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Inspired by the chemistry of mussel adhesive proteins, polydopamine (PDA has been shown as one of the most versatile platforms for altering the properties and incorporating new functionalities to nearby any material surface despite its nature. Rich chemistry of PDA enables broad variety of surface modification and diverse secondary reactions that makes it extremely interesting for a wide range of application including biomedical field, e.g., drug delivery, adhesives, cell adhesion, biosensing. Despite high potential of polydopamine, the lack of deposition control and precision in existed methods limits their applications in microdevices and miniaturized functional systems like, for example, MEMS, microfluidic and sensorics.
Herein, we demonstrate a novel maskless approach for surface micropatterning with polydopamine based on Multiphoton Lithography that overcomes present limitations. Neither strong oxidants, metal ions nor adjustment of pH to alkaline is required by this technique. The spatial resolution down to 0.8 µm has been achieved which is at least an order of magnitude smaller than shown by other existed methods. We are able to control the morphology and thickness of the micropattern by altering fabrication parameters allowing structure gradient.
Apart from the glass substrate, we achieved PDA patterning at surfaces of different nature such as polychlorotrifluoroethylene, polydimethylsiloxane, polyethylene terephthalate, silicon wafers, and fluorinated glass coverslips. Post-modification of polydopamine micropatterns with protein enzyme like trypsin is demonstrated to highlight its sensing potential.
Presented in this work microfabrication technique empowers advanced applications of mussel-inspired materials in single-molecule bioassays, sensors and other complex microdevices.
Moderne Leichtbaustrukturen (Luftfahrt, Eisenbahn, Automotive) aus Faserverbundwerkstoffen (FVW) sind hohen mechanischen und klimatischen Beanspruchungen ausgesetzt. Aussagen über die Lebensdauer und Funktionssicherheit der FVW-Bauteile können eher aus Untersuchungen der mikromechanischen Eigenschaften gewonnen werden als aus der globalen Festigkeit. Die Röntgenrefraktionstopografie ist ein Verfahren zur zerstörungsfreien Bestimmung von inneren Oberflächen in Werkstoffen. Angewendet auf FVW lassen sich Aussagen über die Faserorientierungen, die Fertigungsqualität sowie über Faser-Matrix-Ablösungen und Matrixrisse infolge mechanischer Beanspruchung gewinnen. Nachfolgend wird ein neues Verfahren zur Bestimmung des Zwischenfaserbruchversagens am komplexen Laminat vorgestellt. Hierbei wird das Röntgenrefraktionsverfahren "online bei Zug-Belastung der Probe angewendet.
Mit einer langfristigen Forschungsstrategie begleiten die für die Sicherheit von Mensch und Umwelt zuständigen Bundesoberbehörden (Umweltbundesamt, Bundesinstitut für Risikobe-wertung, Bundesanstalt für Arbeitsschutz und Arbeitsmedizin, Bundesanstalt für Materialfor-schung und -prüfung und Physikalisch-Technische Bundesanstalt) die rasch voranschreiten-de Entwicklung neuer Materialien unter den Gesichtspunkten des Arbeits-, Verbraucher- und Umweltschutzes. Die Strategie steht daher in enger Verbindung zu den öffentlichen Förder-programmen für Nanomaterialien und andere innovative Werkstoffe, z. B. des BMBF („Vom Material zur Innovation“) und der EU („Horizon 2020“).
Die Forschungsstrategie baut auf den bisherigen Ergebnissen der 2008 begonnenen und 2013 erstmals bilanzierten gemeinsamen Forschungsstrategie der Bundesoberbehörden „Nanotechnologie - Gesundheits- und Umweltrisiken von Nanomaterialien"1 auf und erweitert den Blickwinkel auch auf andere Materialinnovationen, bei denen vergleichbare Risiken für Mensch und Umwelt bestehen oder abgeklärt werden müssen. Darüber hinaus greift sie die Idee „anwendungssichere chemische Produkte“2 aus der Initiative „Neue Qualität der Arbeit“ (INQA) des Bundesministeriums für Arbeit und Soziales (BMAS) und das Konzept der nach-haltigen Chemie3 auf, das vom Bundesministerium für Umwelt, Naturschutz, Bau und Reak-torsicherheit (BMUB) unterstützt wird. Durch eine anwendungssichere und umweltverträgli-che Gestaltung innovativer Materialien und ihrer Folgeprodukte sollen nicht akzeptable Risi-ken für Mensch und Umwelt von Anfang an weitgehend ausgeschlossen werden. Dies kann erreicht werden durch
1.
die Verwendung sicherer Materialien ohne Gefahreneigenschaften für Mensch und Umwelt (direkte Anwendungssicherheit) oder
2.
eine Produktgestaltung, die über den gesamten Lebenszyklus emissionsarm und umweltverträglich ist (integrierte Anwendungssicherheit) oder
3.
eine Unterstützung des Anwenders (product stewardship) durch den Hersteller bei technischen, organisatorischen und persönlichen Schutzmaßnahmen zur sicheren Verwendung und Entsorgung des Produktes (unterstützte Anwendungssicherheit).
Die Fortschreibung der Forschungsstrategie soll als Bestandteil des Nanoaktionsplans 2020 der Bundesregierung Beiträge der Ressortforschung zu folgenden Schwerpunkten leisten:
•
Charakterisierung und Bewertung der Risiken von Materialinnovationen
•
Unterstützung von Forschungseinrichtungen und Unternehmen
•
Fortschreiben von Rechtsvorschriften und Praxisempfehlungen
1
http://www.baua.de/nn_47716/de/Themen-von-A-Z/Gefahrstoffe/Nanotechnologie/pdf/Forschungsstrategie.pdf
2 http://www.baua.de/de/Themen-von-A-Z/Gefahrstoffe/Nachhaltige-Chemie/Nachhaltige-Chemie.html
3
http://www.umweltbundesamt.de/themen/chemikalien/chemikalien-management/nachhaltige-chemie
2
•
Gesellschaftliche Akzeptanz
Die Forschungsstrategie soll mit Projekten und anderen forschungsnahen Aktivitäten umge-setzt werden. Dies umfasst die eigene Forschung der Häuser, die extramurale Ausschrei-bung und Vergabe von Forschungsdienstleistungen sowie die Beteiligung an vorwiegend öffentlich geförderten Drittmittelprojekten. Hinzu kommen Aktivitäten im Rahmen der Politik-beratung und der hoheitlichen Aufgaben. Mit inter- und transdisziplinären Ansätzen soll die Risiko- und Sicherheitsforschung enger mit der Innovationsforschung und Materialentwick-lung verknüpft werden. Die Forschungsstrategie ist aufgrund der raschen Entwicklungen auf diesem Gebiet für den Zeitraum bis 2020 angelegt. Die Forschungsziele adressieren die in diesem Zeitraum voraussichtlich umsetzbaren Forschungsansätze. Die Forschungsstrategie wird durch einen Arbeitskreis begleitet und spätestens mit Ablauf des Nanoaktionsplans 2020 evaluiert und angepasst.
Non-isothermal heating rate kinetics was applied to two epoxy resin systems. In situ near-infrared (NIR) measurements were taken with a heatable NIR cell which allowed the cure to be monitored by characteristic absorption bands. An autocatalyzed reaction of the nth order was shown to describe the epoxy conversion curves. Differential Scanning Calorimetry (DSC) was used as a complementary method. The kinetic models developed by both NIR and DSC are in good accordance with experimental epoxy conversion in the in situ NIR setup for single and multiple cure temperature ramps.
A linear calibration curve of the characteristic absorption bands of epoxy normalized to aromatic vibrations was introduced. The curing degree of structural epoxies that were cured according to an industrial temperature cure profile was determined by NIR using the calibration curve. The epoxy conversions of the structural components showed good agreement with the experimental in situ NIR. Several degrees of cure for structural specimens were evaluated by NIR and residual reaction enthalpy by DSC. We present the non-destructive NIR spectroscopy as an alternative to determine fast and non-destructive epoxy conversion, particularly suitable for high degrees of cure on structural components.
Immobilization of silanized DNA on glass: influence of the silane tether on the DNA hybridization
(2010)
Two trifunctional (trimethoxy and triethoxy) and one difunctional (methyldimethoxy) 3-mercaptopropyl-alkoxysilanes were covalently tethered to thiolated DNA oligonucleotides in solution. After deposition as microarrays onto glass, the immobilized DNA probes were tested for hybridization ability by a florescence-based method. The results demonstrate a large enhancement in the fluorescence signal when the functionality of the silane tether is reduced from three to two. An XPS analyses revealed that this is not due to a higher DNA surface density. FTIR spectra of the spin-coated silanes showed that the trifunctional silanes form branched and cyclic siloxane moieties, whereas the difunctional silane generates predominantly short straight siloxane chains. Therefore, the propensity of trifunctional silanes to form more complex networks leads to conformations of the bound DNA which are less favorable for the specific interaction with the complementary strand. The data implicate that further significant improvements in the DNA hybridization ability are possible by adroit choice of the silane system.
Efficient formation of difluoramino (NF2) groups within the polymer matrix upon exposure of polyamides (PA6 and PA12) to elemental fluorine is reported. The reaction was assessed on bulk and thin-film samples by means of RA-FTIR (reflection–absorption FTIR), XPS (X-ray photoelectron spectroscopy), and NMR (nuclear magnetic resonance) techniques. Direct fluorination causes cleavage of the amide C–N bond and concomitant formation of the NF2 chain-end functionalities as evident from an exceptionally large shift (+5 eV) of the N 1s binding energy and an increase of the v(CO) frequency by about 80 cm-1. The structural model is supported by the 19F NMR spectra of volatile reaction products that clearly reveal the presence of the NF2 group.
Today, chemical admixtures like superplasticisers and stabilising agents are extremely important for modern concrete technology. These agents have meanwhile become common practice in concrete technology, but the understanding within the entire system lags far behind their application. The macroscopic rheology of concrete in the presence of superplasticizers strongly depends upon effects on a much smaller scale such as the hydration of the cement, the adsorption of superplasticizers, and the pore solution chemistry.
In recent years, an increasing trend towards investigating and monitoring the contamination of the environment by microplastics (MP) (plastic pieces < 5 mm) has been observed worldwide. Nonetheless, a reliable methodology that would facilitate and automate the monitoring of MP is still lacking. With the goal of selecting practical and standardized methods, and considering the challenges in microplastics detection, we present here a critical evaluation of two vibrational spectroscopies, Raman and Fourier transform infrared (FTIR) spectroscopy, and two extraction methods: thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS) and liquid extraction with subsequent size exclusion chromatography (SEC) using a soil with known contents of PE, PP, PS and PET as reference material. The obtained results were compared in terms of measurement time, technique handling, detection limits and requirements for sample preparation. The results showed that in designing and selecting the right methodology, the scientific question that determines what needs to be understood is significant, and should be considered carefully prior to analysis. Depending on whether the object of interest is quantification of the MP particles in the sample, or merely a quick estimate of sample contamination with plastics, the appropriate method must be selected. To obtain overall information about MP in environmental samples, the combination of several parallel approaches should be considered.
A correlation of adhesion force and electrical conductivity is established for a vanadium oxide and highly oriented pyrolytic graphite (HOPG). Adhesion forces were determined by analysis of pull-off forces obtained from force–distance curves with atomic force microscopy in ultrahigh vacuum, on clean surfaces and with defined contact conditions. The investigated samples include (i) different stoichiometries of Magnéli-type vanadium oxides (V3O5, V4O7, V6O11, and V7O13), which undergo metal-insulator-transitions as a function of temperature, (ii) the (0001) basal plane and the (10–10) prism plane of highly oriented pyrolytic graphite (HOPG), which differ in their respective perpendicular-plane electrical conductivities by several orders of magnitude, and (iii) the (100) surfaces of pure metal single crystals, i.e., silver (Ag), copper (Cu), iron (Fe) and gold (Au). It is shown, that the vanadium oxides as well as the graphite exhibit significantly lower adhesion forces in their electrical conductive state than in their non-electrical conductive state. The values obtained for the electrical conductive states are quantitatively confirmed by the measurements on the single crystal metals.
The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has an enormous influence on the early hydration of cement. The hydration is retarded and the timing of formation and the morphology of hydrates is affected. This short paper presents experimental results about the influence of delayed addition time of PCE SPs on hydration of cement and alite pastes, investigated by isothermal heat flow calorimetry. For cement as well as for alite pastes the hydration is retarded with SP, whereby the high charge PCE has a stronger retarding effect than the low charge PCE. The retardation caused by PCE is much more pronounced for alite than for cement mixes. If PCE is added later to the mix, the induction period is shortened and the hydration is accelerated compared to simultaneous addition. This applies for cement and alite pastes. With delayed PCE addition the alite shows a clearly less retarded setting and main hydration than after simultaneous addition. It is obvious that for alite pastes there is less retardation the later the addition of SP.
The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has an enormous influence on the early hydration of cement. The hydration is retarded and the timing of formation and the morphology of hydrates is affected. This short paper presents experimental results about the influence of delayed Addition time of PCE SPs on hydration of cement and tricalcium aluminate (C3A) pastes, investigated by isothermal heat flow calorimetry. For cement pastes the hydration is retarded with SP, whereby the high charge PCE has a stronger retarding effect than the low charge PCE. With delayed PCE addition the cement shows a less retarded setting than with simultaneous addition. The alteration caused by PCE is much more pronounced for C3A and gypsum mixes than for cement. If the SP is added simultaneous, the exothermic peak of C3A is retarded. However, with delayed addition of SP the hydration is shortened, the gypsum depletion is fastened and the exothermic peak occurs less retarded or even accelerated compared to simultaneous addition. It is obvious that for C3A pastes there is less retardation the later the Addition of SP. Furthermore, the PCE alter the hydration of C3A when added delayed and exhibit changes in kinetics and hydration rates. The rate of reaction in the second stage is lower, discernible in decreased slopes and broader peaks. Besides this, a distinct ramp in the C3A heat flow curves within the first stage of C3A hydration occurs for all pastes with delayed addition of SP, which suggests an accelerated ettringite formation.
The damage caused by ionizing radiation to DNA and proteins is the reason to treat cancer by radiation therapy. A better understanding of the molecular processes and quantification of the different damaging mechanisms is the prerequisite to develop more efficient therapies. Hereby the understanding of the processes involved in the damage to DNA are of key interest due to its central role in reproduction and mutation.
For radiation with low linear energy transfer (LET), most of the damage is caused by the secondary particles produced by scattering of the ionizing radiation with water. Thereby a multitude of species are produced, whereby especially kinetic low energy electrons, prehydrated electrons, OH-radicals and ions are of importance. With higher LET the relative amount of the direct damaging effects increases. This is especially important considering the increased usage of high LET nucleons in radiation therapy. Therefore, the quantification of the contribution to DNA damage of direct and indirect effects and the different secondary species is of high interest due to the increase of radio biological efficiency when applying high LET radiation.
Here we present an approach to investigate the relative contributions to DNA strand break yield for radiation of different LET within a single electron microscope in combination with electron scattering simulations.
Chemical, morphological and accumulation phenomena in ultrashort-pulse laser ablation of TiN in air
(2000)
Ultrashort-pulse laser ablation (F=130 fs, 5=800 nm, repetition rate 2-20 Hz) of titanium nitride was investigated for laser fluences between 0.3 and 4.5 J/cm2 using the direct focusing technique in air. The influence of the laser pulse number and the peak fluence was investigated by means of several surface analytical techniques (optical microscopy, dynamic friction atomic force microscopy, scanning Auger electron microscopy and small-spot electron spectroscopy for chemical analysis). The correlation of the results about optical, physical and chemical properties of the irradiated areas allows us to propose a simple oxidation model, which explains different observed phenomena associated with surface damage such as mound formation and crater widening and clarifies the incubation behavior reported earlier for this material.
We present dynamic plowing nanolithography on polymethylmethacrylate films, performed with a scan-linearized atomic force microscope able to scan up to 250 μm with high resolution. Modifications of the surface are obtained by plastically indenting the film surface with a vibrating tip. By changing the oscillation amplitude of the cantilever, i.e., the indentation depth, surfaces can be either imaged or modified. A program devoted to the control of the scanning process is also presented. The software basically converts the gray scale of pixel images into voltages used to control the dither piezo driving cantilever oscillations. The advantages of our experimental setup and the dependence of lithography efficiency on scanning parameters are discussed. Some insights into the process of surface modifications are presented.
A broadband dielectric study of the dispersions of silica spheres (Aerosil 380) in octylcyanobiphenyl (8CB) with densities between 0.083 and 10 g of silica per 1 cm3 of liquid crystal (LC) is reported. High values of silica densities were achieved for the first time to observe the behaviour of the LC monolayer on the surface of the silica particles. The relaxation characteristic of the bulk LC is noticed especially for the samples with low silica densities. Additionally, a slow relaxation was detected, even at temperatures for which the bulk LC is in the crystalline state. It was assigned to the surface layer of LC molecules. Remarkably, the temperature dependence of the relaxation rates for this slow process shows a behaviour typical for glass-forming liquids.
The physical properties as well as the thickness of the interphase between polymer and reinforcing phase are generally expected to show a strong influence on the macroscopic mechanical properties of composite materials. In this study the scanning force microscope (SFM) has been applied for detecting stiffness gradients near the interface between copper and epoxide. In displacement modulation mode the load exerted by the tip is modulated sinusoidally by vibrating the normal position of the cantilever or the sample. The corresponding amplitude of dynamic cantilever bending is related to local surface stiffness. Thus, using the SFM, the local mechanical properties of the surface under investigation can be probed. When scanning the tip across the reinforcement/polymer interface, the polymeric interphasial zone can be identified with the observed stiffness gradient. For a commercial epoxide based on diglycidyl ether of bisphenol A (DGEBA) cured with an amine-containing hardener, a stiffness gradient was detected that could be fitted by a Gaussian profile typical for diffusional processes. The width of the stiffness gradient was 280 nm. The observation is discussed in terms of interface-induced segregation processes between resin and hardener, as well as heat conduction mechanisms that can occur during the exothermic curing reaction. Both mechanisms are diffusional in nature and, via the local network structure, are expected to show some influence on the local stiffness of the cured epoxy. Copyright © 2000 John Wiley & Sons, Ltd.
Scanning force microscopy (SFM) has been used to assess the local mechanical properties of fibre-reinforced polymers. Using a sinusoidal displacement modulation (DM) and lock-in technique the method allows to characterize local viscoelastic properties with a high lateral resolution. The simultaneous measurement of the local electrical conductivity is proposed which facilitates the interpretation of the mechanical data. The investigation of cross-sections perpendicular to the axis of carbon fibres embedded in PPS delivers some information about the change in local stiffness within the interfacial region. As a first approach, assuming a single-exponential decrease in local stiffness along a radial line from fibre to polymer we find characteristic decay lengths which are distributed in a range between 20 and 80nm. Further, a modified DM-mode is proposed which is expected to provide a contrast enhancement of the signal which is related to local stiffness. This can be achieved by installing an additional feedback loop which keeps constant the amplitude of dynamic indentation (CDI-mode).
Antimony clusters of different shapes and dimensions have been obtained by evaporating antimony on graphite. The dependence of the shape and dimensions of the particles on the evaporation parameters (effective layer thickness, temperature, pressure) is discussed. A characterisation of the different structures is presented. In particular, the decoration of graphite steps is discussed. Clusters have been dislocated by means of dynamic plowing nanolithography, both in vector and in image pattern mode. The dependence of the energy needed to dislocate a cluster on its dimensions and position is discussed.