Method for manufacturing tin(II) oxide powder for replenishing tin component of tin-alloy plating solution, and tin (II) oxide powder manufactured using said method
An object of the present invention is to provide tin(II) oxide powder which has extremely high solubility in an acid or an acidic plating solution, excellent in storage stability in the air and can heighten oxidation-preventive effect of Sn 2+ ion in the plating solution. The method for manufacturing tin(II) oxide powder of the present invention comprises Step ( 11 ) of preparing an aqueous acidic solution containing Sn 2+ ions, Step ( 12 ) of neutralizing the aqueous acidic solution by adding an aqueous alkaline solution to prepare a slurry of tin(II) hydroxide, Step ( 13 ) of dehydrating the prepared slurry to obtain a slurry of tin(II) oxide, Step ( 14 ) of separating the slurry of tin(II) oxide into a solid and a liquid to obtain tin(II) oxide, Step ( 15 ) of treating the obtained tin(II) oxide with an aqueous antioxidant solution, and Step ( 16 ) of vacuum drying the tin(II) oxide treated with the aqueous antioxidant solution.
1. A method for manufacturing tin(II) oxide powder for replenishing a tin component of a tin-alloy plating solution comprising steps of:
preparing an aqueous acidic solution containing Sn 2+ ions;
neutralizing the aqueous acidic solution at a liquid temperature of 30 to 50° C. and at a pH range of 6 to 8 in a nitrogen gas atmosphere by adding an aqueous alkaline solution to prepare a slurry of tin(II) hydroxide;
dehydrating the prepared slurry in a nitrogen gas atmosphere to prepare a slurry of tin(II) oxide;
separating the slurry of tin(II) oxide into a solid and a liquid to obtain tin(II) oxide;
treating the obtained tin(II) oxide with an aqueous antioxidant solution having a concentration of 0.1 to 5% by mass; and
vacuum drying the tin(II) oxide treated with the aqueous antioxidant solution; wherein
the aqueous alkaline solution is an aqueous ammonia solution an ammonium bicarbonate solution or mixture thereof; and
the antioxidant is at least one selected from the group consisting of hydroquinone, catechol, resorcinol, pyrogallol, gallic acid, glucose, galactose, fructose, ribose, xylose, maltose, lactose, hydrazine sulfate, carbohydrazide and sodium cyanotrihydroborate.
2. The method for manufacturing tin(II) oxide powder for replenishing a tin component of a tin-alloy plating solution according to claim 1 , wherein the treatment with the aqueous antioxidant solution is carried out by spraying the aqueous antioxidant solution to the tin(II) oxide powder or dipping the tin(II) oxide powder in the aqueous antioxidant solution.
3. Tin(II) oxide powder for replenishing a tin component of a tin-alloy plating solution manufactured by the method according to claim 1 , wherein the tin(II) oxide powder is coated by the antioxidant, has an average particle diameter with a D 50 value of within 5 to 15 μm, and has a tap density of 0.6 to 1.2 g/cm 3 , the antioxidant is contained in the powder at 100 to 5000 ppm, and the powder has such a dissolution rate that when 0.1 g of the tin(II) oxide powder is added to 100 ml of 100 g/L aqueous alkylsulfonic acid solution at a temperature of 25° C. and stirred, then, it completely dissolves therein within 180 seconds.