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Paper des Monats
- ja (15)
The aim of this study is to develop nanometer-thin epoxy-based films on aluminium alloy AA2024-T3 as a model coating system for high resolution corrosion studies. Spin coating was used for the layer-by-layer (LbL) deposition of poly-(ethylenimine) (PEI) and poly([o-cresyl glycidyl ether]-co-formaldehyde) (CNER) bilayers. The film chemistry and the cross-linking process were characterized by means of Fourier-transform infrared spectroscopy (FTIR).
Ellipsometric data confirmed the linear increase of film thickness. The potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) results indicate the improvement of the film barrier properties with increasing film thickness. Mapping of the topography and the volta potential was performed by means of scanning Kelvin probe force microscopy (SKPFM).
The results indicate the presence of a homogeneous film structure, while the intermetallic phases can still be identified below the coating. The SKPFM Analysis confirmed that the model films are suitable for investigation of corrosion processes at the coating/metal interface.
The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. Complementation and/or filling gaps of published and ongoing standardisation projects on size, shape and number concentration measurements under ISO/TC 229/JWG 2 are offered.
This paper reports a systematic study into the effect of different biomass-derived precursors on the structure and porosity of carbons prepared via catalytic graphitization. Glucose, starch and cellulose are combined with iron nitrate and heated under a nitrogen atmosphere to produce Fe3C nanoparticles, which catalyze the conversion of amorphous carbon to graphitic nanostructures. The choice of organic precursor provides a means of controlling the catalyst particle size, which has a direct effect on the porosity of the material. Cellulose and glucose produce mesoporous carbons, while starch produces a mixture of micro- and mesopores under the same conditions and proceeds via a much slower graphitization step, generating a mixture of graphitic nanostructures and turbostratic carbon. Porous carbons are critical to energy applications such as batteries and electrocatalytic processes. For These applications, a simple and sustainable route to those carbons is essential. Therefore, the ability to control the precise structure of a biomass-derived carbon simply through the choice of precursor will enable the production of a new generation of energy materials.
The intention of the presentation is to inspire a discussion on the needs and challenges for the digitalisation of SOPs. SOPs are available for the disciplines of physical-chemical characterisation, for toxicology, for environmental applications and for exposure applications. Furthermore the SOPs need to be integrated in the regulatory framework and need to be detailed enough for the digital processing. This is highlighted in this presentation.
A detailed calorimetric and dielectric study on two epoxy-based nanocomposite system was performed employing bisphenol A diglycidyl ether (DGEBA) cured with diethylenetriamine (DETA) and methyl tetrahydrophtalic acid anhydride (MTHPA) aas the polymer matrix and taurine-modified MgAL layered double hydroxide (T-LDH) and boehmite as nanofiller. The molecular dynamics investigation revealed an intrinsic structural heterogeneity of the epoxy materials. Moreover the polymer/particle interphase was qualitatively and quantitavely investigated.
Der Vortrag beleuchtet insbesondere die Herausforderungen die sich bei der Dispergierung der Nanopulver aufgrund der hohen Adhäsivkräfte ergeben. Die Bewertung der Probenpräparation ist nur indirekt zugänglich, aber essentiell für die Zuverlässigkeit der Messergebnisse. Anhand von Beispielen werden Lösungsvorschläge aufgezeigt. Der Vortrag schließt mit einem Vorschlag zur Strategie der Herangehensweise bei der Partikelgrößenbestimmung von Nanopulvern.
Standardisation of concentration measurements of extracellular vesicles for medical diagnoses
(2020)
Extracellular vesicles (EVs) are cell-derived particles in body fluids, which have excellent potential as next generation biomarkers for the early diagnosis of common diseases, such as cancer and thrombosis. This project aims to tap into the clinical potential of EVs by developing traceable measurements of number concentration, size distribution, refractive index (RI) and fluorescence intensity of cell-specific EVs in human blood and urine.
To realise our aims, we will develop synthetic reference materials with physical properties resembling EVs (WP1), instrumentation and procedures to standardise EV measurements in clinical laboratories (WP2), and ready-to-use biological test samples (WP3). These will then be evaluated in an inter-laboratory comparison study across a range (>20) of standard flow cytometers in clinical labs (WP4).
A brief introduction to fluorescence spectroscopy will be provided, ranging from typically measured fluorescence quantities over instrument-specific contributions to measured fluorescence signals to selected applications. In this context, an overview of the photoluminescence properties of molecular and nanoscale luminescence reporters will be given including a brief insight into their photophysics and fluorescence standards designed by division Biophotonics for the calibration and instrument performance validation of fluorescence measuring devices will be presented.
A brief introduction to fluorescence spectroscopy will be provided, ranging from typically measured fluorescence quantities over instrument-specific contributions to measured fluorescence signals to selected applications. In this context, an overview of the photoluminescence properties of molecular and nanoscale luminescence reporters will be given including a brief insight into their photophysics and fluorescence standards designed by division Biophotonics for the calibration and instrument performance validation of fluorescence measuring devices will be presented.
The basics of absorption spectroscopy (termed also photometry) will be presented with focus on transparent solutions of different molecular and nanocrystalline absorbers and the ultraviolet (UV), visible (vis), and near-infrared (NIR) spectral region. Thereby, also typical sources of uncertainty will be addressed. Subsequently, several examples for typical applications of absorption measurements in the life and material sciences will be briefly shown ranging from aggregation studies and dye labeling densities of biomolecules (dye-to-biomolecule ratios) over optical assays for thiol and protein quantification to the optical determination of the size of semiconductor nanocrystals using size curves.
You Ask – ACEnano Replies
(2020)
The workshop starts with introductory information about the workshop and the H2020 project ACEnano, followed by two expert round tables, focussing on how the project could address regulator and industry needs, respectively. This is be followed by parallel sessions on tools (based on preferences expressed by those registered to attend, see “Questions”) and finally a question-and-answer session with the attendees.
The experts invited in Round Table 1 have been prepared to answer to questions related to obstacles and advantages for stakeholders such as SMEs to use the ACEnano approaches/tools. Standardisation needs are discussed.
Blueprint for a sustainable new European Centre to support safe innovation for nanotechnology
(2020)
This paper presents the blueprint for the operation of a sustainable and permanent European Centre of collaborating reference laboratories and research centres, to establish a one-stop shop for a wide variety of nanosafety related services, and to provide a central contact point for questions about nanosafety in Europe. The Centre aims to harmonise service provision, and bring novel risk assessment and management approaches closer to practice.
A series of different nanoparticle suspensions (Gold, Latex, and SiO2 in varying concentrations) were microprinted onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 NP/mL and imaged with SEM and TSEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee ring effect.
Data quality is a vast term, which comprises the completeness, relevance (adequacy), and reliability of data. So far, many attempts to assure data quality have been pursued, and evaluation criteria for data quality have been established. One relatively novel but already well-known aspect of data quality refers to the concept of data FAIRness, which states that data should be: findable, accessible, interoperable and re-usable. In order to find, use, and access data, a user has to be guided properly. Such guidelines already exist for regulators and the scientific community. However, a ‘simple’ non-academic user from general society is very unlikely to be able to access or understand such data. Our objective in the H2020 project NANORIGO is to help and guide all types of users (i.e., scientists, regulators, industry workers, citizens, etc.) to access and make use of high-quality data and information from available and suitable data repositories in order to increase the transparency of and trust in nanotechnology.
We demonstrate the potential of time-resolved luminescence spectroscopy for the straightforward assessment and in situ monitoring of the stability of upconversion nanocrystals (UCNPs). Therefore, we prepared hexagonal NaYF4:Yb3+,Er3+ UCNPs with various coatings with a focus on phosphonate ligands of different valency, using different ligand exchange procedures, and studied their dissolution behaviour in phosphate-buffered saline (PBS) dispersions at 20 °C and 37 °C with various analytical methods. The amount of the released UCNPs constituting fluoride ions was quantified by potentiometry using a Fluoride ion-sensitive electrode and particle disintegration was confirmed by transmission electron microscopy studies of the differently aged UCNPs. In parallel, the luminescence features of the UCNPs were measured with special emphasis on the lifetime of the sensitizer emission to demonstrate its suitability as Screening parameter for UCNP stability and changes in particle composition. The excellent correlation between the changes in luminescence lifetime and fluoride concentration highlights the potential of our luminescence lifetime method for UCNP stability screening and thereby indirect monitoring of the release of potentially hazardous fluoride ions during uptake and dissolution in biological systems. Additionally, the developed in situ optical method was used to distinguish the dissolution dynamics of differently sized and differently coated UCNPs.
As one of the widely used analytical methods for the analysis of elemental composition of solid matter, energy dispersive X-ray spectroscopy (EDS) has recently gained significant importance regarding its application to the chemical analysis of nanoparticles, especially in conjunction with the use of a scanning electron microscope (SEM) and the use of the transmission operation mode of SEM (STEM-in-SEM). This development was mainly driven by the technological progress with highly sensitive EDS detectors, such that individual nanoparticles can be quickly inspected with EDS at a SEM. Qualitative information on elemental composition with about 10 nm spatial resolution can be achieved complementary to the high-resolution information of the sample surface morphology within the same scanned area as provided by the electron microscope. Representative examples with successful EDS analysis on nanoparticles are presented, but also limitations of the method are described.
Photoluminescence techniques are amongst the most widely used tools in the life sciences, with new and exciting applications in medical diagnostics and molecular imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from instrument-dependent effects, which are also time-dependent due to aging of instrument-components, and difficulties to measure absolute fluorescence intensities. Moreover, scattering systems require special measurement geometries and the interest in new optical reporters with emission > 1000 nm strategies for reliable measurements in the second diagnostic for the comparison of material performance and the rational design of new fluorophores with improved properties.
Here, we present strategies to versatile method-adaptable liquid and solid fluorescence standards for different fluorescence parameters. Examples are multi-emitter glasses, spectral fluorescence standards, and quantum yield standards for the UV/vis/NIR.
One of the objectives of the EU Project EC4SafeNano (European Centre for Risk Management and Safe Innovation in Nanomaterials & Nanotechnologies) was to test and benchmark the services in order to check their relevance to address identified stakeholder needs, but also to evaluate the governance of the structure delivering the proposed services. The aim is to demonstrate the technical relevance of the services and the overall open structure organisation, including governance rules and operating procedures, by answering relevant identified questions (case studies) selected by a panel of stakeholders. Therefore, a significant part of the project will be devoted to this demonstration of the operational and functional basis of the organized network.
Polymer nanocomposites (PNCs) with inorganic nanofillers dispersed in a polymer matrix have been widely studied from the 1990s, since the pioneering work by Toyota Central Research. The possibility of producing advanced tailor-made, light weight and low-cost materials, inspired academic and commercial research towards numerous potential applications, facilitating PNCs to become a billion-dollar global industry. The introduction of nanoparticles (NPs) to a polymer matrix is expected to result in improved properties. The outstanding performance of PNCs is determined not only by the characteristics of the used components but also by their phase morphology, including the dispersion of NPs and interfacial properties. Understanding of structure-property relationships is particularly important for polymer nanocomposites with high industrial significance, such as epoxy-based materials reinforced with inorganic nanofillers. These PNCs have been successfully adopted by the marine, automotive and aerospace industries, although they are still rarely studied on a fundamental level. Therefore, this thesis aims for a detailed understanding of the structure, molecular mobility and vitrification kinetics first, of two epoxy-based materials with different network structures and second, of the corresponding nanocomposites with different alumina-based nanofillers. The first system considered (EP/T-LDH) was based on bisphenol A diglycidyl ether (DGEBA) cured with diethylenetriamine (DETA) and taurine-modified layered double hydroxide (T-LDH) NPs. The taurine molecule bears additional functionalities that could enhance the interactions between the matrix and the nanofiller, improving the interphase formation. The seconds system (EP/BNP) was based on DGEBA and methyl tetrahydrophtalic acid anhydride (MTHPA) as a hardener, reinforced with boehmite nanoparticles (BNPs). The comparison of the two systems enables for a comparative study on the effect of different hardeners and the morphology and modification of the alumina-based nanofillers on the material behavior. The materials were investigated employing complementary techniques with different sensitivities and frequency windows. The following methodology was used: transmission electron microscopy (TEM), small – and wide – angle X-ray scattering (SAXS/WAXS), broadband dielectric spectroscopy (BDS), calorimetry in a form of conventional DSC and fast scanning calorimetry (FSC), as well as specific heat spectroscopy (SHS) in a form of temperature modulated DSC, temperature modulated FSC and static FSC by calculating the thermal relaxation rates from the cooperativity approach. The FSC method (based on adiabatic chip calorimetry to probe micrometer-sized samples) was successfully employed in this work, exploiting all its possibilities for the first time in literature for a PNC. Moreover, a systematic analysis technique was established to overcome the problem of vague glass transition regions observed for highly loaded PNCs in the heat flow and heat capacity curves.
First, TEM, SAXS/WAXS and indirectly BDS and SHS were employed to obtain the information about the approximate morphology of the PNCs. It was found that epoxy-based materials exhibit a structural heterogeneity in a form of regions with different average crosslinking density. This was indicated by multiple-peak scattering pattern of the polymer matrix and two distinct α-processes (dynamic glass transition) related to the cooperative fluctuation of the epoxy network found by BDS and SHS. This was described for the first time for epoxy-based materials. The two α-relaxations were evidenced differently for the two systems, which is related to different network structures and dipole moments due to the employed hardeners. Nevertheless, structural heterogeneity is an intrinsic feature of these materials, independent of the type of hardener used for the network formation and nanofiller. In addition, matrix inhomogeneities were more pronounced with increasing nanoparticle content. Furthermore, a powerful new technique was applied for X-ray scattering data, using Monte Carlo fits, to describe the NPs dispersion throughout the whole sample volume (as opposed to the local investigations performed by most researches). Additional structural information of the two systems was extracted by BDS and SHS, such as qualitative and quantitative estimation of polymer segments physically adsorbed and/or chemically bonded onto the nanoparticles. Due to the immobilized character of this interphase with respect to the cooperative segmental motions, it is denoted as a rigid amorphous fraction (RAF). For instance, on the contrary to EP/BNP, for EP/T-LDH a dielectrically active process was found, related to the localized fluctuations within RAF. Moreover, the amount of RAF in EP/T-LDH was reaching up to 40 wt % of the system, whereas in EP/BNP it ranged between 1-7 wt %. In the latter case the presence of NPs was found to simultaneously increase and decrease the number of mobile segments, due to the interphase formation and changes in crosslinking density. The difference between the two systems was ascribed to the presence of additional amine functionalities in the T-LDH nanofiller.
Second, employing BDS and SHS, a systematic study on the effect of NPs on the segmental dynamics was performed. For example, depending on the nanofiller, the α-processes related to regions with higher crosslinking density was found to shift to higher and lower temperatures with increasing T-LDH and BNPs concentration, respectively. The observed difference is due to the different synergism of the polymer matrix with the nanofiller.
Third, a detailed investigation of the vitrification kinetics was performed with DSC and FSC. The concentration dependence of the glass transition temperature was found, similar to the behavior of the α-processes. It was shown that, in parallel to the detected main glass transition, epoxy-based materials can exhibit an additional low temperature vitrification mechanism. As expected from the two distinct α-processes, this behavior was however not discussed in prior studies for an unfilled network former. This finding was correlated to the structural heterogeneity evidenced by other techniques.
This thesis, dealing with an in-depth research on the epoxy-based materials that are already successfully employed in numerous applications underlines the necessity of more fundamental research in this field. It shines light on the complexity of these systems and contributes to defining how the structure-property relationships can be determined by combining multiple experimental techniques and analytical methodology.
Low cost, high-efficiency catalysts towards water splitting are urgently required to fulfil the increasing demand for energy. In this work, low-loading (<20 wt%) Ni-confined in layered metal oxide anode catalysts (birnessite and lepidocrocite titanate) have been synthesized by facile ion exchange methodology and subjected to systematic electrochemical studies. It was found that Ni-intercalated on K-rich birnessite (Ni-KMO) presents an onset overpotential (ηonset) as low as 100 mV and overpotential at 10 mA cm−2 (η10) of 206 mV in pH = 14 electrolyte. By combining electrochemical methods and X-ray absorption and emission spectroscopies (XAS and XES), we demonstrate Ni sites are the active sites for OER catalysis and that the Mn3+ sites facilitate Ni intercalation during the ion-exchange process, but display no observable contribution towards OER activity. The effect of the pH and the nature of the supporting electrolyte on the electrochemical performance was also evaluated.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
Aluminum (Al) can be taken up from food, packaging, or the environment and thus reaches the human gastrointestinal tract. Its toxic potential after oral uptake is still discussed. The fate of different solid and ionic Al species during the passage through the digestive tract is the focus of this research, as well as the cellular effects caused by these different Al species. The present study combines the physicochemical processing of three recently studied Al species (metallic Al0, mineral Al2O3, and soluble AlCl3) in artificial digestion fluids with in vitro cell systems for the human intestinal barrier. Inductively coupled plasma mass spectrometry (ICP-MS) and small-angle X-ray scattering (SAXS) methods were used to characterize the Al species in the artificial digestion fluids and in cell culture medium for proliferating and differentiated intestinal Caco-2 cells. Cytotoxicity testing and cellular impedance measurements were applied to address the effects of digested Al species on cell viability and cell proliferation. Microarray-based transcriptome analyses and quantitative real-time PCR were conducted to obtain a deeper insight into cellular mechanisms of action and generated indications for cellular oxidative stress and an influence on xenobiotic metabolism, connected with alterations in associated signaling pathways. These cellular responses, which were predominantly caused by formerly ionic Al species and only at very high concentrations, were not impacted by artificial digestion. A two-directional conversion of Al between ionic species and solid particles occurred throughout all segments of the gastrointestinal tract, as evidenced by the presence of nanoscaled particles. Nevertheless, this presence did not increase the toxicity of the respective Al species.
We synthesized a generation of water-soluble, atomically precise gold nanoclusters (Au NCs) with anisotropic Surface containing a short dithiol pegylated chain (AuMHA/TDT). The AuMHA/TDT exhibit a high brightness (QY ∼ 6%) in the shortwave infrared (SWIR) spectrum with a detection above 1250 nm.
Furthermore, they show an extended half-life in blood (t1/2ß = 19.54 ± 0.05 h) and a very weak accumulation in organs. We also developed a non-invasive, whole-body vascular imaging system in the SWIR window with high-resolution, benefiting from a series of Monte Carlo image processing. The imaging process enabled to improve contrast by 1 order of magnitude and enhance the spatial Resolution by 59%. After systemic administration of these nanoprobes in mice, we can quantify vessel complexity in depth (>4 mm), allowing to detect very subtle vascular disorders non-invasively in bone morphogenetic protein 9 (Bmp9)-deficient mice. The combination of these anisotropic surface charged Au NCs plus an improved SWIR imaging device allows a precise mapping at high-resolution and an in depth understanding of the organization of the vascular network in live animals.
Water-Soluble Aza-BODIPYs: Biocompatible Organic Dyes for High Contrast In Vivo NIR-II Imaging
(2020)
A simple NIR-II emitting water-soluble system has been developed and
applied in vitro and in vivo. In vitro, the fluorophore quickly accumulated in 2D and 3D cell cultures and rapidly reached the tumor in rodents, showing high NIR-II contrast for up to 1 week. This very efficient probe possesses all the qualities necessary for translation to the clinic as well as for the development of NIR-II emitting materials.
facile hydrothermal method to synthesize water-soluble copper indium sulfide (CIS) nanocrystals (NCs) at 150 degrees C is presented. The obtained samples exhibited three distinct photoluminescence peaks in the red, green and blue spectral regions, corresponding to three size fractions, which could be separated by means of size-selective precipitation. While the red and green emitting fractions consist of 4.5 and 2.5 nm CIS NCs, the blue fraction was identified as in situ formed carbon nanodots showing excitation wavelength dependent emission. When used as light absorbers in quantum dot sensitized solar cells, the individual green and red fractions yielded power conversion efficiencies of 2.9% and 2.6%, respectively. With the unfractionated samples, the efficiency values approaching 5% were obtained. This improvement was mainly due to a significantly enhanced photocurrent arising from complementary panchromatic absorption.
Current analyses show a widespread occurrence of microplastic particles in food products and raise the question of potential risks to human health. Plastic particles are widely considered to be inert due to their low chemical reactivity and therefore supposed to pose, if at all only minor hazards. However, variable physicochemical conditions during the passage of the gastrointestinal tract gain strong importance, as they may affect particle characteristics. This study aims to analyze the impact of the gastrointestinal passage on the physicochemical particle characteristics of the five most produced and thus environmentally relevant plastic materials polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate and polystyrene. Scanning electron microscopy (SEM) and subsequent image analysis were employed to characterize microplastic particles. Our results demonstrate a high resistance of all plastic particles to the artificial digestive juices. The present results underline that the main stages of the human gastrointestinal tract do not decompose the particles. This allows a direct correlation between the physicochemical particle characteristics before and after digestion. Special attention must be paid to the adsorption of organic compounds like proteins, mucins and lipids on plastic particles since it could lead to misinterpretations of particle sizes and shapes.
Amphiphilic polymer nanogels (NGs) are promising drug delivery vehicles that extend the application of conventional hydrophilic NGs to hydrophobic cargoes. By randomly introducing hydrophobic groups into a hydrophilic polymer network, loading and release profiles as well as surface characteristics of these colloids can be tuned. However, very little is known about the underlying internal structure of such complex colloidal architectures. Of special interest is the question how the amphiphilic network composition influences the internal morphology and the “fuzzy” surface structure. To shine light into the influence of varying network amphiphilicity on these structural features, we investigated a small library of water-swollen amphiphilic NGs using small-angle X-ray scattering (SAXS). It was found that overall hydrophilic NGs, consisting of pure poly(N-(2-hydroxypropyl)methacrylamide) (PHPMA), display a disordered internal structure as indicated by the absence of a SAXS peak. In contrast, a SAXS peak is present for amphiphilic NGs with various amounts of incorporated hydrophobic groups such as cholesteryl (CHOLA) or dodecyl (DODA). The internal composition of the NGs is considered structurally homologous to microgels. Application of the Teubner–Strey model reveals that hydrophilic PHPMA NGs have a disordered internal structure (positive amphiphilicity factor) while CHOLA and DODA samples have an ordered internal structure (negative amphiphilicity factor). From the SAXS data it can be derived that the internal structure of the amphiphilic NGs consists of regularly alternating hydrophilic and hydrophobic domains with repeat distances of 3.45–5.83 nm.
Iron oxides used as food colorants are listed in the European Union with the number E172. However, there are no specifications concerning the fraction of nanoparticles in these pigments.
Here, seven E172 products were thoroughly characterized. Samples of all colors were analyzed with a Broad spectrum of methods to assess their physico-chemical properties. Small-Angle X-ray Scattering (SAXS), Dynamic Light Scattering (DLS), Transmission Electron Microscopy (TEM), zeta-potential, Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), X-ray diffraction (XRD), Brunauer-Emmett-Teller analysis (BET), Asymmetric Flow Field-Flow Fractionation (AF4) and in vitro cell viability measurements were used.
Nanoparticles were detected in all E172 samples by TEM or SAXS measurements. Quantitative results from both methods were comparable. Five pigments were evaluated by TEM, of which four had a size median below 100 nm, while SAXS showed a size median below 100 nm for six evaluated pigments. Therefore, consumers May be exposed to iron oxide nanoparticles through the consumption of food pigments.
The hexapeptide hIAPP22–27 (NFGAIL) is known as a crucial amyloid core sequence of the human islet amyloid polypeptide (hIAPP) whose aggregates can be used to better understand the wild‐type hIAPP′s toxicity to β‐cell death. In amyloid research, the role of hydrophobic and aromatic‐aromatic interactions as potential driving forces during the aggregation process is controversially discussed not only in case of NFGAIL, but also for amyloidogenic peptides in general. We have used halogenation of the aromatic residue as a strategy to modulate hydrophobic and aromatic‐aromatic interactions and prepared a library of NFGAIL variants containing fluorinated and iodinated phenylalanine analogues. We used thioflavin T staining, transmission electron microscopy (TEM) and small‐angle X‐ray scattering (SAXS) to study the impact of side‐chain halogenation on NFGAIL amyloid formation kinetics. Our data revealed a synergy between aggregation behavior and hydrophobicity of the phenylalanine residue. This study introduces systematic fluorination as a toolbox to further investigate the nature of the amyloid self‐assembly process.
By adding hyaluronic acid (HA) to dioctyl sodium sulfosuccinate (AOT)‐stabilized gold nanotriangles (AuNTs) with an average thickness of 7.5±1 nm and an edge length of about 175±17 nm, the AOT bilayer is replaced by a polymeric HA‐layer leading to biocompatible nanoplatelets. The subsequent reduction process of tetrachloroauric acid in the HA‐shell surrounding the AuNTs leads to the formation of spherical gold nanoparticles on the platelet surface. With increasing tetrachloroauric acid concentration, the decoration with gold nanoparticles can be tuned. SAXS measurements reveal an increase of the platelet thickness up to around 14.5 nm, twice the initial value of bare AuNTs. HRTEM micrographs show welding phenomena between densely packed particles on the platelet surface, leading to a crumble formation while preserving the original crystal structure. Crumbles crystallized on top of the platelets enhance the Raman signal by a factor of around 20, and intensify the plasmon‐driven dimerization of 4‐nitrothiophenol (4‐NTP) to 4,4′‐dimercaptoazobenzene in a yield of up to 50 %. The resulting crumbled nanotriangles, with a biopolymer shell and the absorption maximum in the second window for in vivo imaging, are promising candidates for biomedical sensing.
This paper reports the formation of zinc phosphate nanoparticles from the artificial digestion of zinc chloride. Initially, the formation of amorphous primary particles with a mean radius of 1.1 nm is observed, alongside the formation of larger, protein stabilized aggregates. These aggregates, with a radius of gyration of 37 nm, are observed after 5 minutes of exposure to artificial saliva and are shown to be colloidally stable for a minimum time of two weeks. The initially formed primary particles are thought to consist of amorphous zinc phosphate, which is then transformed into crystalline Zn3(PO4)2·4H2O over the course of two weeks. Our results demonstrate that the interaction of inorganic salts with bodily fluids can induce the formation of de novo nanoparticles, which in turn, provides insights into how zinc‐enriched foods may also facilitate the formation of nanoparticles upon contact with saliva. As such, this may be considered as an undesirable (bio)mineralization.
This poster presents the focused ion beam preparation methodologies developed within the framework of the EU funded EURAMET project ADVENT (Advanced Energy-Saving Technology).
It summarises the key breakthroughs achieved for various in situ investigation techniques, e.g. in situ experiments at the Synchrotron facility BESSY II (IR-SNOM and XRS), TEM and SMM instrumentation.
The created experimental devices from diverse thin-film semiconductor materials paved the way to dynamic structural studies bearing the potential to determine nanoscale correlations between strain and electric fields and, moreover, for the fundamental development of new in situ capabilities.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
Es wurde im Rahmen dieser Arbeit eine neue Methode der Biokonjugation entwickelt, die es ermöglicht humane Antikörper ortspezifisch mit IgG-bindenden Peptiden zu konjugieren. Als Basis fungierte ein Peptid, welches für den Einsatz gezielt modifiziert wurde. So sollte am C-Terminus ein Biotin eingefügt werden, dass für die spätere Detektion der Biokonjugation genutzt werden kann, während am N-Terminus ein Cross-Linker für die kovalente Bindung zum Antikörper eingefügt wurde. Das Biotin wurde mittels Biotin-Lysin eingebaut. Dies hat den Vorteil, dass die modifizierte Aminosäure direkt in der SPPS genutzt werden kann. Auch der Cross-Linker soll schon während der SPPS in das Peptid integriert werden. Als Cross Linker wurden die zwei heterobifunktionellen Succinimidyl(3-bromoacetamid)propionate und Succinimidyl(4-iodacetyl)aminobenzoat untersucht. Die Aktivierung des Peptides mit dem SBAP-Cross-Linker erfolgte am besten im pH-Bereich zwischen 7,0 und 9,0. Die Modifizierung des Peptides mit dem Iodid-Cross-Linker SIAB unter den gleichen Bedingungen zeigte allerdings keine zufriedenstellenden Ergebnisse. Da das erste Peptid allerdings in den Folgeexperimenten sehr gute Ergebnisse zeigte, musste kein weiterer Linker getestet werden. Zusätzlich zu der Cross-Linker-Wahl sollte der Abstand zwischen dem Cross-Linker und dem Grundgerüst des Peptides auf den Einfluss der Bindung untersucht werden. Dazu wurden drei Kontrollpeptide synthetisiert, die entweder um zwei Aminosäuren zwischen dem ursprünglichen N-Terminus des Peptides und dem SBAP-Linker verlängert wurden, keinen SBAP-Linker beinhalten oder die Verlängerung ohne SBAP-Linker besaßen. Die erfolgreiche Synthese aller vier Peptide wurde mittels MALDI-TOF-MS bestätigt.
The employment of type-I pyrethroids for airplane disinfection in recent years underlines the necessity to develop sensing schemes for the rapid detection of these pesticides directly at the point-of-use. Antibody-gated indicator-releasing materials were thus developed and implemented with test strips for lateral-flow assay-based analysis employing a smartphone for readout. Besides a proper matching of pore sizes and gating macromolecules, the functionalization of both the material's outer surface as well as the strips with PEG chains enhanced system performance. This simple assay allowed for the detection of permethrin as a target molecule at concentrations down to the lower ppb level in less than 5 minutes.
Thermoset materials characterization is often limited to solid state analytical techniques such as IR, NMR, DSC, TGA and mechanical testing. Alternatively, their off-gassing behavior can also be evaluated using GC based techniques such as TD-GC-MS, allowing this method to be applied to thermoset materials analyses such as identification, aging characterization, and formulation optimization. As an overview, common thermoset materials were evaluated by analyzing their gaseous degradation products via TGA-based pyrolysis and subsequent TD-GC-MS for the identification of representative volatile signatures. It is thereby possible to distinguish different classes of phenolic materials or cured epoxy resins, as well as their amine or anhydride curatives. Additionally, this method enabled quantification of a volatile fragment (bisphenol A, BPA) which is associated with oxidation of epoxy/amine thermoset materials. The amount of evolved BPA increased linearly with aging time and this trend exhibits linear Arrhenius behavior over the temperature range (80–125 °C) studied, in agreement with oxidation sensitivies based on oxygen consumption data. Further, TD-GC-MS was used to explore how off-gassing of residual anhydride curative from an epoxy/anhydride material depends on formulation stoichiometry. Even in formulations that theoretically contained enough epoxy to consume all anhydride (1:1 stoichiometry), an imperfect final cure state resulted in residual anhydride which could evolve from the material. For such materials, a slightly epoxy-rich formulation is required to ensure that the material contains no residual unreacted anhydride. Analysis of volatiles generated by thermal exposure is an attractive characterization approach enabling compositional analysis as well as complementary diagnostics for materials degradation.
Efficient water electrolysis requires highly active electrodes. The activity of corresponding catalytic coatings strongly depends on material properties such as film thickness, crystallinity, electrical conductivity, and chemical surface speciation. Measuring these properties with high accuracy in vacuum-free and nondestructive methods facilitates the elucidation of structure−activity relationships in realistic environments. Here, we report a novel approach to analyze the optical and electrical properties of highly active oxygen evolution reaction (OER) catalysts via spectroscopic ellipsometry (SE). Using a series of differently calcined, mesoporous, templated iridium oxide films as an example, we assess the film thickness, porosity, electrical resistivity, electron concentration, electron mobility, and interband and intraband transition energies by modeling of the optical spectra. Independently performed analyses using scanning electron microscopy, energy-dispersive X-ray spectroscopy, ellipsometric porosimetry, X-ray reflectometry, and absorption spectroscopy indicate a high accuracy of the deduced material properties. A comparison of the derived analytical data from SE, resonant photoemission spectroscopy, X-ray absorption spectroscopy, and X-ray photoelectron spectroscopy with activity measurements of the OER suggests that the intrinsic activity of iridium oxides scales with a shift of the Ir 5d t2g sub-level and an increase of p−d interband transition energies caused by a transition of μ1-OH to μ3-O species.
Comprehensive Characterization of APTES Surface Modifications of Hydrous Boehmite Nanoparticles
(2020)
Hydrous boehmite (γ-AlOOH) nanoparticles (BNP) show great potential as nanoscale filler for the fabrication of fiber reinforced nanocomposite materials. Notably, the particle−matrix interaction has been demonstrated to be decisive for improving the matrix-dominant mechanical properties in the past years. Tailoring the surface properties of the nanofiller enables to selectively design the interaction and thus to exploit the benefits of the nanocomposite in an optimal way. Here, an extensive study is presented on the binding of (3-aminopropyl)triethoxysilane (APTES), a common silane surface modifier, on BNP in correlation to different process parameters (concentration, time, temperature, and pH). Furthermore, a comprehensive characterization of the modified BNP was performed by using elemental analysis (EA), thermogravimetric analysis (TGA) coupled with mass spectrometry (TGA-MS), and Kaiser’s test (KT). The results show an increasing monolayer formation up to a complete surface coverage with rising APTES concentration, time, and temperature, resulting in a maximal grafting density of 1.3 molecules/nm². Unspecific multilayer formation was solely observed under acidic conditions. Comparison of TGA-MS results with data recorded from EA, TGA, and KT verified that TGA-MS is a convenient and highly suitable method to elucidate the ligand binding in detail.
Phage display biopanning with Illumina next-generation sequencing (NGS) is applied to reveal insights into peptide-based adhesion domains for polypropylene (PP). One biopanning round followed by NGS selects robust PP-binding peptides that are not evident by Sanger sequencing. NGS provides a significant statistical base that enables motif analysis, statistics on positional residue depletion/enrichment, and data analysis to suppress false-positive sequences from amplification bias. The selected sequences are employed as water-based primers for PP-metal adhesion to condition PP surfaces and increase adhesive strength by 100% relative to nonprimed PP.
The oxides, hydroxides, and oxo-hydroxides of iron belong to the most abundant materials on earth. They also feature a wide range of practical applications. In many environments, they can undergo facile phase transformations and crystallization processes.
Water appears to play a critical role in many of these processes. Despite numerous attempts, the role of water has not been fully revealed yet. We present a new approach to study the influence of water in the crystallization and phase transformations of iron oxides.
The approach employs model-type iron oxide films that comprise a defined homogeneous nanostructure. The films are exposed to air containing different amounts of water reaching up to pressures of 10 bar. Ex situ analysis via scanning electron microscopy, Transmission electron microscopy, selected area electron diffraction, and X-ray diffraction is combined with operando near-ambient pressure X-ray photoelectron spectroscopy to follow water-induced changes in hematite nd ferrihydrite. Water proves to be critical for the nucleation of ematite domains in ferrihydrite, the resulting crystallite orientation, and the underlying crystallization mechanism.
The European legislation has responded to the wide use of nanomaterials in our daily life and defined the term “nanoform” in the Annexes to the REACH (Registration, Evaluation, Authorization of Chemicals) Regulation. Now specific information of the nanomaterials is required from the companies when registering the appropriate materials in a dossier.
In the context of REACH eleven physicochemical properties were considered as relevant, of which the following six are essential for registration of nanoforms (priority properties): chemical composition, crystallinity, particle size, particle shape, chemical nature of the surface (“surface chemistry”), and specific surface area (SSA). A key role is the reliable, reproduceable and traceable character of the data of these priority properties.
In this context, we want to discuss which ‘analytical’ information is exactly required to fulfill these conditions. Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) were chosen as the most popular surface analytical methods. Both methods allow a detailed understanding of the surface chemistry with an information depth below ten nanometers. As a rather bulk method for the analysis of nanoforms, Electron Probe Microanalysis (EPMA) in the version with energy dispersive X-ray spectroscopy (EDS) is considered for the quick identification of the main chemical elements present in the sample. Furthermore, Scanning Electron Microscopy (SEM) results are discussed which provide results on particle size and shape. Thus, four of the six priority properties can be obtained with these methods.
Nanoparticles have gained increasing attention in recent years due to their potential and application in different fields including medicine, cosmetics, chemistry, and their potential to enable advanced materials. To effectively understand and regulate the physico-chemical properties and potential adverse effects of nanoparticles, validated measurement procedures for the various properties of nanoparticles need to be developed. While procedures for measuring nanoparticle size and size Distribution are already established, standardized methods for analysis of their surface chemistry are not yet in place, although the influence of the surface chemistry on nanoparticle properties is undisputed. In particular, storage and preparation of nanoparticles for surface analysis strongly influences the analytical results from various methods, and in order to obtain consistent results, sample preparation must be both optimized and standardized. In this contribution, we present, in detail, some standard procedures for preparing nanoparticles for surface analytics. In principle, nanoparticles can be deposited on a suitable substrate from suspension or as a powder. Silicon (Si) Wafers are commonly used as substrate, however, their cleaning is critical to the process. For sample preparation from suspension, we will discuss drop-casting and spin-coating, where not only the cleanliness of the substrate and purity of the suspension but also its concentration play important roles for the success of the preparation methodology.
For nanoparticles with sensitive ligand shells or coatings, deposition as powders is more suitable, although this method requires particular care in fixing the sample.
Methods and materials are presented here, which enable the manufacturing of fine structures using a 3D-printing method known as two-photon polymerization (2PP). As traditional photolithography methods for structuring ceramic slurries do not function with 2PP, due to light scattering on ceramic particles, a novel water-based photoresist with high ceramic loading of extremely well dispersed ceramic nano particles was developed. This photoresist is basically a ceramic slurry containing a photocurable agent and a photoinitiator to be crosslinkable with the 780 nm wavelength femtosecond laser light source of the 2PP machine. It is demonstrated that it is possible to gain a highly transparent and low viscous slurry suitable for 2PP processing. This work shows the development of the slurry, first printing results and the post-printing processes required to form three dimensional ceramic microstructures consisting of alumina toughened zirconia (ATZ).
To simulate the movement of the macroscopic magnetic moment in ferromagnetic systems under the influence of elevated temperatures, the stochastic version of the Landau-Lifshitz (LL) or the Landau-Lifshitz-Gilbert equation with a spin density of one per unit cell has to be used.
To apply the stochastic LL to micromagnetic simulations, where the spin density per unit cell is generally higher, a conversion has to be performed. OOMMF sample files MIF) are provided which can be used to determine the Curie temperature for the classical bulk magnets, iron, nickel and cobalt.
These files contain cell models for TOPAS/Geant4 and the inclusion of nano particles in particle scattering simulations. A simple spherical cell with nanoparticles can be generated in a fast manner. The user has the option to include the following organelles: nucleus, mitochondria, cell membrane. Additionally nanoparticles can be included in the cytosol and at the surface of the nucleus and/or the mitochondria.
The C++ classes in this repository extend the functionality of the TOPAS (http://www.topasmc.org/) Monte-Carlo program, which is itself a wrapper of the Geant4 MCS Toolkit (http://geant4.org). The sourcecode together with examples and scorers are provided.
"If you use this extension please cite the following literature:
Hahn, M.B., Zutta Villate, J.M. "Combined cell and nanoparticle models for TOPAS to study radiation dose enhancement in cell organelles." Sci Rep 11, 6721 (2021).
https://doi.org/10.1038/s41598-021-85964-2 "
The image designed by Natalia Cano Murillo and colleagues shows the cross section of a ternary composite (boehmite/polycarbonate/epoxy, 80μm x 80μm). The surface was measured by AFM kelvin probe microscopy, yielding the surface potential which is shown as 3D‐surface and contour lines. The sample was further subjected to AFM force spectroscopy with a lateral resolution of 1μm², yielding the local Young's modulus, projected in false colors on the 3D surface. The ternary system, containing boehmite nanoparticles, shows a broad distribution of modulus, desirable for optimized macroscopic mechanical properties, such as high stiffness as well as toughness.
Biofouling is a major challenge in the application of textiles, biosensors, and biomedical implants. In the current work, a straightforward method for the solvent-free polymerization of antifouling dendritic polyglycerol (dPG) from mussel-inspired dendritic polyglycerol (MI-dPG) coatings on hydrophilic titanium dioxide (TiO2) and hydrophobic polydimethylsiloxane (PDMS) is reported. Surface characterization is performed by static water contact angle (CA) measurements, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Significant lower CA values are obtained after dPG grafting from MI-dPG-coated TiO2 and MI-dPG coated PDMS. Furthermore, XPS shows a time-dependent increase of the CO bond content upon dPG grafting from MI-dPG-coated TiO2 and MI-dPG-coated PDMS. Analysis of the surface morphology by SEM shows a clear time-dependent increase in the surface roughness upon dPG grafting from MI-dPG-coated TiO2 and MIdPG-coated PDMS. When the viability of two adhesive cell types is studied via LIVE/DEAD staining, a strong reduction in the cell density is observed after the dPG grafting from MI-dPG-coated TiO2 and MI-dPG-coated PDMS (a decrease of >95% in all cases). The combined results show that biocompatible but highly cell-repelling surfaces are efficiently constructed via the grafting of dPG from MI-dPG-coated TiO2 and MI-dPG-coated PDMS.
Antibody-gated indicator delivery (gAID) systems based on mesoporous silica nano- and microparticle scaffolds are a promising class of materials for the sensitive chemical detection of small-molecule analytes in simple test formats such as lateral flow assays (LFAs) or microfluidic chips. Their architecture is reminiscent of drug delivery systems, only that reporter molecules instead of drugs are stored in the voids of a porous host particle. In addition, the pores are closed with macromolecular “caps” through a tailored “gatekeeping” recognition chemistry so that the caps are opened when an analyte has reacted with a “gatekeeper”. The subsequent uncapping leads to a release of a large number of indicator molecules, endowing the system with signal amplification features. Particular benefits of such systems are their modularity and adaptability. With the example of the immunochemical detection of type-I pyrethroids by fluorescent dye-releasing gAID systems, the influence of several tuning modes on the optimisation of such hybrid sensory materials is introduced here. In particular, different mesoporous silica supports (from nano- and microparticles to platelets and short fibres), different functionalisation routes and different loading sequences were assessed. The materials’ performances were evaluated by studying their temporal response behaviour and detection sensitivity, including the tightness of pore closure (through the amount of blank release in the absence of analyte) and the release kinetics. Our results indicate that the better the paratope-accommodating Fab region of the antibody “cap” fits into the host material's pore opening, the better the closing/opening mechanism can be controlled. Because such materials are well-suited for LFAs, performance assessment included a test-strip format besides conventional assays in suspension. In combination with dyes as indicators and smartphones for read-out, simple analytical tests for use by untrained personnel directly at a point-of-need such as an aeroplane cabin can be devised, allowing for sensitivities down to the μg kg−1 range in <5 min with case-required selectivities.
Multidrug resistance resulting from a variety of defensive pathways in Cancer has become a global concern with a considerable impact on the mortality associated with the failure of traditional chemotherapy. Therefore, further research and new therapies are required to overcome this challenge. In this work, a cyclic R10 peptide (cR10) is conjugated to polyglycerol-covered nanographene oxide to engineer a nanoplatform for the surmounting of multidrug resistance. The nuclear translocation of the nanoplatform, facilitated by cR10 peptide, and subsequently, a laser-triggered release of the loaded doxorubicin result in efficient anticancer activity confirmed by both in vitro and in vivo experiments. The synthesized nanoplatform with a combination of different features, including active nucleus-targeting, highloading capacity, controlled release of cargo, and photothermal property, provides a new strategy for circumventing multidrug resistant cancers.
In this work the flexural rigidity of individual large diameter multi-walled carbon nanotubes (MWCNTs) was investigated. The bending modulus were obtained by detecting the resonance frequencies of mechanically excited cantilevered carbon nanotubes using the so-called dynamic scanning electron microscopy technique, and applying the Euler–Bernoulli beam theory. For the nanotubes studied, we determined a modulus of up to 160 GPa. This agrees with values reported by other authors for MWCNTs produced by catalytic chemical vapor deposition, however, it is 6-8 times smaller than values reported for single and multi-walled carbon nanotubes produced by arc-discharge synthesis. Toxicological studies with carbon nanotubes have been showing that inhaled airborne nanofibers that reach the deep airways of the respiratory system may lead to serious, asbestos-like lung diseases. These studies suggested that their toxicity critically depends on the fiber flexural rigidity, with high rigidity causing cell lesions. To complement the correlation between observed toxicological effects and fiber rigidities, reliable and routinely applicable measurement techniques for the flexural rigidity of nanofibers are required.
Controlling thickness and tightness of surface passivation shells is crucial for many applications of core–shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the applicationrelevant functionality like a high photoluminescence (PL) quantum yield, calling for a whole nanoobject approach. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. In addition to demonstrating the potential of this novel whole nanoobject approach for determining architectures of small nanoparticles, the presented results also highlight challenges faced by different sizing and structural analysis methods and method-inherent uncertainties.
Raman spectroscopic signature of ectoine conformations in bulk solution and crystalline state
(2020)
Recent crystallographic results revealed conformational changes of zwitterionic ectoine upon hydration. By means of confocal Raman spectroscopy and density functional theory calculations, we present a detailed study of this transformation process as part of a Fermi resonance analysis. The corresponding findings highlight that all resonant couplings are lifted upon exposure to water vapor as a consequence of molecular binding processes. The importance of the involved molecular groups for water binding and conformational changes upon hydration is discussed. Our approach further Shows that the underlying rapid process can be reversed by carbon dioxide saturated atmospheres. For the first time, we also confirm that the conformational state of ectoine in aqueous bulk solution coincides with crystalline ectoine in its dihydrate state, thereby highlighting the important role of a few bound water molecules.
This dataset is a complete set of raw, processed and analyzed data, complete with Jupiter notebooks, associated with the manuscript mentioned in the title.
In the manuscript, we provide a "systems architecture"-like overview and detailed discussions of the methodological and instrumental components that, together, comprise the "MOUSE" project (Methodology Optimization for Ultrafine Structure Exploration). Through this project, we aim to provide a comprehensive methodology for obtaining the highest quality X-ray scattering information (at small and wide angles) from measurements on materials science samples.
A major source of capacity fade of the common vanadium redox flow battery (VRFB) is the vanadium ion transport through the separator. However, different transport models disagree significantly in the diffusion coefficient for the different V species and the influence of different transport mechanisms. The underlying hypothesis of this work is that reactions inside the membrane are partly responsible for these discrepancies. Accordingly, it was investigated if redox reactions inside the nanoscopic water body of Nafion 117 can occur. X-ray absorption near edge structure spectroscopy (XANES) was used to distinguish between the different V species inside hydrated Nafion 117 and novel PVDF-based membranes. It was validated that the speciation of vanadium can be performed using the pre-edge peak energy and intensity. The experiments were performed as follows: strips of the membrane were exposed from one site to a V3+ solution (green) and from the other site to a VO2+ solution (yellow). The ions could diffuse into the membrane from both sides. A change of color of the membrane strip was observed. The blue color in the middle of the strip indicated that VO2+ was formed where V3+ and VO2+ got in contact. Using XANES this reaction inside Nafion was proven.
The antibacterial features of natural pine/spruce rosin are well established, yet the functionality in various thermoplastics has not been surveyed. This work focuses on the processing of industrial grade purified rosin mixed with polyethylene (PE), polypropylene (PP), polylactic acid (PLA), polyamide (PA) and corn starch based biopolymer (CS). Homopolymer masterbatches were extrusion-compounded and melt-spun to form fibres for a wide range of products, such as filters, reinforcements, clothing and medical textiles. Due to the versatile chemical structure of rosin, it was observed compatible with all the selected polymers. In general, the rosin-blended systems were shear-thinning in a molten condition. The doped fibres spun of PE and PP indicated adequate melt-spinning capability and proper mechanical properties in terms of ultimate strength and Young's modulus. The antibacterial response was found dependent on the selected polymer. Especially PE with a 10 wt% rosin content showed significant antibacterial effects against Escherichia coli DH5α and Staphylococcus aureus ATCC 12598 when analysed in the Ringer's solution for 24 h.
Aldehyde moieties on 2D-supports or microand nanoparticles can function as anchor groups for the attachment of biomolecules or as reversible binding sites for proteins on cell surfaces. The use of aldehyde-based materials in bioanalytical and medical settings calls for reliable methods to detect and quantify this functionality. We report here on a versatile concept to quantify the accessible aldehyde moieties on particle surfaces through the specific binding and subsequent release of small reporter molecules such as fluorescent dyes and nonfluorescent chromophores utilizing acylhydrazone formation as a reversible covalent labeling strategy. This is representatively demonstrated for a set of polymer microparticles with different aldehyde labeling densities. Excess reporter molecules can be easily removed by washing, eliminating inaccuracies caused by unspecific adsorption to hydrophobic surfaces. Cleavage of hydrazones at acidic pH assisted by a carbonyl trap releases the fluorescent reporters rapidly and quasi-quantitatively and allows for their fluorometric detection at low concentration. Importantly, this strategy separates the signal-generating molecules from the bead surface. This circumvents common issues associated with light scattering and signal distortions that are caused by binding-induced changes in reporter fluorescence as well as quenching dye−
dye interactions on crowded particle surfaces. In addition, we demonstrate that the release of a nonfluorescent chromophore via disulfide cleavage and subsequent quantification by absorption spectroscopy gives comparable results, verifying that both assays
are capable of rapid and sensitive quantification of aldehydes on microbead surfaces. These strategies enable a quantitative
comparison of bead batches with different functionalization densities, and a qualitative prediction of their coupling efficiencies in bioconjugations, as demonstrated in reductive amination reactions with Streptavidin.
If the particle size decreases, the ratio of surface area to volume increases considerably. This provides benefits for all surface-driven processes that run faster or at lower temperatures than larger particles. However, handling and characterization of the nanopowders are much more difficult. Particularly polydisperse powders with irregular shape, as grinding products, represent a challenge. Granulometry in the submicron and nanoscale often leads to incorrect results without knowledge of particle morphology.
This presentation demonstrates potentials of using the volume-specific surface area (SV or VSSA) in the granulometric characterization of nanopowders, for instance, correlations between the volume-specific surface area and the median particle size are discussed considering the particle morphology and the model of the logarithmic normal distribution.
Moreover, the presentation deals with the optimal dispersion of nanopowders during sample preparation. Indirect ultrasound device with defined cooling was developed to prevent both contamination by sonotrode abrasion and sample changes by heat.
Successful granulometric characterization of nanopowders demands both improved dispersion technology and very often an effective combination of two or more measurement methods.
Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Nach einem Vergleich der Ergebnisse mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet.
The 44th Meeting of the Versailles Project on Advanced Materials and Standards (VAMAS) Steering Committee has just taken place at NIST in Boulder (CO, USA). BAM participates with significant contributions in Technical Working Areas on nanoparticle and surface chemistry characterization, but also has positioned itself to new global material challenges and trends in the developement of advanced materials and their characterization, such as thermal properties, self-healing materials, and micro- and nanoplastic.
Everything SAXS
(2019)
Experimenting on MAUS
(2019)
Nanocomposites based on MgAL layered double hydroxides (LDH) and an epoxy resin were prepared and investigated by a combination of complementary methods. As epoxy resin Bisphenol A diglycidyl ether (DGEBA) was used with Diethylenetriamine as curing agent. The LDH was modified with taurine, which acts as an additional crosslinking agent due to its amine groups. The epoxy resin was cured in a presence of the nanofiller, which was added to the system in various concentrations. X-ray scattering, by combination of SAXS and WAXS was used to characterize the morphology of the obtained nanocomposites. These investigations show that the filler is distributed in the matrix as small stacks of ca. 10 layers. The molecular dynamics of the system, as probe for structure, was investigated by broadband dielectric spectroscopy. In addition to the - and -relaxation (dynamic glass transition), characteristic for the unfilled materials, a further process was found which was assigned to localized fluctuations of segments physically adsorbed or chemically bonded to the nanoparticles. The dielectric -relaxation is shifted to higher temperatures for the nanocomposites in comparison to the pure material but depends weakly on the content of nanoparticles. Further, for the first time Flash DSC was employed to a thermosetting system to investigate the glass transition behavior of the nanocomposites. The heating rates were converted in to relaxation rates. For low concentrations of the nanofiller the thermal data overlap more or less with that of the pure epoxy. For higher concentrations the thermal data are shifted significantly to higher temperatures. This is discussed in terms the cooperativity approach to the glass transition.
What to measure? is a key question in nanoscience, and it is not straightforward to address as different physicochemical properties define a nanoparticle sample. Most prominent among these properties are size, shape, surface charge, and porosity. Today researchers have an unprecedented variety of measurement techniques at their disposal to assign precise numerical values to those parameters. However, methods based on different physical principles probe different aspects, not only of the particles themselves, but also of their preparation history and their environment at the time of measurement. Understanding these connections can be of great value for interpreting characterization results and ultimately controlling the nanoparticle structure–function relationship. Here, the current techniques that enable the precise measurement of these fundamental nanoparticle properties are presented and their practical advantages and disadvantages are discussed. Some recommendations of how the physicochemical parameters of nanoparticles should be investigated and how to fully characterize these properties in different environments according to the intended nanoparticle use are proposed. The intention is to improve comparability of nanoparticle properties and performance to ensure the successful transfer of scientific knowledge to industrial real‐world applications.
Femtosecond laser-induced periodic surface structures: from light localization to applications
(2019)
This presentation reviews the current state in the field of Laser-induced Periodic Surface Structures (LIPSS). These surface nanostructures are a universal phenomenon and can be generated on almost any material by irradiation with intense linearly polarized laser radiation. LIPSS are formed in a “self-ordered” way and are often accompanying material processing applications. They can be produced following a single-step process and enable surface functionalization through the adaption of optical, mechanical and chemical surface properties. Their structural sizes typically range from several micrometers down to less than 100 nanometers exhibiting a clear correlation with the polarization direction of the laser radiation. Various types of surface structures are classified, relevant control parameters are identified, and their material specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics, through time-resolved optical experiments and theoretical simulations. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
Formation of interphases between inorganic nanofillers and thermoplastic matrices are usually correlated to short-range interactions which does not exceed more than tens of nanometers away from the surface of the filler. Nevertheless, in nanocomposites with thermosetting matrices, the effect of nanofillers on the properties of the matrix is not limited to the immediate vicinities, but a long-range property alteration of the bulk polymer may be observed. The interaction between nanofillers and the polymer can disturb the curing reaction and alters the chemical, physical and mechanical properties of the polymer network in the matrix phase. In our studies, we aim to investigate short and long-range interphases of a nanocomposite system consisting of a thermosetting matrix (DGEBA) filled with an inorganic nanoparticle (boehmite). For this purpose, a combination of atomic force microscopy (AFM)-based approaches is implemented. Scanning kelvin probe microscopy (SKPM) was used to map the compositional contrast and the interphase with different electrical properties than the bulk. The mechanical properties of the interphase were probed by high resolution intermodulation AFM. (ImAFM). Furthermore, infrared spectroscopy AFM (AFM-IR) is used to investigate the chemical structure of the matrix at different distances from the nanoparticle. SKPM and (AFM-IR) measurements both show a long-range (to 10 µm) effect of boehmite on the chemical structure and surface potential of the bulk epoxy, respectively, whereas ImAFM force measurements reveals a short-range mechanical interphase between the filler and the matrix. The AFM-IR demonstrated the existence of unreacted anhydride hardener at the interphase. This indicates the preferential absorption of anhydride on the surface of boehmite. The consequence of such a selective interaction between the inorganic filler and the epoxy components is disturbance of the epoxy-hardener stoichiometric ratio, the curing mechanism. and the alteration of bulk properties of the matrix.
Spherical mesoporous bioactive glasses in the silicon dioxide (SiO2)-phosphorus pentoxide (P2O5)–calcium oxide (CaO) system with a high specific surface area of up to 300m2/g and a medium pore radius of 4 nm were synthesized by using a simple one-pot surfactant-assisted sol–gel synthesis method followed by calcination at 500–700°C. The authors were able to control the particle properties by varying synthesis parameters to achieve microscale powders with spherical morphology and a particle size of around 5–10 mm by employing one structure-directing agent. Due to a high Calcium oxide content of 33·6mol% and a phosphorus pentoxide content of 4·0mol%, the powder showed very good bioactivity up to 7 d of immersion in simulated Body fluid. The resulting microspheres are promising materials for a variety of life science applications, as further processing – for example, granulation – is unnecessary. Microspheres can be applied as materials for powder-based additive manufacturing or in stable suspensions for drug release, in bone cements or fillers.
The freeze casting technique assisted with cryo thiol-ene photopolymerization is successfully employed for the fabrication of macroporous polymer-derived silicon oxycarbide with highly aligned porosity. It is demonstrated that the free radical initiated thiol-ene click reaction effectively cross-linked the vinyl-containing liquid polysiloxanes into infusible thermosets even at low temperatures. Furthermore, mixed solution- and suspension-based freeze casting is employed by adding silica nanopowders. SiOC/SiO2 foams with almost perfect cylindrical shapes are obtained, demonstrating that the presence of nano-SiO2 does not restrict the complete photoinduced cross-linking. The post-pyrolysis HF acid treatments of produced SiOC monoliths yields hierarchical porosities, with SiOC/SiO2 nanocomposites after etching demonstrating the highest specific surface area of 494 m2/g and pore sizes across the macro-, meso- and micropores ranges. The newly developed approach gives a versatile solution for the fabrication of bulk polymer-derived ceramics with controlled porosity.
New reference material candidates for traceable size measurement of nonspherical nanoparticles
(2019)
Size measurement of nanoparticles (NP) becomes a challenging analytical problem when non-spherical shapes must be traceably measured. However, most industrial NPs have irregular shapes and broad size distribution making it often more complex to follow European regulatory to identify a material as a nanomaterial according to which accurate measurement of the smallest dimension and its size Distribution is necessary.
The European research project nPSize - Improved traceability chain of nanoparticle size measurements aims to fill this gap by developing potential non-spherical reference nanoparticles, measurement procedures and physical modelling to improve the traceability chain, comparability and compatibility for NP size measurements between different methods. Therefore, new model NP with well-controlled shape has been synthesized and are supposed to be systematically characterized using the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering.
Following NP candidates are under investigation with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-100 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). In addition, sample preparation procedures as well as measurement analysis procedures with evaluation of appropriate measurands and descriptors for each material class and method are being developed to support standardization. To underpin the traceability of the size measurement of nonspherical NP, physical modelling of the signals in e.g. electron microscopy techniques will be used and in combination, the implementation of machine learning is aimed to facilitate measurement Analysis procedures, especially regarding the accurate thresholding/segmentation of the NPs.
In this study, femtosecond laser-induced sub-micrometer structures are generated to modify polyethylene (PE) surface topographies. These surfaces were subjected to bacterial colonization studies with Escherichia coli and Staphylococcus aureus as test strains. The results reveal that the nanostructures do not influence S. aureus coverage, while the adhesion of E. coli is reduced.
Fresnoite glass with excess SiO2 exhibits oriented surface crystallization, in contrast to the stoichiometric glass composition. Recent EBSD studies documented that the crystals in BTS (2BaO-TiO2-xSiO2, x=0-3) can occur in a distinct [101]-orientation perpendicular to the surface and claimed that this orientation is not a result of growth selection. During these previous studies, however, the effect of surface preparation and surrounding atmosphere during the crystallization experiments were not considered. As these parameters may influence crystal orientation, we studied the surface crystallization of a BTS glass (2BaO-TiO2–2.75SiO2) under controlled conditions with the help of light, electron and polarisation microscopy as well as EBSD. Heat treatments for one hour at 840°C of fractured BTS glass surfaces in air resulted in a large number of not-separable surface crystals. This large number of crystals can be caused by dust particles, which act as nucleation agents. As crystal growth velocity could further be influenced by humidity, our experiments are performed in a filtered and dried air atmosphere. The crystal morphology and orientation will be analysed in dependence of the sample preparation and a differing surrounding atmosphere.
Characterization of early crystallization stages in surface-crystallized diopside glass-ceramics
(2019)
Structure formation in glass-ceramics by means of surface crystallization is a challenging open question and remains elusive to definite answers. In several glass-ceramic systems, oriented crystal layers have been observed at the immediate surface, including diopside and some fresnoite systems. However, it is still open to debate, whether oriented surface crystallization is the result of oriented nucleation or growth selection effects. In the same vein, there is still discussion whether surface nucleation is governed by surface chemistry effects or by defects serving as active nucleation sites.
In order to help answer these questions, annealing experiments at 850°C have been performed on a MgO·CaO·2SiO2 glass, leading to the crystallization of diopside at the surface. Different annealing durations and surface treatment protocols (i.a. lapping with diamond slurries between 16 µm and 1 µm grain size) have been applied. Particular focus has been put on earliest crystallization stages, with crystal sizes down to about 200 nm. The resultant microstructure has been analyzed by electron backscatter diffraction (EBSD) and two different kinds of textures have been observed, with the a- or b-axis being perpendicular to the sample surface and the c-axis lying in the sample plane. Even at shortest annealing durations, a clear texture was present in the samples. Additionally, selected samples have been investigated with energy-dispersive x-ray spectroscopy in the scanning transmission electron microscope (STEM-EDX). The diopside crystals have been found to exhibit distinguished submicron structure variations and the glass around the crystals was shown to be depleted of Mg.
NanoDefiner e-Tool: An Implemented Decision Support Framework for Nanomaterial Identification
(2019)
The European Commission’s recommendation on the definition of nanomaterial (2011/696/EU) established an applicable standard for material categorization. However, manufacturers face regulatory challenges during registration of their products. Reliable categorization is difficult and requires considerable expertise in existing measurement techniques (MTs). Additionally, organizational complexity is increased as different authorities’ registration processes require distinct reporting.
The NanoDefine project tackled these obstacles by providing the NanoDefiner e-tool: A decision support expert system for nanomaterial identification in a regulatory context. It providesMT recommendations for categorization of specific materials using a tiered approach (screening/confirmatory), and was constructed with experts from academia and industry to be extensible, interoperable, and adaptable for forthcoming revisions of the nanomaterial definition. An implemented MT-driven material categorization scheme allows detailed description. Its guided workflow is suitable for a variety of user groups. Direct feedback and explanation enable transparent decisions. Expert knowledge is Held in a knowledge base for representation of MT performance criteria and physicochemical particle type
properties. Continuous revision ensured data quality and validity. Recommendations were validated by independent case studies on industry-relevant particulate materials. Besides supporting material identification and registration, the free and open-source e-tool may serve as template for other expert systems within the nanoscience domain.
The characteristics of TiO2 coatings can greatly influence their final performance in large-scale applications. In the present study self-assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with e.g. silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3- aminopropyl)triethoxysilane (APTES) or (3-aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino-groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino-groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape and specific surface area have been functionalized. FTIR, TGA, SEM/EDS, XPS, Auger electron spectroscopy (AES) and ToF-SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA.
New reference material candidates for traceable size measurement of non-spherical nanoparticles
(2019)
New model nanoparticles with well-controlled shape were synthesized within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. Their systematic characterization takes place by the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering. Following reference nanoparticle candidates are under investigation with respect to their homogeneity and stability: titania nanoplatelets (10-15 nm x 50-100 nm), titania bipyramides (~60 nm x 40 nm), titania acicular particles (100 nm x 15-20 nm; aspect ratio 5.5/6), gold nanorods (~10 nm x 30 nm), and gold nanocubes (~55 nm x 55 nm x 55 nm).
Based on the three-phase model of semi-crystalline polymers, we determined all phase fractions of the NiAl-LDH/PLLA nanocomposites in dependence on the concentration of the nanofiller. Moreover, the rigid amorphous fraction (RAF) was separated into the RAFcrystal and the RAFfiller unbiasedly. A detailed comparison to the related nanocomposite system MgAl-LDH/PLLA was made considering that Mg and Ni have different atomic weights. As a first result is was found that NiAl-LDH/PLLA displays a higher crystallization rate compared to MgAl-LDH/PLLA, which is related to the different morphologies of the two nanocomposite systems. For both systems RAFcrystal increases with increasing concentration of the nanofiller. This means in the case of the nanocomposite not each crystal produces the same amount of RAF, as often assumed. Also, RAFfiller increases with the concentration for both systems but in a different way. This is discussed considering again the different morphologies of both nanocomposites.
The particle size distribution is considered the most relevant information for nanoscale property identification and material characterization. The current OECD test guideline on particle size and size distribution (TG 110) is not applicable to ‘nano-sized’ objects. In this project we thus develop a new OECD test guideline for the measurement of the size and size distribution of particles and fibers with at least one dimension in the nanoscale. A fiber is defined as an object having an aspect ratio of length/diameter l/d >3. The width and length of each fiber should be measured concurrently.
In order to measure the particle size distributions, many techniques are available. 9 methods for particles and 2 methods for fibres have been tested in a prevalidation study and appropriate methods will be compared in an interlaboratory round robin test starting in February 2019.
The properties of nanomaterials are influenced not only by their chemical composition but also by physical properties (such as size, geometry and crystal structure). For the reliable determination and assessment of behaviour and effects of nanomaterials as well as for the determination of the exposure of humans and environment a comprehensive physical-chemical characterization of nanomaterials is essential. This is an important prerequisite to identify them as nanomaterials and to interpret and compare test results and - in future – to forecast interaction and effects of nanomaterials.
In 2006, the OECD launched a sponsorship program for the testing of nanomaterials in which 11 nanomaterials were thoroughly investigated using a variety of methods. The aim of the project was, among other things, to find out where problems occur and where there are gaps in the measurement and test procedures and where are changes required. An important outcome of the sponsorship program was the finding that the OECD Test Guidelines should in several cases be extended to the specific needs in testing of nanomaterials. The existing standardized test methods of the OECD for physical-chemical characterization have not been developed for nanomaterials in particular. A high demand for an extension of the test guidelines was identified. Germany complied with the OECD's request in 2017 and has agreed to extend the “Test Guideline on Particle Size Distribution / Fiber Length and Diameter Distributions Test Guideline” for Manufactured Nanomaterials (MN). UBA commissioned BAM and BAuA with the preparation of the Test Guideline. The aim of the project is the development of a harmonized test protocol for a valid and reproducible determination of particle size and size distribution which is one of the most relevant physical-chemical properties for MNs.
Different measuring methods provide different results for the size distribution of the particles. This is caused by the different measuring principles of the methods. Each method measures a specific parameter that ultimately determines particle size. First, the measured quantity differs for each method (Scattered light intensity, 2D image / projection, electric mobility, etc.). Second, the calculated diameters of the MN may differ (Feret Diameter, Area Projection, Mobility Diameter, Aerodynamic Diameter, Hydrodynamic Diameter). Third, a measuring method provides a size distribution which is measured either mass-based, surface-based or number-based. A conversion between the results requires additional parameters and thus possibly increases the measurement error.
In addition to the technical differences, the individual parameters are strongly influenced by the structure and material of the nanoparticles. For example, a surface functionalization can lead to very different results in the size distribution. The suitability of measurement methods differs with the material of the MN. As a result, two very different results can be measured for the particle size distribution using two different methods, which are nevertheless both correct. Several large projects in recent years therefore concluded that nanomaterials should be characterized by at least two complementary method. Imaging techniques are regarded as one of these methods for the characterization, the complementary methods are supposed to be statistical methods.
The different results for the size distribution of nanomaterials become problematic for the registration of new MN. A comparable and reproducible size distribution is a prerequisite for a standardized registration. In the future, the particle size distribution in the EU will also decide on the classification of a substance as a nanomaterial or as a non-nanomaterial. Especially in borderline cases, a standardized and comparable measurement methodology is therefore essential.
The new OECD test guideline will address the following four main steps in the determination of the length and width distributions of fibers: sample preparation, image acquisition, data evaluation and uncertainty analysis. As the sample preparation has to be optimized for each material, general quality criteria will be given in the protocol. For full visibility of a fiber the appropriate resolution has to be chosen. In the data evaluation the length and diameter of each fiber will be determined concurrently to allow for application of different regulatory definitions. The quality of the results critically depends on the sample preparation as well as the data evaluation. In this step the classification rules have to be formulated and followed accurately in order to optimize reproducibility of the method. The SOP will be validated in an international round robin test, which is planned for 2018/2019.
In recent years, the improved understanding of the formation of laser-induced periodic surface structures (LIPSS) has led to an emerging variety of applications that modify the optical, mechanical and chemical properties of many materials. Such structures strongly depend on the laser beam polarization and are formed usually after irradiation with ultrashort linearly polarized laser pulses. The most accepted explanation for the origin of the structures is based on the interference of the incident laser radiation with electromagnetic surface waves that propagate or scatter at the surface of the irradiated materials. This leads to an intensity modulation that is finally responsible for the selective ablation in the form of parallel structures with periods ranging from hundreds of nanometers up to some micrometers. The versatility when forming such structures is based on the high reproducibility with different wavelength, pulse duration and repetition rate laser sources, customized micro- and nanometric spatial resolutions, and the compatibility with industrially relevant processing speeds when combined with fast scanning devices. In this contribution, we review the latest applications in the rapidly emerging field of surface functionalization through LIPSS, including biomimetic functionalities on fluid transport, control of the wetting properties, specific optical responses in technical materials, improvement of tribological performance on metallic surfaces and bacterial and cell growth for medical devices, among many others.
Challenges in Traceable Size Measurement of Non-Spherical, Non-Monodisperse Nanoparticles - nPSize
(2019)
Size measurement of nanoparticles (NP) becomes a challenging analytical problem when non-spherical shapes must be traceably measured. However, most industrial NPs have irregular shapes and broad size distribution making it often more complex to follow European regulatory to identify a material as a nanomaterial according to which accurate measurement of the smallest dimension and its size Distribution is necessary.
The European research project nPSize - Improved traceability chain of nanoparticle size measurements aims to fill this gap by developing potential non-spherical reference nanoparticles, measurement procedures and physical modelling to improve the traceability chain, comparability and compatibility for NP size measurements between different methods. Therefore, new model NP with well-controlled shape has been synthesized and are supposed to be systematically characterized using the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering.
Following NP candidates are under investigation with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-100 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). In addition, sample preparation procedures as well as measurement analysis procedures with evaluation of appropriate measurands and descriptors for each material class and method are being developed to support standardization. To underpin the traceability of the size measurement of nonspherical NP, physical modelling of the signals in e.g. electron microscopy techniques will be used and in combination, the implementation of machine learning is aimed to facilitate measurement Analysis procedures, especially regarding the accurate thresholding/segmentation of the NPs.zeige mehr
The efficient and sensitive detection of pathogenic microorganisms in aqueous environments, such as water used in medical applications, drinking water, and cooling water of industrial plants, requires simple and fast methods suitable for multiplexed detection such as flow cytometry (FCM) with optically encoded carrier beads. For this purpose, we combine fluorescent Cd-free Ag−In−S ternary quantum dots (t-QDs) with fluorescence Lifetimes (LTs) of several hundred nanoseconds and superparamagnetic Fe3O4 nanoparticles (SPIONs) with mesoporous CaCO3 microbeads to a magneto-fluorescent bead platform that can be surface-functionalized with bioligands, such as antibodies. This inorganic bead platform enables immuno-magnetic separation, target enrichment, and target quantification with optical readout. The beads can be detected with steady-state and time-resolved fluorescence microscopy and flow cytometry (FCM). Moreover, they are suited for readout by time gated emission. In the following, the preparation of these magneto-fluorescent CaCO3 beads, their spectroscopic and analytic characterization, and their conjugation with bacteria-specific antibodies are presented as well as proof-of-concept measurements with Legionella pneumophila including cell cultivation and plating experiments for bacteria quantification. Additionally, the possibility to discriminate between the long-lived emission of the LT-encoded capture and carrier CaCO3 beads and the short-lived Emission of the dye-stained bacteria with time-resolved fluorescence techniques and single wavelength excitation is demonstrated.
In summary, we report a highly modular solid TTA-UC system comprising of a crystalline, thermally stable PCN222(Pd) MOF with CA-coated MOF channels and with a DPA annihilator embedded in a solution-like environment in the MOF channels. This solid material displays blue upconverted delayed emission with a luminescence lifetime of 373 us, a threshold value of 329 mW*cm-2 and a triplet–triplet energy transfer efficiency of 82%. This optical application adds another facet to the versatile chemistry of PCN-222 MOFs. The design concept is also applicable to other TTA-UC pairs and enables tuning of the UCL color, for example, by replacing DPA with other dyes as exemplarily shown for 2,5,8,11-tetra-tert-butyl-perylene, that yields UCL at 450 nm. Current work aims to reduce the oxygen sensitivity and to increase the retention of the trapped annihilators in organic environments, for example, by tuning the chain length of the carboxylic acid and by coating the MOF surface. In addition, the TTA-UC efficiency will be further enhanced by reducing the reabsorption of the UC emission caused by Pd(TCPP) and by optimizing the sensitizer/annihilator interface.
It was found for inorganic/polymer nanocomposites that a so-called Rigid Amorphous Phase (RAF) is formed in the interfacial region by adsorption of polymer segments onto the nanoparticles. The segmental dynamics of RAF is expected to be altered, as compared to the pure matrix, which might percolate into the entire system, affecting the overall nanocomposite properties. Here, the structure and molecular mobility of epoxy-based PNCs with different nanofillers (layered double hydroxide and boehmite) was studied by a combination of calorimetric and X-Ray scattering techniques. Temperature modulated DSC (TMDSC) showed that depending on the nanofiller, RAF can reach up to 40 wt % of the system or, on the contrary, the overall mobility of the matrix might increase due to the presence of particles. Such contrasting results, including the high amount of RAF, which was never shown before for epoxy-based PNCs, emphasize the importance of interfaces. Additionally, glass transition and glassy dynamics were investigated by a novel technique, Flash DSC (heating rates up to 10 kK/s) employed for the first time to a thermosetting system and electrospun fibers, which did not result in their degradation. It was used to study both the vitrification kinetics and glassy dynamics of the PNCs, for instance further confirming the presence of RAF and its impact on the overall material properties.
Extracellular vesicles (EV) are cell-derived particles in body fluids, which have excellent potential as next-generation biomarkers. The exploitation of EV requires reliable measurements, which is currently very difficult, as most EV are smaller than 200 nm. At present, flow cytometry (FCM) is the most appropriate technique for EV analysis in biological samples, as FCM is readily available in many clinical laboratories and allows to identify cell-specific EV at high throughput. However, due to technical variations between different FCM instruments, EV concentration measurements are currently not well comparable between most laboratories. Therefore, EV reference materials and standardized reference methods are urgently needed to calibrate flow rate, light scattering intensity, and fluorescence intensity of FCM in the sub-micrometer size range. This requires a better matching of the optical properties of calibration beads and EV as can be realized with current polystyrene calibration beads.
The EMPIR project 18HLT01 “MetVes II” aims to develop synthetic reference materials and traceable measurement methods to standardize EV measurements. The reference materials should resemble EV properties, so that calibrations are reliable and do not require a change of acquisition settings. Hence, the reference materials should contain particles with a traceable number concentration in the range of 109–1012 particles/mL to calibrate flow rate, a traceable size with discrete diameters between 50–1000 nm and a refractive index (RI) in the range of 1.37–1.42 to calibrate scattering intensity, and a traceable fluorescence intensity between 100–100,000 molecules of equivalent soluble fluorochromes (MESF). At BAM, various approaches to prepare such low-RI nanometer-sized reference materials will be studied, preliminary results of the primary characterization of these candidate reference particles will be presented, and possible applications besides FCM-based EV detection will be outlined.
Zeolitic imidazolate frameworks (ZIFs) have been widely investigated for their use in separation, gas adsorption, catalysis, and biotechnology. Their practical applications, however, can be hampered by their structural instability in humid acidic conditions. Here, guided by density functional theory calculations, we demonstrate that the acidic stability of two polymorphic ZIFs (i.e., ZIF-8 and ZIF-L) can be enhanced by the incorporation of functional groups on polypeptides or DNA. A range of complementary synchrotron investigations into the local chemical structure and bonding environment suggest that the enhanced acidic stability arises from the newly established coordinative interactions between the Zn centers and the inserted carboxylate (for polypeptides) or phosphate (for DNA) groups, both of which have lower pKas than the imidazolate ligand. With functional biomolecular homologs (i.e., enzymes), we demonstrate a symbiotic stability reinforcement effect, i.e., the encapsulated biomolecules stabilize the ZIF matrix while the ZIF exoskeleton protects the enzyme from denaturation.
Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EPMA and µ-XRF
(2019)
The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification.
Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results.
Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode.
Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values.
As resistance to traditional drugs emerges for treatment of Virus infections, the need for new methods for virus inhibition increases. Graphene derivatives with large surface areas have shown strong activity against different viruses. However, the inability of current synthetic protocols to accurately manipulate the structure of graphene sheets in order to control their antiviral activity remains a major challenge. In this work, a series of graphene derivatives with defined polyglycerol sulfate and fatty amine functionalities have been synthesized and their interactions with herpes simplex Virus type 1 (HSV-1) are investigated. While electrostatic interactions between polyglycerol sulfate and virus particles trigger the binding of graphene to virus, alkyl chains induce a high antiviral activity by secondary hydrophobic interactions. Among graphene sheets with a broad range of alkyl chains, (C3–C18), the C12-functionalized sheets showed the highest antiviral activity, indicating the optimum synergistic effect between electrostatic and hydrophobic interactions, but this derivative was toxic against the Vero cell line.
In contrast, sheets functionalized with C6- and C9-alkyl chains showed low toxicity against Vero cells and a synergistic Inhibition of HSV-1. This study shows that antiviral agents against HSV-1 can be obtained by controlled and stepwise functionalization of graphene sheets and may be developed into antiviral agents for future biomedical applications.
An inter-laboratory comparison on the particle size, expressed as mean diameter d, of nanoscaled SiO2 (#14 BAM Silica (see NanoValid DoW, D.5.41/5.42)) has been performed. The majority of participants used Dynamic Light Scattering (DLS). A few used Electron Microscopy as method. Following methods had been applied by only one partner, respectively: Small Angle X-ray Scattering, Analytical Ultracentrifugation, Atomic Force Microscopy and Atomizer with electric mobility spectrometer.
BAM provides leading expertise in preparation, characterisation and application of fluorescent reference standards and biomedical relevant nanomaterials, as well as in traceable, absolute, and quantitative fluorometric measurements of transparent and scattering systems in the ultraviolet, visible, and near infrared spectral region. BAM will prepare solid low-RI particles in WP1, will develop reference methods to determine the fluorescence intensity and RI of reference materials in WP2, and will measure the fluorescence intensity of EVs in biological test samples of WP3.
The composites combining aluminum and silica nanoparticles with the addition of tetramethylammonium hydroxide (Al-SiO2(T)) and butanol (Al-SiO2(B)) as mixing media have been successfully fabricated. Corrosion behavior of Al-SiO2 composites before and after exposure in 1M NaCl solution was examined using potentiodynamic polarization (Tafel curve analysis). The study was also equipped with scanning electron microscopy (SEM), energy dispersive X-ray (EDX), and X-ray diffraction (XRD) investigations. Before exposure, Al-SiO2(T) exhibited the best corrosion resistance. Performance improvement was indicated by Al-SiO2(B) up to 10 times better than Al-SiO2(T) after exposure. The increased SiO2 content did not significantly enhance the corrosion resistance of the composites. The Al-SiO2 composites with 5% SiO2 content showed very high corrosion resistance (as the optimum composition). Furthermore, pitting corrosion was observed in the Al-SiO2 composites, indicated by the formation of corrosion products at grain boundaries. The product was affected by the presence of SiO2 in the Al matrix and the NaCl environment at 90 °C (approach to synthetic geothermal media: Na+, Cl, H+, OH-). Our study revealed the presence of γ-Al2O3, γ-Al(OH)3, and Al(OH)2Cl as the dominant corrosion products.
Laser-induced periodic surface structures: from nanoscaled light localization to applications
(2019)
In this contribution the current state in the field of Laser-Induced Periodic Surface Structures (LIPSS) is reviewed. This includes the mechanisms of formation and current applications, particularly the colorization of technical surfaces, the control of surface wetting properties, the tailoring of surface colonization by bacterial biofilms, and the improvement of the tribological performance of nanostructured metal surfaces.
An inter-laboratory comparison on the surface charge, expressed as zeta potential ζ, of nanoscaled SiO2 has been performed using #14 BAM Silica (see D.5.41/5.42) nanoparticles. The comparability of results delivered by participants has been tested.
The Task 5.4 of NanoValid is designed to test, compare and validate current methods to measure and characterize physicochemical properties of selected engineered nanoparticles. The measurand is Surface charge expressed as zeta-Potential. The measurements are to be accompanied by estimates of the uncertainties at a confidence level of 95%, deduced from the standard uncertainties. Therefore an uncertainty budget comprising statistical (Type A) and systematic (Type B) errors has to be established and delivered for the measurand. The protocol comprises two Annexes addressing the establishment of uncertainty budgets following GUM. The final goal of the comparison is to identify those methods of measurement which have potential as reference methods in pc characterization of nanoparticles for the determination of a given measurand.
This Report describes an inter-laboratory comparison aiming on the establishment of the used method (BET) as a reference method. Another purpose was the certification of the porous reference material #15 BAM Titania as CRM BAM-P110 (cf. D 5.41/42). The certified values determined by nitrogen ad-sorption at 77.3 K according to the international standards ISO 15901-2 and ISO 9277 are summarized in the Table below.
A central challenge to ensure the sustainable production and use of nanotechnologies is to understand and effectively control the risks along the industrial innovation value chain. Knowledge about nanotechnology processes and nanosafety issues (hazards, fate, risk...) is growing rapidly but the effective use of this knowledge for risk management by market actors is lagging behind.
EC4SafeNano (European Centre for Risk Management and Safe Innovation in Nanomaterials and Nanotechnologies) promotes a harmonized vision of expertise in risk assessment and management for the public and private sectors to enable the safe development and commercialization of nanotechnology.
EC4SafeNano is operated together by major European risk institutes with the support of numerous associated partners, gathering all stakeholders involved in Nanomaterials and Nanotechnologies (regulators, industry, society, research, service providers...).
In a case study the surface chemical transformations upon 2 different ageing procedures (long-term UV irradiation or swimming pool water) of a representative set of titanium dioxide nanoparticles has been investigated. The materials have been analyzed by various analytical techniques. Each method addresses different aspects of the complex endpoint surface chemistry. The multi technique approach allows evaluation of the capabilities and limitations of the applied methods regarding their suitability to address the endpoint surface chemistry and their sensitivity to identify even small surface chemical transformations.
Results:
- To obtain a comprehensive picture, it is insufficient to concentrate on a single analysis technique.
- By using time-of-flight secondary ion mass spectrometry (ToF-SIMS) in combination with principal component analysis (PCA) it was possible to identify even subtle changes in the surface chemistry of the investigated materials.
- A general trend that was observed for the UV-aged samples is the decrease of organic material on the nanomaterial surface.
This project has received funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement No 723623.