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A comprehensive insight into the parameters that influence the synthesis of Ag2MoO4 semiconductors via experimental design

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Abstract

This study characterized and statistically evaluated the influence of three parameters that potentially affect the synthesis of Ag2MoO4, which have not previously been investigated in conjunction. The study focused on the concentration of a dispersant (polyvinylpyrrolidone, PVP, mmol−1), aging time (h), and pH to evaluate the effects of these factors on the physio-chemical properties of the as-produced semiconductors. Particularly, this study aims to better understand the synthesis of metastable α-Ag2MoO4, which is poorly studied, and explore how minor modifications to the chosen parameters, under mild conditions, can impact its formation. To optimize the production of the α-phase, eleven Ag2MoO4 catalysts were produced by complete factorial experimental design, varying the aforementioned parameters. XRD results revealed that only two samples presented crystalline α-Ag2MoO4 and were significantly influenced by PVP concentration, pH, and their interaction. Additionally, prolonged aging favored an α to β transformation, reducing α content from 68 to 8%. These transformations are correlated with the thermodynamic stability of the crystal, which attempts to reach a more stable matrix. Furthermore, acidic pH modified the stabilization of Ag+ with PVP, enabling the formation of α-Ag2MoO4. The presence of the α phase was further confirmed by TGA/DTA, FTIR, and Raman spectroscopies results. Only PVP concentration significantly affected particle size, increasing it from ~ 4 to 8 μm upon PVP addition. Moreover, several morphologies were observed (butterfly like, potato like, coral like, polygons, etc.), potentially influencing their catalytic and antibacterial activities. Furthermore, a mechanism was proposed to elucidate how these factors affected the particles’ formation.

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Data and code availability

The data that support the findings of this study are available from the corresponding author, Daniela Gier Della Rocca, upon reasonable request.

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Acknowledgements

The authors are grateful to the financial support from Brazil’s Coordination of Improvement of Higher Education Personnel (CAPES—Brazil) [Grant number 001, Project 88881.142487/2017-01] and from the National Council for Scientific and Technological Development (CNPq—Brazil) [Grant Nos. 405892/2013 6 and 142059/2019-6]. As well as LCME (Central Laboratory of Electronic Microscopy) for FEG-SEM images, Nanotec (Laboratory of Nanotechnology Applications in Civil Construction) for XRD analysis, EQA-UFSC analysis center for BET and FTIR spectroscopy analyses, and LINDEN (Interdisciplinary Laboratory for the Development of Nanostructures) for zeta potential and Raman spectroscopy analyses, respectively. E.R.A. and E.R.C. thank Ministerio de Ciencia e Innovación of Spain, projects PID2021-126235OB-C32 and TED2021-130756B-C31 and FEDER funds.

Funding

The Coordination of Improvement of Higher Education Personnel (CAPES—Brazil) [Grant code 001] and Brazil’s National Council for Scientific and Technological Development (CNPq—Brazil) [Grant Nos. 405892/2013 6 and 142059/2019–6] provided financial support. E.R.A. and E.R.C. thank Ministerio de Ciencia e Innovación of Spain, projects PID2021-126235OB-C32 and TED2021-130756B-C31 and FEDER funds.

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Authors and Affiliations

  1. Laboratory of Energy and Environment, Department of Chemical and Food Engineering, Federal University of Santa Catarina, Florianópolis, Brazil

    Daniela G. Della Rocca, Mariana Schneider, Fernanda C. Fraga, Agenor De Noni Júnior & Regina F. P. M. Moreira

  2. Laboratory of Bioinorganic and Crystallography, Department of Chemistry, Federal University of Santa Catarina, Florianópolis, Brazil

    Rosely A. Peralta

  3. Departament of Inorganic Chemistry, Science Faculty, University of Málaga, Malaga, Spain

    Elena Rodríguez-Aguado & Enrique Rodríguez-Castellón

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  1. Daniela G. Della Rocca
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  2. Mariana Schneider
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  3. Fernanda C. Fraga
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Contributions

The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript. The authors contributed equally. DGDR, ADNJ, and RFPMM conceived the project and developed the concept. DGDR, MS, FCF, ERA, ERC, and RAP conducted the material preparation, experiments, and data analysis. DGDR drafted this manuscript. MS, FCF, ERA, ERC, ADNJ, RAP, and RFPMM reviewed and edited the manuscript. All authors discussed and commented on the manuscript. All authors read and approved the final manuscript.

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Correspondence to Daniela G. Della Rocca.

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Regina de Fatima Peralta Muniz Moreira reports financial support was provided by the Federal University of Santa Catarina.

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Della Rocca, D.G., Schneider, M., Fraga, F.C. et al. A comprehensive insight into the parameters that influence the synthesis of Ag2MoO4 semiconductors via experimental design. J Mater Sci: Mater Electron 34, 1500 (2023). https://doi.org/10.1007/s10854-023-10897-7

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