Comparison of Clusters Produced from Sb 2 Se 3 Homemade Polycrystalline Material, Thin Films, and Commercial Polycrystal
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J. Am. Soc. Mass Spectrom. (2019) DOI: 10.1007/s13361-019-02346-9
RESEARCH ARTICLE
Comparison of Clusters Produced from Sb2Se3 Homemade Polycrystalline Material, Thin Films, and Commercial Polycrystalline Bulk Using Laser Desorption Ionization with Time of Flight Quadrupole Ion Trap Mass Spectrometry Fei Huang,1 Lubomír Prokeš,1 Petr Němec,2 Virginie Nazabal,2,3 Josef Havel1 1
Department of Chemistry, Faculty of Science, Masaryk University, Kamenice 5/A14, 62500, Brno, Czech Republic Department of Graphic Arts and Photophysics, Faculty of Chemical Technology, University of Pardubice, Studentská 573, 53210, Pardubice, Czech Republic 3 Institut des Sciences Chimiques de Rennes, UMR-CNRS 6226, Equipe Verres et Céramiques, Université de Rennes 1, 35042, Rennes, France 2
Abstract. This study compared Sb2Se3 material in the form of commercial polycrystalline bulk, sputtered thin film, and homemade polycrystalline material using laser desorption ionization (LDI) time of flight mass spectrometry with quadrupole ion trap mass spectrometry. It also analyzed the stoichiometry of the SbmSen clusters formed. The results showed that homemade Sb2Se3 bulk was more stable compared to thin film; its mass spectra showed the expected cluster formation. The use of materials for surface-assisted LDI (SALDI), i.e., graphene, graphene oxide, and C60, significantly increased the mass spectra intensity. In total, 19 SbmSen clusters were observed. Six novel, high-mass clusters—Sb4Se4+, Sb5Se3-6+, and Sb7Se4+—were observed for the first time when using paraffin as a protective agent. Keywords: Antimony selenide, Clusters, Laser desorption ionization, Paraffin, Chalcogenides Received: 25 July 2019/Revised: 11 September 2019/Accepted: 29 October 2019
Introduction
S
b2Se3 is known in nature as the mineral antimonselite. The crystal and electronic structure of antimony selenide as well as its vibrational properties were previously determined [1–4]. Generally, the SbmSen system is an important member of chalcogenide materials. Under typical experimental conditions of chalcogenide glass synthesis, the glass-forming region in the SbmSen system is limited to rather low antimony content (up to 30%) and smaller glass batches often face phase separation problems [5–7]. On the other hand, it is possible to fabricate
Electronic supplementary material The online version of this article (https:// doi.org/10.1007/s13361-019-02346-9) contains supplementary material, which is available to authorized users. Correspondence to: Josef Havel; e-mail: [email protected]
amorphous, stoichiometric, and thin Sb2Se3 films by physical vapor deposition techniques such as radiofrequency magnetron sputtering [8] or thermal evaporation [9]. Moreover, Sb2Se3 forms stable glasses and amorphous thin films with other glassforming selenides like GeSe2 [10–13]. Today, SbmSen materials, especially in the form of thin films, have been widely studied as for memory switching application [14, 15], as glassceramic or antimony selenide thin films for solar cells [16–20], as Sb2
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