Nano
Filtern
Dokumenttyp
- Zeitschriftenartikel (347)
- Vortrag (338)
- Posterpräsentation (100)
- Forschungsdatensatz (50)
- Sonstiges (20)
- Beitrag zu einem Tagungsband (16)
- Buchkapitel (10)
- Beitrag zu einem Sammelband (10)
- Forschungsbericht (9)
- Zeitschriftenheft (Herausgeberschaft für das komplette Heft) (6)
Sprache
- Englisch (870)
- Deutsch (52)
- Spanisch (2)
- Mehrsprachig (1)
Schlagworte
- Nanoparticles (124)
- Nano (70)
- SAXS (64)
- XPS (60)
- Laser-induced periodic surface structures (LIPSS) (59)
- Fluorescence (53)
- Quantum yield (51)
- Electron microscopy (48)
- Nanoparticle (46)
- X-ray scattering (46)
Organisationseinheit der BAM
- 6 Materialchemie (659)
- 6.1 Oberflächen- und Dünnschichtanalyse (345)
- 1 Analytische Chemie; Referenzmaterialien (184)
- 1.2 Biophotonik (159)
- 6.6 Physik und chemische Analytik der Polymere (134)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (129)
- 6.2 Material- und Oberflächentechnologien (90)
- 5 Werkstofftechnik (61)
- 4 Material und Umwelt (46)
- 5.4 Multimateriale Fertigungsprozesse (33)
- 6.3 Strukturanalytik (27)
- 7 Bauwerkssicherheit (27)
- 4.2 Material-Mikrobiom Wechselwirkungen (26)
- 9 Komponentensicherheit (25)
- 9.5 Tribologie und Verschleißschutz (20)
- 4.1 Biologische Materialschädigung und Referenzorganismen (19)
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (17)
- 1.5 Proteinanalytik (14)
- 6.7 Materialsynthese und Design (14)
- 8 Zerstörungsfreie Prüfung (14)
- 5.1 Mikrostruktur Design und Degradation (13)
- 5.6 Glas (10)
- 8.5 Röntgenbildgebung (9)
- VP Vizepräsident (9)
- VP.1 eScience (9)
- 1.9 Chemische und optische Sensorik (8)
- 6.0 Abteilungsleitung und andere (7)
- 1.0 Abteilungsleitung und andere (5)
- 7.6 Korrosion und Korrosionsschutz (5)
- 1.1 Anorganische Spurenanalytik (4)
- 7.4 Baustofftechnologie (4)
- 1.8 Umweltanalytik (3)
- P Präsident (3)
- 1.7 Organische Spuren- und Lebensmittelanalytik (2)
- 3 Gefahrgutumschließungen; Energiespeicher (2)
- 5.2 Metallische Hochtemperaturwerkstoffe (2)
- 5.5 Materialmodellierung (2)
- 8.0 Abteilungsleitung und andere (2)
- 9.0 Abteilungsleitung und andere (2)
- 9.4 Integrität von Schweißverbindungen (2)
- P.0 Präsident und andere (2)
- 1.3 Instrumentelle Analytik (1)
- 1.4 Prozessanalytik (1)
- 2 Prozess- und Anlagensicherheit (1)
- 2.1 Sicherheit von Energieträgern (1)
- 3.0 Abteilungsleitung und andere (1)
- 3.5 Sicherheit von Gasspeichern (1)
- 4.5 Kunst- und Kulturgutanalyse (1)
- 5.0 Abteilungsleitung und andere (1)
- 5.3 Polymere Verbundwerkstoffe (1)
- 6.4 Materialinformatik (1)
- 7.1 Baustoffe (1)
- 7.2 Ingenieurbau (1)
- 8.1 Sensorik, mess- und prüftechnische Verfahren (1)
- 8.4 Akustische und elektromagnetische Verfahren (1)
- 8.6 Faseroptische Sensorik (1)
- 9.2 Versuchsanlagen und Prüftechnik (1)
- 9.3 Schweißtechnische Fertigungsverfahren (1)
- MP Mitglied des Präsidiums (1)
- MP.0 Mitglied des Präsidiums und andere (1)
- PST Präsidiale Stabsstelle (1)
Paper des Monats
- ja (15)
In our (dramatically understaffed) X-ray scattering laboratory, developing a systematic, holistic methodology let us provide scattering and diffraction information for more than 2100 samples for 200+ projects led by 120+ collaborators. Combined with automated data correction pipelines, and our analysis and simulation software, this led to more than 40 papers in the last 5 years with just over 2 full-time staff members.
This year, our new, modular synthesis platform has made more than 1000 additional samples for us to analyse and catalogue. By virtue of the automation, the synthesis of these samples is automatically documented in excruciating detail, preparing them for upload and exploitation in large-scale materials databases.
This talk is intended to spark ideas and invite collaborations by providing an overview of: 1) the current improvements in our wide-range X-ray scattering laboratory methodology, and 2) introducing our open, modular robotic platform for systematic sample preparation.
Hierarchically porous, high‐surface‐area silica materials are excellent candidates for multiple applications like catalysis and environmental remediation. Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on‐demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK‐12 slurries were robocasted into monoliths, containing different ratios of uncalcined COK‐12 and sodium bentonite (0–25 wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69 vs. 0.32) and higher yield stresses (96 vs. 259 Pa) compared to pure COK‐12 ones. Monoliths were printed in woodpile structures and calcined at 600°C. Micro‐CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20 ± 0.07 to 1.0 ± 0.3 MPa) with increasing binder/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK‐12 was retained. The structures exhibited open porosities of 52 ± 4% and showed higher specific mesopore volumes, and increased average mesopore size (6 vs. 8 nm) compared to COK‐12. Small‐angle x‐ray scattering analysis revealed an increased lattice parameter (10.3 vs. 11.0 nm) and reduced wall thickness (3.1 nm vs. 4.1 nm) of the COK‐12 in the monoliths. These properties indicate suitability for their application as porous supports and adsorbents.
Due to the extremely high specific surface area of nanoparticles and corresponding potential for adsorption, the results of surface analysis can be highly dependent on the history of the particles, particularly regarding sample preparation and storage. The sample preparation method has, therefore, the potential to have a significant influence on the results. This report describes an interlaboratory comparison (ILC) with the aim of assessing which sample preparation methods for ToF-SIMS analysis of nanoparticles provided the most intra- and interlaboratory consistency and the least amount of sample contamination. The BAM reference material BAM-P110 (TiO2 nanoparticles with a mean Feret diameter of 19 nm) was used as a sample representing typical nanoparticles. A total of 11 participants returned ToF-SIMS data,in positive and (optionally) negative polarity, using sample preparation methods of “stick-and-go” as well as optionally “drop-dry” and “spin-coat.” The results showed that the largest sources of variation within the entire data set were caused by adventitious hydrocarbon contamination or insufficient sample coverage, with the spin-coating protocol applied in this ILC showing a tendency toward insufficient sample coverage; the sample preparation method or the participant had a lesser influence on results.
Test artifact for fs-LDW
(2023)
Ionic Liquid Crystals are ionic liquids that exhibit liquid crystalline mesomorphism together with ionic conductivity. As known confined liquid crystal mesophases can show an anomalous dynamics and phase behavior. Investigations considering the factors controlling the macroscopic properties of ILCs in confinement are scare in the literature. This study reports the molecular mobility, and the phase transition behavior of a guanidinium based columnar ILC confined in the nanopores of self-ordered anodic aluminum oxide membranes of various pore diameters (25 – 180 nm) using Broadband Dielectric Spectroscopy (BDS), calorimetry and X-ray scattering. It is aimed to reveal in which way the pore size as well as the pore surface wettability (hydrophobic or hydrophilic) alters the molecular dynamics, and phase transition behavior for this system. These properties are crucial for applications. The DSC investigations reveal: (i) the phase transition temperature for the transition from the plastic crystalline to the crystalline-liquid state has non-monotonic dependence versus the inverse pore diameter and (ii) the transition from the liquid crystalline to the isotropic phase is suppressed for all nanoconfined samples. This transition suppressed in the thermal signal was evidenced by BDS and X-ray scattering. It is discussed as a continuous phase transition taking place in the pores instead of a discontinuous first order transition as observed for the bulk. BDS investigations show different relaxation processes for the bulk and the nanoconfined ILC. Molecular origins for various relaxation processes are discussed and suggested. It is further shown that the self-assembly of this ILC is dynamic in nature which might apply for other ILCs too. The obtained results will have implications for the nanoscale applications of ionic liquid crystals.
Bulk metallic glasses (BMG) are amorphous metal alloys known for their unique physical and mechanical properties. In the present study, the formation of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on the Zr-based BMGs Zr46Cu46Al8, Zr61Cu25Al12Ti2, Zr52.5Cu17.9Al10Ni14.6Ti5 (Vit105) and Zr57Cu15.4Al10Ni12.6Nb5 (Vit106) was investigated as a function of their different chemical composition. For this purpose, LIPSS were generated on the sample surfaces in an air environment by fs-laser irradiation (λ = 1025 nm, τ = 300 fs, frep = 100 kHz). The surface topography was characterized by scanning electron microscopy and atomic force microscopy. Moreover, the impact of LIPSS formation on the structure and chemical surface composition was analyzed before and after fs-laser irradiation by X-ray diffraction and X-ray photoelectron spectroscopy as well as by transmission electron microscopy in combination with energy dispersive X-ray spectroscopy. Despite the different chemical composition of the investigated BMGs, the fs-laser irradiation resulted in almost similar properties of the generated LIPSS patterns. In the case of Zr61Cu25Al12Ti2, Vit105 and Vit106, the surface analysis revealed the preservation of the amorphous state of the materials during fs-laser irradiation. The study demonstrated the presence of a native oxide layer on all pristine BMGs. In addition, fs-laser irradiation results in the formation of laser-induced oxide layers of larger thickness consisting of an amorphous ZrAlCu-oxide. The precise laser-structuring of BMG surfaces on the nanoscale provides a versatile alternative to thermoplastic forming of BMG surfaces and is of particular interest for the engineering of functional material surfaces.
Iron Oxide Nanocubes as a New Certified Reference Material for Nanoparticle Size Measurements
(2023)
The rational design and increasing industrial use of nanomaterials require a reliable characterization of their physicochemical key properties like size, size distribution, shape, and surface chemistry. This calls for nanoscale reference materials (nanoRMs) for the validation and standardization of commonly used characterization methods closely matching real-world nonspherical nano-objects. This encouraged us to develop a nonspherical nanoRM of very small size consisting of 8 nm iron oxide nanocubes (BAM-N012) to complement spherical gold, silica, and polymer nanoRMs. In the following, the development and production of this nanoRM are highlighted including the characterization by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) as complementary methods for size and shape parameters, homogeneity and stability studies, and calculation of a complete uncertainty budget of the size features. The determination of the nanocubes’ edge length by TEM and SAXS allows a method comparison. In addition, SAXS measurements can also provide the mean particle number density and the mass concentration. The certified size parameters, area equivalent circular diameter and square edge length, determined by TEM with a relative expanded uncertainty below 9%, are metrologically traceable to a natural constant for length, the very precisely known (111) lattice spacing of silicon. Cubic BAM-N012 qualifies as a certified nanoRM for estimating the precision and trueness, validation, and quality assurance of particle size and shape measurements with electron microscopy and SAXS as well as other sizing methods suitable for nanomaterials. The production of this new iron oxide nanocube RM presents an important achievement for the nanomaterial community, nanomaterial manufacturers, and regulators.
The basic principles of generation of electrons and X-rays and the operation of SEM/EDS instruments are presented. Examples, recent successes and challenges in the analysis of nano-structures are given. Multi-method analytical approaches with the focus on imaging the nanoscale are highlighted. Details on the sample preparation and persepective on the automated analysis (sample preparation, measurement, data analyis and storage) are given. Metrological aspects, standardisation, and reference materials are also emphasized by examples.
With femtosecond-laser direct writing (fs-LDW) maturing in all aspects as a manufacturing technology, a toolset for quality assurance must be developed. In this work we introduce a first of its kind test artifact. Test artifacts are standardized 3D models with specific geometric features to evaluate the performance of writing parameters. Test artifacts are already common in other 3D additive manufacturing technologies e.g. selective laser melting. The test artifact introduced in this work was developed in particular to accommodate the high geometrical resolution of fs-LDW structures and the limited possibilities to examine the resulting structure. Geometric accuracy, surface adhesion as well as confocal Raman spectroscopy results were considered when evaluating the design of the test artifact. We will explain the individual features and design considerations of our fs-LDW test artifact. The difference between two slicers, Cura and 3DPoli, and the implications on measured feature sizes and the general shape is quantified. The measured geometries are used to derive a general design guide for a specific combination of photoresists, laser power and scanning speed and to analyze the geometric accuracy of a structure produced using these guidelines. The shown test artifact is publicly available as STL file on GitHub (https://github.com/BAMresearch/2PP-TestArtifact) and in the supplement.
Surface-functionalized polymer beads encoded with molecular luminophores and nanocrystalline emitters such as semiconductor nanocrystals, often referred to as quantum dots (QDs), or magnetic nanoparticles are broadly used in the life sciences as reporters and carrier beads. Many of these applications require a profound knowledge of the chemical nature and total number of their surface functional groups (FGs), that control bead charge, colloidal stability, hydrophobicity, and the interaction with the environment and biological systems. For bioanalytical applications, also the
number of groups accessible for the subsequent functionalization with, e.g., biomolecules or targeting ligands is relevant. In this study, we explore the influence of QD encoding on the amount of carboxylic acid (COOH) surface FGs of 2 μm polystyrene microparticles (PSMPs). This is done for frequently employed oleic acid and oleylamine stabilized, luminescent core/shell CdSe QDs and two commonly used encoding procedures. This included QD addition during bead formation by a thermally induced polymerization reaction and a post synthetic swelling procedure. The accessible number of COOH groups on the surface of QD-encoded and pristine beads was quantified by two colorimetric assays, utilizing differently sized reporters and electrostatic and covalent interactions. The results were compared to the total number of FGs obtained by a conductometric titration and Fourier transform infrared spectroscopy (FTIR). In addition, a comparison of the impact of QD and dye encoding on the bead surface chemistry was performed. Our results demonstrate the influence of QD encoding and the QD-encoding strategy on the number of surface FG that is ascribed to an interaction of the QDs with the carboxylic acid groups on the bead surface. These findings are of considerable relevance for applications of nanoparticle-encoded beads and safe-by-design concepts for nanomaterials.