Formation of Titanium Sulfide from Titanium Oxycarbonitride by CS 2 Gas

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Previously this group reported that a good quality titanium metal powder can be produced from titanium sulfides by electrochemical OS process. In this study, the sulfurization procedure was examined to synthesize titanium sulfide from titanium oxycarbonitride by CS2 gas. The experiments were carried out in the temperature range of 1173 K to 1523 K (900 C to 1250 C) in a tube reactor with continuously flowing argon (Ar) as carrier gas of CS2. The formation of titanium sulfide phases from the commercial TiN, TiC, and TiO powders was studied as the initial step. Then, TiO0.02C0.13N0.85 coming from ilmenite was sulfurized to prepare single phase of titanium sulfide. The products were characterized by X-ray diffraction, and the morphology of the sulfides was rigorously investigated, and the sulfur, oxygen, and carbon contents in the products were analyzed. The process was remarkably dependent on the temperature and time. TiN and TiO0.02C0.13N0.85 powders could be fully converted to the single phase of Ti2.45S4 (Ti2+xS4) at 1473 K (1200 C) in 3.6 ks. The maximum weight gain of TiN sample was ~ 55.3 pct indicating a full conversion of TiN to Ti2S3 phase. The carbon and oxygen contents in this sulfide prepared from the oxycarbonitride were about 1.8 wt pct C and 1.4 wt pct O, respectively. Therefore, the titanium sulfide could be a promising feedstock for the production of commercial grade titanium powder. https://doi.org/10.1007/s11663-018-1278-8  The Minerals, Metals & Materials Society and ASM International 2018

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INTRODUCTION

THE Ti-S system includes many compounds, namely, Ti6S, Ti3S, Ti2S, TiS, Ti1+xS, Ti4S5, Ti16S21, Ti2.67S4, TiS2, and TiS3.[1,2] Among these compounds, TiS2, hexagonal-layered structure (P3m1), is one of the most promising compounds reported for engineering applications. The excellent physical properties of TiS2 are high electrical conductivity at room temperatures and low density (1.4 9 103 ohm1 cm1)[3] (3.25 g cm3) compared to commercial thermoelectric materials such as PbTe (8.24 g cm3).[4] In addition, sulfur (S) doping has been used for narrowing band gap energy of materials, for example, band gap energy of ELTEFAT AHMADI is with the Division of Materials Science and Engineering, Faculty of Engineering, Hokkaido University, N13W8, Kita-ku, Sapporo 060-8628, Japan and also with the School of Materials & Mineral Resources Engineering, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia. YUTA YASHIMA and RYOSUKE O. SUZUKI are with the Division of Materials Science and Engineering, Faculty of Engineering, Hokkaido University. Contact e-mail: [email protected], URL: http:// www.eng.hokudai.ac.jp/labo/ecopro/rosuzuki/ SHEIKH ABDUL REZAN is with the School of Materials & Mineral Resources Engineering, Universiti Sains Malaysia. Manuscript submitted October 10, 2017.

METALLURGICAL AND MATERIALS TRANSACTIONS B

1.4 eV reported for Ti2xSx compared to 2.3 eV for TiO2.[5] Two-dimensional (2D)-layered materials have also exhibited exciting properties due to the distinct electroni