銅キレート剤を用いた鋼中硫化物分析法の開発

• Published in: 鉄と鋼 Vol. 104; no. 11; pp. 634 - 639
• Main Authors: 水上, 和実, 板橋, 大輔, 相本, 道宏, 西藤, 将之
• Format: Journal Article
• Language: Japanese
• Published: 一般社団法人 日本鉄鋼協会 2018
• Subjects: AES; copper sulfide; CUSH; electrolytic dissolution; inclusion; SEM; SPEED method; Triethylenetetramine
• ISSN: 0021-1575; 1883-2954
• DOI: 10.2355/tetsutohagane.TETSU-2018-056

Copper sulfide (CuxS) has been frequently observed in steel samples, prepared using selective potentiostatic etching by electrolytic dissolution (SPEED). It is often the case that CuxS is detected unexpectedly from the precipitates extracted from steel samples by selective potentiostatic etching, although such CuxS formation during the heat treatment conducted is not anticipated by the thermodynamic equilibrium calculations.In this study, we observed such artificial CuxS along with manganese sulfide (MnS) precipitates, which were extracted from steel materials by SPEED, using secondary electron microscope (SEM) equipped with energy dispersive X-ray spectroscopy (EDX) and Auger electron spectroscopy. These CuxS-MnS sulfide complex would be formed by the following mechanism: as the solubility of CuxS is far bigger (i.e. 10 times or more) than that of MnS, Cu2+ ion dissolved from steel matrix would be exchanged with Mn2+ ion on the MnS surface during the etching process, leading to a formation of CuxS-MnS sulfide complex.In order to suppress the formation of such CuxS, we propose the use of following electrolyte: a non-aqaueous solutions of 4% methyl salicylate + 1% salicylic acid + 1% tetramethylammonium chloride (TMAC) + 5% Triethylenetetramine (TET) in volume fraction, in methyl alcohol (Cu ion selective hold etching by electrolytic dissolution, abridged as CUSH electrolyte). Then, this electrolyte was applied to precipitates in steel samples. It was effective to prevent the formation of sulfides in electrolyte, with the effect of metallic (Cu2+, Ag+, Pb+, etc.) chelating ability of TET.