TY - JOUR A1 - Heinekamp, Christian A1 - Palmer, Tahlia M. A1 - Al‐Sabbagh, Dominik A1 - May, Anastasia A1 - Prinz, Carsten A1 - Michalik, Stefan A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - Pre‐Activation as a Route for Tuning the Kinetics of Mechanochemical Transformations N2 - Learning to control reaction kinetics is essential for translating any chemical technology into real‐world application. Based on time‐resolved in situ powder X‐ray diffraction data, we demonstrate the opportunity to tune mechanochemical reaction rates through the pre‐activation of the starting reagents. For three model co‐crystal systems, the pre‐activation of the most stable reagent yields up to a ca 10‐fold increase in the reaction rate, whilst negligible kinetic enhancement is seen when the less stable reagent is pre‐activated. Moreover, we demonstrate how the polymorphic outcome of mechano‐co‐crystallization is also sensitive to pre‐activation of the starting material. Our results suggest that reproducibility of mechanochemical processes requires detailed understanding over the origin and history of reagent powders, whilst providing a new conceptual framework to design and control mechanochemical reactions. KW - Mechanochemistry KW - In situ synthesis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649409 DO - https://doi.org/10.1002/anie.202516632 SN - 1433-7851 SP - 1 EP - 7 PB - Wiley VHC-Verlag AN - OPUS4-64940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - Bhattacharya, Biswajit A1 - Rodríguez Sánchez, Noelia A1 - Gugin, Nikita T1 - Advancing sustainable synthesis through in situ monitoring and industrial scale-up of mechanochemical processes N2 - Mechanochemistry has emerged as a powerful approach for sustainable materials synthesis and processing, with significant potential to meet the UN Sustainable Development Goals. This presentation will highlight our recent advancements in understanding, monitoring, and scaling-up mechanochemical transformations, focusing on the balance between fundamental understanding of reaction mechanisms and its practical applications in energy storage and energy transfer materials. Our research has made significant strides in elucidating the fundamental mechanisms of mechanochemical reactions. We have investigated delayed polymorphism under mechanochemical conditions, revealing new insights into the interplay between mechanical impact, thermal effects, and structural transformations in molecular crystals. By employing variable temperature ball milling, we have demonstrated unprecedented control over polymorphic forms in organic cocrystals, opening new avenues for tailoring material properties. A central focus of our work has been the development and application of time-resolved in situ monitoring techniques for mechanochemical processes. Our research on real-time synchrotron X-ray diffraction has enabled unprecedented insights into reaction pathways and kinetics. Recently, we have successfully applied energy-dispersive X-ray diffraction for time-resolved in situ monitoring of reactive extrusion, marking a significant step towards ‘lighting up’ industrial-scale mechanochemistry. Bridging fundamental understanding with practical applications, we have explored the mechanochemical synthesis of functional materials for energy storage and transfer, making process in the mechanochemical synthesis of highly proton-conductive metal phosphonates, demonstrating the potential of mechanochemistry to manufacture advanced materials for energy applications. Addressing the challenges of industrial scale-up, we have investigated the role of solvent polarity in mechanochemical reactions, providing valuable guidance for optimizing organic syntheses such as the Knoevenagel condensation. This work contributes to our broader efforts to develop more efficient and sustainable chemical manufacturing processes. Looking to the future, we will discuss emerging directions in mechanochemistry, including the development of continuous flow processes and the integration of machine learning approaches for reaction prediction and optimization. As we anticipate the next decade of research, we envision mechanochemistry playing an increasingly crucial role in sustainable chemical manufacturing and materials processing, with far-reaching implications for addressing global energy and environmental challenges. T2 - Mech’cheM 2025: New forces in Mechanochemistry Conference CY - Montpellier, France DA - 04.06.2025 KW - Phosphonates KW - Biocomposites PY - 2025 AN - OPUS4-64845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - Bhattacharya, Biswajit A1 - Rodríguez Sánchez, Noelia A1 - Gugin, Nikita T1 - Mechanochemical innovations for sustainable synthesis of framework materials and industrial scaleup N2 - Mechanochemistry has emerged as a powerful approach for sustainable materials synthesis and processing, with significant potential to meet the UN Sustainable Development Goals. This presentation will highlight our recent advancements in understanding, monitoring, and scaling-up mechanochemical synthesis of framework materials, focusing on the balance between fundamental understanding of reaction mechanisms and its practical applications in energy storage and energy transfer materials. A central focus of our work has been the development and application of time-resolved in situ monitoring techniques for mechanochemical processes. Our research on real-time synchrotron X-ray diffraction has enabled unprecedented insights into reaction pathways and kinetics. Recently, we have successfully applied energy-dispersive X-ray diffraction for time-resolved in situ monitoring of reactive extrusion, marking a significant step towards ‘lighting up’ industrial-scale mechanochemistry. Bridging fundamental understanding with practical applications, we have explored the mechanochemical synthesis of functional materials for energy storage and transfer, making process in the mechanochemical synthesis of highly proton-conductive metal phosphonates, demonstrating the potential of mechanochemistry to manufacture advanced materials for energy applications. T2 - 17. international-conference für Materialchemie CY - Edinburgh, United Kingdom DA - 07.07.2025 KW - MOF KW - Synchrotron KW - ZIF PY - 2025 AN - OPUS4-64841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hemingway, Jack M. A1 - Quayle, Heather M. A1 - Byrne, Cian A1 - Pulham, Colin R. A1 - Mondal, Subrata A1 - Michalchuk, Adam A1 - Morrison, Carole A. T1 - Predicting impact sensitivities for an extended set of energetic materials via the vibrational up-pumping model: Molecular-based structure–property relationships identified N2 - We have applied the vibrational up-pumping model to predict the mechanically-induced impact sensitivities of 33 molecular energetic crystals. Overall, the current model successfully identifies and ranks the compounds that are most sensitive to mechanical initiation, but offers poorer differentiation between compounds with lower sensitivity. Further developments to include the effects of trigger bond activation led to significant improvements in predictive capability. We show that this structure–property model highlights the importance of molecular flexibility in predicting impact sensitivity, and furthermore, we show that the Kier molecular flexibility index, which can be obtained from a SMILES string, offers a simple molecular-based descriptor that goes some way towards predicting the sensitivity of energetic materials. KW - Vibrational KW - Pyrazoles KW - Comprising KW - Electronic PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632651 DO - https://doi.org/10.1039/d5cp00852b SN - 1463-9076 VL - 27 IS - 22 SP - 11640 EP - 11648 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-63265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Speight, Isaiah R. A1 - Ardila-Fierro, Karen J. A1 - Hernández, José G. A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - García, Felipe A1 - Colacino, Evelina A1 - Mack, James T1 - Ball milling for mechanochemical reactions N2 - Mechanochemistry is an emerging field with the potential to pave the way for sustainable chemistry. Although the use of mechanical force to initiate chemical reactions has been recognized for millennia, it has often taken a backseat to thermal and photonic methods. Over the past 30 years, mechanochemistry has seen a resurgence of interest, attracting researchers across the globe. Despite its proven ability to address numerous challenges within the chemical community, mechanochemistry remains on the periphery. This Primer serves as a valuable guide for conducting mechanochemical reactions by ball milling, offering an overview of the processes, methods, tools and terminology necessary to embark on research in this field. It also highlights persistent hurdles such as equipment standardization, understanding the impact of new discoveries and the lack of predictability of reaction outcomes. The Primer’s focus is on how mechanochemical ball milling is used in various chemical transformations, distinguishing it from other forms of mechanochemistry discussed in the literature. With a promising future, this Primer serves as a gateway for those aspiring to contribute to the field’s advancement. KW - Mechanochemistry KW - Ball milling KW - Upscaling PY - 2025 DO - https://doi.org/10.1038/s43586-025-00401-2 SN - 2662-8449 VL - 5 IS - 1 SP - 1 EP - 18 PB - Springer Science and Business Media LLC AN - OPUS4-63447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudziak, Mateusz A1 - Riechers, Birte A1 - Maaß, Robert A1 - Michalchuk, Adam A1 - Schönhals, Andreas A1 - Szymoniak, Paulina T1 - Beyond conventional calorimetry: Unlocking thermal characterization with fast scanning techniques N2 - Fast scanning calorimetry (FSC) has emerged as a transformative technique in thermal analysis, enabling the investigation of rapid and kinetically driven thermal transitions that are inaccessible to conventional differential scanning calorimetry. This review highlights the capabilities enabled by FSC for studying a wide range of materials under extreme thermal conditions, including polymers, pharmaceuticals, metallic glasses, nanocomposites, and hydrogels. By employing ultrafast heating and cooling rates, FSC allows for the suppression of crystallization, resolution of weak transitions, and analysis of thermally labile or size-limited samples. The technique is particularly valuable for probing glass transitions, relaxation phenomena, and phase behavior in systems with complex morphologies or confined geometries. Case studies demonstrate the use of FSC in characterizing vitrification, physical aging, and interfacial dynamics, as well as its application in emerging fields such as additive manufacturing, supramolecular systems, and neuromorphic materials. Together, these examples underscore the role that FSC plays in advancing the understanding of structure-property relationships across diverse material classes. KW - Flash DSC KW - Calorimetry KW - Glass transition PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647405 DO - https://doi.org/10.1016/j.tca.2025.180177 VL - 754 SP - 1 EP - 14 PB - Elsevier B.V. AN - OPUS4-64740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - Casali, Lucia A1 - May, Anastasia T1 - Real-Time Monitoring and Temperature Control for Optimized Polymorph Engineering N2 - Integrating real-time monitoring with precise temperature control and mechanochemical processing represents a transformative approach to the controlled engineering of polymorphic forms in molecu-lar solids. Combining these methodologies overcomes the limitations of traditional solution-based or purely thermal approaches, enabling access to metastable or otherwise elusive polymorphs under milder and more sustainable conditions. Recent studies have shown that mechanochemical trans-formations proceed through distinct kinetic stages, including prolonged induction periods that can be tuned by adjusting the mechanical energy input[1]. These induction periods are associated with pro-cesses of mechanical activation, such as the accumulation of defects and increased surface energy, which lower the effective energy barriers for polymorphic transitions. Crucially, it is the total accumu-lated mechanical energy, rather than the duration or intensity of milling alone, that dictates the onset of polymorphic conversion, offering a new dimension of kinetic control[2-5]. Variable temperature ball milling reveals that the temperature required to induce polymorphic trans-formations can be significantly lower than under conventional thermal methods. For instance, tran-sitions that typically require high temperatures under equilibrium conditions can be achieved at sub-stantially lower temperatures in the presence of mechanical activation. This has been demonstrated in cocrystal systems such as nicotinamide-pimelic acid and isonicotinamide-glutaric acid, where the transition temperature was lowered by up to 25°C[2,3]. Real-time, in situ powder X-ray diffraction and temperature monitoring are essential for capturing transient phases and elucidating the interplay between thermal and mechanical effects. This confirms that combining mechanical energy with con-trolled temperature not only accelerates transformation kinetics, but also expands the accessible polymorphic landscape [2,3]. Collectively, these advances underscore the potential of real-time monitored, temperature-controlled mechanochemistry as a robust platform for the selective design and manufacturing of polymorphs. This approach provides unprecedented control over solid-state reactivity and opens new avenues for the sustainable and targeted engineering of functional materials and pharmaceuticals. T2 - 13th Bologna´s convention on Crystal Forms - CF@Bo n.13 University of Bologna CY - Bologna, Italy DA - 07.09.2025 KW - Plymorhism KW - Pre-activation PY - 2025 AN - OPUS4-64839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - Stolar, Jasna A1 - Falkenhagen, Jana A1 - Bhattacharya, Biswajit A1 - Gugin, Nikita A1 - Casali, Lucia T1 - Mechanochemical pathways to sustainability: from molecular insights to applications N2 - Mechanochemical Innovations for Sustainable Synthesis of Framework Materials and Industrial ScaleUp Mechanochemistry has emerged as a powerful approach for sustainable materials synthesis and processing, with significant potential to meet the UN Sustainable Development Goals. This presentation will highlight our recent advancements in understanding, monitoring, and scaling-up mechanochemical synthesis of framework materials, focusing on the balance between fundamental understanding of reaction mechanisms and its practical applications in energy storage and energy transfer materials. A central focus of our work has been the development and application of time-resolved in situ monitoring techniques for mechanochemical processes. Our research on real-time synchrotron X-ray diffraction has enabled unprecedented insights into reaction pathways and kinetics. Recently, we have successfully applied energy-dispersive X-ray diffraction for time-resolved in situ monitoring of reactive extrusion, marking a significant step towards ‘lighting up’ industrial-scale mechanochemistry. Bridging fundamental understanding with practical applications, we have explored the mechanochemical synthesis of functional materials for energy storage and transfer, making process in the mechanochemical synthesis of highly proton-conductive metal phosphonates, demonstrating the potential of mechanochemistry to manufacture advanced materials for energy applications. T2 - GDCh Universität Marburg CY - Marburg, Germany DA - 10.02.2025 KW - Situ investigation KW - Nanoparticles KW - Metal phosphonates PY - 2025 AN - OPUS4-64844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -