Ball Mill Synthesis of Bulk Quaternary Cu₂ZnSnSe₄ and Thermoelectric Studies

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• 作者：Kunal J. Tiwari ; D. S. Prem Kumar ; Ramesh Chandra Mallik…
• 关键词：Ball mill synthesis ; x ; ray diffraction ; CZTSe ; thermoelectric properties
• 刊名：Journal of Electronic Materials
• 出版年：2017
• 出版时间：January 2017
• 年：2017
• 卷：46
• 期：1
• 页码：30-39
• 全文大小：
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Optical and Electronic Materials; Characterization and Evaluation of Materials; Electronics and Microelectronics, Instrumentation; Solid State Physics;
• 出版者：Springer US
• ISSN：1543-186X
• 卷排序：46

文摘

In this work, quaternary chalcogenide Cu₂ZnSnSe₄ (CZTSe) was synthesized using a mechanochemical ball milling process and its thermoelectric properties were studied by electrical resistivity, Seebeck coefficient, and thermal conductivity measurements. The synthesis process comprises three steps viz., wet ball milling of the elemental precursors, vacuum annealing, and densification by hot pressing. The purpose of this is to evaluate the feasibility of introducing wet milling in place of vacuum melting in solid state synthesis for the reaction of starting elements. We report the structural characterization and thermoelectric studies conducted on samples that were milled at 300 rpm and 500 rpm. X-ray diffraction (XRD) analysis showed the existence of multiple phases in the as-milled samples, indicating the requirement for heat treatment. Therefore, the ball milled powders were cold pressed and vacuum annealed to eliminate the secondary phases. Annealed samples were hot pressed and made into dense pellets for further investigations. In addition to XRD, energy dispersive spectroscopy (EDS) studies were performed on hot pressed samples to study the composition. XRD and EDS studies confirm CZTSe phase formation along with ZnSe secondary phase. Electrical resistivity and Seebeck coefficient measurements were done on the hot pressed samples in the temperature range 340–670 K to understand the thermoelectric behaviour. Thermal conductivity was calculated from the specific heat capacity and thermal diffusivity values. The thermoelectric figure of merit zT values for samples milled at 300 rpm and 500 rpm are ∼0.15 and ∼0.16, respectively, at 630 K, which is in good agreement with the values reported for solid state synthesized compounds.