TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Michalchuk, Adam A1 - Cakir, Cafer Tufan A1 - Haider, M. B. A1 - Yusenko, Kirill A1 - Radtke, Martin A1 - Reinholz, U. A1 - Emmerling, Franziska T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - AfLS3 CY - Online meeting DA - 14.11.2021 KW - Dipsersive XAS KW - Mechanochemistry KW - Time-resolved KW - In situ PY - 2021 AN - OPUS4-56256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Michalchuk, Adam A1 - Cakir, Cafer Tufan A1 - Yusenko, Kirill A1 - Radtke, Martin A1 - Reinholz, U. A1 - Emmerling, Franziska T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - Denver X-ray Conference: DXC 2021 CY - Online meeting DA - 02.08.2021 KW - Dispersive XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2021 AN - OPUS4-56257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - European Conference on X-ray Spectrometry 2022 CY - Bruges, Belgium DA - 27.06.2022 KW - XAS KW - Mechanochemictry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - Advances X ray Analytics Seminar at TU Berlin CY - Berlin, Germany DA - 14.06.2022 KW - XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in cocrystal formations: in situ investigations of mechanochemical syntheses N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. We discuss our recent results investigating the formation of (polymorphic) cocrystals. First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented.6 Furthermore, X-ray diffraction and in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat. Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds. T2 - CSEC Seminar University of Edinburgh CY - Edinburgh, Scotland DA - 16.05.2019 KW - Mechanochemistry KW - Acoustic levitation KW - In situ PY - 2019 AN - OPUS4-48098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ studies of mechanochemistry: a force of synthesis N2 - Recent results in the field of mechanisms and kinetics of mechanochemical reactions. T2 - Seminar GFZ Potsdam CY - Postdam, Germany DA - 28.03.2018 KW - In situ KW - XRD KW - Rietveld PY - 2018 AN - OPUS4-46992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Synchrotron X-ray Investigations N2 - Summary of the techniques available at the BAMline and µspot BEamline. T2 - Workshop Humboldt University and Hebrew University of Jerusalem CY - Berlin, Germany DA - 09.10.2018 KW - In situ KW - XRD PY - 2018 AN - OPUS4-46993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - May the Force be with you - Mechanochemical syntheses studied in situ N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - Seminar Universität Montpellier CY - Montpellier, France DA - 24.01.2019 KW - Mechanochemistry KW - In situ PY - 2019 AN - OPUS4-47261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in mechanochemical processes using real-time in situ investigations N2 - Use of synchrotron radiation for special sample conditions. Recent work of the group at BESSY II. T2 - DESY Usermeeting Satelite Workshop CY - Hamburg, Germany DA - 22.01.2019 KW - XRD KW - In situ KW - Rietveld KW - Synchrotron PY - 2019 AN - OPUS4-47262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanistic investigations of mechanosyntheses N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms often remain unclear. In the last years, we have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. A further development is the in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. [5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. Based on these data, metastable polymorphs of cocrystals and coordination polymorphs could be isolated and struc-turally characterized. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - Beilstein Symposium MECHANOCHEMISTRY: MICROSCOPIC AND MACROSCOPIC ASPECTS CY - Rüdesheim, Germany DA - 13.11.2018 KW - Mechanochemistry KW - Phosphonates KW - In situ PY - 2018 AN - OPUS4-46758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -