TY - CONF
A1 - Ryll, Tom William
T1 - Researching automation of gypsum recycling
N2 - This poster illustrates the recent work on a setup for automated in-situ analysis of gypsum recycling processes. Analysis in synchrotron X-rays, Raman- and UV-vis spectroscopy are made possible with this compact and mobile setup. First results from Raman spectroscopy on the conversion of gypsum to bassanite in hypersaline solutions are presented and future plans on optimization are formulated.
T2 - ANAKON 2025
CY - Leipzig, Germany
DA - 10.03.2025
KW - Recycling
KW - Automation
KW - Synchrotron-X-ray-diffraction
KW - Raman-spectroscopy
KW - Gypsum
PY - 2025
AN - OPUS4-62706
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 - Ghiringhelli, Luca M.
A1 - Baldauf, Carsten
A1 - Bereau, Tristan
A1 - Brockhauser, Sandor
A1 - Carbogno, Christian
A1 - Chamanara, Javad
A1 - Cozzini, Stefano
A1 - Curtarolo, Stefano
A1 - Draxl, Claudia
A1 - Dwaraknath, Shyam
A1 - Fekete, Ádám
A1 - Kermode, James
A1 - Koch, Christoph T.
A1 - Kühbach, Markus
A1 - Ladines, Alvin Noe
A1 - Lambrix, Patrick
A1 - Himmer, Maja-Olivia
A1 - Levchenko, Sergey V.
A1 - Oliveira, Micael
A1 - Michalchuk, Adam
A1 - Miller, Ronald E.
A1 - Onat, Berk
A1 - Pavone, Pasquale
A1 - Pizzi, Giovanni
A1 - Regler, Benjamin
A1 - Rignanese, Gian-Marco
A1 - Schaarschmidt, Jörg
A1 - Scheidgen, Markus
A1 - Schneidewind, Astrid
A1 - Sheveleva, Tatyana
A1 - Su, Chuanxun
A1 - Usvyat, Denis
A1 - Valsson, Omar
A1 - Wöll, Christof
A1 - Scheffler, Matthias
T1 - Shared metadata for data-centric materials science
N2 - The expansive production of data in materials science, their widespread sharing and repurposing requires educated support and stewardship. In order to ensure that this need helps rather than hinders scientific work, the implementation of the FAIR-data principles (Findable, Accessible, Interoperable, and Reusable) must not be too narrow. Besides, the wider materials-science community ought to agree on the strategies to tackle the challenges that are specific to its data, both from computations and experiments. In this paper, we present the result of the discussions held at the workshop on “Shared Metadata and Data Formats for Big-Data Driven Materials Science”. We start from an operative definition of metadata, and the features that a FAIR-compliant metadata schema should have. We will mainly focus on computational materials-science data and propose a constructive approach for the FAIRification of the (meta)data related to ground-state and excited-states calculations, potential-energy sampling, and generalized workflows. Finally, challenges with the FAIRification of experimental (meta)data and materials-science ontologies are presented together with an outlook of how to meet them.
KW - Library and Information Sciences
KW - Statistics, Probability and Uncertainty
KW - Computer Science Applications
KW - Education
KW - Information Systems
KW - Statistics and Probability
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584846
DO - https://doi.org/10.1038/s41597-023-02501-8
VL - 10
IS - 1
SP - 1
EP - 18
PB - Springer Science and Business Media LLC
AN - OPUS4-58484
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 - Michalchuk, Adam
T1 - On the physical processes of mechanochemically induced transformations in molecular solids
N2 - Initiating or sustaining physical and chemical transformations with mechanical force – mechanochemistry – provides an opportunity for more sustainable chemical processes, and access to new chemical reactivity.
KW - Molecular solids
KW - Transformation
KW - Destabilisation
KW - Instabilities
KW - Common phenomenon
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621755
DO - https://doi.org/10.1039/d4cc04062g
IS - 99
SP - 1
EP - 12
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-62175
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Driscoll, Laura L.
A1 - Driscoll, Elizabeth H.
A1 - Dong, Bo
A1 - Sayed, Farheen N.
A1 - Wilson, Jacob N.
A1 - O’Keefe, Christopher A.
A1 - Gardner, Dominic J.
A1 - Grey, Clare P.
A1 - Allan, Phoebe K.
A1 - Michalchuk, Adam
A1 - Slater, Peter R.
T1 - Under pressure: offering fundamental insight into structural changes on ball milling battery materials
N2 - Synthesis of Li ion battery materials via ball milling has been a huge area of growth, leading to new high-capacity electrode materials, such as a number of promising disordered rocksalt (DRS) phases. In prior work, it was generally assumed that the synthesis was facilitated simply by local heating effects during the milling process. In this work, we show that ball milling Li2MoO4 leads to a phase transformation to the high pressure spinel polymorph and we report electrochemical data for this phase. This observation of the formation of a high pressure polymorph shows that local heating effects alone cannot explain the phase transformation observed (phenakite to spinel) and so indicates the importance of other effects. In particular, we propose that when the milling balls collide with the material, the resulting shockwaves exert a localised pressure effect, in addition to local heating. To provide further support for this, we additionally report ball milling results for a number of case studies (Li2MnO3, Li2SnO3, Nb2O5) which reinforces the conclusion that local heating alone cannot explain the phase transformations observed. The work presented thus provides greater fundamental understanding of milling as a synthetic pathway and suggests potential strategies to prepare such samples without milling (e.g., doping to create internal chemical pressure). In addition, we suggest that further research is needed into the effect of the use of milling as a route to smaller particles, since we believe that such milling may also be affecting the surface structure of the particles through the influence of the shockwaves generated.
KW - Pollution
KW - Nuclear Energy and Engineering
KW - Sustainability and the Environment
KW - Environmental Chemistry
KW - Renewable Energy
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590086
DO - https://doi.org/10.1039/d3ee00249g
VL - 16
IS - 11
SP - 5196
EP - 5209
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59008
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 - JOUR
A1 - Linberg, Kevin
A1 - Szymoniak, Paulina
A1 - Schönhals, Andreas
A1 - Emmerling, Franziska
A1 - Michalchuk, Adam
T1 - The Origin of Delayed Polymorphism in Molecular Crystals Under Mechanochemical Conditions
N2 - We show that mechanochemically driven polymorphic transformations can require extremely long induction periods, which can be tuned from hours to days by changing ball milling energy. The robust design and interpretation of ball milling experiments must account for this unexpected kinetics that arises from energetic phenomena unique to the solid state. Detailed thermal analysis, combined with DFT simulations, indicates that these marked induction periods are associated with processes of mechanical activation. Correspondingly, we show that the pre‐activation of reagents can also lead to marked changes in the length of induction periods. Our findings demonstrate a new dimension for exerting control over polymorphic transformations in organic crystals. We expect mechanical activation to have a much broader implication across organic solid‐state mechanochemistry.
KW - General Chemistry
KW - Catalysis
KW - Organic Chemistry
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589219
DO - https://doi.org/10.1002/chem.202302150
SN - 0947-6539
SP - e202302150
PB - Wiley
AN - OPUS4-58921
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Michalchuk, Adam
A1 - Delogu, Francesco
T1 - Fundamental basis of mechanochemical reactivity
N2 - This themed collection includes a collection of articles on the fundamental basis of mechanochemical reactivity.
KW - Mechanochemical
KW - Metal-organic
KW - Transformation
KW - Dimerization
PY - 2024
DO - https://doi.org/10.1039/d4cp90153c
SP - 1
EP - 3
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-61500
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 - RPRT
A1 - Kittner, Maria
A1 - Altmann, Korinna
A1 - Hamann, Sven
A1 - Weyer, Rüdiger
A1 - Kalbe, Ute
T1 - Bewertung der Freisetzung von Mikroplastik aus Sportböden auf Kunststoffbasis - Abschlussbericht
N2 - Die Europäische Kommission hat 2023 ein Verbot zum bewussten Austrag von Mikroplastik (MP) in die Umwelt beschlossen, das auch für die Verwendung von synthetischen Gummi-Granulaten (v. a. EPDM) in Sportböden gilt. In Deutschland gibt es laut DFB ca. 5100 Kunstrasenplätze. In der EU beläuft sich die Anzahl laut ECHA auf 13,000 Kunstrasen- und 47,000 Bolzplätze, Tendenz steigend. Das Hauptziel des Projektes war es daher, eine Massenbilanz für die Freisetzung von MP zu erstellen, um so eine Schätzung des MP-Austrags pro Kunstrasenplatz und Jahr zu ermöglichen. Dafür werden die MP-Emissionen von drei Kunstrasenszenarien in verschiedenen Zuständen (ungealtert, künstlich gealtert und in Echtzeit gealtert) verglichen: die Vergangenheit (Kunstrasen: fossilbasiert, EPDM-Füllung), die Gegenwart (der in Europa am häufigsten installierte Rasen) und die Zukunft (Rasen mit recycelten Grasfasern, keine synthetische Füllung sondern z.B. Quarzsand oder Korkschrott). Dazu werden fabrikneue Kunststoffrasen und EPDM-Granulat unter Laborbedingungen beschleunigt gealtert, um die Freiland-Beanspruchung eines Kunststoffrasens in circa 15 Jahren abzubilden. Die Verwendung spezieller Mikrofiltertiegel in Lysimeter-Experimenten ermöglicht die Abschätzung der Partikelgrößen des emittierten MP, was eine Grundbedingung für die Bewertung einer potenziellen Gesundheitsgefährdung für Menschen ist. Ergänzend wurden weitere umweltrelevante Schadstoffausträge aus den Kunststoffrasen quantifiziert.
KW - Mikroplastik
KW - Kunststoffrasen
KW - Schadstoffe
KW - Bewitterung
KW - Lysimeter
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633114
DO - https://doi.org/10.26272/opus4-63311
N1 - Das Projekt wurde gefördert vom Bundesinstitut für Bau-, Stadt- und Raumforschung (BBSR) im Auftrag des Bundesministeriums für Wohnen, Stadtentwicklung und Bauwesen (BMWSB) aus Mitteln des Innovationsprogramms Zukunft Bau. Aktenzeichen: FKZ 10.08.18.7-22.02. Projektlaufzeit: 09.2022 bis 03.2025.
SP - 1
EP - 75
PB - Bundesanstalt für Materialforschung und -prüfung (BAM)
CY - Berlin
AN - OPUS4-63311
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - INPR
A1 - Miliūtė, Aistė
ED - Bustamante, Joana
ED - Karafiludis, Stephanos
ED - Zöllner, Moritz
ED - Eddah, Mustapha
ED - Emmerling, Franziska
ED - Mieller, Björn
ED - George, Janine
ED - Stawski, Tomasz
T1 - Synthesis and phase purity of the negative thermal expansion material ZrV2O7
N2 - 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 the purity and homogeneity of ZrV2O7 samples. Our findings indicate that different synthesis methods significantly impact the material's characteristics. The solid-state reaction provided high-purity material through extended milling time and repeated calcination cycles, while the sol-gel reaction enabled a “near-atomic” level of mixing and, therefore, homogenous phase-pure ZrV2O7. We confirmed purity via X-ray diffraction and Raman spectroscopy, highlighting differences between phase-pure and multiphase ceramics. These analytical techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, we were able to interpret the Raman spectra and visualise Raman active atom vibrations. We show that phase purity enables the unbiased characterisation of material properties such as negative thermal expansion.
KW - NTE
KW - Sol-gel
KW - Solid-state
KW - Ab-initio
KW - XRD
KW - Raman
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613643
DO - https://doi.org/10.26434/chemrxiv-2024-d4sj9
SN - 2573-2293
VL - 2024
SP - 1
EP - 60
PB - American Chemical Society
CY - Washington, D.C.
AN - OPUS4-61364
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dorau, Kristof
A1 - Rückamp, Daniel
A1 - Weber, Christian
A1 - Scheeder, Georg
A1 - Reßing, Ronja
A1 - Peth, Stephan
A1 - Otto, Philipp
A1 - Altmann, Korinna
A1 - Fries, Elke
A1 - Hoppe, Martin
T1 - Characterization and spatial distribution of mesoplastics in an arable soil
N2 - AbstractExtraction of plastic particles from soil is challenging and, thus, exceptionally little spatial information on plastic distribution at the field scale has been gathered. However, for environmental risk assessment, adequate sampling should complement coherent plastic profiling. In this study, we investigated the spatial distribution of mesoplastics (MePs; from 5 mm up to 130 mm) in arable soil (Haplic Cambisol) managed intensively by 12 years of compost application. Geo‐referenced samples (n = 128) and five different sampling designs (n = 45) of variable sampling volume (from 2 to 300 L) were collected at a three hectare study site in Northern Germany (0–30 cm soil depth). Soil properties such as pH and soil organic carbon (SOC) were measured to evaluate dispersion measures of these data. In total, we found 259 MePs with a predominance of transparent packaging foils made of polyethylene and coloured fibres of polypropylene. Average particle metrics were a projection area of 47 (3–400) mm2, a Feret diameter of 18.5 (5.4–130) mm and a mass of 1.89 (0.11–221) mg. Caution is advised when measuring the particle mass due to still strongly adhering soil material, especially for fibre bundles with 0.544 mg soil mg−1 particle. We recommend using a 0.1 mol L−1 tetrasodium pyrophosphate solution to purify MePs by removing attached soil before weighing for further environmental risk assessment. The MePs count with a median value of 0.50 (0–3.2) particles kg−1 and median mass of 2.26 (0–221) mg kg−1 featured the highest coefficient of variation (CV) with 103% and 187%, respectively. This is 10–20 times larger in comparison to the CV of SOC (9.2%) and even 50–93 times larger than CV of soil pH (2.2%). This leads to the need of larger sample numbers to delineate plastic metrics in comparison with soil properties to identify a reliable mean value of the field within a predefined allowable error. Mesoplastics in the soil were characterized by a pure nugget effect variogram (no spatial correlation), revealed no intrafield variability and the sample volume yielded inconclusive results. Sampling for plastics in soil should either (i) drastically increase the sample number for a single field or (ii) communicate transparently that the allowable error is by far enhanced in comparison with classical soil properties like pH and SOC. More systematic studies featuring geo‐spatial analysis of MePs and smaller‐sized plastics in soils are required to propose adequate sampling designs across multiple land uses and plastics fingerprints. A larger database would, thereupon, pave the way for best‐practice guides on how to treat ‘outliers’ and search for robust estimators for spatial mapping of plastics in soils.
KW - Large microplastics
KW - Microplastics
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-617772
DO - https://doi.org/10.1111/ejss.70016
VL - 75
IS - 6
SP - 1
EP - 16
PB - Wiley
AN - OPUS4-61777
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gugin, Nikita
A1 - Yusenko, Kirill
A1 - King, Andrew
A1 - Meyer, Klas
A1 - Al-Sabbagh, Dominik
A1 - Villajos Collado, José Antonio
A1 - Emmerling, Franziska
T1 - Lighting up industrial mechanochemistry: Real-time in situ monitoring of reactive extrusion using energy-dispersive X-ray diffraction
N2 - Mechanochemistry is an environmentally friendly synthetic approach that enables the sustainable production of a wide range of chemicals while reducing or eliminating the need for solvents. Reactive extrusion aims to move mechanochemistry from its conventional gram-scale batch reactions, typically performed in laboratory ball mills, to a continuous, large-scale process. Meeting this challenge requires in situ monitoring techniques to gain insights into reactive extrusion and its underlying processes. While the effectiveness of in situ Raman spectroscopy in providing molecular-level information has been demonstrated, our study uses energy-dispersive X-ray diffraction to monitor reactive extrusion in real time at the crystalline level. Our results provide previously unavailable control over the reactive extrusion process, promoting its perception as an industrially feasible green alternative to traditional solvent-based syntheses.
KW - Mechanochemistry
KW - Reactive extrusion
KW - Green chemistry
KW - In situ studies
KW - Time-resolved in situ
KW - TRIS
KW - Synchrotron radiation
KW - Scalable synthesis
KW - Solid-state reactions
KW - Reaction mechanisms
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613969
DO - https://doi.org/10.1016/j.chempr.2024.07.033
VL - 10
IS - 11
SP - 1
EP - 16
PB - Elsevier B.V.
AN - OPUS4-61396
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wimmer, L
A1 - Hoang, M V N
A1 - Schwarzinger, J
A1 - Jovanovic, V
A1 - Adelkovic, B
A1 - Velickovic, T C
A1 - Meisel, T C
A1 - Waniek, T
A1 - Weimann, Christiane
A1 - Altmann, Korinna
A1 - Dailey, L A
T1 - A quality-by-design inspired approach to develop PET and PP nanoplastic test materials for use in in vitro and in vivo biological assays
N2 - Micro- and nanoplastics have become environmental pollutants of concern, receiving increased attention from consumers, scientists, and policymakers. The lack of knowledge about possible impacts on wildlife and human health requires further research, for which well-characterized testmaterials are needed. A quality-bydesign (QbD) driven approachwas used to produce sterile, endotoxinmonitored nanoplastics of polyethylene terephthalate (PET) and polypropylene (PP) with a size fraction of >90% below 1 μm and high yield of >90%. Glycerol was used as a versatile and biocompatible liquid storage medium which requires no further exogenous dispersing agent andmaintained colloidal stability, sterility (0 CFU mL−1), and low endotoxin levels (<0.1 EU mL−1) for more than one year of storage at room temperature. Further, the glycerol vehicle showed no biological effect on the tested human bronchial cell line Calu-3 up to 0.8% (w/v). Given the concentration of 40 mg g−1 nanoplastics in the glycerol stock, this corresponds to a nanoplastic concentration of 320 μg mL−1. The surfactant-free nanoplastics are dispersible in bio-relevant media from the glycerol stock without changing size characteristics and are suitable for in vitro and in vivo research.
KW - Microplastics
KW - Reference materials
KW - Nanoplastics
KW - Polymer 3R
KW - Glycerol
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629934
DO - https://doi.org/10.1039/D4EN01186D
SN - 2051-8161
VL - 12
IS - 5
SP - 2667
EP - 2686
PB - Royal Society of Chemistry
CY - Cambridge
AN - OPUS4-62993
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Starkholm, A.
A1 - Al-Sabbagh, Dominik
A1 - Sarisozen, S
A1 - von Reppert, A
A1 - Rössle, M
A1 - Ostermann, Markus
A1 - Unger, E
A1 - Emmerling, Franziska
A1 - Kloo, L
A1 - Svensson, P
A1 - Lang, F
A1 - Maslyanchuk, O.
T1 - Green Fabrication of Sulfonium-Containing Bismuth Materials for High-Sensitivity X-Ray Detection
N2 - Organic–inorganic hybrid materials based on lead and bismuth have recently been proposed as novel X- and gamma-ray detectors for medical imaging, non-destructive testing, and security, due to their high atomic numbers and facile preparation compared to traditional materials like amorphous selenium and Cd(Zn)Te. However, challenges related to device operation, excessively high dark currents, and long-term stability have delayed commercialization. Here, two novel semiconductors incorporating stable sulfonium cations are presented, [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5, synthesized via solvent-free ball milling and fabricated into dense polycrystalline pellets using cold isostatic compression, two techniques that can easily be upscaled, for X-ray detection application. The fabricated detectors exhibit exceptional sensitivities (14 100–15 190 µC Gyair−1 cm−2) and low detection limits (90 nGyair s−1 for [(CH3CH2)3S]6Bi8I30 and 78 nGyair s−1 for [(CH3CH2)3S]AgBiI5), far surpassing current commercial detectors. Notably, they maintain performance after 9 months of ambient storage. The findings highlight [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5 as scalable, cost-effective and highly stable alternatives to traditional semiconductor materials, offering great potential as X-ray detectors in medical and security applications.
KW - Mechanochemistry
KW - X-ray detectors
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630306
DO - https://doi.org/10.1002/adma.202418626
SP - 1
EP - 10
PB - Wiley VHC-Verlag
AN - OPUS4-63030
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez-Sánchez, Noelia
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Prinz, Carsten
A1 - Prieto-Laria, P.
A1 - Ruiz-Salvador, A.R.
A1 - Ballesteros, M.
T1 - Engineering a multivariate cobalt metal–organic framework for high photocatalytic activity: the impact of mixed ligands and metal incorporation in a visible light-driven heterogeneous photo-Fenton reaction for water treatment
N2 - Metal–organic frameworks (MOFs) have attracted increasing attention for the removal of organic pollutants in wastewater via photocatalysis. Here, we design a multivariate modification of ZIF-9 to tune its electronic properties for use in visible light photocatalysis. A controllable synthesis of ZIF-9 and its multivariate forms with the incorporation of copper and the 2-imidazolecarboxaldehyde (ica) ligand was carried out. The materials are tested for the removal of the model dye methylene blue (MB) by a heterogeneous photo-Fenton-like reaction at neutral pH and room temperature. Cu-ZIF-9-ica (UPO-3) shows high photocatalytic activity under both visible and ultraviolet A (UVA) light, achieving 94% MB degradation in 45 min, compared to 65% MB degradation in 120 min using bare ZIF-9. The study revealed a first-order rate constant of 0.0475 min−1 for Cu-ZIF-9-ica compared to 0.0088 min−1 for ZIF-9 under visible light. The improvement of the catalyst was clearly attributed to the co-incorporation of Cu and the ica ligand in the MOF, which reduces the band gap, in agreement with DFT calculations. Reproducibility and recyclability tests proved that Cu-ZIF-9-ica can be used for at least 3 cycles without a significant loss of efficiency, making it a promising material for the study and application of wastewater treatment.
KW - Metal-Organic Framework (MOF)
KW - Heterogeneous photo-Fenton
KW - ZIF-9
KW - Methylene Blue
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630797
DO - https://doi.org/10.1039/d4na00954a
SN - 2516-0230
VL - 7
IS - 8
SP - 2255
EP - 2265
PB - Royal Society of Chemistry
AN - OPUS4-63079
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Visileanu, Emilia
A1 - Catalin Grosu, Marian
A1 - Tiberiu Miclea, Paul
A1 - Altmann, Korinna
A1 - Brossell, Dirk
T1 - Methods for the collection and characterization of airborne particles in the textile industry
N2 - Airborne particulate matter is one of the main air pollutants. Their impact on mortality, and the occurrence of pulmonary and cardiovascular complications, have been the subject of numerous studies. Airborne particles are complex mixtures of organic and inorganic substances from different sources of particle emissions. Particulate Matter (PM) particles are classified according to their aerodynamic diameter expressed in µm and can vary from coarse (PM 10) to fine (less than PM 2.5). These diameter considerations are fundamental because they condition the penetration of particles into the bronchopulmonary system and the body. In recent years, there has been an interest in so-called “ultra-fine” particles, with a diameter of 0.1 µm (or 100 nm), or PM 0.1. They are nanoparticles and their impact on human health is not yet clear.With more than 1.5 million employees, textiles and clothing is a diverse sector that plays an important role in the European manufacturing industry, producing a turnover of €162 billion.An important component of the solid particles that generate air pollution in the textile industry is microplastics (MP) and nano plastics (NP), which also include microfibers (<5mm) and nanofibers (<100 nm), respectively. The particles released into the air during fiber and yarn processing range from 1 µg/m3 to 50 µg/m3.The paper presents the results of the determination of indoor and outdoor air concentration levels in textile companies, to identify the areas with the highest concentration level, by using an online recording system such as the Laser Aerosol Spectrometer MINI LAS model 11-E. The total concentration level TSP (µg/m3), the fractions PM 10(µg/m3), PM 2.5(µg/m3), PM1(µg/m3), as well as the total number of particles TC (1/l), were shown. It was noted that TSP is approximately at the same level both indoors and outdoors, but the fractions of PM10, PM2.5, and PM1 have much higher values indoors than outdoors with possible consequences on workers' health.The next step was the collection of fibers, namely micro and nano plastic particles from the vicinity of the workplaces of polyester, polyamide, and polypropylene fibers processing units in the textile industry in Romania, to obtain a sufficient quantity for laboratory analysis to determine the size and shape of the particles as well as their chemical composition. Two types of pumps were used, differentiated by their operating parameters: TECORA SKYPOST with airflow of 38 l/min and GILAIRPLUS with airflow 2l/min. Filters made of different materials with different diameters and pore sizes were used, namely: quartz filters (ø 47 mm, and ø 37 mm) on a TECORA SKYPOST type pump, polycarbonate nucleopore coated with a gold membrane (ø 25 mm) and silica filter (ø 9 mm) on GILAIRPLUS type pump.Using descriptive statistics, the calculation of correlation coefficients highlighted a strong correlation between the variables: "Collected mass/ Air concentration" and "Collected mass/ Air volume" for all diameters of the filters.The highest collected particle volume, determined by weighing the filters before and after collection, was obtained with the quartz filters (ø 47 mm) at an airflow of 38 l/min. The particles collected (polyester, polyamide, polypropylene) in the first stage were analyzed by SEM and thermogravimetric and it was found that the quartz filters absorbed the particles inside, with very few remaining on the surface. Thus no known methods can be used to perform analysis for particles collected on quartz filters. The number of particles on the filters was insufficient for analysis either because of the collection parameters used or because of the loss of particles during transport. As a result, in the next step, the use of 9 mm Si filters using the GILAIRPLUS pump at an airflow rate of 2l/min was chosen.To improve the transport conditions and avoid the loss of the particles and keep them on the surface of the filters, two methods were applied:- after weighing the filters were reintroduced into the collection pump holder;- a filtration system for airborne micro-nano plastics was designed and manufactured to selectively collect and transport PM10 and PM1 particles collected on SI filters.In both cases, SEM, Raman mapping, and GS-MS microscopy were used for analysis.Several times more PM10 than PM1 (74.5µg compared to 12.5 µg) was found. In all cases, both particles and fibers showed the same Raman fingerprint.The GS-MS analyses showed some contamination of the workspaces with particles other than the processed fibers. The presence of non-notifiable substances was also observed.The most viable filters are Si filters with a pore size of 10 microns to 1 micron and the use of the selected collection and transport filter system. In the following a filter system will be applied for collection on Au membrane-coated polycarbonate filters.
T2 - 5th International Conference on Human Systems Engineering and Design: Future Trends and Applications (IHSED 2023)
KW - Microplastics
KW - Textiles
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624442
DO - https://doi.org/10.54941/ahfe1004132
VL - 112
SP - 212
EP - 223
PB - AHFE International
AN - OPUS4-62444
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Ciornii, Dmitri
T1 - Identification of toxicologically relevant functional groups on micro- and nanoplastic particles’ surface by means of X-Ray photoelectron spectroscopy
N2 - Microplastic and nanoplastic particles (MNP) are spread all over the world in various types, shapes and sizes making it very challenging to accurately analyse them. Each sampling procedure, sample preparation method and detection technique needs suitable reference materials to validate the method for accurate results. Furthermore, the effects of these MNPs should be evaluated by risk and hazard assessment with test particles close to reality. To better understand MNP behavior and aid in clarification of their interactions with organisms, we produced several MNP materials by top-down procedure and characterized their properties. Since surface properties mostly determine particles’ toxicity, the aim of the present study was to determine which functional groups are present on MNPs and how the surface can be affected by the production process and particle’s environment.
T2 - SETAC 34th Meeting
CY - Seville, Spain
DA - 05.05.2024
KW - Microplastics
KW - Nanoplastics
KW - Polypropylene
KW - XPS
KW - SEM
PY - 2024
AN - OPUS4-60037
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Altmann, Korinna
T1 - Realitätsnahe Referenzmaterialien für die Mikroplastik-Analytik und Vergleichsuntersuchungen
N2 - Zur Validierung und Harmonisierung von verschiedenen Methoden in der Mikroplastik-Analytik werden polymere Referenzmaterialien benötigt. In diesem Vortrag wird dargestellt, was bisher an der BAM zu Referenzmaterialien für die Mikroplastik-Analytik entwickelt wurde, wo es hingehen soll und ein Überblick über bisher gelaufene Vergleichsuntersuchungen gebracht.
T2 - Kick-off Meeting "Mikroplastik in Lebensmitteln"
CY - Online meeting
DA - 03.12.2020
KW - Mikroplastik
KW - Referenzmaterial
KW - Vergleichsuntersuchungen
KW - Ringversuche
PY - 2020
AN - OPUS4-51743
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tscheuschner, Georg
A1 - Ponader, Marco
A1 - Raab, Christopher
A1 - Weider, Prisca S.
A1 - Hartfiel, Reni
A1 - Kaufmann, Jan Ole
A1 - Völzke, Jule L.
A1 - Bosc-Bierne, Gaby
A1 - Prinz, Carsten
A1 - Schwaar, T.
A1 - Andrle, Paul
A1 - Bäßler, Henriette
A1 - Nguyen, Khoa
A1 - Zhu, Y.
A1 - Mey, A. S. J. S.
A1 - Mostafa, A.
A1 - Bald, I.
A1 - Weller, Michael G.
T1 - Efficient Purification of Cowpea Chlorotic Mottle Virus by a Novel Peptide Aptamer
N2 - The cowpea chlorotic mottle virus (CCMV) is a plant virus explored as a nanotechnological platform. The robust self-assembly mechanism of its capsid protein allows for drug encapsulation and targeted delivery. Additionally, the capsid nanoparticle can be used as a programmable platform to display different molecular moieties. In view of future applications, efficient production and purification of plant viruses are key steps. In established protocols, the need for ultracentrifugation is a significant limitation due to cost, difficult scalability, and safety issues. In addition, the purity of the final virus isolate often remains unclear. Here, an advanced protocol for the purification of the CCMV from infected plant tissue was developed, focusing on efficiency, economy, and final purity. The protocol involves precipitation with PEG 8000, followed by affinity extraction using a novel peptide aptamer. The efficiency of the protocol was validated using size exclusion chromatography, MALDI-TOF mass spectrometry, reversed-phase HPLC, and sandwich immunoassay. Furthermore, it was demonstrated that the final eluate of the affinity column is of exceptional purity (98.4%) determined by HPLC and detection at 220 nm. The scale-up of our proposed method seems to be straightforward, which opens the way to the large-scale production of such nanomaterials. This highly improved protocol may facilitate the use and implementation of plant viruses as nanotechnological platforms for in vitro and in vivo applications.
N2 - Das Cowpea Chlorotic Mottle Virus (CCMV) ist ein Pflanzenvirus, das als nanotechnologische Plattform erforscht wird. Der robuste Selbstorganisationsmechanismus seines Kapsidproteins ermöglicht die Verkapselung und gezielte Abgabe von Medikamenten. Darüber hinaus kann das Kapsid-Nanopartikel als programmierbare Plattform für die Präsentation verschiedener molekularer Komponenten verwendet werden. Im Hinblick auf künftige Anwendungen ist eine effiziente Produktion und Reinigung von Pflanzenviren von entscheidender Bedeutung. In etablierten Protokollen stellt die notwendige Ultrazentrifugation aufgrund von Kosten, schwieriger Skalierbarkeit und Sicherheitsaspekten eine erhebliche Einschränkung dar. Darüber hinaus bleibt die Reinheit des endgültigen Virusisolats oft unklar. Hier wurde ein fortschrittliches Protokoll für die Reinigung von CCMV aus infiziertem Pflanzengewebe entwickelt, wobei der Schwerpunkt auf Effizienz, Wirtschaftlichkeit und Reinheit lag. Das Protokoll beinhaltet eine Fällung mit Polyethylenglycol (PEG 8000), gefolgt von einer Affinitätsextraktion mit einem neuartigen Peptid-Aptamer. Die Effizienz des Protokolls wurde mithilfe von Größenausschluss-Chromatographie (SEC), MALDI-TOF-Massenspektrometrie, Umkehrphasen-HPLC und Sandwich-Immunoassay validiert. Darüber hinaus wurde nachgewiesen, dass das endgültige Eluat der Affinitätssäule eine außergewöhnliche Reinheit (98,4 %) aufweist, die durch HPLC und Detektion bei 220 nm bestimmt wurde. Die Skalierung der von uns vorgeschlagenen Methode scheint einfach zu sein, was den Weg für eine größer angelegte Produktion solcher Nanomaterialien ebnet. Dieses stark verbesserte Protokoll könnte die Verwendung und Umsetzung von Pflanzenviren als nanotechnologische Plattformen für In-vitro- und In-vivo-Anwendungen erleichtern.
KW - Affinity chromatography
KW - Nanoparticles
KW - Nanoscience
KW - Carrier protein
KW - Encapsulation
KW - Combinatorial peptide library
KW - Peptide binder
KW - Vigna unguiculata
KW - Augenbohne
KW - Schlangenbohne
KW - Pflanzenvirus
KW - Plant virus
KW - Upscaling
KW - Commercialization
KW - Reference material
KW - Nanocarrier
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572645
DO - https://doi.org/10.3390/v15030697
VL - 15
IS - 3
SP - 1
EP - 24
PB - MDPI
CY - Basel, Schweiz
AN - OPUS4-57264
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Liu, Yanchen
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Montoro, Luciano A.
A1 - Liu, Hao
A1 - Liu, Ye
A1 - Emmerling, Franziska
A1 - Russo, Patrícia A.
A1 - Pinna, Nicola
T1 - A partially disordered crystallographic shear block structure as fast-charging negative electrode material for lithium-ion batteries
N2 - A well-ordered crystalline structure is crucial in battery electrodes, as the dimensionality and connectivity of the interstitial sites inherently influence Li+ ions diffusion kinetics. Niobium tungsten oxides block structures, composed of ReO3-type blocks of specific sizes with well-defined metal sites, are promising fast-charging negative electrode materials. Structural disorder is generally detrimental to conductivity or ion transport. However, here, we report an anomalous partially disordered Nb12WO33 structure that significantly enhances Li-ion storage performance compared to the known monoclinic Nb12WO33 phase. The partially disordered phase consists of corner-shared NbO6 octahedra blocks of varied sizes, including 5×4, 4×4, and 4×3, with a disordered arrangement of distorted WO4 tetrahedra at the corners of the blocks. This structural arrangement is robust during lithiation/delithiation, exhibiting minor local structure changes during cycling. It enables accelerated Li-ion migration, resulting in promising fast-charging performance, namely, 62.5 % and 44.7 % capacity retention at 20 C and 80 C, respectively. This study highlights the benefits of introducing disorder into niobium tungsten oxide shear structures, through the establishment of clear structure-performance correlations, offering guidelines for designing materials with targeted properties.
KW - Lithium ion batteries
KW - Oxides
KW - XANES
KW - XRD
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637994
DO - https://doi.org/10.1038/s41467-025-61646-9
SN - 2041-1723
VL - 16
IS - 1
SP - 1
EP - 15
PB - Springer Science and Business Media LLC
AN - OPUS4-63799
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heinekamp, Christian
A1 - Roy, Arkendu
A1 - Karafiludis, Stephanos
A1 - Kumar, Sourabh
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Stawski, Tomasz M.
A1 - Miliūtė, Aistė
A1 - von der Au, Marcus
A1 - Ahrens, Mike
A1 - Braun, Thomas
A1 - Emmerling, Franziska
T1 - Zirconium fluoride-supported high-entropy fluoride: a catalyst for enhanced oxygen evolution reaction
N2 - 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 electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDX) as well as inductively coupled plasma-mass spectrometry (ICP-MS). Additional investigations on the local structure were performed using extended X-ray absorption fine structure spectroscopy (EXAFS) and pair distribution function (PDF) analysis. The catalyst shows significant potential for oxygen evolution reaction (OER) in alkaline media with a current density of 100 mA cm−2 at approximately 1.60 V, thus outperforming benchmark materials such as IrO2, despite a significant reduction in electrochemical mass loading. A potential mechanism is suggested based on free energy calculation using DFT calculations.
KW - OER
KW - HEA
KW - CCMAT
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637116
DO - https://doi.org/10.1039/D4TA08664C
SN - 2050-7488
VL - 13
IS - 26
SP - 20383
EP - 20393
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-63711
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dittmar, Stefan
A1 - Weyrauch, Steffen
A1 - Reemtsma, Thorsten
A1 - Eisentraut, Paul
A1 - Altmann, Korinna
A1 - Ruhl, Aki S.
A1 - Jekel, Martin
T1 - Settling Velocities of Tire and Road Wear Particles: Analyzing Finely Graded Density Fractions of Samples from a Road Simulator and a Highway Tunnel
N2 - The terminal settling velocity is considered the most critical parameter determining the transport of tire and road wear particles (TRWP) in aquatic environments. Nonetheless, no respective empirical data has been reported so far. In this study, particle samples from a road simulator and a highway tunnel were investigated with a validated imaging method. Different density and size fractions of both samples were measured separately, acquiring sizes and settling velocities of more than 30,000 individual particles. In addition, tire marker polymers were analyzed for each fraction via thermal extraction desorption-gas chromatography/mass spectrometry. Finally, the acquired particle data was combined according to the fractions’ estimated tire contents in order to deduce detailed probability distributions of particle size and settling velocity for the actual TRWP from both samples. Weighted by TRWP-incorporated tire mass, median diameters of 54 and 44 μm as well as median settling velocities of 0.65 and 0.22 mm/s were found for TRWP from the road simulator and highway tunnel, respectively. This study thus provides the first ever empirical data on TRWP settling velocities in water, which can be highly valuable input for modeling the environmental transport of TRWP and for dimensioning TRWP retention systems.
KW - Microplastics
KW - TED-GC/MS
KW - Sinking velocities
KW - Transport
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635449
DO - https://doi.org/10.1021/acs.est.5c04165
SN - 0013-936X
VL - 59
IS - 26
SP - 13434
EP - 13446
PB - American Chemical Society (ACS)
AN - OPUS4-63544
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Das, Prasenjit
A1 - Chakraborty, Gouri
A1 - Yang, Jin
A1 - Roeser, Jérôme
A1 - Küçükkeçeci, Hüseyin
A1 - Nguyen, Anh Dung
A1 - Schwarze, Michael
A1 - Gabriel, Jose
A1 - Penschke, Christopher
A1 - Du, Shengjun
A1 - Weigelt, Vincent
A1 - Khalil, Islam E.
A1 - Schmidt, Johannes
A1 - Saalfrank, Peter
A1 - Oschatz, Martin
A1 - Rabeah, Jabor
A1 - Schomäcker, Reinhard
A1 - Emmerling, Franziska
A1 - Thomas, Arne
T1 - The Effect of Pore Functionality in Multicomponent Covalent Organic Frameworks on Stable Long‐Term Photocatalytic H2 Production
N2 - AbstractIn nature, organic molecules play a vital role in light harvesting and photosynthesis. However, regarding artificial water splitting, the research focus is primarily on inorganic semiconductors. Although organic photocatalysts have high structural variability, they tend to exhibit lower quantum efficiencies for water splitting than their inorganic counterparts. Multicomponent reactions (MCRs) offer an attractive route to introduce different functional units into covalent organic frameworks (COFs) and enable semiconducting properties and high chemical stability, creating promising materials for long‐term photocatalytic applications, such as H2 production. Herein, five highly crystalline donor‐acceptor based, 4‐substituted quinoline‐linked MCR‐COFs are presented that are prepared via the three‐component Povarov reaction. The pore functionality is varied by applying different vinyl derivatives (e.g., styrene, 2‐vinyl pyridine, 4‐vinylpyridine, 4‐vinyl imidazole, 2,3,4,5,6‐pentafluorostyrene), which has a strong influence on the obtained photocatalytic activity. Especially an imidazole‐functionalized COF displays promising photocatalytic performance due to its high surface area, crystallinity, and wettability. These properties enable it to maintain its photocatalytic activity even in a membrane support. Furthermore, such MCR‐COFs display dramatically enhanced (photo)chemical stability even after long‐term solar light irradiation and exhibit a high and steady H2 evolution for at least 15 days.
KW - Sstability
KW - Covalent organic frameworks
KW - Pore functionality
KW - Long-term H2 production
KW - Multicomponent reactions
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639787
DO - https://doi.org/10.1002/aenm.202501193
SN - 1614-6832
SP - 1
EP - 10
PB - Wiley VHC-Verlag
AN - OPUS4-63978
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Go, Eun Sul
A1 - Hong, Eun Ji
A1 - Lee, Ji Yeong
A1 - Stolar, Tomislav
A1 - Peterson, Gregory I.
A1 - Emmerling, Franziska
A1 - Kim, Kyoungsoo
A1 - Kim, Jeung Gon
T1 - Insights into Mechanochemical Solid-State Ball-Milling Reaction: Monitoring Transition from Heterogeneous to Homogeneous Conditions
N2 - As mechanochemical synthesis has advanced significantly, there has been intense interest in understanding the underlying mechanisms of these reactions. Given that many mechanochemical processes are conducted in the solid-state without solvation yet sometimes yield faster reactions than those in solution, we sought to address the following question: Are mechanochemical reactions homo- or heterogeneous? To investigate, we employed a model system involving the mixing and copolymerization of l-lactide (LLA) and d-lactide (DLA), monitored through powder X-ray diffraction (PXRD), nuclear magnetic resonance, and differential scanning calorimetry. In situ and ex situ PXRD analyses of the mixture of LLA and DLA showed that vibratory ball milling rapidly transformed the initially heterogeneous lactide mixture into a homogeneous phase within one min due to collisions between the balls and the jar. By varying the milling conditions, we were able to regulate the level of mixing, which subsequently influenced the copolymerization outcomes. In the solid-state ball-milling copolymerization of LLA and DLA in the presence of a catalyst and initiator, multiblock copolymers of poly(l-lactic acid) and poly(d-lactic acid) were formed within one min during the early stage of the reaction, when incomplete mixing of the monomers led to a process governed by phase heterogeneity. In contrast, prolonged polymerization promoted conditions approaching homogeneity, ultimately yielding atactic poly(lactic acid). This transition from heterogeneous to homogeneous reactions is a distinctive feature compared to conventional homogeneous reactions, potentially leading to mechano-exclusive reaction designs.
KW - Mechanochemistry
KW - Ball-milling
KW - Homogeneous reaction
KW - Heterogeneous reaction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638008
DO - https://doi.org/10.1021/jacsau.5c00322
SN - 2691-3704
VL - 5
IS - 6
SP - 2720
EP - 2727
PB - American Chemical Society (ACS)
AN - OPUS4-63800
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Feiler, Torvid
A1 - Emmerling, Franziska
A1 - Bhattacharya, Biswajit
T1 - Sustainable mechanochemical approach for the selective synthesis of multicomponent organic solids: real-time in situ insights
N2 - Crystalline multicomponent organic solids (MOSs) such as cocrystals and ionic cocrystals hold immense potential in diverse functional applications, ranging from pharmaceuticals to optoelectronics. However, conventional solution-based crystallization methods often result in polymorphic mixtures and lack precise control over product composition. Herein, we report a comparative investigation of solution crystallization versus mechanochemical synthesis for constructing MOSs from 9-anthracenecarboxylic acid (ACA) and 4,4 '-bipyridine (BPY). Solution-based approaches consistently yielded concomitant formation of neutral cocrystal (CC) and ionic cocrystal (ICC) forms, regardless of the solvent used. The resulting multicomponent solids were comprehensively characterized using a combination of single crystal X-ray diffraction, powder X-ray diffraction, Fourier-transform infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. In contrast, mechanochemical methods, including neat grinding (without solvent) and liquid-assisted grinding (with minimum solvent), enabled selective formation of either a phase pure CC or ICC form. Less polar and nonpolar organic solvents favor the kinetic CC, while polar water promotes formation of the thermodynamically stable ICC. Time-resolved in situ powder X-ray diffraction (TRIS-PXRD) captures the dynamic evolution of solid-state phases and reveals the complete transformation of the CC into ICC under neat grinding or water-assisted conditions. This study highlights the powerful role of mechanochemistry and in situ monitoring in steering solid-state reactivity and offers a sustainable pathway for the targeted and scalable synthesis of pure multicomponent organic materials.
KW - Cocrystal
KW - Synchrotron X-ray powder diffraction
KW - Time-resolved in situ investigation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641409
DO - https://doi.org/10.1039/D5CE00663E
SN - 1466-8033
SP - 1
EP - 9
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64140
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Falkenhagen, Jana
T1 - Coupling of chromatographic and spectrometric techniques for polymer characterization
N2 - Coupling of chromatographic and spectrometric techniques for polymer characterization; focus topics: LCxMALDI-TOF-MS and UPLC x ESI-TOF-MS
T2 - 16. Tagung des Arbeitskreises Polymeranalytik
CY - Online meeting
DA - 22.03.2022
KW - Liquid chromatography
KW - Mass spectrometry
KW - Polymers
KW - Two-dimensional chromatography (2D-LC)
PY - 2022
AN - OPUS4-54567
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Karafiludis, Stephanos
A1 - Scoppola, E.
A1 - Wolf, S.E.
A1 - Kochovski, Z.
A1 - Matzdorff, D.
A1 - Van Driessche, A. E. S.
A1 - Hövelmann, J.
A1 - Emmerling, Franziska
A1 - Stawski, Tomasz M.
T1 - Evidence for liquid-liquid phase separation during the early stages of Mg-struvite formation
N2 - 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. Specifically, indirect evidence suggests the involvement of an amorphous precursor and the occurrence of multi-step processes in struvite formation, which would indicate non-classical paths of nucleation and crystallization. In this study, we use synchrotron-based in situ x-ray scattering complemented by cryogenic transmission electron microscopy to obtain new insights from the earliest stages of struvite formation. The holistic scattering data captured the structure of an entire assembly in a time-resolved manner. The structural features comprise the aqueous medium, the growing struvite crystals, and any potential heterogeneities or complex entities. By analysing the scattering data, we found that the onset of crystallization causes a perturbation in the structure of the surrounding aqueous medium. This perturbation is characterized by the occurrence and evolution of Ornstein-Zernike fluctuations on a scale of about 1 nm, suggesting a non-classical nature of the system. We interpret this phenomenon as a liquid-liquid phase separation, which gives rise to the formation of the amorphous precursor phase preceding actual crystal growth of struvite. Our microscopy results confirm that the formation of Mg-struvite includes a short-lived amorphous phase, lasting >10 s.
KW - Physical and theoretical chemistry
KW - Non-classical crystallization
KW - Struvite
KW - Liquid-liquid-phase-separation
KW - Nucleation
KW - Crystallization
KW - In-situ scattering
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584766
DO - https://doi.org/10.1063/5.0166278
SN - 1089-7690
VL - 159
IS - 13
SP - 1
EP - 12
PB - AIP Publishing
CY - Woodbury, NY
AN - OPUS4-58476
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stawski, Tomasz
A1 - Karafiludis, Stephanos
A1 - Pimentel, Carlos
A1 - Montes-Hernández, German
A1 - Kochovski, Zdravko
A1 - Bienert, Ralf
A1 - Weimann, Karin
A1 - Emmerling, Franziska
A1 - Scoppola, Ernesto
A1 - Van Driessche, Alexander E.S.
T1 - Solution-driven processing of calcium sulfate: The mechanism of the reversible transformation of gypsum to bassanite in brines
N2 - 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 c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the better-known behaviour of the bassanite phase in low-salt environments. In low-salinity aqueous solutions, bassanite is considered to be metastable with respect to gypsum and anhydrite, and therefore gypsum-to-bassanite conversion does not occur in pure water. Interestingly, the high-salinity transformation of gypsum-to-bassanite has been reported by many authors and used in practice for several decades, although its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures was inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline phase for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios.
KW - Industrial and Manufacturing Engineering
KW - Strategy and Management
KW - General Environmental Science
KW - Renewable Energy, Sustainability and the Environment
KW - Building and Construction
KW - Calcium sulfate
KW - Gypsum
KW - Bassanite
KW - Scattering
KW - Raman
KW - In situ
KW - Synchrotron
KW - BESSY
KW - MySpot
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594698
UR - https://www.sciencedirect.com/science/article/pii/S0959652624004591#appsec1
DO - https://doi.org/10.1016/j.jclepro.2024.141012
SN - 0959-6526
VL - 440
SP - 1
EP - 12
PB - Elsevier B.V.
AN - OPUS4-59469
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Edzards, Joshua
A1 - Saßnick, Holger-Dietrich
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Valencia, Ana M.
A1 - Emmerling, Franziska
A1 - Beyer, Sebastian
A1 - Cocchi, Caterina
T1 - Effects of Ligand Substituents on the Character of Zn-Coordination in Zeolitic Imidazolate Frameworks
N2 - 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 widespread interest in these materials, fundamental questions regarding the zinc coordination environment remain poorly understood. By focusing on zinc(II)2-methylimidazolate (ZIF-8) and its tetrahedrally coordinated analogues with Br-, Cl-, and H-substitution in the 2-ring position, we aim to clarify how variations in the local environment of Zn impact the charge distribution and the electronic properties of these materials. Our results from densityfunctional theory confirm the presence of a Zn coordinative bond with a large polarization that is quantitatively affected by different substituents on the organic ligand. Moreover, our findings suggest that the variations in the Zn coordination induced by the functionalization have a negligible effect on the electronic structure of the considered compounds. On the other hand, halogen terminations of the ligands lead to distinct electronic contributions in the vicinity of the frontier region which ultimately reduce the band gap size by a few hundred millielectron volts. Experimental results obtained from X-ray absorption spectroscopy (Zn K-edge) confirm the trends predicted by theory and, together with them, contribute to a better understanding of the structure−property relationships that are needed to tailor ZIFs for target applications.
KW - Surfaces
KW - Physical and Theoretical Chemistry
KW - General Energy
KW - Electronic
KW - Coatings and Films
KW - Optical and Magnetic Materials
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589117
DO - https://doi.org/10.1021/acs.jpcc.3c06054
SN - 1932-7447
VL - 127
IS - 43
SP - 21456
EP - 21464
PB - American Chemical Society (ACS)
AN - OPUS4-58911
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zuffa, Caterina
A1 - Cappuccino, Chiara
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Maini, Lucia
T1 - Liquid reagents are not enough for liquid assisted grinding in the synthesis of [(AgBr)(n-pica)]n
N2 - This study investigates the mechanochemical reactions between AgBr 3-picolylamine and 4-picolylamine. The use of different stoichiometry ratios of the reagents allows [(AgBr)(n-pica)]n and [(AgBr)2(n-pica)]n to be obtained, and we report the new structures of [(AgBr)2(3-pica)]n and [(AgBr)2(4-pica)]n which are characterized by the presence of the following: (a) infinite inorganic chains, (b) silver atom coordinated only by bromide atoms and (c) argentophilic interactions. Furthermore, we studied the interconversion of [(AgBr)(n-pica)]n/[(AgBr)2(n-pica)]n by mechanochemical and thermal properties. The in situ experiments suggest that [(AgBr)(3-pica)]n is kinetically favoured while [(AgBr)2(3-pica)]n is converted into [(AgBr)(3-pica)]n only with a high excess of the ligand. Finally, the liquid nature of the ligands is not sufficient to assist the grinding process, and the complete reaction is observed with the addition of a small quantity of acetonitrile.
KW - Mechanochemistry
KW - Complex
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594755
DO - https://doi.org/10.1039/d3cp04791a
SN - 1463-9076
SP - 1
EP - 10
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59475
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Villajos Collado, José Antonio
A1 - Bienert, M.
A1 - Gugin, Nikita
A1 - Emmerling, Franziska
A1 - Maiwald, Michael
T1 - A database to select affordable MOFs for volumetric hydrogen cryoadsorption considering the cost of their linkers
N2 - 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 storage capacity. However, such extensive use of MOFs for this application requires the selection of affordable structures, easy to produce and made from feasible metallic and organic components. Herein, we introduce a MOF database detailing the crystallographic and porous properties of 3600 existing MOFs made from industrially relevant metals and their organic composition. The comparison of the available minimum costs of linkers allowed the creation of a database to select affordable structures with high potential for volumetric hydrogen storage by cryoadsorption, considering their composition based on individual or mixed building blocks. A user inter� face, available online, facilitates the selection of MOFs based on the properties or names of structures and linkers.
KW - MOF´s
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583619
DO - https://doi.org/10.1039/d3ma00315a
VL - 4
IS - 18
SP - 4226
EP - 4237
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58361
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scheurrell, Kerstin
A1 - B. Martins, Inês C.
A1 - Murray, Claire
A1 - Emmerling, Franziska
T1 - Exploring the role of solvent polarity in mechanochemical Knoevenagel condensation: in situ investigation and isolation of reaction intermediates
N2 - 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 solvents with different polarities (liquid-assisted grinding). The reaction was monitored using time-resolved in situ Raman spectroscopy and powder X-ray diffraction (PXRD). Our results indicate a direct relationship between solvent polarity and reaction kinetics, with higher solvent polarity leading to faster product (2-(4-nitrobenzylidone)malononitrile) formation. For the first time, we were able to isolate and determine the structure of an intermediate 2-(hydroxy(4-nitrophenyl)methyl)malononitrile based on PXRD data.
KW - Physical and Theoretical Chemistry
KW - General Physics and Astronomy
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588071
DO - https://doi.org/10.1039/D3CP02883F
SN - 1463-9076
VL - 25
IS - 35
SP - 23637
EP - 23644
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58807
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Peters, Stefan
A1 - Kunkel, Benny
A1 - Cakir, Cafer Tufan
A1 - Kabelitz, Anke
A1 - Witte, Steffen
A1 - Bernstein, Thomas
A1 - Bartling, Stephan
A1 - Radtke, Martin
A1 - Emmerling, Franziska
A1 - Abdel-Mageed, Ali Mohamed
A1 - Wohlrab, Sebastian
A1 - de Oliveira Guilherme Buzanich, Ana
T1 - Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy
N2 - A novel setup for dispersive X-ray absorption spectroscopy (XAS) with simultaneous resolution of space, time and energy for in situ characterization of solid materials is demonstrated.
KW - Dispersive XAS
KW - Catalysis
KW - In situ
KW - Structure analysis
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584924
DO - https://doi.org/10.1039/d3cc03277a
SN - 1359-7345
SP - 1
EP - 4
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58492
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heinekamp, Christian
A1 - Kneiske, Sönke
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Ahrens, Mike
A1 - Braun, Thomas
A1 - Emmerling, Franziska
T1 - A fluorolytic sol-gel route to access an amorphous Zr fluoride catalyst: A useful tool for C-F bond activation
N2 - 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 stream of CHClF2. The behaviour of different Zr(IV) precursors in a sol–gel reaction with anhydrous isopropanol/HF solution was investigated. The subsequent post-fluorination step was optimised in its temperature ramp and confirmed the necessity of a fluorination of the generated xerogels to obtain catalytic activity. The process is discussed in the context of the analysis of the materials using Brunauer–Emmett–Teller analysis (BET), powder X-ray diffraction (XRD), infrared spectroscopy (IR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The local structure of the amorphous catalyst was elucidated by extended X-ray absorption fine structure spectroscopy (EXAFS).
KW - Catalysis
KW - Heterogeneous catalysis
KW - C-F bond activation
KW - Postfluorination
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593433
DO - https://doi.org/10.1039/D3CY01439H
SN - 2044-4761
SP - 1
EP - 8
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59343
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Paul, Sagar
A1 - Dolai, Malay
A1 - Nanda Goswami, Juli
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Drew, Michael G. B.
A1 - Chattopadhyay, Shouvik
A1 - Sarkar, Rabi Sankar
A1 - Sunil, Appu
A1 - Novitchi, Ghenadie
A1 - Moreno-Pineda, Eufemio
A1 - Wernsdorfer, Wolfgang
T1 - From strong to weak interaction: Reconciling SQUID and μSQUID-EPR data in anomalous Co(ii) dimers
N2 - Magnetic molecules have been proposed as scaffolds for novel quantum technologies, ranging from quantum sensing and quantum memory to multilevel quantum bits (qudits) and fault-tolerant quantum computation. Integration of magnetic molecules into cutting-edge applications hinges on a deep understanding and tunability of their spin states. To date, the strategic manipulation of the local environment of the ion and careful selection of the magnetic core have enabled the desired tunability and scalability of the spin states. For such goals, however, extracting the anisotropic parameters that dictate the characteristics of the Spin Hamiltonian is challenging, especially for molecules consisting of multiple magnetic cores. We address these challenges by studying two cobalt(II) dinuclear systems, complicated by inherent spin–orbit coupling. We explore the magnetic properties of these systems in two temperature regimes: (i) at sub-Kelvin temperatures employing single crystals at 30 mK using a unique μSQUID-EPR technique that examines the microwave absorption peaks in the magnetisation data and their variation with field angle and frequency; and (ii) in bulk employing convectional SQUID magnetometry above 2 K i.e., χMT(T) and M(H). Unexpectedly, sub-Kelvin temperature investigations reveal a negligible interaction, whereas the SQUID data reveal a much stronger interaction between the Co(II) ions. An understanding of these data is developed based on a strong coupling model and the coupling of two moieties with a spin-effective ground state.
KW - cOBALT(II)-complex
KW - In situ complex formation
KW - Magnetic property
KW - Crystal structure
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641421
DO - https://doi.org/10.1039/D5QI01387A
SN - 2052-1553
SP - 1
EP - 13
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64142
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mishra, Rajesh K.
A1 - Minussi, F.B.
A1 - Kumari, Priyanka
A1 - Shahi, Rohit R.
A1 - Yadav, R.P.
A1 - Emmerling, Franziska
A1 - Araújo, E.B.
T1 - Effect of sintering temperature on structural, microstructural, and dielectric properties of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 multi-cations high entropy oxides
N2 - The study reports the effect of sintering temperature on structural, microstructural, and dielectric properties of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 spinel high-entropy oxides (HEOs) synthesized through the solid-state mechanochemistry method. The sintering of the ceramic powders was accomplished at three different temperatures (1000 ◦C, 1100 ◦C, and 1250 ◦C), followed by air quenching. XRD analysis along with Le-Bail refinement confirms that 1100 ◦C and 1250 ◦C sintered oxides comprised of a single cubic spinel phase (Fd3m), while 1000 ◦C sintered oxide contains constituent oxides and a spinel phase. The phase formation of oxides sintered at 1100 ◦C and 1250 ◦C has also been confirmed by Raman spectroscopic analysis. Microstructural analysis revealed that the aggregated particle size increases with the rise in sintering temperature. With the change in sintering temperature, the dielectric behavior of the ceramic changed extensively. The 1100 ◦C sintered ceramic exhibits high frequency-dependent behavior, whereas the 1250 ◦C sintered ceramic yields low frequency-dependent behavior. The 1250 ◦C sintered HEO exhibits low-loss tangent (tan δ = 0.01) with higher dielectric permittivity (εʹ = 44) at high frequency (1 MHz) compared to the 1100 ◦C sintered ceramic and many other conventional dielectrics.
Fractal concept and impedance analysis have been employed to correlate the microstructure-dielectric property relation of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 spinel HEOs. The found Hurst exponent values for both different temperature-sintered HEOs are less than 0.5, indicating the anti-persistent behavior. This signifies that the height variations at neighboring pixels are negatively correlated. The present work is of fundamental importance in employing fractal analysis for the first time on spinel HEOs and correlating their properties. It also shows that processing conditions can effectively tailor the dielectric properties of the materials.
KW - Multi-cations high entropy oxide
KW - Mechanochemistry
KW - Spinel structure
KW - Fractal and impedance spectroscopic analysis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647584
DO - https://doi.org/10.1016/j.ceramint.2025.09.256
SN - 0272-8842
VL - 51
IS - 27
SP - 55341
EP - 55354
PB - Elsevier Ltd.
AN - OPUS4-64758
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Karafiludis, Stephanos
A1 - Standl, Jacob
A1 - Ryll, Tom W.
A1 - Schwab, Alexander
A1 - Prinz, Carsten
A1 - Wolf, Jakob B.
A1 - Kruschwitz, Sabine
A1 - Emmerling, Franziska
A1 - Völker, Christoph
A1 - Stawski, Tomasz M.
T1 - High-Entropy Phosphate Synthesis: Advancements through Automation and Sequential Learning Optimization
N2 - Transition metal phosphates (TMPs) are extensively explored for electrochemical and catalytical applications due to their structural versatility and chemical stability. Within this material class, novel high-entropy metal phosphates (HEMPs)─containing multiple transition metals combined into a single-phase structure─are particularly promising, as their compositional complexity can significantly enhance functional properties. However, the discovery of suitable HEMP compositions is hindered by the vast compositional design space and complex or very specific synthesis conditions. Here, we present a data-driven strategy combining automated wet-chemical synthesis with a Sequential Learning App for Materials Discovery (SLAMD) framework (Random Forest regression model) to efficiently explore and optimize HEMP compositions. Using a limited set of initial experiments, we identified multimetal compositions in a single-phase crystalline solid. The model successfully predicted a novel Co0.3Ni0.3Fe0.2Cd0.1Mn0.1 phosphate octahydrate phase, validated experimentally, demonstrating the effectiveness of the machine learning approach. This work highlights the potential of integrating automated synthesis platforms with data-driven algorithms to accelerate the discovery of high-entropy materials, offering an efficient design pathway to advanced functional materials.
KW - Metal phosphates
KW - High entropy
KW - Sequential learning
KW - Automated synthesis
KW - MAP
KW - Random forest
KW - Machine learning
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641554
DO - https://doi.org/10.1021/acs.cgd.5c00549
SN - 1528-7483
VL - 25
IS - 19
SP - 7989
EP - 8001
PB - American Chemical Society (ACS)
CY - Washington, DC
AN - OPUS4-64155
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Batteas, James
A1 - Blank, Kerstin G.
A1 - Colacino, Evelina
A1 - Emmerling, Franziska
A1 - Friščić, Tomislav
A1 - Mack, James
A1 - Moore, Jeffrey
A1 - Rivas, Maria Elena
A1 - Tysoe, Wilfred
T1 - Moving mechanochemistry forward
N2 - Arguably mechanochemistry is one of the oldest, and at the same time one of the newest, areas of chemistry. One of the oldest, because it has been theorized that early hominids were able to develop rapidly due to their ability to heat and mechanically process their food to make it easier to digest. Old, because the ancient Greeks knew that mechanically activating stones (consisting of cinnabar) with vinegar in a copper pestle and mortar caused them to convert into mercury. We might be forgiven for thinking that this could have led our alchemical forbears to wonder if there were other stones that might also be persuaded to convert into gold. Early chemical luminaries such as Michael Faraday and Wilhelm Röntgen dabbled in mechanochemistry. However, in the late 19th and early 20th centuries, the field developed separately in many areas. Perhaps most significantly, synthetic chemists realized that reactions could be carried out with surprisingly high yields and selectivities by shaking them in a ball mill, and that they could even make novel compounds that their colleagues just using heat were not able to. Physicists were mechanically rearranging atoms into new configurations (i.e., doing chemistry) using exotic means such as atomic force microscope tips and optical tweezers. Scientists and engineers studying the formation of lubricious and anti-wear films realized that they were mechanochemically formed. Biochemists found molecular motor proteins, such as myosin and kinesin, that were able to convert chemical energy into motion or, vice versa, mechanical energy into the biochemical energy storage molecule adenosine triphosphate. In 2023, this confluence of advances convinced the Royal Society of Chemistry that the time was ripe to establish a new journal dedicated to the field of mechanochemistry. It is rare that a journal has the privilege of helping to create a new sub-branch of chemistry but, having done so, it has the obligation of helping to define the field and, optimistically, suggesting how the field might develop. This editorial has two major goals. The first is to bring to the attention of the scientific community the challenges faced by the field to set people thinking about how they might contribute and, second, to form the basis for more thorough discussions in the future. The sub-topics below outline current thoughts brought forward from members of our editorial board. We lay out areas and topics here with the intent of establishing a new editorial series, which we invite the community to contribute to, and outline topics and hopefully lay out challenges, which will enable us as a community to come together to move mechanochemistry forward.
KW - Mechanochemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646086
DO - https://doi.org/10.1039/d4mr90021a
SN - 2976-8683
VL - 2
IS - 1
SP - 10
EP - 19
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64608
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ferreira, Daniela R.
A1 - Portet, Anaïs
A1 - Alves, Paula C.
A1 - Rijo, Patrícia
A1 - Gomes, Clara S. B.
A1 - Duarte, M. Teresa
A1 - Halasz, Ivan
A1 - Colacino, Evelina
A1 - Emmerling, Franziska
A1 - André, Vânia
T1 - Modulating the crystalline forms of silver–sulfadiazine complexes by mechanochemistry
N2 - Mechanochemical synthesis of pharmaceutical compounds has gained significant attention due to its potential to overcome traditional synthetic challenges while offering the possibility of improving the physicochemical properties of drugs. This study delves into the mechanochemical synthesis of silver sulfadiazine (AgSD) coordination compounds, obtained under different mechanochemical stress and processing conditions. The aim of this work was to investigate the influence of mechanochemical conditions on the selectivity in the preparation of AgSD coordination compounds. Through a series of experiments, we demonstrate the successful synthesis of two different AgSD coordination networks, using high-energy ball milling. By strategically manipulating the starting materials and milling parameters — including milling time, milling frequency, type of mechanical stress (as determined by different milling devices), and the presence of co-milling agents — we were able to control the product outcome. As a result, we achieved two different forms of silver-sulfadiazine metal frameworks, one of which was not previously disclosed. The crystal structure of the new form, obtained from high resolution PXRD synchrotron data, was compared with the previously known structure of a silver sulfadiazine compound. The in-depth antimicrobial activity systematic study of these AgSD forms on the generic systems showed increased antibacterial activity when compared to sulfadiazine. This research sheds light on the mechanochemical synthesis of silver sulfadiazine complexes. The obtained knowledge may guide the development of novel synthetic strategies for other drug molecules, leading to improved drug performance, stability, and therapeutic outcomes.
KW - Mechanochemistry
KW - Structure solution
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646099
DO - https://doi.org/10.1039/d5ce00572h
SN - 1466-8033
SP - 1
EP - 12
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64609
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez-Sánchez, Noelia
A1 - Prinz, Carsten
A1 - Bienert, Ralf
A1 - Ballesteros, Menta
A1 - Ruiz Salvador, A. Rabdel
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Mechanochemical ZIF-9 formation: in situ analysis and photocatalytic enhancement evaluation
N2 - 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 diffraction, we provide real-time insights into the formation dynamics of ZIF-9 during mechanosynthesis. Our results show that mechanochemically synthesised ZIF-9 exhibits superior photocatalytic activity compared to its solvothermally prepared counterpart, achieving a 2-fold increase in methylene blue degradation rate. This research not only advances our understanding of the synthesis and properties of ZIF-9, but also demonstrates the potential of mechanochemical approaches in the development of high-performance, sustainably produced materials for water treatment and other environmental applications.
KW - MOFs
KW - ZIF
KW - Time-resolved in situ investigation
KW - Photocatalysis synchrotron X-ray powder diffraction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641416
DO - https://doi.org/10.1039/D4MR00114A
SN - 2976-8683
VL - 2
IS - 1
SP - 116
EP - 126
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64141
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lopes, Chrystal
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Leyssens, Tom
A1 - Dupray, Valérie
A1 - Brandel, Clement
A1 - Cartigny, Yohann
T1 - Efficient racemization of the pharmaceutical compound Levetiracetam using solvent-free mechanochemistry
N2 - 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 the tremendous potential of mechanochemistry. In this study, we highlight the importance of mixing efficiency regarding data reproducibility, and we show, in particular, that water contamination has a negative impact on the reaction rate. Moreover, in situ X-ray diffraction gives us first insights into the mechanisms involved in the solid state during the mechanochemical racemization process.
KW - Mechanochemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646108
DO - https://doi.org/10.1039/d4mr00103f
SN - 2976-8683
VL - 2
IS - 1
SP - 83
EP - 90
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64610
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Macchietti, Laura
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Braga, Dario
A1 - Grepioni, Fabrizia
T1 - Deriving kinetic insights from mechanochemically synthesized compounds using multivariate analysis (MCR-ALS) of powder X-ray diffraction data
N2 - 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 Resolution-Alternating Least Squares (MCR-ALS) method on powder X-ray diffraction (PXRD) data of mechanochemical processes by studying the system theophylline (TP) and malonic acid (MA) in a 1 : 1 stoichiometric ratio at different milling conditions. We have highlighted the strengths and weaknesses of the MCR-ALS method, and we demonstrated why it may be an alternative route to obtain quantitative information on mechanochemical kinetics.
KW - Mechanochemistry
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646115
DO - https://doi.org/10.1039/d3mr00013c
SN - 2976-8683
VL - 1
IS - 1
SP - 106
EP - 115
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64611
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pavlidis, Sotirios
A1 - Teutloff, Christian
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Krause, Konstantin B.
A1 - Emmerling, Franziska
A1 - Bittl, Robert
A1 - Abbenseth, Josh
T1 - A Crystalline Bismuth(II) Radical Anion: Synthesis, Characterization, and Reactivity
N2 - AbstractWe report the synthesis of a planarized tris‐amidobismuthane supported by a rigid, bulky NNN pincer ligand, which enforces a T‐shaped geometry at the bismuth center. The Bi(NNN) complex features a low‐lying LUMO with distinct Bi(6p) orbital character as shown by DFT calculations. Cyclic voltammetry reveals a fully reversible one‐electron reduction at E1/2 = –1.85 V versus Fc0/+ in THF. Chemical reduction with KC8 in the presence of 4,7,13,16,21,24‐hexaoxa‐1,10‐diazabicyclo[8.8.8]hexacosane (222‐crypt) enables the isolation of an unprecedented Bi(II) radical anion in high isolated yields. Multi‐frequency EPR, X‐ray absorption spectroscopy and SQUID magnetometry complemented by theoretical calculations confirm localization of the unpaired electron on the bismuth center. Preliminary reactivity studies display radical reactivity as shown by single‐electron transfer chemistry and radical coupling reactions.
KW - Bi(III)
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644143
DO - https://doi.org/10.1002/anie.202515545
SN - 1433-7851
VL - 64
IS - 49
SP - 1
EP - 6
PB - Wiley VHC-Verlag
AN - OPUS4-64414
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Chapartegui-Arias, Ander
A1 - Raysyan, A.
A1 - Belenguer, A. M.
A1 - Jaeger, Carsten
A1 - Tchipilov, Teodor
A1 - Prinz, Carsten
A1 - Abad Andrade, Carlos Enrique
A1 - Beyer, S.
A1 - Schneider, Rudolf
A1 - Emmerling, Franziska
T1 - Tailored mobility in a zeolite imidazolate framework (ZIF) antibody conjugate
N2 - Zeolitic imidazolate framework (ZIF) hybrid fluorescent nanoparticles and ZIF antibody conjugates have been synthesized, characterized, and employed in lateral-flow immunoassay (LFIA). The bright fluorescence of the conjugates and the possibility to tailor their mobility gives a huge potential for diagnostic assays. An enzyme-linked immunosorbent assay (ELISA) with horseradish peroxidase (HRP) as label, proved the integrity, stability, and dispersibility of the antibody conjugates, LC-MS/MS provided evidence that a covalent link was established between these metal-organic frameworks and lysine residues in IgG antibodies.
KW - ZIF
KW - ELISA
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532096
DO - https://doi.org/10.1002/chem.202100803
SN - 0947-6539
SN - 1521-3765
VL - 27
IS - 36
SP - 9414
EP - 9421
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-53209
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Casali, L.
A1 - Broll, V.
A1 - Ciurili, S.
A1 - Braga, D.
A1 - Emmerling, Franziska
A1 - Gepioni, F.
T1 - Facilitating Nitrification Inhibition through Green, Mechanochemical Synthesis of a Novel Nitrapyrin Complex
N2 - Nitrapyrin (NP) is applied to cultivated soils to inhibit the enzymatic activity of ammonia monooxygenase (AMO), but its poor aqueous solubility and high volatility severely limit its application. β-Cyclodextrin (β-CD) is commonly used to form inclusion complexes with hydrophobic molecules, improving water solubility and stability upon complexation. Here we report on the mechanochemical synthesis of the inclusion complex β-CD·NP, characterized via a combination of solid-state techniques, including exsitu and in situ X-ray diffraction, Raman and NMR spectroscopies, transmission electron microscopy, and energy dispersive X-ray spectroscopy. The pure inhibitor NP was also structurally characterized. The β-CD·NP complex presents improved solubility and thermal stability, and still inhibits the enzymatic activity of AMO with high efficacy. All results indicate that the inclusion of NP into β-CD represents a viable route for the preparation of a novel class of inhibitors, with improved properties related to stability, water solubility, and good inhibition activity.
KW - Mechanochemistry
KW - Nitrification
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537154
DO - https://doi.org/10.1021/acs.cgd.1c00681
SN - 1528-7505
VL - 21
IS - 10
SP - 5792
EP - 5799
PB - ACS Publications
AN - OPUS4-53715
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heilmann, Maria
A1 - Prinz, Carsten
A1 - Bienert, Ralf
A1 - Wendt, R.
A1 - Kunkel, B.
A1 - Radnik, Jörg
A1 - Hoell, A.
A1 - Wohlrab, S.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Emmerling, Franziska
T1 - Size-Tunable Ni–Cu Core–Shell Nanoparticles—Structure, Composition, and Catalytic Activity for the Reverse Water–Gas Shift Reaction
N2 - A facile and efficient methodology is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core–shell nanoparticles (NPs) for application in catalysis. The diameter of the NPs is tuned in a range from 6 nm to 30 nm and to adjust the Ni:Cu ratio from 30:1 to 1:1. Furthermore, the influence of different reaction parameters on the final NPs is studied. The NPs are structurally characterized by a method combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray absorption fine structure, and X-ray photoelectron spectroscopy. Using these analytical methods, it is possible to elucidate a core–shell–shell structure of all particles and their chemical composition. In all cases, a depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core–shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction) independent of size and Ni:Cu ratio.
KW - Nanoparticles
KW - Core-shell
KW - Catalysis
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543606
DO - https://doi.org/10.1002/adem.202101308
SN - 1438-1656
SP - 1
EP - 13
PB - Wiley VCH
AN - OPUS4-54360
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dudziak, Mateusz
A1 - Topolniak, Ievgeniia
A1 - Silbernagl, Dorothee
A1 - Altmann, Korinna
A1 - Sturm, Heinz
T1 - Long-time behavior of surface properties of microstructures fabricated by multiphoton lithography
N2 - The multiphoton lithography (MPL) technique represents the future of 3D microprinting, enabling the production of complex microscale objects with high precision. Although the MPL fabrication parameters are widely evaluated and discussed, not much attention has been given to the microscopic properties of 3D objects with respect to their surface properties and time-dependent stability. These properties are of crucial importance when it comes to the safe and durable use of these structures in biomedical applications. In this work, we investigate the surface properties of the MPL-produced SZ2080 polymeric microstructures with regard to the physical aging processes during the post-production stage. The influence of aging on the polymeric microstructures was investigated by means of Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS). As a result, a time-dependent change in Young’s Modulus, plastic deformation, and adhesion and their correlation to the development in chemical composition of the surface of MPL-microstructures are evaluated. The results presented here are valuable for the application of MPL-fabricated 3D objects in general, but especially in medical technology as they give detailed information of the physical and chemical time-dependent dynamic behavior of MPL-printed surfaces and thus their suitability and performance in biological systems.
KW - Multiphoton lithography
KW - Additive manufacturing
KW - Microfabrication
KW - SZ2080 negative photo-resist
KW - Young´s modulus
KW - Aging
KW - Surface properties
KW - X-ray photoelectron spectroscopy
KW - Atomic force microscopy
KW - Force-distance-curve
PY - 2021
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542166
DO - https://doi.org/10.3390/nano11123285
SN - 2079-4991
VL - 11
IS - 12
SP - 1
EP - 12
PB - MDPI
CY - Basel
AN - OPUS4-54216
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Müller, Axel
A1 - Altmann, Korinna
A1 - Kocher, B.
A1 - Braun, U.
T1 - Determination of tire wear markers in soil samples and their distribution in a roadside soil
N2 - Tire wear (TW) constitutes a significant source of microplastic in terrestrial ecosystems. It is known that particles emitted by roads can have an effect up to 100 m into adjacent areas. Here, we apply for the first-time thermal extraction desorption gas chromatography-mass spectrometry (TED-GC/MS) to determine TW in soil samples by detection of thermal decomposition products of styrene-butadiene rubber (SBR), without additional enrichment. Additionally, zinc contents were determined as an elemental marker for TW. Mixed soil samples were taken along three transects along a German motorway in 0.3, 2.0, and 5.0 m distance from the road. Sampling depths were 0–2, 2–5, 5–10, and 10–20 cm. Four fine fractions, 1 000–500, 500–100, 100–50, and <50 μm, were analyzed.
TW contents based on SBR ranged from 155 to 15 898 mg kg−1. TW contents based on zinc were between 413 and 44 812 mg kg−1. Comparison of individual values of SBR and zinc reveals SBR as a more specific marker. Results confirm that most TW ends up in the topsoil within a 2 m distance.
The sampling strategy resulted in representative data for a larger area. Standard deviations of quadruple TED-GC/MS determination of SBR were <10% for all grain size fractions. TED-GC/MS is a suitable analytical tool for determining TW in soil samples without the use of toxic chemicals, enrichment, or special sample preparation.
KW - Microplastic
KW - TED-GC/MS
KW - Tire wear
PY - 2022
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543344
DO - https://doi.org/10.1016/j.chemosphere.2022.133653
VL - 294
SP - 1
EP - 8
PB - Elsevier Ltd.
AN - OPUS4-54334
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -