Oxidation-resistant metallic tin
US-12129529-B2 · Oct 29, 2024 · US
US11118276B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11118276-B2 |
| Application number | US-201715775731-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 2, 2017 |
| Priority date | Mar 9, 2016 |
| Publication date | Sep 14, 2021 |
| Grant date | Sep 14, 2021 |
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Provided is high purity tin having purity of 5N (99.999% by mass), which can suppress generation of particles. According to the high purity tin, the number of particles each having a particle diameter of 0.5 μm or more is 50,000 or less per a gram.
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What is claimed is: 1. High purity tin product having a purity of 5N (99.999% by mass) or more, the high purity tin product containing high purity tin and insoluble residue particles wherein the number of insoluble residue particles each having a particle diameter of 0.5 μm or more is greater than 0 and up to 50,000 per gram, and wherein the number of insoluble residue particles are determined by placing a 5 g sample of the high purity tin product in 200 mL hydrochloric acid having a 6N concentration for one hour, heating the sample to 140° C. for 48 hours to dissolve the sample, cooling the sample, diluting the sample with 500 mL pure water and then measuring a number of particles in a portion of the sample using a particle counter according to JIS B9925: 2010. 2. The high purity tin product according to claim 1 , wherein the number of insoluble residue particles each having a particle diameter of 0.5 μm or more is greater than 0 and up to 10,000 per gram. 3. The high purity tin product according to claim 1 , wherein each of concentrations of iron, copper, lead and sulfur contained in the high purity tin is 0.5 ppm by mass or less. 4. The high purity tin product according to claim 1 , wherein a concentration of antimony is 1 ppm by mass or less. 5. The high purity tin product according to claim 1 , wherein a concentration of oxygen is less than 5 ppm by mass. 6. A method for producing high purity tin product according to claim 1 , comprising: a step (1) of providing primary refined electrodeposited tin on a surface of a cathode by carrying out electrolytic refining in an electrolytic bath partitioned into an anode chamber and a cathode chamber by disposing a diaphragm between an anode and a cathode, said electrolytic bath containing a sulfuric acidic solution of tin sulfate as an electrolytic solution and raw material tin as said anode, said raw material tin having a lead content of 20 ppm by mass or less, an iron content of 5 ppm by mass or less, a copper content of 0.5 ppm by mass or less, an antimony content of 5 ppm by mass or less and the total content of silver, arsenic, bismuth, cadmium, copper, iron, indium, nickel, lead, antimony and zinc of 30 ppm by mass or less, while adding to at least said cathode chamber a smoothing agent for reducing a surface area of electrodeposited tin, wherein said step (1) comprises withdrawing at least a part of said tin sulfate solution on said anode chamber side, removing lead and an oxide sludge in said withdrawn tin sulfate solution, and supplying said tin sulfate solution resulting from the removal of lead and the oxide sludge to said cathode chamber; a step (2) of providing needle shaped secondary refined electrodeposited tin on a surface of said cathode by carrying out electrolytic refining in an electrolytic bath containing said primary refined electrodeposited tin or cast tin resulting from heating, melting and casting of said primary refined electrodeposited tin as an anode and a hydrochloric acidic solution of tin chloride as an electrolytic solution, wherein said step (2) comprises withdrawing at least a part of said tin chloride solution from said electrolytic bath, removing particles which can be removed by filtration in said tin chloride solution and remaining components of said smoothing agent carried from the step (1), and then recycling to said electrolytic bath again said tin chloride solution from which said particles and said remaining components of said smoothing agent have been removed; and a step (3) comprising melting and casting said needle shaped secondary refined electrodeposited tin in a reducing gas atmosphere. 7. The method for producing high purity tin product according to claim 6 , wherein said smoothing agent comprises a nonionic surfactant composed of a compound having a structure in which one or more hydroxyl groups are bonded to an aryl group(s) directly or via one or more methylene groups and/or one or more ethylene oxide groups. 8. The method for producing high purity tin product according to claim 6 , wherein said smoothing agent comprises polyoxyethylene alkyl phenyl ether. 9. The method for producing high purity tin product according to claim 6 , wherein said step (1) further comprises adding an antioxidant to said tin sulfate solution together with said smoothing agent.
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