# Modular Reactor for In Situ X-ray Scattering, Spectroscopy, and ATR-IR Studies of Solvothermal Nanoparticle Synthesis Tjark R. L. Groene,¹ Sani Y. Harouna-Mayer,^1,2 Melike Gumus Akcaalan,¹ Jagadesh Kopula Kesavan,^1,2 Lars Klemeyer,^1,2 Sarah-Alexandra Hussak,^1,3 Lukas Grote,¹ Davide Derelli,¹ Francesco Caddeo,¹ Cecilia Zito,^1,2 Paul Stützle,¹ Dorota Speer,¹ Ann-Christin Dippel,³ Blanka Detlefs,⁴ Yannik Appiarius,⁵ Axel Jacobi von Wangelin,⁵ Dorota Koziej^1,2*
University of Hamburg, Institute for Nanostructure and Solid-State Physics, Center for Hybrid Nanostructures, Luruper Chaussee 149, 22761 Hamburg, Germany

he Hamburg Center for Ultrafast Imaging, 22761 Hamburg, Germany

Deutsches Elektronen-Synchrotron DESY, Notkestraße 85, 22607 Hamburg, Germany.

ESRF, The ESRF, The European Synchrotron, 71 Avenue des Martyrs, CS40220, 38043 Grenoble, Cedex 9, France

University of Hamburg, Department of Chemistry, Martin Luther King Platz 6, 20146 Hamburg,

We describe a novel reaction reactor for in situ X-ray scattering and spectroscopy with liquid or gas injection capabilities. The reactor enables autoclave-like conditions for solvothermal synthesis, with heating up to 200 °C at pressures of up to 8 bar, as well as cooling to −20 °C to decelerate rapid reduction processes such as those occurring during cluster formation. Optional ATR IR or injection can be performed simultaneously by the choice of different caps for the inlet. While conventional ex situ techniques usually provide information only on the final products, the underlying reaction mechanisms often remain obscured, potentially missing crucial intermediate steps. However, a deeper insight into the reaction step is of great interest to tailor material properties, especially for those at the nanoscale.[1],[2],[3] To shine a light on these mechanisms, our multi-purpose in situ cell standardises reaction procedures across a wide range of non-invasive monitoring methods with a strong focus on high flux synchrotron radiation. Capabilities of the cell to fetch complexation and cluster intermediates have been demonstrated for Cu3PdN, ZnS and Fe3O4 nanoparticles.[4],[5],[6]

Cansell, F. and Aymonier, C. (2009) The Journal of Supercritical Fluids, 47(3), pp. 508–516.
Deshmukh, R. and Niederberger, M. (2017), Chemistry – A European Journal, 23(36), pp. 8542–8570.
Terraschke, H. (2023) Nanostructured Materials: Applications, Synthesis and In-Situ Characterization.
Sani Y. Harouna-Mayer, Small, Vol 21,33 (2025) (https://doi.org/10.1002/smll.202506838)
L. Klemeyer et al., JACS, Vol. 146, 49, 10 S. (2024) (https://doi.org/10.1021/jacs.4c10257)
L. Klemeyer et al., ACS Nano, 19, 28, 25710–25719 (2025) (https://doi.org/10.1021/acsnano.5c02875)

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