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Paper des Monats
- ja (11)
Stable crack growth was measured for nominal dry and water-bearing (6 wt%) soda-lime silicate glasses in double cantilever beam geometry and combined with DMA studies on the effects of dissolved water on internal friction and glass transition, respectively. In vacuum, a decreased slope of logarithmic crack growth velocity versus stress intensity factor is evident for the hydrous glass in line with an increase of b-relaxation intensity indicating more energy Dissipation during fracture. Further, inert crack growth in hydrous glass is found to be divided into sections of different slope, which indicates different water related crack propagation mechanism. In ambient air, a largely extended region II is observed for the hydrous glass, which indicates that crack growth is more sensitive to ambient water.
The corrosion resistance of aluminium surfaces is closely linked to the surfacecstate after a grinding process. For years, iron‐containing abrasive materials were suspected to lead to increased corrosion susceptibility after processing of aluminium surfaces. To prove a possible correlation between the iron content of an abrasive and the corrosion behaviour of aluminium components, scientific investigations and experimentally practical corrosion tests are necessary.
For the current investigation, specimens of a technical Al‐Si alloy from the same batch were used. The test specimens were mechanically ground with various resin‐bonded model abrasives containing different iron contents. The performed corrosion tests did not reveal a negative influence of the different iron‐containing abrasives on the corrosion behaviour of the Al–Si alloy.
However, the most sensitive measuring method (electrochemical noise)
showed differences in the surface activity depending on the type of abrasive.
Synthesis, characterization, electrochemistry, and photophysics of novel homo- and heteroleptic ruthenium(II) complexes [Ru(cpmp)2] 2+ (22+) and [Ru(cpmp)(ddpd)]2+ (32+) bearing the tridentate ligands 6,2’’-carboxypyridyl-2,2’-methylamine-pyridylpyridine (cpmp) and N,N’-dimethyl-N,N’-dipyridin-2-ylpyridine-2,6-diamine (ddpd) are reported. The complexes possess one (32+) or two (22+) electron-deficient dipyridyl ketone fragments as electron accepting sites enabling intraligand charge transfer (ILCT), ligand-toligand charge transfer (LL’CT) and low-energy metal-to-ligand charge transfer (MLCT) absorptions. The latter peak around 544 nm (green light). 22+ shows 3MLCT phosphorescence in the red to near-infrared spectral region at room temperature in deaerated acetonitrile solution with an emission quantum yield of 1.3 % and a 3MLCT lifetime of 477 ns, while 3
2+ is much less luminescent. This different behaviour is ascribed to the energy gap law and the shape of the parasitic excited 3MC state potential energy surface. This study highlights the importance of the excited state energies and geometries for the actual excited state dynamics. Aromatic and aliphatic amines reductively quench the excited state of 22+ paving the way to photocatalytic applications using low-energy green light as exemplified with the green-light sensitized thiol-ene click reaction.
Even though being the subject of natural scientific research for many decades, the system CaSO4–H2O, consisting of the five crystalline phases gypsum, bassanite, and the anhydrites III, II, and I, has left many open questions for research. Raman spectroscopy was used because of its structural sensitivity and in situ measurement capability to obtain further insight by studying phase transitions in both ex situ and in situ experiments. The findings include significant contributions to the completeness and understanding of Raman spectroscopic data of the system. The dehydration path gypsum–bassanite–anhydrite III was shown to have strong parallels to a physical drying process, which depends on many parameters beyond the burning temperature. Raman band width determination was demonstrated to enable the quantitative discrimination of α-bassanite and β-bassanite as well as the postulated three sub-forms of anhydrite II (AII), which are all based on differences in crystallinity. In the latter case, the observed continuous structural variations over increasing burning temperatures were elucidated as a combination of decreasing surface areas and healing of crystal lattice defects. We propose an only two-fold sub-division of AII into reactive “disordered AII” and much less reactive “crystalline AII” with a transition temperature of 650°C ± 50 K.
Detection of Multiple Cracks in Four-Point Bending Tests Using the Coda Wave Interferometry Method
(2020)
The enlargement of the cracks outside the permitted dimension is one of the main causes for the reduction of service life of Reinforced Concrete (RC) structures. Cracks can develop due to many causes such as dynamic or static load. When tensile stress exceeds the tensile strength of RC, cracks appear. Traditional techniques have limitations in early stage damage detection and localisation, especially on large-scale structures. The ultrasonic Coda Wave Interferometry (CWI) method using diffuse waves is one of the most promising methods to detect subtle changes in heterogeneous materials, such as concrete. In this paper, the assessment of the CWI method applied for multiple cracks opening detection on two specimens based on four-point bending test is presented. Both beams were monitored using a limited number of embedded Ultrasonic (US) transducers as well as other transducers and techniques (e.g., Digital Image Correlation (DIC), LVDT sensors, strain gauges, and Fiber Optics Sensor (FOS)). Results show that strain change and crack formation are successfully and efficiently detected by CWI method even earlier than by the other techniques. The CWI technique using embedded US transducers is undoubtedly a feasible, efficient, and promising method for long-term monitoring on real infrastructure.
Thousands of antibodies for diagnostic and other analytical purposes are on the market. However, it is often difficult to identify duplicates, reagent changes, and to assign the correct original publications to an antibody. This slows down scientific progress and might even be a cause of irreproducible research and a waste of resources. Recently, activities were started to suggest the sole use of recombinant antibodies in combination with the open communication of their sequence. In this case, such uncertainties should be eliminated. Unfortunately, this approach seems to be rather a long-term vision since the development and manufacturing of recombinant antibodies remain quite expensive in the foreseeable future. Nearly all commercial antibody suppliers also may be reluctant to publish the sequence of their antibodies, since they fear counterfeiting. De novo sequencing of antibodies is also not feasible today for a reagent user without access to the hybridoma clone. Nevertheless, it seems to be crucial for any scientist to have the opportunity to identify an antibody undoubtedly to guarantee the traceability of any research activity using antibodies from a third party as a tool. For this purpose, we developed a method for the identification of antibodies based on a MALDI-TOF MS fingerprint. To circumvent lengthy denaturation, reduction, alkylation, and enzymatic digestion steps, the fragmentation was performed with a simple formic acid hydrolysis step. Eighty-nine unknown monoclonal antibodies were used for this study to examine the feasibility of this approach. Although the molecular assignment of peaks was rarely possible, antibodies could be easily recognized in a blinded test, simply from their mass-spectral fingerprint. A general protocol is given, which could be used without any optimization to generate fingerprints for a database. We want to propose that, in most scientific projects relying critically on antibody reagents, such a fingerprint should be established to prove and document the identity of the used antibodies, as well as to assign a specific reagent to a datasheet of a commercial supplier, public database record, or antibody ID.
Nano-carrier systems such as liposomes have promising biomedical applications. Nevertheless, characterization of these complex samples is a challenging analytical task. In this study a coupled hydrodynamic chromatography-single particle-inductively coupled plasma mass spectrometry (HDC-spICP-MS) approach was validated based on the technical specification (TS) 19590:2017 of the international organization for standardization (ISO). The TS has been adapted to the hyphenated setup. The quality criteria (QC), e.g., linearity of the calibration, transport efficiency, were investigated. Furthermore, a cross calibration of the particle size was performed with values from dynamic light scattering (DLS) and transmission electron microscopy (TEM). Due to an additional Y-piece, an online-calibration routine was implemented. This approach allows the calibration of the ICP-MS during the dead time of the chromatography run, to reduce the required time and enhance the robustness of the results. The optimized method was tested with different gold nanoparticle (Au-NP) mixtures to investigate the characterization properties of HDC separations for samples with increasing complexity. Additionally, the technique was successfully applied to simultaneously determine both the hydrodynamic radius and the Au-NP content in liposomes. With the established hyphenated setup, it was possible to distinguish between different subpopulations with various NP loads and different hydrodynamic diameters inside the liposome carriers.
Hydrogen-charged supermartensitic steel samples were used to systematically investigate imaging artifacts in neutron radiography. Cadmium stencils were placed around the samples to shield the scintillator from excessive neutron radiation and to investigate the influence of the backlight effect. The contribution of scattered neutrons to the total detected intensity was investigated by additionally varying the sample-detector distance and applying a functional correlation between distance and intensity. Furthermore, the influence of the surface roughness on the edge effect due to refraction was investigated.
Supramolecular copolymerization driven by integrative self-sorting of hydrogen-bonded rosettes
(2020)
Molecular recognition to preorganize noncovalently polymerizable supramolecular complexes is a characteristic process of natural supramolecular polymers, and such recognition processes allow for dynamic self-alteration, yielding complex polymer systems with extraordinarily high efficiency in their targeted function. We herein show an example of such molecular recognition-controlled kinetic assembly/disassembly processes within artificial supramolecular polymer systems using six-membered hydrogen-bonded supramolecular complexes (rosettes). Electron-rich and poor monomers are prepared that kinetically coassemble through a temperature-controlled protocol into amorphous coaggregates comprising a diverse mixture of rosettes. Over days, the electrostatic interaction between two monomers induces an integrative self-sorting of rosettes. While the electron-rich monomer inherently forms toroidal homopolymers, the additional electrostatic interaction that can also guide rosette association allows helicoidal growth of supramolecular copolymers that are comprised of an alternating array of two monomers. Upon heating, the helicoidal copolymers undergo a catastrophic transition into amorphous coaggregates via entropy-driven randomization of the monomers in the rosette.
Spectroscopy in Catalysis
(2020)
Knowledge-based catalyst development is always an interaction between preparation, analysis and catalytic testing. Only if these three factors fit together can success be expected. For the analytic side of this triangle, spectroscopic methods play a crucial role. Whereas with diffraction, scattering and microscopy, decisive insights into the structure and morphology of the catalysts can be obtained, spectroscopy produces new knowledge about the chemical nature of the catalyst, e.g., its bonding and valence states.
Connecting Diffraction-Based Strain with Macroscopic Stresses in Laser Powder Bed Fused Ti-6Al-4V
(2020)
The laser powder bed fusion (LPBF) production process often results in large residual stress (RS) in the parts. Nondestructive techniques to determine RS are badly needed. However, a reliable quantification of macro-RS (i.e., stress at the component level) by means of diffraction-based techniques is still a great challenge, because the link between diffraction-based strain and macro-RS is not trivial. In this study, we experimentally determine (by means of in-situ synchrotron radiation diffraction) this link for LPBF Ti-6Al-4V. We compare our results with commonly used models to determine the so-called diffraction elastic constants (DECs). We show that LPBF materials possess different DECs than wrought alloys, simply because their microstructural and mechanical properties are different. We also show that the existing models can be used to calculate DECs only if high accuracy of the RS values is not required. If the peculiarities of the microstructure have to be taken into account (as is the case of additively manufactured materials), a radically new approach is desirable.
Explaining Deviatoric Residual Stresses in Aluminum Matrix Composites with Complex Microstructure
(2020)
The residual stresses in multiphase metal Matrix composites with both random planar-oriented short fibers and particles were studied by neutron diffraction and by a model based on the reformulation of classic Maxwell’s homogenization method. Contrary to common understanding and state-of-the-art models, we experimentally observed that randomly oriented phases possess non-hydrostatic residual stress. The recently developed modeling Approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses Accounting for the interaction of random oriented phases with fibers having preferential orientation.
Ring–Ring Equilibration in Solid, Even-Numbered Cyclic Poly(l-lactide)s and their Stereocomplexes
(2020)
Even-numbered cyclic poly(d-lactide) and poly(l-lactide) are prepared by ringexpansion polymerization. The cyclic pol(l-lactide) is annealed either at 120 or at 160 °C for several days. The progress of transesterification in the solid state is monitored by the formation of odd-numbered cycles via matrix-assisted laser desorption/ionization-time of flight mass spectrometry. The changes of the crystallinity are monitored by differential scanning calorimetry, wideand small-angle x-ray scattering (WAXS and SAXS) measurements. Despite total even-odd equilibration at 160 °C, the crystallinity of poly(l-lactide) is not reduced. Furthermore, the crystallinity of the stereocomplexes of both cyclic polylactides do not decrease or vanish, as expected, when a blocky or random stereosequence is formed by transesterification. This conclusion is confirmed by 13C NMR spectroscopy. These measurements demonstrate that transesterification is a ring–ring equilibration involving the loops on the surfaces of the lamellar crystallites thereby improving crystallinity and 3D packing of crystallites without significant broadening of the molecular weight distribution.
Cyclic poly(L-lactide)s were prepared by ring-opening polymerization combined with simultaneous polycondensation (ROPPOC) in bulk at 160 ° with dibutyltin bis(4-cyanophenoxide) as catalyst. It is demonstrated by MALDI TOF mass spectrometry and 1H NMR end group analyses that cycles are formed by endto-end cyclization in addition to “back-biting” transesterification. Formation of high molar mass cyclic poly L-lactide)s by means of several more reactive ROPPOC catalysts presented previously and in new experiments is discussed. These experimental results, together with theoretical arguments, prove that part of the Jacobson–Stockmayer theory is wrong. The critical monomer concentration, above which end-toend cyclization is seemingly impossible, does not exist and reversible like irreversible polycondensations can theoretically proceed up to 100% conversion, so that finally all reaction products will necessarily adopt a cyclic architecture.
The catalytic behavior of iron phthalocyanine (FePc)-sensitized magnetic nanocatalysts was evaluated for their application in the oxidative treatment of Bisphenol A (BPA) under mild environmental conditions. Two types of FePc (Fe(II)Pc and Fe(III)Pc), which are highly photosensitive compounds, were immobilized on the surface of functionalized magnetite. The nanomaterials were characterized by high resolution transmission electron microscopy (HR-TEM), X-ray difraction (XRD), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analyses (TGA). The generation of singlet Oxygen by nanomaterials was also investigated. In the presence of UVA light exposure (365nm) and 15mM H2O2, the M@Fe(III)Pc photocatalyst gave the best results; for a catalyst concentration of 2.0gL −1, around 60% BPA was removed after 120min of reaction. These experimental conditions were further tested under natural solar light exposure, for which also M@Fe(III)Pc exhibited enhanced oxidative catalytic activity, being able to remove 83% of BPA in solution. The water samples were less cytotoxic after treatment, this being confrmed by the MCF-7 cell viability assay.
Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature
(2020)
The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products.
Welding of 13CrMoV9-10 vanadium steel requires care due to an increased susceptibility to stress relief cracking during post weld heat treatment. Previous research into the crack formation in creep-resistant steels has focused on thermal and metallurgical factors; however, little knowledge has been gathered regarding the crack formation during post weld heat treatment considering real-life restraint conditions. This work is subdivided in two parts. Part I showed that an increasing heat input during submerged arc welding under restraint led to an increasing stress level in the joint prior to the post weld heat treatment. The magnitude of stress relief cracking observed in the heat-affected zone after the post weld heat treatment is affected by the heat input. In Part II of this work, the cracks and the associated microstructure which occurred under restraint were studied. The application of a Special acoustic emission analysis indicated that the cracks formed in a temperature range between 300 and 500 °C during the post weld heat treatment. The toughness in the heat-affected zone of the restrained welds was affected by the welding heat input.
Microstructural analyses of all specimens revealed accelerated aging due to precipitation of carbides during post weld heat treatment under restraint.
The avoidance of failures during the fabrication or operation of petrochemical reactors made of creep-resistant, low-alloy steels as 13CrMoV9-10 requires still research despite over 60 years of international investigations in the field of stress relief cracking. The quality of modern base materials and filler metals leads to the fact that previously known crack causes, such as impurities of S or P, recede into the background. Rather, the causes are increasingly to be found in the fabrication process. Investigations on the influence of heat control on the stresses in welded components and thus on the stress relief cracking sensitivity under realistic manufacturing conditions are not yet available. This work is subdivided in two parts. Part 1 of this study focused on the effect of heat control during submerged arc welding on the stresses. For this purpose, a testing facility was applied, which allows to observe the forces and moments accumulating during welding or heat treatment in a component-like specimen under shrinkage restraint. The stress acting in the specimen increases with higher preheat/interpass temperatures and higher heat input. During the heat treatment, the stresses are relieved. Nevertheless, cracks are formed already during heating. The total crack length correlates with the heat input.
Thermographic reconstruction of defects that lie in the bulk of a sample is a difficult task because entropy production during heat diffusion leads to information loss. To reconstruct defects one has to solve an inverse heat conduction problem. The quality of the reconstruction is closely related to the information content of the observed data set that is reflected by the decreasing ability to spatially resolve a defect with growing defect depth. In this work we show a 2D reconstruction of rectangular slots with different width-to-depth ratios in a metallic sample. For this purpose, we apply the virtual wave concept and incorporate positivity and sparsity as prior information to overcome the diffusion-based information loss partially. The reconstruction is based on simulated and experimental pulse thermography data. In the first reconstruction step, we compute a virtual wave field from the surface temperature data. This allows us, in the second step, to use ultrasonic backpropagation methods for image reconstruction.
Heterodyne Eddy Current Testing Using Magnetoresistive Sensors for Additive Manufacturing Purposes
(2020)
In recent years additive manufacturing technologies have become widely popular. For complex functional components or low volume production of workpieces, laser powder bed fusion can be used. High safety requirements, e.g. in the aerospace sector, demand extensive quality control. Therefore, offline non-destructive testing methods like computed tomography are used after manufacturing. Recently, for enhanced profitability and practicality online non-destructive testing methods, like optical tomography have been developed. This paper discusses the applicability of eddy current testing with magnetoresistive sensors for laser powder bed fusion parts. For this purpose, high spatial resolution giant magnetoresistance arrays are utilized for testing in combination with a single wire excitation coil. A heterodyne principle minimizes metrology efforts. This principle is compared to conventional signal processing in an eddy current testing setup using an aluminum test sample with artificial surface defects. To evaluate the influence of the powder used in the manufacturing process on eddy current testing and vice versa, a laser powder bed fusion mock-up made from stainless steel powder (316L) is used with artificial surface defects down to 100 µm. This laser powder bed fusion specimen was then examined using eddy current testing and the underlying principles.
Currently, sulfate-reducing bacteria (SRB) is regarded as the main culprit of microbiologically influenced corrosion (MIC), mainly due to the low reported corrosion rates of other microorganisms. For example, the highest reported corrosion rate for methanogens is 0.065 mm/yr. However, by investigating methanogen-induced microbiologically influenced corrosion (Mi-MIC) using an in-house developed versatile multiport flow test column, extremely high corrosion rates were observed. We analyzed a large set of carbon steel beads, which were sectionally embedded into the test columns as substrates for iron-utilizing methanogen Methanobacterium IM1. After 14 days of operation using glass beads as fillers for section separation, the highest average corrosion rate of Methanobacterium IM1 was 0.2 mm/yr, which doubled that of Desulfovibrio ferrophilus IS5 and Desulfovibrio alaskensis 16109 investigated at the same conditions. At the most corroded region, nearly 80% of the beads lost 1% of their initial weight (fast-corrosion), resulting in an average corrosion rate of 0.2 mm/yr for Methanobacterium IM1-treated columns. When sand was used as filler material to mimic sediment conditions, average corrosion rates for Methanobacterium IM1 increased to 0.3 mm/yr (maximum 0.52 mm/yr) with over 83% of the beads having corrosion rates above 0.3 mm/yr. Scanning electron images of metal coupons extracted from the column showed methanogenic cells were clustered close to the metal surface. Methanobacterium IM1 is a hydrogenotrophic methanogen with higher affinity to metal than H2. Unlike SRB, Methanobacterium IM1 is not restricted to the availability of sulfate concentration in the environment. Thus, the use of the multiport flow column provided a new insight on the corrosion potential of methanogens, particularly in dynamic conditions, that offers new opportunities for monitoring and development of mitigation strategies. Overall, this study shows under certain conditions methanogenic archaea can cause higher corrosion than SRB, specific quantifications, i.e., maximum, average, and minimum corrosion rates can be determined, and that spatial statistical evaluations of MIC can be carried out.
On the influence of crystallography on creep of circular notched single crystal superalloy specimens
(2020)
The present work contributes to a better understanding of the effect of stress multiaxiality on the creep behavior of single crystal Ni-base superalloys. For this purpose we studied the creep deformation and rupture behavior of double notched miniature creep tensile specimens loaded in three crystallographic directions [100], [110] and [111] (creep conditions: 950 °C and 400 MPa net section stress). Crystal plasticity finite element method (CPFEM) was used to analyze the creep stress and strain distributions during creep. Double notched specimens have the advantage that when one notch fails, the other is still intact and allows to study a material state which is close to rupture. No notch root cracking was observed, while microstructural damage (pores and micro cracks) were frequently observed in the center of the notch root region. This is in agreement with the FEM results (high axial stress and high hydrostatic stress in the center of the notched specimen). Twinning was observed in the notch regions of [110] and [111] specimens, and <112> {111} twins were detected and analyzed using orientation imaging scanning electron microscopy. The present work shows that high lattice rotations can be detected in SXs after creep fracture, but they are associated with the high strains accumulated in the final rupture event.
The subject of this study is how, and to what extent, Varestraint/Transvarestraint test results are influenced by both testing parameters and characteristics of evaluation methods. Several different high-alloyed martensitic LTT (low Transformation temperature) filler materials, CrNi and CrMn type, were selected for examination due to their rather distinctive solidification cracking behaviour, which aroused interest after previous studies. First, the effects of different process parameter sets on the solidification cracking response were measured using standard approaches. Subsequently, microfocus X-ray computer tomography (μCT) scans were performed on the specimens. The results consistently show sub-surface cracking to significant yet varying extents. Different primary solidification types were found using wavelength dispersive X-ray (WDX) analysis conducted on filler metals with varying Cr/Ni equivalent ratios. This aspect is regarded as the main difference between the CrNiand CrMn-type materials in matters of cracking characteristics. Results show that when it comes to testing of modern highperformance alloys, one set of standard Varestraint testing parameters might not be equally suitable for all materials. Also, to properly accommodate different solidification types, sub-surface cracking has to be taken into account.
The interaction of different charged polymers, namely anionic polycarboxylate
superplasticizer (PCE) and neutral polyethylene glycol (PEG) with potassium ions, and their effect on the yield stress of highly concentrated glass bead suspension (GBS), were studied under different concentrations of potassium ions ([K+]). It was found that, compared to the neutral PEG, the negatively charged PCE can be adsorbed on glass beads (GB), and then decreases the yield stress of GBS. The increasing concentration of free polymer in the interstitial liquid phase with the increased polymer dosage leads to the higher yield stress of GBS, which may be caused by the higher Depletion force. In addition, this effect is also related to the charge density of the polymer and the [K+] in the solution. Along with the increase in [K+], the yield stress of GBS increases significantly with the addition of PCE, but this cannot be observed with PEG, which indicates that potassium ions can interact with negatively charged PCE instead of the neutral PEG. At last, the interparticle Forces between two single GB with adsorbed PCE in solutions containing [K+] and PCE were measured by colloidal probe atomic force microscopy to better understand the interaction of the charged polymer with counterions.
An ultrasonic vibration post-treatment procedure was suggested for additively manufac-tured lattices. The aim of the present research was to investigate mechanical properties andthe differences in mechanical behavior and fracture modes of Ti6Al4V scaffolds treated withtraditional powder recovery system (PRS) and ultrasound vibration (USV). Scanning electronmicroscopy (SEM) was used to investigate the strut surface and the fracture surface mor-phology. X-ray computed tomography (CT) was employed to evaluate the inner structure,strut dimensions, pore size, as well as the surface morphology of additively manufacturedporous scaffolds. Uniaxial compression tests were conducted to obtain elastic modulus,compressive ultimate strength and yield stress. Finite element analysis was performedfor a body-centered cubic (BCC) element-based model and for CT-based reconstructiondata, as well as for a two-zone scaffold model to evaluate stress distribution during elasticdeformation. The scaffold with PRS post treatment displayed ductile behavior, while USVtreated scaffold displayed fragile behavior. Double barrel formation of PRS treated scaffoldwas observed during deformation. Finite element analysis for the CT-based reconstructionrevealed the strong impact of surface morphology on the stress distribution in comparisonwith BCC cell model because of partially molten metal particles on the surface of struts,which usually remain unstressed.
Nanotechnology has enabled the discovery of a multitude of novel materials exhibiting unique physicochemical (PChem) properties compared to their bulk analogues. These properties have led to a rapidly increasing range of commercial applications; this, however, may come at a cost, if an association to long-term health and environmental risks is discovered or even just perceived. Many nanomaterials (NMs) have not yet had their potential adverse biological effects fully assessed, due to costs and time constraints associated with the experimental assessment, frequently involving animals. Here, the available NM libraries are analyzed for their suitability for integration with novel nanoinformatics approaches and for the development of NM specific Integrated Approaches to Testing and Assessment (IATA) for human and environmental risk assessment, all within the NanoSolveIT cloud-platform. These established and well-characterized NM libraries (e.g. NanoMILE, NanoSolutions, NANoREG, NanoFASE, caLIBRAte, NanoTEST and the Nanomaterial Registry (>2000 NMs)) contain physicochemical characterization data as well as data for several relevant biological endpoints, assessed in part using harmonized Organisation for Economic Co-operation and Development (OECD) methods and test guidelines.
Integration of such extensive NM information sources with the latest nanoinformatics methods will allow NanoSolveIT to model the relationships between NM structure (morphology), properties and their adverse effects and to predict the effects of other NMs for which less data is available. The project specifically addresses the needs of regulatory agencies and industry to effectively and rapidly evaluate the exposure, NM hazard and risk from nanomaterials and nano-enabled products, enabling implementation of computational ‘safe-by-design’ approaches to facilitate NM commercialization.
Laser material processing is an emerging technology that generates surface functionalities on the basis of optical, mechanical, or chemical properties. In the form of laser surface texturing (LST), it has attracted a remarkable amount of research to tailor surface properties towards various tribological applications. The main advantages of this single-step, laser-based technology are the contactless machining, featuring a high flexibility, efficiency, and speed, along with the excellent quality of the processed products. LST can be applied precisely localized to sub-micrometric areas, but, via laser beam scanning, it is also feasible for structuring large surface areas at the square meter size.
This Special Issue focuses on the latest developments concerning the tribological performance of laser-generated periodic surface nano- and microstructures and their applications. This includes the laser-based processing of different surface patterns, such as “self-organized” laser-induced periodic surface structures (LIPSS, ripples), grooves, micro-spikes, hierarchical hybrid nano-/micro-structures, microfeatures generated by direct laser interference patterning (DLIP), or even dimples or other topographic geometries shaped by direct laser modification or ablation. The applications of these periodically nano- and micro-patterned surfaces may improve the lubricated or non-lubricated tribological performance of surfaces in conformal and even non-conformal contact through a reduction of wear, a variation of the coefficient of friction, altered load carrying capacity, etc., resulting in energy saving, improved reliability, increased lifetimes as well as durability, leading in turn to extended maintenance intervals/reduced down-time. This can be beneficial in terms of bearings, gears, engines, seals, cutting tools, or other tribological components. Fundamental aspects addressed may involve the investigation of the relevant physical and chemical effects accompanying the laser-generated nano- and microscale topographies, such as alterations of the material structures, the hardness, superficial oxidation, the role of additives contained in lubricants, surface wettability, micro-hydrodynamic effects, etc.
For this Special Issue we aim to attract both academic and industrial researchers and would like to provide a bridge between research in the fields of tribology and laser material processing in order to foster the current knowledge and present new ideas for future applications and new technologies.
Ectoine is a small zwitterionic osmolyte and compatible solute, which does not interfere with cell metabolism even at molar concentrations. Plasmid DNA (pUC19) was irradiated with ultraviolet radiation (UV-C at 266 nm) under quasi physiological conditions (PBS) and in pure water in the presence and absence of ectoine (THP(B)) and hydroxyectoine (THP(A)). Different types of UV induced DNA damage were analysed: DNA single-strand breaks (SSBs), abasic sites and cyclobutane pyrimidine dimers (CPDs). A complex interplay between these factors was observed with respect to the nature and occurrence of DNA damage with 266 nm photons. In PBS, the cosolutes showed efficient protection against base damage, whilst in pure water, a dramatic shift from SSB damage to base damage was observed when cosolutes were added. To test whether these effects are caused by ectoine binding to DNA, further experiments were conducted: small-angle X-ray scattering (SAXS), surface-plasmon resonance (SPR) measurements and Raman spectroscopy. The results show, for the first time, a close interaction between ectoine and DNA. This is in stark contrast to the assumption made by preferential exclusion models, which are often used to interpret the behaviour of compatible solutes within cells and with biomolecules. It is tentatively proposed that the alterations of UV damage to DNA are attributed to ectoine influence on nucleobases through the direct interaction between ectoine and DNA.
Material defects in fiber reinforced polymers such as delaminations can rapidly degrade the material properties or can lead to the failure of a component. Pulse thermography (PT) has proven to be a valuable tool to identify and quantify such defects in opaque materials. However, quantification of delaminations within semitransparent materials is extremely challenging. We present an approach to quantify delaminations within materials being semitransparent within the wavelength ranges of the optical excitation sources as well as of the infrared (IR) camera. PT experimental data of a glass fiber reinforced polymer with a real delamination within the material were reconstructed by one dimensional (1D) mathematical models. These models describe the heat diffusion within the material and consider semitransparency to the excitation source as well to the IR camera, thermal losses at the samples surfaces and a thermal contact resistance between the two layers describing the delamination. By fitting the models to the PT data, we were able to determine the depth of the delamination very accurately. Additionally, we analyzed synthetic PT data from a 2D simulation with our 1D-models to show how the thermal contact resistance is influenced by lateral heat flow within the material.
This paper reports results from in situ electrochemical X-ray absorption near-edge spectroscopy (XANES) studies of the corrosion processes on model thin iron films in the presence of iron reducing bacteria Shewanella putrefaciens. Here we investigate the electrochemical activity of two cultures grown in the presence and absence of Fe(III) citrate in the culture medium. The XANES spectra and the OCP data of the Fe sample incubated with the culture grown in absence of Fe(III) did not show any significant changes during twenty hours of monitoring. In the case of the culture grown in Fe(III) containing medium, an accelerated dissolution of the iron film was observed together with the formation of a mixed Fe(II)-Fe(III) hydroxide surface layer. The open circuit potential (OCP) steadily approached the free corrosion potential of iron in neutral chloride containing electrolytes, indicating a continuous dissolution process without passivation.
Ultrashort pulse laser processing of materials allows for precise machining with high accuracy. By increasing the repetition rate to several 100 kHz, laser machining becomes quick and cost-effective. Ultrafast laser processing at high repetition rates and peak intensities above 10^13 W/cm^2 can cause a potential hazard by generation of unwanted x-ray radiation. Therefore, radiation protection must be considered. For 925 fs pulse duration at a center wavelength of 1030 nm, the x-ray emission in air at a repetition rate of 400 kHz was investigated up to a
peak intensity of 2.6 × 10^14 W/cm^2. Based on the presented measurements, the properties of potential shielding materials will be discussed. By extending our previous works, a scaling of the x-ray radiation emission to higher peak intensities up to 10^15 W/cm^2 is described, and emitted x-ray doses are predicted.
In this contribution, chemical, structural, and mechanical alterations in various types of femtosecond laser-generated surface structures, i.e., laser-induced periodic surface structures (LIPSS, ripples), Grooves, and Spikes on titanium alloy, are characterized by various surface analytical techniques, including X-ray diffraction and glow-discharge optical emission spectroscopy. The formation of oxide layers of the different laser-based structures inherently influences the friction and wear performance as demonstrated in oil-lubricated reciprocating sliding tribological tests (RSTTs) along with subsequent elemental mapping by energy-dispersive X-ray analysis. It is revealed that the fs-laser scan processing (790 nm, 30 fs, 1 kHz) of near-wavelength-sized LIPSS leads to the formation of a graded oxide layer extending a few hundreds of nanometers into depth, consisting mainly of amorphous oxides. Other superficial fs-laser-generated structures such as periodic Grooves and irregular Spikes produced at higher fluences and effective number of pulses per unit area present even thicker graded oxide layers that are also suitable for friction reduction and wear resistance. Ultimately, these femtosecond laser-induced nanostructured surface layers efficiently prevent a direct metal-to-metal contact in the RSTT and may act as an anchor layer for specific wear-reducing additives contained in the used engine oil.
The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually referred to as ANFO, is extensively used in the mining industry as a bulk explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the complex pore structure of the AN prills. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. Importantly, oil retention measurements (qualifying the efficiency of ANFO as explosives) correlate well with the specific surface area determined by XCT. XCT can therefore be employed non-destructively; it can accurately evaluate and characterise porosity in ammonium nitrate prills, and even predict their efficiency.
Hydrocarbons fuel our economy. Furthermore, intermediate goods and consumer products are often hydrocarbon-based. Beside all the progress they made possible, hydrogen-containing substances can have severe detrimental effects on materials exposed to them. Hydrogen-assisted failure of iron alloys has been recognised more than a century ago. The present study aims to providing further insight into the degradation of the austenitic stainless steel AISI 304L (EN 1.4307) exposed to hydrogen. To this end, samples were electrochemically charged with the hydrogen isotope deuterium (2H, D) and analysed by scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). It was found that deuterium caused a phase transformation from the original γ austenite into ε- and α’-martensite. Despite their low solubility for hydrogen, viz. deuterium, the newly formed phases showed high deuterium concentration which was attributed to the increased density of traps. Information about the behaviour of deuterium in the material subjected to external mechanical load was gathered. A four-point-bending device was developed for this purpose. This allowed to analyse in-situ pre-charged samples in the ToF-SIMS during the application of external mechanical load. The results indicate a movement of deuterium towards the regions of highest stress.
Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation.
We describe and demonstrate a novel experimental approach to measure broadband, amplitude- and phase-resolved scattering spectra of single nanoparticles with 10-nm spatial resolution. Nanofocusing of Surface plasmon polaritons (SPPs) propagating along the shaft of a conical gold taper is used to create a spatially isolated, spectrally broad nanoscale light source at ist very apex. The interference between these incident SPPs and SPPs that are backpropagating from the apex leads to the formation of an inherently phase-stable interferogram, which we detect in the far field by partially scattering SPPs off a small protrusion on the taper shaft. We show that these interferograms allow the reconstruction of both the amplitude and phase of the local optical near fields around individual nanoparticles optically coupled to the taper apex. We extract local light scattering spectra of particles and quantify line broadenings and spectral shifts induced by tip-sample coupling. Our experimental findings are supported by corresponding finite-difference time-domain and coupled dipole simulations and Show that, in the limit of weak tip-sample coupling, the measurements directly probe the projected local density of optical states of the plasmonic system. The combination of a highly stable inline interferometer with the inherent optical background suppression through nanofocusing makes it a promising tool for the locally resolved study of the spectral and temporal optical response of coupled hybrid nanosystems.
Separation technology as a sub-discipline of thermal process engineering is one of the most critical steps in the production of chemicals, essential for the quality of intermediate and end products.
The discipline comprises the construction of facilities that convert raw materials into value-added products along the value chain. Conversions typically take place in repeated reaction and separation steps—either in batch or continuous processes. The end products are the result of several production and separation steps that are not only sequentially linked, but also include the treatment of unused raw materials, by-products and wastes. Production processes in the process industry are particularly susceptible to fluctuations in raw materials and other influences affecting product quality. This is a challenge, despite increasing fluctuations, to deliver targeted quality and simultaneously meet the increasing dynamics of the market, at least for high value fine chemicals. In order to survive successfully in a changed environment, chemical companies must tread new paths. This includes the potential of digital technologies. The full integration and intelligent networking of systems and processes is progressing hesitantly. This contribution aims to encourage a more holistic approach to the digitalization in thermal process engineering by introduction of integrated and networked systems and processes.
Municipal solid waste incineration (MSWI) is one of the leading technologies for municipal solid waste (MSW) treatment in Europe. Incineration bottom ash (IBA) is the main solid residue from MSWI, and its annual European production is about 20 million tons. The composition of IBA depends on the composition of the incinerated waste; therefore, it may contain significant amounts of ferrous and non-ferrous (NFe) metals as well as glass that can be recovered. Technologies for NFe metals recovery have emerged in IBA treatment since the 1990s and became common practice in many developed countries. Although the principles and used apparatus are nearly the same in all treatment trains, the differences in technological approaches to recovery of valuable components from IBA – with a special focus on NFe metals recovery – are summarized in this paper.
The analysis of pollen chemical composition is important to many fields, including agriculture, plant physiology, ecology, allergology, and climate studies. Here, the potential of a combination of different spectroscopic and spectrometric methods regarding the characterization of small biochemical differences between pollen samples was evaluated using multivariate statistical approaches. Pollen samples, collected from three populations of the grass Poa alpina, were analyzed using Fourier-transform infrared (FTIR) spectroscopy, Raman spectroscopy, surface enhanced Raman scattering (SERS), and matrix assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS). The variation in the sample set can be described in a hierarchical framework comprising three populations of the same grass species and four different growth conditions of the parent plants for each of the populations. Therefore, the data set can work here as a model system to evaluate the classification and characterization ability of the different spectroscopic and spectrometric methods. ANOVA Simultaneous Component Analysis (ASCA) was applied to achieve a separation of different sources of variance in the complex sample set. Since the chosen methods and sample preparations probe different parts and/or molecular constituents of the pollen grains, complementary information about the chemical composition of the pollen can be obtained. By using consensus principal component analysis (CPCA), data from the different methods are linked together. This enables an investigation of the underlying global information, since complementary chemical data are combined. The molecular information from four spectroscopies was combined with phenotypical information gathered from the parent plants, thereby helping to potentially link pollen chemistry to other biotic and abiotic parameters.
Mechanical flexibility in single crystals of covalently bound materials is a fascinating and poorly understood phenomenon. We present here the first example of a plastically flexible one-dimensional (1D) coordination polymer. The compound [Zn(m-Cl)2(3,5-dichloropyridine)2]n is flexible over two crystallographic faces. Remarkably, the single crystal remains intact when bent to 1808. A combination of microscopy, diffraction, and spectroscopic studies have been used to probe the structural response of the crystal lattice to mechanical bending. Deformation of the covalent polymer chains does not appear to be responsible for the observed macroscopic bending. Instead, our results suggest that mechanical bending occurs by displacement of the coordination polymer chains. Based on experimental and theoretical evidence, we propose a new model for mechanical flexibility in 1D coordination polymers. Moreover, our calculations propose a cause of the different mechanical properties of this compound and a structurally similar elastic material
Spatial heterodyne spectroscopy (SHS) is a novel spectral analysis technique that is being applied for Raman spectroscopy of minerals. This paper presents the theoretical basis of SHS and its application for Raman measurements of calcite, quartz and forsterite in marble, copper ore and nickel ore, respectively. The SHS measurements are done using a broadband (518–686 nm) and resolving power R ≈ 3000 instrument. The spectra obtained using SHS are compared to those obtained by benchtop and modular dispersive spectrometers. It is found that SHRS performance in terms of resolution is comparable to that of the benchtop spectrometer and better than the modular dispersive spectrometer, while the sensitivity of SHRS is worse than that of a benchtop spectrometer, but better than that of a modular dispersive spectrometer. When considered that SHS components are small and can be packaged into a handheld device, there is interest in developing an SHS-based Instrument for mobile Raman spectroscopy. This paper evaluates the possibility of such an application.
The quantitative analysis of microstructural features is a key to understanding the micromechanical behavior of metal matrix composites (MMCs), which is a premise for their use in practice. Herein, a 3D microstructural characterization of a five-phase MMC is performed by synchrotron X-ray computed tomography (SXCT). A workflow for advanced deep learning-based segmentation of all individual phases in SXCT data is shown using a fully convolutional neural network with U-net architecture. High segmentation accuracy is achieved with a small amount of training data. This enables extracting unprecedently precise microstructural parameters (e.g., volume fractions and particle shapes) to be input, e.g., in micromechanical models.
Numerous new tin catalysts that enable the synthesis of cyclic polylactides with broad variation in their molecular mass were recently developed. The abundance of cyclics in matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectra is, however, frequently reported to greatly exceed that of linears. Thus, the MALDI ionization behavior of various end-capped linear poly(L-lactide)s and one cyclic poly(L-lactide) was investigated and compared.
Neat compounds and various blends of cyclic and linear species were prepared and studied under identical conditions with regard to sample preparation and instrumental condition, except for the laser power. For this purpose, two different MALDI-TOF mass spectrometers were applied.
Our results reveal that cyclics indeed show a slightly better ionization in MALDI, although their ionization as a neat compound seems to be less effective than that of linear polylactides. The ionization of most linear polylactides investigated does not depend on the end group structure. However, linear polylactides containing 12-bromododecyl end groups reveal an unexpected saturation effect that is not caused by fragmentation of the polymer or the end group, or by electronic saturation of the detector digitizer. Furthermore, polylactides with a 2-bromoethyl end group did not show such a saturation effect.
An overestimation of cyclic species in MALDI-TOF mass spectra of poly(L-lactide)s must be considered, but the commonly assumed peak suppression of linear polymers in mixtures of both structures can be excluded.
Many standardised durability testing methods have been developed for Portland cement-based concretes, but require validation to determine whether they are also applicable to alkali-activated materials. To address this question, RILEM TC 247-DTA ‘Durability Testing of Alkali-Activated Materials’ carried out round robin testing of carbonation and chloride penetration test methods, applied to five different alkali-activated concretes based on fly ash, blast furnace slag or metakaolin. The methods appeared overall to demonstrate an intrinsic precision comparable to their precision when applied to conventional concretes. The ranking of test outcomes for pairs of concretes of similar binder chemistry was satisfactory, but rankings were not always reliable when comparing alkali-activated concretes based on different precursors. Accelerated carbonation testing gave similar results for fly ash-based and blast furnace slag-based alkali-activated concretes, whereas natural carbonation testing did not. Carbonation of concrete specimens was observed to have occurred already during curing, which has implications for extrapolation of carbonation testing results to longer service life periods. Accelerated chloride penetration testing according to NT BUILD 443 ranked the tested concretes consistently, while this was not the case for the rapid chloride migration test. Both of these chloride penetration testing methods exhibited comparatively low precision when applied to blast furnace slag-based concretes which are more resistant to chloride ingress than the other materials tested.
The suitability of common analytical methods for the determination of active substances from wood preservatives in aged wood samples was investigated during an interlaboratory study. Permethrin, propiconazole and tebuconazole were quantified in 1.5 and 8 year-old wood samples by gas chromatography and liquid chromatography. Generally, the applied Methods yielded reliable results for these samples. However, wood components can coelute with propiconazole and tebuconazole during liquid chromatography. Optimization of separation might be required if UV detection is applied.
Current and future requirements to industrial analytical infrastructure—part 2: smart sensors
(2020)
Complex processes meet and need Industry 4.0 capabilities. Shorter product cycles, flexible production needs, and direct assessment of product quality attributes and raw material attributes call for an increased need of new process analytical technologies (PAT) concepts. While individual PAT tools may be available since decades, we need holistic concepts to fulfill above industrial needs. In this series of two contributions, we want to present a combined view on the future of PAT (process analytical technology), which is projected in smart labs (Part 1) and smart sensors (Part 2). Part 2 of this feature article series describes the future functionality as well as the ingredients of a smart sensor aiming to eventually fuel full PAT functionality. The smart sensor consists of (i) chemical and process information in the physical twin by smart field devices, by measuring multiple components, and is fully connected in the IIoT 4.0 environment. In addition, (ii) it includes process intelligence in the digital twin, as to being able to generate knowledge from multi-sensor and multi-dimensional data. The cyber-physical system (CPS) combines both elements mentioned above and allows the smart sensor to be self-calibrating and self-optimizing. It maintains its operation autonomously. Furthermore, it allows—as central PAT enabler—a flexible but also target-oriented predictive control strategy and efficient process development and can compensate variations of the process and raw material attributes. Future cyber-physical production systems—like smart sensors—consist of the fusion of two main pillars, the physical and the digital twins. We discuss the individual elements of both pillars, such as connectivity, and chemical analytics on the one hand as well as hybrid models and knowledge workflows on the other. Finally, we discuss its integration needs in a CPS in order to allow is versatile deployment in efficient process development and advanced optimum predictive process control.
The competitiveness of the chemical and pharmaceutical industry is based on ensuring the required product quality while making optimum use of plants, raw materials, and energy. In this context, effective process control using reliable chemical process analytics secures global competitiveness. The setup of those control strategies often originate in process development but need to be transferable along the whole product life cycle. In this series of two contributions, we want to present a combined view on the future of PAT (process analytical technology), which is projected in smart labs (part 1) and smart sensors (part 2). In laboratories and pilot plants, offline chemical analytical methods are frequently used, where inline methods are also used in production. Here, a transferability from process development to the process in operation would be desirable. This can be obtained by establishing PAT methods for production already during process development or scale-up. However, the current PAT (Bakeev 2005, Org Process Res 19:3–62; Simon et al. 2015, Org Process Res Dev 19:3–62) must become more flexible and smarter. This can be achieved by introducing digitalization-based knowledge management, so that knowledge from product development enables and accelerates the integration of PAT. Conversely, knowledge from the production process will also contribute to product and process development. This contribution describes the future role of the laboratory and develops requirements therefrom. In part 2, we examine the future functionality as well as the ingredients of a smart sensor aiming to eventually fuel full PAT functionality—also within process development or scale-up facilities (Eifert et al. 2020, Anal Bioanal Chem).
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.
We present here our methodological approach applied to the study of Egyptian inks in Late Antiquity. It is based on an interdisciplinary strategy, bringing together a variety of disciplines from humanities and natural sciences, and it aims at systematically collecting a statistically relevant amount of data regarding the composition of the inks. The application of a wellestablished, non-invasive protocol that includes near-infrared imaging and X-ray fluorescence spectroscopy for in situ measurements enables the identification and characterisation of inks dating from the end of Late Antiquity onwards. However, sometimes this method limits our understanding when characterising more ancient inks. Trying to overcome these limitations, the potential of a new device for the characterisation of organic compounds is here explored by conducting preliminary tests on mock samples.
In this work, we present the results from 77 codicological units that include some of the earliest manuscripts of our corpus that presently lists 159 units.