Franziska Emmerling

Bundesanstalt für Materialforschung und -prüfung | BAM · Department of Analytical Chemistry (Dpt.1)

James Batteas, et al., introduce the field of mechanochemistry in “Moving mechanochemistry forward”.

Extended hydrogen initiatives promote the urgency of research on water splitting technologies and therein oxygen evolution reaction catalysts being developed. A route to access a ZrF4 supported high-entropy fluoride catalyst using a facile sol-gel route is presented. The high-entropy character of the catalyst was confirmed by scanning transmission...

Efficient treatment of persistent pollutants in wastewater is crucial for sustainable water management and environmental protection. This study addresses this challenge by investigating the mechanochemical synthesis and photocatalytic performance of ZIF-9, a cobalt-based zeolitic imidazolate framework. Using synchrotron-based powder X-ray diffracti...

The integration of multiple elements in a high‐entropy state is crucial in the design of high‐performance, durable electrocatalysts. High‐entropy metal hydroxide organic frameworks (HE‐MHOFs) are synthesized under mild solvothermal conditions. This novel crystalline metal–organic framework (MOF) features a random, homogeneous distribution of cation...

Chemistry traditionally relies on reactions in solution, but this method is increasingly problematic due to the scale of chemical processes and their economic and environmental impact. Handling residual chemical waste, including solvents, incurs significant costs and environmental pressure. Conversely, novel chemical approaches are needed to addres...

We present the racemization of an active pharmaceutical ingredient Levetiracetam using a novel approach. We demonstrate the design of a 100% solvent-free process that proceeds by high energy milling inside a regular mixer mill. The kinetics of the racemization process is drastically improved compared to the solution-based approach and illustrates t...

A well-ordered structure with high crystallinity is crucial in various applications, particularly in electrode materials for batteries. The dimensionality and connectivity of the interstitial sites, determined by the crystal structure, inherently influence Li+ ions diffusion kinetics. Niobium tungsten oxides block structures, which are built by the...

Chemistry traditionally relies on reactions in solution, but this method is increasingly problematic due to the scale of chemical processes and their economic and environmental impact. Handling residual chemical waste, including solvents, incurs significant costs and environmental pressure. Conversely, novel chemical approaches are needed to addres...

Phase transformations during high-energy ball milling, being a tool of mechanochemistry, are interesting due to the possible production of metastable phases without the need of artificially introducing high temperatures and...

Mechanochemistry is drawing the attention of the pharmaceutical industry given its potential for sustainable material synthesis and manufacture. Scaling mechanochemical processes to the industry level remains a challenge due to...

Synthesis of pure, homogeneous, and reproducible materials is key for the comprehensive understanding, design, and tailoring of material properties. In this study, we focus on the synthesis of ZrV2O7, a material known for its negative thermal expansion properties. We investigate the influence of solid-state and wet chemistry synthesis methods on th...

In materials science, traditional techniques for analyzing layered structures are essential for obtaining information about local structure, electronic properties and chemical states. While valuable, these methods often require high vacuum environments and have limited depth profiling capabilities. The grazing exit x-ray absorption near-edge struct...

The synthesis of the first pincer ligand featuring a strictly T-shaped group 15 element and its coordination behaviour towards transition metals is described. The platform is itself derived from a trianionic redox non-innocent NNN scaffold. In addition to providing a rigid coordination environment to constrain a Bi centre in a T-shaped geometry to...

Kinetics information on the progress of the mechanochemical reactions is key to their understanding and subsequent scale-up. For crystalline materials, the most robust and tested method for obtaining kinetic data is the Quantitative Phase Analysis (QPA) via Rietveld refinement. In this work, we tested the feasibility of the Multivariate Curve Resol...

The Simons process is an electrochemical fluorination (ECF) process for the synthesis of organofluorine compounds. Despite the wide application of the process, the underlying mechanism and the nature of the...

Mechanochemistry routinely provides solid forms (polymorphs) that are difficult to obtain by conventional solution-based methods, making it an exciting tool for crystal engineering. However, we are far from identifying the full scope of mechanochemical strategies available to access new and potentially useful solid forms. Using the model organic co...

This study investigates the mechanochemical reactions between AgBr 3-picolylamine or 4-picolylamine. The use of different stoichiometry ratio of the reagents allows to obtain [(AgBr)(n-pica)]n and [(AgBr)2(n-pica)]n and we report the...

Crystalline materials that exhibit reversible mechanical responses upon exposure to external stimuli have garnered significant attention due to their potential applications in various fields. Herein, we report crystal of (2Z,...

Molecular crystals that exhibit photomechanical responses hold great promise as photoactuators and other smart materials in various fields. Here, we synthesized two new barbituric acid derivative crystals (crystals 1 and...

Photoresponsive molecular crystals sparked interest due to potential application prospects. We have achieved dual mechanical responses of cyanostilbene based crystal BN. The crystal exhibited both stress induced mechanical flexibility and...

Correction for ‘Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy’ by Stefan Peters et al. , Chem. Commun. , 2023, 59 , 12120–12123, https://doi.org/10.1039/D3CC03277A.

A setup for dispersive X-ray absorption spectroscopy (XAS) with spatial, temporal and energy resolution is presented. Through investigation of Mo/HZSM-5 catalyst during the dehydro-aromatization of methane we observed a reduction...

Here, we elucidate non-classical multistep crystallization pathways of transition metal phosphates from aqueous solutions. We followed precipitation processes of M-struvites, NH4MPO4•6H2O, and M-phosphate octahydrates, M3(PO4)2•8H2O, where M = Ni, Co, NixCo1-x by using in-situ scattering and spectroscopy-based techniques, supported by elemental mas...

Here, we show that calcium sulfate dihydrate (gypsum) can be directly, rapidly and reversibly converted to calcium sulfate hemihydrate (bassanite) in high salinity solutions (brines). The optimum conditions for the efficient production of bassanite in a short time (< 5 min) involve the use of brines with [NaCl] > 4 M and maintaining a temperature,...

Due to their favorable properties and high porosity, zeolitic imidazolate frameworks (ZIFs) have recently received much limelight for key technologies such as energy storage, optoelectronics, sensorics, and catalysis. Despite the widespread interest in these materials, fundamental questions regarding the zinc coordination environment remain poorly...

An exceptional HF transfer reaction by C-F bond activation of fluoropentane and a subsequent hydrofluorination of alkynes at room temperature is reported. An amorphous Lewis-acidic Zr chlorofluoride serves as heterogeneous...

Mechanochemistry has proven to be a highly effective method for the synthesis of organic compounds. We studied the kinetics of the catalyst-free Knoevenagel reaction between 4-nitrobenzaldehyde and malononitrile, activated and driven by ball milling. The reaction was investigated in the absence of solvents (neat grinding) and in the presence of sol...

Physical adsorption at cryogenic temperature (cryoadsorption) is a reversible mechanism that can reduce the pressure of conventional compressed gas storage systems. Metal–organic framework (MOF) materials are remarkable candidates due to the combination of high specific surface area and density which, in some cases, provide a high volumetric storag...

In this article, we present a novel one-pot mechanochemical reaction for the surface activation of lignin. The process involves environmentally friendly oxidation with hydrogen peroxide, depolymerization of fractions with high molecular mass, and introduction of new carbonyl functions into the lignin backbone. Kraft lignin was ground with sodium pe...

Chemically synthesized iron is in demand for biomedical applications due to its large saturation magnetization compared to iron oxides. The polyol process, suitable for obtaining Co and Ni particles and their alloys, is laborious in synthesizing Fe. The reaction yields iron oxides, and the reaction pathway remains unexplored. This study shows that...

The precipitation of struvite, a magnesium ammonium phosphate hexahydrate (MgNH4PO4⋅6H2O) mineral, from wastewater is a promising method for recovering phosphorous. While this process is commonly used in engineered environments, our understanding of the underlying mechanisms responsible for the formation of struvite crystals remains limited. Specif...

Transition metal phosphates (TMPs) have attracted interest as materials for (electro-) catalysis, and electrochemistry due to their low-cost, stability, and tunability. In this work, an automated synthesis platform was used for the preparation of transition metal phosphate crystals to efficiently explore the multidimensional parameter space, determ...

Mechanically flexible coordination polymers (CPs) represent new directions for advanced materials design. We herein report unprecedented complexity in the design of isostructural mechanically flexible CPs, with elastic, plastic, and delaminating properties. Ab initio simulations show how these properties can be rationalised by analysis of the simul...

With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and le...

Mechanochemistry has proven to be a highly effective method for the synthesis of organic compounds. We studied the kinetics of the catalyst-free Knoevenagel reaction between 4-nitrobenzaldehyde and malononitrile, activated and driven by ball milling. The reaction was investigated in the absence of solvents (neat grinding) and in the presence of sol...

Here, we describe how to synthesise proton-conductive transition metal phosphates (TMPs) by direct thermal processing of precursor M-struvites, NH4MPO4·6H2O, with M = Ni2+, Co2+. In the as-derived TMP phases their thermal history and bulk proton conductivity were linked with the structural information about the metal coordination, phosphate groups,...

Crystalline porous materials are recognized as promising proton conductors for the proton exchange membrane (PEM) in fuel cell technology owing to their tunable framework structure. However, it is still a challenging bulk synthesis for real-world applications of these materials. Herein, we report the mechanochemical gram-scale synthesis of two isos...

An anion‐doped aluminium chlorofluoride AlCl0.1F2.8(OTeF5)0.1 (ACF‐teflate) was synthesized. The material contains pentafluoroorthotellurate (teflate) groups, which mimic fluoride ions electronically, but are sterically more demanding. They are embedded into the amorphous structure. The latter was studied by PDF analysis, EXAFS data and MAS NMR spe...

In this study, we propose the use of nondestructive, depth-resolved, element-specific characterization using grazing exit X-ray absorption near-edge structure spectroscopy (GE-XANES) to investigate the corrosion process in compositionally complex alloys (CCAs). By combining grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry and a pnCCD...

Mechanically flexible single crystals of molecular materials offer potential for a multitude of new directions in advanced materials design. Before the full potential of such materials can be exploited, insight into their mechanisms of action must be better understood. Such insight can be only obtained through synergistic use of advanced experiment...

We present how mesoporosity can be engineered in transition metal phosphate (TMPs) materials in a template-free manner. The method involves the transformation of a precursor metal phosphate phase, called M-struvite (NH4MPO4·6H2O, M = Mg2+, Ni2+, Co2+, NixCo1-x2+). It relies on the thermal decomposition of crystalline M-struvite precursors to an amo...

Mechanically dual-responsive molecular crystals substantially gained interest among researchers due to their significant application in various fields. Incorporation of disparate mechanical responses in the same crystalline material is still a...

Mechanically flexible molecular crystals have emerged as a fascinating class of materials with the ability to undergo substantial deformation without compromising their structural integrity. We report here four 3,5-di-tert-butyl salicylaldehyde...

A route to a ZrF4 catalyst active in room temperature Friedel-Crafts and dehydrofluorination reactions was developed via a fluorolytic sol-gel route, which was followed by a postfluorination step using a...

Lignin is a highly underused resource. The complex and heterogeneous structure poses a challenge to industry and science. Problems are high polydispersity, high-molar-mass and insufficient functional groups. In this article, we present a mechanochemical one-pot reaction that depolymerises high-molecular-mass fractions by environmentally friendly hy...

Clerodin was isolated from the medicinal plant Clerodendrum infortunatum, and CSD search showed the first crystal structure of clerodin by a single-crystal X-ray diffraction study. We checked its binding potential with target proteins by docking and conducted network pharmacology analysis, ADMET analysis, in silico pathway analysis, normal mode ana...

Fluorescent plastically bendable crystals are a promising alternative to silicon‐based materials for fabricating photonic integrated circuits, owing to their optical attributes and mechanical compliance. Mechanically bendable plastic organic crystals are rare. Their formation requires anisotropic intermolecular interactions and slip planes in the c...

We obtained three 4-(1-Napthylvinyl) pyridine based cocrystals (1–3) and studied its structure mechanical property correlation which aimed towards various applications for photo switches, mechanical actuators etc. Selection of coformer molecules is important in fine tuning mechanical property outcome of synthesized cocrystals. Amongst three cocryst...