Low-Pressure Microwave Plasma Reduction of Iron and Copper Salt Compounds at Low Temperatures for Oxidation State Alteration and Functional Applications

Mirco Weber; Anna Scheglov; Wiebke Dörries; Johann Benedikt Meyer; Wolfgang Viöl

doi:10.3390/ma16083221

Low-Pressure Microwave Plasma Reduction of Iron and Copper Salt Compounds at Low Temperatures for Oxidation State Alteration and Functional Applications

Materials (Basel). 2023 Apr 19;16(8):3221. doi: 10.3390/ma16083221.

Authors

Mirco Weber^{1

2}, Anna Scheglov¹, Wiebke Dörries¹, Johann Benedikt Meyer², Wolfgang Viöl^{1

3}

Affiliations

¹ Faculty of Engineering and Health, HAWK University of Applied Sciences and Arts, Von-Ossietzky-Straße 98/100, 37085 Göttingen, Germany.
² Institute of Inorganic Chemistry, Georg August University of Göttingen, Tammannstraße 4, 37077 Göttingen, Germany.
³ Application Center for Plasma and Photonics, Fraunhofer Institute for Surface Engineering and Thin Films, Von-Ossietzky-Straße 100, 37085 Göttingen, Germany.

Abstract

The influence of plasma-reduction treatment on iron and copper compounds at different oxidation states was investigated in this study. For this purpose, reduction experiments were carried out with artificially generated patina on metal sheets and with metal salt crystals of iron(II) sulfate (FeSO₄), iron(III) chloride (FeCl₃), and copper(II) chloride (CuCl₂), as well as with the metal salt thin films of these compounds. All the experiments were carried out under cold low-pressure microwave plasma conditions; the main focus was on plasma reduction at a low pressure in order to evaluate an implementable process in a parylene-coating device. Usually, plasma is used within the parylene-coating process as a supporting tool for adhesion improvement and micro-cleaning efforts. This article offers another useful application for implementing plasma treatment as a reactive medium in order to apply different functionalities by an alteration in the oxidation state. The effect of microwave plasmas on metal surfaces and metal composite materials has been widely studied. In contrast, this work deals with metal salt surfaces generated from a solution and the influence of microwave plasma on metal chlorides and sulfates. While the plasma reduction of metal compounds commonly succeeds with hydrogen-containing plasmas at high temperatures, this study shows a new reduction process that reduces iron salts at temperatures between 30 and 50 °C. A novelty of this study is the alteration in the redox state of the base and noble metal materials within a parylene-coating device with the help of an implemented microwave generator. Another novelty of this study is treating metal salt thin layers for reduction purposes in order to provide the opportunity to include subsequent coating experiments to create parylene metal multilayers. Another new aspect of this study is the adapted reduction process of thin metal salt layers consisting of either noble or base metals, with an air plasma pre-treatment prior to the hydrogen-containing plasma-reduction procedure.

Keywords: low-pressure plasma reduction inclusion; metal salt films; microwave plasma; reduction strategy.

Abstract

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