the blackening bath additionally comprises a water soluble chloride salt. 21. The bath of claim 18 , wherein the thiocyanate salt is selected from the group consisting of sodium thiocyanate, potassium thiocyanate, and lithium thiocyanate. 22. The bath of claim 18 , wherein the highly soluble nitric acid salt is selected from the group consisting of sodium nitrate, potassium nitrate, and lithium nitrate. 23. The bath of claim 18 , wherein the strong base is selected from the group consisting of sodium hydroxide, potassium hydroxide, and lithium hydroxide. 24. The bath of claim 18 , wherein the blackening bath additionally comprises about 0.2 wt. % to about 5 wt. % of a molybdate salt.
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