TY - JOUR A1 - Shovo, Redoy Gazi A1 - Thünemann, Andreas A1 - Katcharava, Zviadi A1 - Marinvo, Anja A1 - Hoppe, Richard A1 - Woltersdorf, Georg A1 - Du, Mengxue A1 - Androsch, Rene A1 - de Souza e Silva, Juliana Martins A1 - Busse, Karste A1 - Binder, Wolfgang H. T1 - Generating Tagged Micro- and Nanoparticles of Poly(ethylene furanoate) and Poly(ethylene terephthalate) as Reference Materials N2 - Detecting nanoplastic particles in environmental samples and biological tissues remains a significant challenge, especially in view of newly emerging polymers, not yet commercially exploited. Fluorescent labeling provides a tagging strategy to overcome this limitation by reducing the detection limit of individual particles, especially for small-sized particles. We present a method for producing labeled nanoparticles (NP/MP) of poly(ethylene terephthalate) (PET) and poly(ethylene furanoate) (PEF), tagged with Alexa Fluor 633 or Alexa Fluor 647. Our preparations used mechanical grinding or solvent-based approaches (confined impinging jet mixing, ((CIJ, precipitation), generating particles with hydrodynamic diameters of 200–700 nm, displaying long-term stability in water of up to 57 days. Stable suspensions with concentrations of the particles ranging from 10 µg/mL (surfactant-free, by solvent mixing) to 5.88 mg/mL (precipitation, containing surfactant) were generated with zeta-potentials from −5 to −50 mV. Characterization of the nanoparticles by SEC, DSC, and XRD showed no significant changes in molecular weight, thermal behavior, or crystallinity via the solvent-based methods, compared to the pristine polymer, highlighting their suitability for producing standardized nanoparticle dispersions. Fluorescence spectroscopy of the Alexa-dye-labeled particles confirmed the successful incorporation of the Alexa dyes, so improving monitoring of their biological profiles of the PEF-MP/NPs. s-SNOM (near field imaging) could identify individual PEF-particles sized ∼200 nm by direct imaging. KW - Reference Materials KW - Nanoplastics KW - Microplastics KW - Polymer KW - Fluorescence PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655531 DO - https://doi.org/10.1002/marc.202500839 SN - 1521-3927 VL - 47 IS - 4 SP - 1 EP - 11 PB - Wiley VHC-Verlag CY - Weinheim AN - OPUS4-65553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Risse, Kerstin A1 - Nikiforidis, Constantinos V. A1 - Morris, Imogen A1 - Thünemann, Andreas A1 - Drusch, Stephan T1 - Regulating the heat stability of protein-phospholipid stabilised oil-water emulsions by changing the phospholipid headgroup or fatty acyl chain N2 - Stabilising oil–water emulsions remains a central challenge across food, pharmaceutical and cosmetic applications. β-lactoglobulin (β-LG) and phospholipids (PLs) can act synergistically at oil-water interfaces: PLs adsorb rapidly, while β-LG forms a viscoelastic protein network that enhances long-term stability. However, competitive adsorption between proteins and PLs can disrupt interfacial structure. In addition, for commercial production, emulsions are often exposed to heat treatment during or after manufacture, for instance due to food safety requirements. Yet, the combined effects of PL structure and heat treatment on interfacial organisation and emulsion stability remain poorly understood. Here we show that PL saturation and processing temperature jointly determine interfacial organisation, protein-PL interactions and emulsion stability. Using β-LG-PL emulsions, we combined ζ-potential measurements, small-angle X-ray scattering (SAXS), micro-differential scanning calorimetry (μDSC), X-ray diffraction and confocal laser scanning microscopy (CLSM) to link interfacial composition with functional stability. Below the β-LG denaturation temperature (≤75 °C), saturated PLs promoted partial unfolding of β-LG at the interface without displacement, producing mixed protein-PL networks with enhanced viscoelasticity and stability. Unsaturated PLs displaced β-LG, yielding less elastic interfaces and promoting protein aggregation in the bulk. At ≥75 °C, increased hydrophobicity intensified protein-protein interactions irrespective of PL type. Our findings reveal that saturated PLs shift the β-LG denaturation temperature upward by restricting molecular mobility, without preventing quaternary-level protein-protein interactions. Thermal denaturation, regardless of PL type, promoted interfacial multilayer formation at 90 °C. These results provide a mechanistic framework for tailoring emulsion stability via lipid saturation and processing temperature. KW - Small-angle X-ray scattering KW - SAXS KW - Nanostructure KW - Reference Method KW - Colloid KW - Nanoparticle PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648956 DO - https://doi.org/10.1016/j.jcis.2025.139530 SN - 0021-9797 VL - 705 SP - 1 EP - 25 PB - Elsevier Inc. AN - OPUS4-64895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mikhlin, Yuri A1 - Muzikansky, Anya A1 - Zysler, Melina A1 - Thünemann, Andreas A1 - Zitoun, David T1 - Emerging electrochemistry of high-concentration colloids: Redox-activity, wide potential window and electrophoretic transport of iron oxide nanoparticles N2 - High-concentration, steric stabilizer free colloids and particularly their electrochemical behavior remains almost unexplored. Herein, we report on the electrochemistry (cyclic voltammetry, impedance spectroscopy, etc.) of highly concentrated aqueous colloidal dispersion up to 800 g/L of citrate-capped ∼11 nm Fe3-xO4 nanoparticles (NPs) without background electrolyte on glassy carbon electrodes. X-ray photoelectron spectroscopy was applied to analyze the reaction products. Solid-state Fe(II)/Fe(III) conversion was concluded to determine the cathodic and anodic faradaic reactions of the particles, with the currents depending on approximately square root of the concentration. The electrochemical reactions are coupled with the electrophoretic transfer of the negatively charged NPs on toward the anode, with the ohmic-type behavior in the bulk demonstrated by the nearly linear voltametric cathodic curves and frequency-independent impedance above ∼10–100 Hz. Accumulation and clogging of the NPs retards diffusion near anode. Hydrogen and especially oxygen evolution are arrested, and very large oxidation overpotentials result in extraordinary wide, up to 12 V, electrochemical window of water stability. The findings shed light onto basic features of the electrochemistry of high-concentration colloids without added electrolyte and their potential applications in redox flow batteries, electrophoretic deposition and beyond. KW - Nanoplastics KW - SAXS KW - Small-angle X-ray scattering PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644340 DO - https://doi.org/10.1016/j.jcis.2025.139247 SN - 0021-9797 VL - 703 SP - 1 EP - 18 PB - Elsevier Inc. AN - OPUS4-64434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartczak, Dorota A1 - Sikora, Aneta A1 - Goenaga-Infante, Heidi A1 - Altmann, Korinna A1 - Drexel, Roland A1 - Meier, Florian A1 - Alasonati, Enrica A1 - Lelong, Marc A1 - Cado, Florence A1 - Chivas-Joly, Carine A1 - Fadda, Marta A1 - Sacco, Alessio A1 - Rossi, Andrea Mario A1 - Pröfrock, Daniel A1 - Wippermann, Dominik A1 - Barbero, Francesco A1 - Fenoglio, Ivana A1 - Booth, Andy M. A1 - Sørensen, Lisbet A1 - Igartua, Amaia A1 - Wouters, Charlotte A1 - Mast, Jan A1 - Barbaresi, Marta A1 - Rossi, Francesca A1 - Piergiovanni, Maurizio A1 - Mattarozzi, Monica A1 - Careri, Maria A1 - Caebergs, Thierry A1 - Piette, Anne-Sophie A1 - Parot, Jeremie A1 - Giovannozzi, Andrea Mario T1 - Multiparameter characterisation of a nano-polypropylene representative test material with fractionation, light scattering, high-resolution microscopy, spectroscopy, and spectrometry methods N2 - Reference and quality control materials with comparable physicochemical properties to nanoplastic contaminants present in environmental and food nanoplastics are currently lacking. Here we report a nanoplastic polypropylene material prepared using a top-down approach involving mechanical fragmentation of larger plastics. The material was found to be homogeneous and stable in suspension and has been characterised for average particle size, size distribution range, particle number concentration, polypropylene mass fraction and inorganic impurity Content using a wide range of analytical methods, including AF4, cFFF, PTA, (MA)DLS, MALS, SEM, AFM, TEM, STEM, EDS,Raman, ICP-MS and pyGC-MS. The material was found to have a broad size distribution, ranging from 50 nm to over 200 nm, with the average particle size value dependent on the technique used to determine it. Particle number concentration ranged from 1.7–2.4 × 1010 g−1 , according to PTA. Spectroscopy techniques confirmed that the material was polypropylene, with evidence of aging due to an increased level of oxidation. The measured mass fraction was found to depend on the marker used and ranged between 3 and 5 μg g−1 . Inorganic impurities such as Si, Al, Mg, K, Na, S, Fe, Cl and Ca were also identified at ng g−1 levels. Comparability and complementarity across the measurement methods and techniques is also discussed. KW - Polypropylene KW - Nanoplastics KW - Analytics KW - Reference material KW - Scattering methods PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654680 DO - https://doi.org/10.1039/D5EN00917K SN - 2051-8153 SP - 1 EP - 15 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aliyah, K. A1 - Berger, A. A1 - Lazaridis, T. A1 - Appel, C. A1 - Prehal, C. A1 - Menzel, A. A1 - Guizar-Sicairos, M. A1 - Smales, Glen J. A1 - Pauw, Brian Richard A1 - Gasteiger, H. A. A1 - Gubler, L. A1 - Büchi, F. N. A1 - Eller, J. T1 - Impact of Microporous Layer Composition on the Water Content in the Membrane Electrode Assembly of Polymer Electrolyte Fuel Cells N2 - Polymer electrolyte fuel cells are paramount for future emission-free mobility. One of the vital challenges for prospering commercialization of PEFCs is water management in the cells. A microporous layer (MPL) is typically positioned between the gas Diffusion layer (GDL) and the catalyst layer (CL) to boost the cell performance and facilitate water management. In this study, three different MPLs were investigated, namely, carbon black-based MPLs with different PTFE binder contents (20 wt % PTFE as a base case and 40 wt % PTFE), as well as perforated MPLs with micron-sized pores coated on the same GDL- Substrate (Freudenberg H14). The water content in the membrane, catalyst layers (CL), and MPLs was explored using operando scanning small- and wide-angle X-ray scattering (S/WAXS). At Tcell = 80 °C, relative humidity = 100%, pabs = 3 bar, the MPL with larger pores exhibits slightly higher performance than the base case, while a considerably lower cathode CL and MPL saturation levels were observed for the MPL. In contrast, the MPL with higher amounts of PTFE binder shows lower performance than the base case, with considerably higher cathode CL and MPL saturation levels. 3D representations of how the pores could be filled in the cathode CLs were obtained from operando SAXS profiles using representative structure modeling for the different materials and operating conditions. KW - Polymer electrolyte fuel cell KW - Catalyst layer saturation KW - Microporous layer saturation KW - Membrane hydration KW - Small and wide-angle scattering KW - MOUSE KW - SAXS KW - X-ray scattering KW - Energy storage materials PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656691 DO - https://doi.org/10.1021/acsami.5c22540 SN - 1944-8244 SP - 1 EP - 17 PB - American Chemical Society (ACS) AN - OPUS4-65669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saeed, A. M. A1 - Saied, M. A. A1 - Szymoniak, Paulina A1 - Altmann, Korinna A1 - Schönhals, Andreas A1 - Fahmy, Alaa T1 - High performance novel polyelectrolyte membrane consisting of polyvinyl alcohol-phenylsilanol-polypyrrole N2 - The synthesis of composite membranes based on PVA, PPy, and sulfonated–hydrolyzed TMPS was investigated for application in proton–exchange membrane fuel cells. FT–IR confirmed the hydrolysis of TMPS through the appearance of Si–OH vibrations, disappearance of Si–O–CH3 bands, reduced CH3 stretching intensity (2840 cm− 1), and successful sulfonation of the phenyl ring (1030 cm− 1). XPS verified the introduction of sulfonic acid groups by identifying S2p peaks between 166–170 eV. Scanning electron microscopy (SEM) showed an incorporation of PPy and that the membrane morphology altered by silanol leading to an increased surface roughness and inducing phase separation in comparison to pure PVA. The PVA–PPy–Si membrane which did not undergo phase separation demonstrated improved mechanical stability (maximum stress 5.91 MPa), reduced methanol uptake (22%, lower than Nafion’s 30%), and enhanced thermal resistance compared to PVA–PPy and PVA–Si. It also exhibited a high ion–exchange capacity (1.5mmol g− 1, exceeding Nafion® at 0.9mmol g− 1 ) and a proton conductivity of 0.036 S/cm, twice that of Nafion 117. These combined properties identify the PVA–PPy–Si composite as a promising high–performance polyelectrolyte membrane for fuel cell applications. KW - Polyelectrolyte membrane PY - 2026 DO - https://doi.org/10.1016/j.apsusc.2026.166495 SN - 1873-5584 VL - 731 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-65627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monroy, José del Refugio A1 - Deshpande, Tejas A1 - Schlecht, Joël A1 - Douglas, Clara A1 - Stirling, Robbie A1 - Grabicki, Niklas A1 - Smales, Glen Jacob A1 - Kochovski, Zdravko A1 - Fabozzi, Filippo Giovanni A1 - Hecht, Stefan A1 - Feldmann, Sascha A1 - Dumele, Oliver T1 - Homochiral versus racemic 2D covalent organic frameworks N2 - The synthesis of homochiral two-dimensional covalent organic frameworks (2D COFs) from chiral π-conjugated building blocks is challenging, as chiral units often lead to misaligned stacking interactions. In this work, we introduce helical chirality into 2D COFs using configurationally stable enantiopure and racemic [5]helicenes as linkers in the backbone of 2D [5]HeliCOFs as powders and films. Through condensation with 1,3,5-triformylbenzene (TFB) or 1,3,5-triformylphloroglucinol (TFP), our approach enables the efficient formation of a set of homochiral and racemic 2D [5]HeliCOFs. The resulting carbon-based crystalline and porous frameworks exhibit distinct structural features and different properties between homochiral and racemic counterparts. Propagation of helical chirality into the backbone of the crystalline frameworks leads to the observation of advanced chiroptical properties in the far-red visible spectrum, along with a less compact structure compared with the racemic frameworks. Homogeneous thin films of [5]HeliCOFs disclosed photoluminescent properties arising from the controlled growth of highly ordered π-conjugated lattices. The present study offers insight into general chiral framework formation and extends the Liebisch−Wallach rule to 2D COFs. KW - Chirality KW - Covalent organic frameworks KW - Diffraction KW - Lattices KW - Thin films PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633755 DO - https://doi.org/10.1021/jacs.5c01004 SN - 0002-7863 VL - 147 IS - 21 SP - 17750 EP - 17763 PB - American Chemical Society (ACS) CY - Washington, DC AN - OPUS4-63375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adamski, Paweł A1 - Zgrzebnicki, Michał A1 - Albrecht, Aleksander A1 - Jurkowski, Artur A1 - Wojciechowska, Agnieszka A1 - Ekiert, Ewa A1 - Sielicki, Krzysztof A1 - Mijowska, Ewa A1 - Smales, Glen J. A1 - Maximenko, Alexey A1 - Moszyński, Dariusz T1 - Ammonia synthesis over γ-Al2O3 supported Co-Mo catalysts N2 - Novel ammonia synthesis catalysts are sought due to energetic transformation and increasing environmental consciousness. Materials containing cobalt and molybdenum are showing state-of-art activities in ammonia synthesis. The application of γ-alumina support was proposed to enhance the properties of Co-Mo nanoparticles. The wet impregnation of the support was conducted under reduced pressure. The active catalysts were obtained by ammonolysis of precursors. The chemical and phase composition, as well as morphology, porosity, and surface composition of precursors and catalysts, were characterized. The Co-Mo nanoparticles phase composition as well as their size and dispersion were determined using X-ray absorption spectroscopy utilizing synchrotron radiation, electron microscopy, and X-ray scattering. The catalytic activity was tested in the ammonia synthesis process under atmospheric pressure. The activity and stability of the supported catalysts were compared with unsupported cobalt molybdenum nitride Co3Mo3N, revealing the superiority of the present approach. KW - Ammonia synthesis KW - Supported catalyst KW - Cobalt molybdenum nitrides KW - Scattering KW - X-ray scattering KW - Gamma-alumina KW - Stability PY - 2025 DO - https://doi.org/10.1016/j.mcat.2025.114907 SN - 2468-8231 VL - 575 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-64827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - del Rocío Silva-Calpa, Leydi A1 - de Souza Bernardes, Andrelaine A1 - de Avillez, Roberto Ribeiro A1 - Smales, Glen J. A1 - Camarena, Mariella Alzamora A1 - Ramos Moreira, Carla A1 - Zaitsev, Volodymyr A1 - Archanjo, Braulio Soares A1 - Letichevsky, Sonia T1 - From support to shell: An innovative design of air-stable nano zero-valent iron–nickel catalysts via structural self-assembly N2 - This work presents the design of air-stable core–shell zero-valent iron–nickel nanofilaments supported on silica and zeolite, developed to overcome the oxidation limitations of nano zero-valent iron in environmental catalysis. The nanofilaments feature ∼ 100 nm iron–nickel cores surrounded by ultrafine iron-rich threads embedded with aluminates and silicates, originating from partial support dissolution during synthesis. By varying the iron reduction time, three catalysts were prepared: one on silica reduced for 30 min, and two on zeolite reduced for 30 and 15 min. They were thoroughly characterized using nitrogen physisorption, X-ray diffraction, electron microscopy with elemental analysis, Mössbauer spectroscopy, and small-angle X-ray scattering. The zeolite-supported catalyst reduced for 15 min showed the highest activity for hexavalent chromium reduction (rate constant 8.054 min−1), attributed to a higher fraction of reactive iron–nickel phases formed under shorter reduction. Its tailored core–shell structure improves air stability and surface reactivity, highlighting its potential as a next-generation zero-valent iron nanocatalyst for aqueous remediation KW - nanofilaments KW - Core–shell nanostructures KW - Air-stable nanomaterials KW - Structure-controlled FeNi nanoparticles KW - Hexavalent chromium reduction KW - X-ray scattering KW - MOUSE PY - 2025 DO - https://doi.org/10.1016/j.mtcomm.2025.114142 SN - 2352-4928 VL - 49 SP - 1 EP - 15677 PB - Elsevier Ltd. AN - OPUS4-65087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Berry, Charlotte A. A1 - Reinart, Katre A1 - Smales, Glen J. A1 - Wilkinson, Holly N. A1 - Hardman, Matthew J. A1 - Marchesini, Sofia A1 - Lee, William A1 - Nery, Eveliny Tomás A1 - Moghaddam, Zarrin A1 - Hoxha, Agron A1 - Felipe-Sotelo, Mónica A1 - Gutierrez-Merino, Jorge A1 - Carta, Daniela T1 - Hierarchically porous copper and gallium loaded sol–gel phosphate glasses for enhancement of wound closure N2 - In this work, we have developed hierarchically porous phosphate-based glasses (PPGs) as novel materials capable of promoting wound closure and simultaneously delivering antibacterial effects at the glass-biological tissue interface. PPGs are characterised by extended porosity, which enhances the controlled release of therapeutic ions, whilst facilitating cell infiltration and tissue growth. Two series of PPGs in the systems P2O5–CaO–Na2O–CuO and P2O5–CaO–Na2O–Ga2O3 with (CuO and Ga2O3 0, 1, 5 and 10 mol%) were manufactured using a supramolecular sol–gel synthesis strategy. Significant wound healing promotion (up to 97%) was demonstrated using a human ex vivo wound model. A statistically significant reduction of the bacterial strains Staphylococcus aureus and Escherichia coli was observed in both series of PPGs, particularly those containing copper. All PPGs exhibited good cytocompatibility on keratinocytes (HaCaTs), and analysis of PPG dissolution products over a 7-day period demonstrated controlled release of phosphate anions and Ca, Na, Cu, and Ga cations. These findings indicate that Cu- and Ga-loaded PPGs are promising materials for applications in soft tissue regeneration given their antibacterial capabilities, in vitro biocompatibility with keratinocytes and ex vivo wound healing properties at the biomaterial-human tissue interface. KW - Porous glass KW - Phosphates KW - Wound healing materials KW - Antibacterial KW - X-ray scattering KW - MOUSE PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650867 DO - https://doi.org/10.1039/d5tb01945a SN - 2050-750X VL - 13 IS - 48 SP - 15662 EP - 15677 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -