Modular Reactor for In Situ X-ray Scattering, Spectroscopy, and ATR-IR Studies of Solvothermal Nanoparticle Synthesis

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Auteurs principaux: Harouna-Mayer, Sani Y., Akcaalan, Melike Gumus, Kesavan, Jagadesh Kopula, Groene, Tjark R. L., Klemeyer, Lars, Hussak, Sarah-Alexandra, Grote, Lukas, Derelli, a Davide, Caddeo, Francesco, Zito, Cecilia, Stützle, Paul, Speer, Dorota, Dippel, Ann-Christin, Detlefs, Blanka, Appiarius, Yannik, von Wangelin, Axel Jacobi, Koziej, Dorota
Format: Preprint
Publié: 2025
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author Harouna-Mayer, Sani Y.
Akcaalan, Melike Gumus
Kesavan, Jagadesh Kopula
Groene, Tjark R. L.
Klemeyer, Lars
Hussak, Sarah-Alexandra
Grote, Lukas
Derelli, a Davide
Caddeo, Francesco
Zito, Cecilia
Stützle, Paul
Speer, Dorota
Dippel, Ann-Christin
Detlefs, Blanka
Appiarius, Yannik
von Wangelin, Axel Jacobi
Koziej, Dorota
author_facet Harouna-Mayer, Sani Y.
Akcaalan, Melike Gumus
Kesavan, Jagadesh Kopula
Groene, Tjark R. L.
Klemeyer, Lars
Hussak, Sarah-Alexandra
Grote, Lukas
Derelli, a Davide
Caddeo, Francesco
Zito, Cecilia
Stützle, Paul
Speer, Dorota
Dippel, Ann-Christin
Detlefs, Blanka
Appiarius, Yannik
von Wangelin, Axel Jacobi
Koziej, Dorota
contents 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 cell 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, pressures 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 ATR-IR spectroscopy.
format Preprint
id arxiv_https___arxiv_org_abs_2510_06770
institution arXiv
publishDate 2025
record_format arxiv
spellingShingle Modular Reactor for In Situ X-ray Scattering, Spectroscopy, and ATR-IR Studies of Solvothermal Nanoparticle Synthesis
Harouna-Mayer, Sani Y.
Akcaalan, Melike Gumus
Kesavan, Jagadesh Kopula
Groene, Tjark R. L.
Klemeyer, Lars
Hussak, Sarah-Alexandra
Grote, Lukas
Derelli, a Davide
Caddeo, Francesco
Zito, Cecilia
Stützle, Paul
Speer, Dorota
Dippel, Ann-Christin
Detlefs, Blanka
Appiarius, Yannik
von Wangelin, Axel Jacobi
Koziej, Dorota
Materials Science
Instrumentation and Detectors
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 cell 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, pressures 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 ATR-IR spectroscopy.
title Modular Reactor for In Situ X-ray Scattering, Spectroscopy, and ATR-IR Studies of Solvothermal Nanoparticle Synthesis
topic Materials Science
Instrumentation and Detectors
url https://arxiv.org/abs/2510.06770