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Hampel, Marco ; Schenderlein, Matthias ; Schary, Christian ; Dimper, Matthias ; Özcan Sandikcioglu, Özlem
High resolution analysis of corrosion processes on stainless steels is a challenging task. The application of local electrochemical techniques such as scanning electrochemical microscopy (SECM) has opened new possibilities for the detection of corrosion products and activity on metallic surfaces. However, due to its stochastic nature, the analysis of pitting corrosion requires being at the right place at the right time. Scanning over large areas at a high resolution not only leads to long scan durations but also leaves many short-lived processes undetected. In this paper we present the combined automated operation of SECM and wire multi-electrodes connected to a multi-electrode analyzer (MMA). The inter-electrode currents between 25 wire electrodes connected via zero resistance ammeters (ZRA) are measured by the MMA at open circuit potential (OCP) and the electrodes reporting anodic currents are detected automatically to be analyzed by means of SECM. The results demonstrate the successful application of this methodology for the detection of unstable and stable pitting processes on 304 stainless steel in a corrosive aqueous environment.
The Scope of the Workshop was to provide a forum for discussion on progress in development, characterisation and application of reference nanomaterials. Results of recently finsihed national and international research projects have been presented. Moreover, the need for future developments have been addressed.
Attendees of teh Workshop were expected to be experts from academia, research institutes, regulatory bodies and industry working or interested in the area of reference nanomaterials.
The following structure of Workshop was planned: the main focus of the first day was on reference material needs and development, while teh second day was focussed on reference materials characterisation and standardisation.
Over 111 participants frm 13 countries and teh European Joint Research Centre have regsitered for the Workshop with 16 platform presentations and 42 poster contributions grouped in 2 sessions and 10 topical areas.
A summary of the observations, analysis and conclusions of the Workshop is made including an overview table of links to information on existing reference nanomaterials.
An overview of the activities in the field of surface and microbeam analysis at BAM-6.1 is given with focus on physico-chemical characterization at the nanoscale. Ideas of potential joint activities are presented: structural and chemical analysis of graphene, deposition techniques for nanoparticles, EBSD on steel for a broader range of methods, instruments and types of steel, soft X-ray Analysis of low-Z materials, analysis of mesoporous thin films, etc.
Das EMPIR-Förderprogramm wird kurz erläutert und laufende Projekte aus der Nanotechnologie werden vorgestellt. Der Schwerpunkt liegt auf Standardisierungsprojekten, die gemeinsam mit ISO/TC 229 'Nanotechnologies' und CEN/TC 352 'Nanotechnologies' zu neuen Normen führen sollten. Als Beispiel für laufende Nanotechnologie-Projekte mit Koordination aus Deutschland werden MagNaStand (PTB) und nPSize (BAM) gegeben.
Ball mass is an important parameter that is known to have an influence on the outcome of a mechanochemical reaction induced by ball-milling. A standard way of modifying the ball mass is to change the size of the ball made of the same material. In this case, however, a change in mass is accompanied by a simulatneous change in the ball size. It is therefore not possible to disentangle the effects of mass and Surface area in these cases. In the present work we report the results of experiments with specially designed and manufactured balls in which (1) milling ball mass is held constant, but their size differs, and (2) the ball mass is altered, with the diameter of the milling ball being held constant. Using the cocrystallisation of theophylline + nicotinamide as a case study it was found that both diameter and ball mass play crucial roles in determining the rate of a mechanochemical reaction. For comparison, we have also used milling balls with the same size (different mass), and others with the same mass (different size) made of different materials, as would be “traditional”. It was found that, despite having the same size, the lightest milling ball (nylon) was the most efficient in initiating the co-crystallisation, presumably due to the sorption of EtOH. Hence, the results of this manuscript also demonstrate how milling ball material can in fact be the most influential parameter, and potentially counterintuitive to classical mechanics.
Yin, Huajie ; Chapala, P. ; Bermeshev, M. ; Pauw, Brian Richard ; Schönhals, Andreas ; Böhning, Martin
Superglassy polymers with a large fractional free volume have emerged as novel materials with a broad range of applications, especially in the field of membrane separations. Highly permeable addition-type substituted polynorbornenes with high thermal resistance and chemical stability are among the most promising materials. The major obstacle for extending the practical membrane application is their strong tendency to physical aging, leading to a partial decline in their superior transport performance over time. In the present study, broadband dielectric spectroscopy with complementary X-ray scattering techniques were employed to reveal changes in microporous structure, molecular mobility, and conductivity by systematic
comparison of two polynorbornenes with different numbers of trimethylsilyl side groups. Their response upon heating (aging) was compared in terms of structure, dynamics, and charge transport behavior. Furthermore, a detailed analysis of the observed
Maxwell−Wagner−Sillars polarization at internal interfaces provides unique information about the microporous structure in the
solid films. The knowledge obtained from the experiments will guide and unlock potential in synthesizing addition-type polynorbornenes with versatile properties.
View into the depths of copolymer microstructure by a special approach of LC-MS data evaluation
(2019)
It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. This is and will remain a challenge for analysts.
First a very short overview will be given concerning the common liquid separation techniques for polymers (SEC, LAC, LCCC, GELC) coupled to soft ionization mass spectrometric methods like MALDI and ESI-MS with focus on their limitations. For very broadly distributed samples or chemical very similar species the superposition of different separation mechanisms in chromatography is unavoidable or the separation efficiency cannot be optimized.
Different ionization probabilities and species of the same nominal mass with completely different structures are just two problems of mass spec of complex polymer mixtures.
Subsequently, different examples will be shown how these limitations in some cases could be outsmarted.
First example will be the separation of statistical EO-PO copolymers of different chemical compositions by end group functionality and the quantification of end group fractions over the whole CCD. Here an UP-LCCC / ESI-TOF-MS coupling is applied.
Further for different kinds of polymers it will be shown how it could be realized to obtain information on small isobaric/isomeric topological heterogeneities by coupling UP-SEC / ESI-TOF-MS.
All results are based on the data processing of reconstructed ion chromatograms of single mass traces of complex ESI-MS spectra.
In this study, the molecular dynamics of a series of dipole functionalized triphenylene-based discotics, forming a columnar mesophase, were investigated by broadband dielectric spectroscopy (BDS). In addition to conductivity and localized dynamics, glassy dynamics were also observed. At higher temperatures an α1-processes and at low temperatures an α2 processes were detected having a completely different temperature dependence of its relaxation times. Different molecular assignments of α1- and α2-processes are suggested. The phase behavior of the material was explored under helium purge down to 100 K by differential scanning calorimetry (DSC). Besides the phase transition temperatures and enthalpies, one or two thermal glass transitions were found for all the materials. Moreover, the glassy dynamics were further investigated by Flash DSC, which is a chip-based calorimetry technique allowing for fast heating and cooling rates as high as 10000K/s.
High performance polymers of intrinsic microporosity (PIMs) have emerged as novel materials with broad applications from gas separation to electronic devices. Sufficiently rigid, even contorted polymer chains show only limited molecular mobility, therefore undergo inefficient packing and give rise to intrinsic microporosity with pore size generally smaller than 1 nm and BET surface areas larger than 700 m2/g. Further performance optimization and long-term stability of devices incorporating PIMs rely on our understanding of structure-processing-property relationships and physical aging, in which glass transition plays a key role. Up to now no glass transition temperature (Tg) of PIMs could be detected with conventional thermal analysis techniques before degradation. Decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this. This was achieved by employing fast scanning calorimetry (FSC) based on a chip sensor, which is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. FSC provides definitive evidence of glass transition of a series of PIMs with a special consideration on the chain rigidity. The determined glass transition temperature of these PIMs follows the order of the rigidity of their backbone structures. FSC provides the first clear-cut experimental evidence of the glass transition of PIM-EA-TB with a Tg of 663 K, PIM-1 of 644 K and PIM-DMDPH-TB of 630 K at a heating rate of 1Χ104 K/s. Local fluctuations are featured in glass transition of highly rigid PIMs. As conformational changes are prevented by the backbone rigidity, the glass transition must rather be assigned to local small scale fluctuations.
Polymeric membranes represent a low-cost, energy efficient solution for gas separation. Recently polymers of intrinsic microporosity (PIMs) have emerged as prestigious membrane materials featuring a large concentration of pores smaller than 1 nm, a BET surface area larger than 700 m2/g and high gas permeability and selectivity. Unusual chain structure combining rigid segments with sites of contortion gives rise to the intrinsic microporosity. However, this novel class of glassy polymers are prone to pronounced physical aging. The initial microporous structures approach a denser state via local small scale fluctuataions, leading to a dramatic reduction in the gas permeabilities. For the first time, dielectric relaxation spectroscopy with state-of-the-art high-resolution analyzers was employed to investigate three representative PIMs with a systematic change in chain rigidity: PIM-EA-TB 〉 PIM-1 〉 PIM-MDPH-TB. The molecular mobility, the charge transport and their response upon heating (aging) in the polymers were measured in a broad temperature range through isothermal frequency scans during different heating / cooling cycles. Multiple dielectric processes following Arrhenius behavior were observed for the investigated polymers. Local fluctuations, Maxwell-Wagner-Sillars (MWS) polarization and structural relaxation phenomena were discussed and attempted to be correlated with the structural features of PIMs. Moreover, all PIMs showed conductivity in the glassy state. The significant increase in the conductivity with increasing temperature far below the glass transition temperature of PIMs is explained in terms of the loosely packed microporous structure and the formation of local intermolecular agglomerates due to interaction of π-electrons in aromatic moieties of the polymer backbone.