Etch solutions having bis(perfluoroalkylsulfonyl)imides, and use thereof to form anode foils with increased capacitance
US-10072349-B2 · Sep 11, 2018 · US
US11230794B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11230794-B2 |
| Application number | US-201916276319-A |
| Country | US |
| Kind code | B2 |
| Filing date | Feb 14, 2019 |
| Priority date | Dec 2, 2016 |
| Publication date | Jan 25, 2022 |
| Grant date | Jan 25, 2022 |
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Anode foil, preferably aluminum anode foil, is etched using a process of treating the foil in an electrolyte bath composition comprising a perfluoroalkylsulfonate, a sulfate, a halide, and an oxidizing agent. The anode foil is etched in the electrolyte bath composition by passing a direct current charge through the bath. The etched anode foil is suitable for use in an electrolytic capacitor.
Opening claim text (preview).
What is claimed is: 1. An aqueous electrolyte bath composition for etching anode foil, comprising: a sulfate; a halide; an oxidizing agent; and a C 1 -C 8 perfluoroalkylsulfonate in an amount ranging from about 10 to 90 parts per million (ppm). 2. The composition of claim 1 , wherein said C 1 -C 8 perfluoroalkylsulfonate is present in the electrolyte bath composition in an amount ranging from about 20 to about 70 ppm. 3. The composition of claim 1 , wherein the C 1 -C 8 perfluoroalkylsulfonate comprises nonafluorobutanesulfonic acid (FBSA) and/or a salt thereof. 4. The composition of claim 1 , wherein the C 1 -C 8 perfluoroalkylsulfonate is an alkali metal nonafluorobutanesulfonate. 5. The composition of claim 4 , wherein the alkali metal is potassium. 6. The composition of claim 1 wherein: the C 1 -C 8 perfluoroalkylsulfonate is selected from the group consisting of nonafluorobutanesulfonic acid (FBSA), potassium perfluoroalkylsulfonate (KFBS), and mixtures thereof, the sulfate is sulfuric acid and said electrolyte bath composition comprises about 0.8% by weight to about 1.0% by weight sulfuric acid, the halide is hydrochloric acid and said electrolyte bath composition comprises about 0.5% by weight to about 3% by weight hydrochloric acid, and the oxidizing agent is sodium perchlorate and said electrolyte bath composition comprises about 2% by weight to about 6% by weight sodium perchlorate. 7. The composition of claim 6 , wherein said electrolyte bath composition comprises: about 0.92% by weight sulfuric acid; about 0.62% by weight hydrochloric acid; and about 3.5% by weight sodium perchlorate. 8. The composition of claim 7 , wherein the C 1 -C 8 perfluoroalkylsulfonate is FBSA and/or KFBS. 9. The composition of claim 8 , further comprising diethanolamine (DEA). 10. A method of etching an anode foil, comprising: passing a direct current (DC) charge through an anode foil while the anode foil is immersed in an aqueous electrolyte bath, wherein said aqueous electrolyte bath comprises: a sulfate; a halide; an oxidizing agent; and a C 1 -C 8 perfluoroalkylsulfonate in an amount ranging from about 10 to 90 parts per million (ppm); such that the anode foil is etched. 11. The method of claim 10 , wherein the C 1 -C 8 perfluoroalkylsulfonate is provided as an aqueous solution of C 1 -C 8 perfluoroalkylsulfonic acid and/or a salt thereof. 12. The method of claim 11 , wherein the C 1 -C 8 perfluoroalkylsulfonic acid or salt thereof is nonafluorobutanesulfonic acid (FBSA) and/or potassium nonafluorobutanesulfonate (KFBS). 13. The method of claim 10 , wherein the anode foil is etched so as to form branched tunnels in the anode foil. 14. The method of claim 10 , wherein the anode foil is etched so as to form tunnels in the anode foil, and further comprising: widening the tunnels after etching the anode foil. 15. The method of claim 10 , further comprising: making a capacitor that includes the etched anode foil as an anode. 16. The composition of claim 1 , wherein the foil is immersed in the bath. 17. The composition of claim 16 , wherein the bath etches tunnels in the foil. 18. The composition of claim 1 , wherein the bath further comprises: an amine base. 19. The composition of claim 18 , wherein the amine base is selected from a group consisting of: ethanolamine, diethanolamine, triethanolamine, ethylamine, diethylamine, triethyamine, methylamine, dimethylamine, trimethylamine, and ammonia. 20. The composition of claim 1 , wherein the bath has a composition of 4 to 9.
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