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As heterogeneous catalysis is a surface-dependent process, nickel compounds in the form of microparticles (MPs), and particularly nanoparticles (NPs), improve the catalytic activity of Ni-based catalysts due to their high specific surface area. Solvothermal synthesis, which has so far been neglected for the synthesis of Ni-based methanation catalysts, was used in this study to synthesize nickel and nickel oxide MPs and NPs with a narrow size distribution. Solvothermal synthesis allows for the control of both the chemical composition of the resulting Ni catalysts and their physical structure by simply changing the reaction conditions (solvent, temperature, or concentration of reactants). Only non-toxic substances were used for synthesis in this study, meaning that the whole synthesis process can be described as environmentally friendly. Solvothermally prepared Ni compounds were subsequently transformed into nickel oxide by means of high-temperature decomposition, and all of the prepared Ni-based compounds were tested as catalysts for CO2 methanation. The best catalysts prepared in this study exhibited a CO2 conversion rate of nearly 95% and a selectivity for methane close to 100%, which represent thermodynamic limits for this reaction at the used temperature. These results are commonly achieved with much more complex catalytic composites containing precious metals, while here we worked with pure nickel and its oxides, in the form of micro- or nanoparticles, only.<\/jats:p>","DOI":"10.3390\/nano15171379","type":"journal-article","created":{"date-parts":[[2025,9,8]],"date-time":"2025-09-08T08:06:32Z","timestamp":1757318792000},"page":"1379","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["The Solvothermal Method: An Efficient Tool for the Preparation of Ni-Based Catalysts with High Activity in CO2 Methanation"],"prefix":"10.3390","volume":"15","author":[{"given":"Arkadii","family":"Bikbashev","sequence":"first","affiliation":[{"name":"Department of Physical Chemistry, Faculty of Science, Palack\u00fd University Olomouc, 17. 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Heyrovsk\u00fd Institute of Physical Chemistry, Czech Academy of Sciences, Dolejskova 2155\/3, 18223 Prague, Czech Republic"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Robert","family":"Prucek","sequence":"additional","affiliation":[{"name":"Department of Physical Chemistry, Faculty of Science, Palack\u00fd University Olomouc, 17. Listopadu 12, 77900 Olomouc, Czech Republic"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5429-9966","authenticated-orcid":false,"given":"Ale\u0161","family":"Pan\u00e1\u010dek","sequence":"additional","affiliation":[{"name":"Department of Physical Chemistry, Faculty of Science, Palack\u00fd University Olomouc, 17. 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