Journal Article

PUBDB-2026-00066

http://join2-wiki.gsi.de/foswiki/pub/Main/Artwork/join2_logo100x88.png Modular reactor for in situ X-ray scattering, spectroscopy and ATR-IR studies of solvothermal nanoparticle synthesis

Harouna-Mayer, S. (Corresponding author)Extern* ; Gumus Akcaalan, M.CFEL*MPG*Extern* ; Kopula Kesavan, J.Extern*XFEL.EU* ; Groene, T. R. L.Extern* ; Klemeyer, L.Extern*DESY* ; Hussak, S.-A.Extern*DESY* ; Grote, L. ; Derelli, D. ; Caddeo, F. ; Zito, C.Extern* ; Stützle, P. ; Speer, D. ; Dippel, A.-C.DESY* ; Detlefs, B. ; Appiarius, Y. ; Jacobi von Wangelin, A. ; Koziej, D.Extern*

2026
IUCr Chester

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Please use a persistent id in citations: doi:10.1107/S1600577525009634  doi:10.3204/PUBDB-2026-00066

Abstract: Understanding the chemical processes that occur during the solvothermal synthesis of functional nanomaterials is essential for their rational design and optimization for specific applications. However, these processes remain poorly understood, primarily due to the limitations of conventional ex situ characterization techniques and the technical challenges associated with in situ studies, particularly the design and implementation of suitable reactors. Here, we present a versatile reactor suitable for in situ X-ray scattering, X-ray spectroscopy and infrared spectroscopy studies performed during solvothermal synthesis under autoclave-like, inert conditions. The reactor enables precise control of the temperature between −20°C and 200°C, pressure up to 8 bar, magnetic stirring, and injection of gas or liquids. The reactor's capabilities are demonstrated by comprehensively studying the solvothermal synthesis of magnetite nanoparticles from iron acetyl­acetonate in benzyl alcohol through in situ X-ray scattering and spectroscopy, and attenuated total reflection infrared (ATR-IR) spectroscopy.

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Contributing Institute(s):

1. FS-PETRA (FS-PETRA)
2. Experimentebetreuung PETRA III (FS-PET-D)

Research Program(s):

1. 632 - Materials – Quantum, Complex and Functional Materials (POF4-632) (POF4-632)
2. 6G3 - PETRA III (DESY) (POF4-6G3) (POF4-6G3)
3. DFG project G:(GEPRIS)390715994 - EXC 2056: CUI: Tiefe Einblicke in Materie (390715994) (390715994)
4. 05K22GU7 - Untersuchung photoaktiver Nanomaterialien durch Hochenergie-Röntgenstrahl Streumethoden: Messzellen für Atome, Cluster und Nanokristalle (BMBF-05K22GU7) (BMBF-05K22GU7)
5. 05K20GUA - Verbundprojekt 05K2020 - 2019-06104 XStereoVision: Stereoskopische Röntgenmikroskopie zur Untersuchung von Nukleation, Wachstum und Aufbau von Nanopartikeln in 3D (BMBF-05K20GUA) (BMBF-05K20GUA)

Experiment(s):

1. PETRA Beamline P21.1 (PETRA III)

Appears in the scientific report 2026

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