Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (244)
- Vortrag (120)
- Posterpräsentation (32)
- Beitrag zu einem Tagungsband (29)
- Beitrag zu einem Sammelband (28)
- Sonstiges (18)
- Forschungsbericht (7)
- Buchkapitel (2)
- Corrigendum (1)
Sprache
- Englisch (363)
- Deutsch (117)
- Mehrsprachig (1)
Schlagworte
- XPS (93)
- NEXAFS (58)
- ToF-SIMS (41)
- SIMS (18)
- Surface analysis (18)
- ESCA (14)
- Plasma polymerization (13)
- Nanoparticles (11)
- Plasma (11)
- AES (10)
Organisationseinheit der BAM
- 6 Materialchemie (66)
- 6.1 Oberflächen- und Dünnschichtanalyse (66)
- 4 Material und Umwelt (6)
- 4.1 Biologische Materialschädigung und Referenzorganismen (6)
- 6.3 Strukturanalytik (3)
- 9 Komponentensicherheit (3)
- 9.0 Abteilungsleitung und andere (3)
- 5 Werkstofftechnik (2)
- 5.1 Materialographie, Fraktographie und Alterung technischer Werkstoffe (2)
- 1 Analytische Chemie; Referenzmaterialien (1)
Eingeladener Vortrag
- nein (120)
Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM.
The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1-xAs and InxGa1 xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers a plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013.
The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and stability of the suspension. In this study, a systematic step-wise approach is carried out to identify optimal sonication conditions in order to achieve a stable dispersion. This approach has been adopted and shown to be suitable for several nanomaterials (cerium oxide, zinc oxide, and carbon nanotubes) dispersed in deionized (DI) water. However, with any change in either the nanomaterial type or dispersing medium, there needs to be optimization of the basic protocol by adjusting various factors such as sonication time, power, and sonicator type as well as temperature rise during the process. The approach records the dispersion process in detail. This is necessary to identify the time Points as well as other above-mentioned conditions during the sonication process in which there may be undesirable changes, such as damage to the particle surface thus affecting surface properties. Our goal is to offer a harmonized approach that can control the Quality of the final, produced dispersion. Such a guideline is instrumental in ensuring dispersion quality repeatability in the nanoscience community, particularly in the field of nanotoxicology.
Magnetic iron oxide nanoparticle clusters (mnpc) coated with organic stabilizers were investigated using scanning transmission x-ray microscopy (STXM). Simultaneous surface and bulk sensitive Fe L3 edge absorption spectra, obtained using a photomultiplier tube and a channeltron, were used to detect subtle changes in the oxidation state in the surface and bulk of Iron Oxide mnpc.
The effectiveness of this mode of STXM operation is demonstrated for These nanoparticle clusters.
A sealable ultrathin window sample cell for the study of liquids by means of soft X-ray spectroscopy
(2017)
A new sample cell concept for the analysis of liquids or solid-liquid interfaces using soft X-ray spectroscopy is presented, which enables the complete sealing of the cell as well as the Transport into vacuum via, for example, a load-lock system. The cell uses pressure monitoring and active as well as passive pressure regulation systems, thereby facilitating the full control over the pressure during filling, sealing, evacuation, and measurement. The cell design and sample preparation as well as the crucial sealing procedure are explained in detail. As a first proof-of-principle experiment, successful nitrogen K-edge fluorescence yield near-edge X-ray absorption fine structure experiments of a biomolecular solution are presented. For this purpose, it is shown that the careful evaluation of all involved parameters, such as window type or photon flux, is desirable for optimizing the experimental result.
Role of metal cations in plasmon-catalyzed oxidation: A case study of p-aminothiophenol dimerization
(2017)
The mechanism of the plasmon-catalyzed reaction of p-aminothiophenol (PATP) to 4,4′-dimercaptoazobenzene (DMAB) on the surface of metal nanoparticles has been discussed using data from surface-enhanced Raman scattering of DMAB. Oxides and hydroxides formed in a plasmon-catalyzed process were proposed to play a central role in the reaction. Here, we report DMAB formation on gold nanoparticles occurring in the presence of the metal cations Ag+, Au3+, Pt4+, and Hg2+. The experiments were carried out under conditions where formation of gold oxide or hydroxide from the nanoparticles can be excluded and at high pH where the formation of the corresponding oxidic species from the metal ions is favored. On the basis of our results, we conclude that, under these conditions, the selective oxidation of PATP to DMAB takes place via formation of a metal oxide from the ionic species in a plasmon-catalyzed process. By evidencing the necessity of the presence of the metal cations, the reported results underpin the importance of metal oxides in the reaction.
Water and aqueous reagents are essential in any biological process or system. But apart from a few special low vapor-pressure cases, liquids have not been accessible to any technique requiring UHV conditions. EnviroESCA opens up this exciting field of applications.
In this paper first results from water based samples are presented as a proof of concept to demonstrate the special capabilities of EnviroESCA analyzing liquid samples. The following solutions were investigated under near ambient pressure conditions: i.) water, ii.) brine, iii.) an oil in water dispersion, iv.) aqueous iron(II) sulfate heptahydrate, and v.) a suspension of nano silver particles in water.
A controlled, reproducible, gram-scale method is reported for the covalent functionalization of graphene Sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. The reaction between commercially available 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized sheets. The different reactivities of the chlorine substituents on the functionalized graphene allow stepwise post-modification by manipulating the temperature.
This new method provides unique access to defined bifunctional 2D nanomaterials, as exemplified by chiral surfaces and multifunctional hybrid architectures.
The use of duplex stainless steels (DSS) in energy related applications is well known. Nowadays, DSS steels become more favorable than austenitic steels due to the outstanding mechanical properties, the good corrosion resistance and the lower nickel content. However, the use of the duplex grade in acidic environments such as seawater often leads to severe degradation of the structural integrity of the steel by hydrogen-induced/assisted cracking (HAC) phenomena, which can eventually result in premature failure. Hydrogen assisted degradation and cracking of steels are active fields of research even though this topic is intensively studied for more than a century. A bottleneck is the analytical validation of the theoretical models proposed ion the literature at the sub-micron scale.
Industrial and the research communities see a need for an accurate analytical method by which it is possible to image the distribution of hydrogen in the microstructure of a steels or and other alloys. Among the very few available methods hydrogen imaging methods, Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) has the principal capability for mapping of hydrogen in a steel’s microstructure. The combination of ToF-SIMS with multivariate data analysis (MVA), electron microscopy (SEM) and electron-backscattered diffraction (EBSD) is a powerful approach for providing chemical and structural information. The use of data fusion techniques has been shown recently to enhance the better understanding of the hydrogen induced degradation processes in in a DSS steel.
CCQM has established a framework of comparisons to demonstrate the international comparability of chemical measurements. The key point is the establishment of comparable measurements, with traceability to internationally or nationally stated references.
Originally initiated by Dr Martin P Seah, NPL, the Surface Analysis Working Group (SAWG) has been formally founded in 2003. The following terms of reference were presented to CCQM in April 2002. CCQM ratified the group as a full working group of CCQM in April 2003 with these terms of reference:
- to develop pilot studies and carry out key comparisons of national measurement standards for surface and micro/nano-analysis;
- to assist in identifying and establishing inter-laboratory work to improve the traceability of surface and micro/nano-analysis;
- to establish and update a work plan to be adopted by CCQM;
- to discuss and review the scope of the working group and to liase with other working groups related to nanotechnology.
Following the 2016 meeting, the Key Comparison K-129 "Measurement of atomic fractions in Cu(In,Ga)Se2 Films" lead by KRISS and the Key Comparison K-136 on "BET specific surface area of nanoporous Al2O3" lead by UNIIM&BAM have been finished in 2016.
The 15th meeting of SAWG will focus on
- survey on CMC claim submitted with reference to K-129 and K-136.
- the overall and SAWG specific aspects of the CCQM Strategy process,
- a joint meeting with the Inorganic Working Group addressing number concentrations of nano particles,
- discussion of future comparisons.