Synthesis of Iron Group Metal Sulfides from the Elements under Hydrothermal Condition

Abstract

Iron group metal sulfides were synthesized from the elements under hydrothermal condition. For nickel sulfides, two kinds of nickel metal powder, coarse powder passed through 63 mm mesh and fine powder passed through 3 mm mesh, were used as the starting materials. The reaction with the coarse Ni powder gave NiS with appreciable amount of Ni, Ni 3 S 2 , and Ni 9 S 8 . Pure NiS was obtained by the reaction with the fine Ni powder at 240? C for 10 h. The lowest nickel sulfide Ni 3 S 2 was obtained as a single phase product of the reaction if the coarse Ni powder was used. From these results, the fine and coarse powders were found to be suitable for the syntheses of NiS and Ni 3 S 2 , respectively. The lowest cobalt sulfide Co 9 S 8 was obtained almost as a single phase though the XRD pattern of the product showed some unidentified peaks. Pure Co 9 S 8 was obtained by washing the reaction product with HNO 3 . In the Fe-S system, FeS was obtained with a small amount of Fe 3 O 4 .

Syntheses of Bi2X3 (X = S, Se, Te) from elements under hydrothermal conditions

“…In contrast, we have studied a simple hydrothermal reaction using only an elemental metal and an elemental chalcogen as starting materials. In this manner, we have succeeded in synthesizing the binary metal sulfides of CuS [17,18], Cu 2 S [18], Ag 2 S [18], NiS [19], Co 9 S 8 [19], Ni 3 S 2 [19], ZnS [20], and CdS [20], and the complex ternary metal sulfides of Ag 3 CuS 2 [21] and AgCuS [21]. Among these sulfides, we have observed interesting particle shapes, such as polyhedral CuS and Cu 2 S. We considered whether this simple approach can possibly be applied to the synthesis of Bi 2 X 3 (X = S, Se, Te).…”

Simple synthesis of zinc sulfide and cadmium sulfide under hydrothermal conditions

“…We have found that pure CuS is obtained easily at low temperature, 60°C. 4),5) Silver sulfide (Ag 2 S), 5) iron sulfide (FeS), 6) cobalt sulfide (Co 9 S 8 ), 6) nickel sulfides (NiS, Ni 3 S 2 ), 6) and complex sulfides AgCuS 7) and Ag 3 CuS 2 7) can also be prepared under similar conditions.…”

Preparation of NiS[sub 2] Using Spark-Plasma-Sintering Process and Its Electrochemical Properties

“…12,13 The low melting point ͑ca. 120°C͒ and volatilization of sulfur generally makes the control of composition difficult with these reactions.…”

“…Recently, a low-temperature synthesis procedure has been developed and several nickel sulfides, such as Ni 3 S 2 , Ni 3 S 4 , and NiS, have been prepared by precipitation reactions or hydrothermal synthesis. [12][13][14] However, the single phase with higher sulfur content, that is NiS 2 , has not yet been reported thus far, and therefore, its electrochemical property has not yet been clarified up to date.…”