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CERAMICS INTERNATIONAL · 2023 · IF 5.2

Carbothermal-sulfurization of TiO2 into Ti2SC MAX phase in TiO2/C/FeS2 ternary system

Sheng Pang,Zhenqian Zhang,Liangwei Cong,Youpeng Xu,Guoyu Qian,Dong Wang,Laishi Li,Yusheng Wu,Zhi Wang

The conventional method for synthesizing Ti 2 SC depends on the reaction between TiS and TiC, which requires the utilization of costly Ti, TiC, or TiS 2 powders. Utilizing TiO 2 as the raw material for the synthesis of Ti 2 SC enables the cost-effective preparation of this compound. However, the optimization of the TiO 2 /C/X n S m (sulfides) system is of utmost importance when aiming to synthesize Ti 2 SC through carbothermal-sulfurization of TiO 2 , as the formation temperature of TiS and TiC greatly depends on the X n S m . In this study, the identification of the thermodynamically dominant region for the formation of TiS and TiC in the TiO 2 /C/X n S m systems was conducted by utilizing various sulfides (63 types). Considering factors such as the challenges associated with removing by-products, accessibility, and toxicity, FeS 2 was ultimately chosen as a highly promising candidate. Thanks to the low melting point of FeS 2 , Ti 3 O 5 , the preliminary carbothermal reduction product of TiO 2 , has achieved rapid-deep deoxidation and phase reconstruction processes in the molten phase. Meanwhile, unlike the conventional solid-solid sintering reaction , which often results in residual reactants that are challenging to eliminate. This novel one-step phase transformation process that occurs in the molten phase exhibits minimal impurity phases, apart from the by-product Fe. Ti 2 SC with a purity greater than 99 wt% was obtained when the TiO 2 /C/FeS 2 was pickled to remove Fe after sintering at 1600 °C for 5 min. This work will provide the theoretical basis and a new path for the low-cost preparation of sulfur-containing MAX phases.

CAS / MDL: 1317-40-4
研究领域: 材料科学 · 化学工程
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JOURNAL OF ALLOYS AND COMPOUNDS · 2025 · IF 6.3

Conversion of Nb2O5 to NbS2 for the Preparation of Niobium Nanopowder through Solid Cathode Electrolysis in Molten Chlorides

Changsheng Wu,Zhiyong Wang,Xianbo Jin

Niobium (Nb) is primarily used as the active material in Nb electrolytic capacitors in the form of metallic fine powder. Unlike traditional methods of preparing niobium powder through chemical or electrochemical reduction of metal compounds in molten salts, we report here the efficient preparation of Nb nanopowder via electrolysis of NbS 2 in the NaCl-KCl melt at 973   K. The NbS 2 is simply synthesized by carbo-sulfidation of Nb 2 O 5 . The following electro-desulfidation in the molten electrolyte converts solid NbS 2 into Nb nanopowder at the cathode, with S 2- ions moving to the anode and being oxidized to gaseous sulfur. The reduction path was verified to be NbS 2 → L x NbS 2 → NbS 2-w → Nb. Through constant cell electrolysis at 2.9   V, NbS 2 is rapidly reduced to nodular Nb nanopowder (50-100   nm), with a Current efficiency and energy consumption of approximately 94% and 3.58   kW·h kg⁻¹ Nb, respectively.

研究领域: 材料科学 · 电化学 · 纳米技术 · 冶金学
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