Sepiolite-PAN intercalation used as Si3N4 forming precursor

Silicon nitride (Si₃N₄) formation was investigated using sepiolite and polyacrylonitrile as silicon and carbon source, respectively. It was found that purified sepiolite could readily adsorb a sufficient amount of acrylonitrile (AN) reagent without pre-treatment. Polymerisation of sepiolite-AN mixtures and subsequent cyclization of the polymerised complex yielded a precursor, which was found ideal as a starting material in carbothermal reduction-nitridation (CRN) for the formation of silicon nitride powders. The quantity of silicon nitride, grain size and morphology were found to be dependent on the reaction conditions and starting reagent. Fine grain size, high surface area (up to approx. 12.4 m²/g) powders of mainly -Si₃N₄ were obtained via pyrolysis of sepiolite-PAN complex after 4 h heating at 1400°C in 1000 ml/min nitrogen flow with a heating rate of 300°C/h. Mg retained in the molecular structure of the mineral must have promoted the formation of -grains in CRN process.     

Broadband detection electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry to reveal enzymatically and chemically induced deamidation reactions within peptides.

Among the numerous forms of chemical degradation of peptides or proteins, deamidation is one of the alterations observed most frequently. In this irreversible reaction, a glutamine or an asparagine side chain is hydrolyzed to glutamic acid or aspartic acid, respectively (conversion of NH2 to OH). Besides its influence in the deterioration of biotechnological and food products, deamidation represents a defined posttranslational modification reaction with respect to proteomics. Here mass spectrometric techniques play a leading role in determining posttranslational modifications. However, not all mass spectrometers are able to resolve signal differences of 0.0193 Da (mass difference of 12CO vs 13CNH) for singly charged molecules, the mass difference between the first isotopic signal of an asparagine/glutamine-containing peptide and the monoisotopic signal of the corresponding partially deamidated aspartate/glutamate derivative. To detect partial deamidation within peptides, advantage has been taken of the ability of Fourier transform ion cyclotron resonance mass spectrometry to perform very high mass resolution. In this work, we investigated up to triply charged ions produced by electrospray ionization using direct infusion. Although the special heterodyne detection mode enables higher mass resolution than the routinely used broadband detection, often only a small mass window can be investigated. Using broadband detection, we were able to resolve ions with a difference of m/z 0.0064 to detect partially deamidated peptides formed either enzymatically or under acidic and basic conditions.     

Die Historizität der Verdatung: Konzepte,Werkzeuge und Praktiken im 19. Jahrhundert

This essay explores the use of the concept of “data” during the nineteenth century. It traces the development of manual data driven research decades before the introduction of Hollerith machines and electronic computers. Census statisticians in late-nineteenth century Prussia employed moveable paper tools to assemble numerical information in novel ways; their actions fundamentally recast processes of compilation. The paper considers the epistemic impact of moving data inscribed on tons of paper, reconstructing the logistics of a circulatory compilation system spread across the Prussian capital. The movement of data in Wilhelmine Berlin reached outward from the statistical bureau to encompass the homes of many women, enlisted in a minutely-orchestrated putting out system. The essay scrutinizes the social and intellectual requirements necessary to classify, sort, and aggregate the information on the loose paper slips fast and without error. For all of their inventiveness, Prussian statisticians were neither the first nor the only ones to gather, process and visualize data in imaginative ways. As this essay demonstrates, many so-called “Baconian” sciences developed similar tools and practices to those of Prussian statisticians. Making and moving data sparked historical sensitivity in disciplines well beyond population statistics, from taxonomy to paleontology, yielding unexpected revelations.     

Level set topology optimization of structural problems with interface cohesion

This paper presents a finite element topology optimization framework for the design of two‐phase structural systems considering contact and cohesion phenomena along the interface. The geometry of the material interface is described by an explicit level set method, and the structural response is predicted by the extended finite element method. In this work, the interface condition is described by a bilinear cohesive zone model on the basis of the traction‐separation constitutive relation. The non‐penetration condition in the presence of compressive interface forces is enforced by a stabilized Lagrange multiplier method. The mechanical model assumes a linear elastic isotropic material, infinitesimal strain theory, and a quasi‐static response. The optimization problem is solved by a nonlinear programming method, and the design sensitivities are computed by the adjoint method. The performance of the presented method is evaluated by 2D and 3D numerical examples. The results obtained from topology optimization reveal distinct design characteristics for the various interface phenomena considered. In addition, 3D examples demonstrate optimal geometries that cannot be fully captured by reduced dimensionality. The optimization framework presented is limited to two‐phase structural systems where the material interface is coincident in the undeformed configuration, and to structural responses that remain valid considering small strain kinematics. Copyright © 2017 John Wiley & Sons, Ltd.     

The periodic tableau: Form and colours in the first 100 years

While symbolic colour use has always played a conspicuous role in science research and education, the use of colour in historic diagrams remains a lacuna in the history of science. Investigating the colour use in diagrams often means uncovering a whole cosmology that is not otherwise explicit in the diagram itself. The periodic table is a salient and iconic example of non‐mimetic colour use in science. Andreas von Antropoff's (1924) rectangular table of recurrent rainbow colours is famous, as are Alcindo Flores Cabral's (1949) application of colour in his round snail form, using the RGB scheme, and Mazurs's (1967) pine tree system, consisting of warm and cold colours that he attributed to specific groups of elements—an attribution that we can relate back to humoralism and alchemy. From the first periodic tables in the 19th century, individual researchers have used different colour regimes. While standardization may play an obvious role in chemistry and its diagrams, all the more impressive is the anarchistic use of colour in the various diagrams which continue to be created. This article focuses on periodic tables in chemical journals and text books, and explores and compares the development of colour codes found in the few existing polychrome diagrams from the 1920s to the 1970s.     

Laser beam melting of aluminum alloys with hull-core build strategy by using an initial meso-scale simulation

Laser beam melting (LBM) of aluminum alloys is gaining a wide popularity in different industrial applications as an alternative technology for the production of individual and complex parts. A long build time and the high amount of experimental work for optimizing or finding new process parameters are two of the current challenges for reaching an industrial maturity. This paper proposes an efficient way to determine new process parameters for aluminum alloy aluminum-silicon10-magnesium with highest build-up rates by using a 3D finite element model on the mesoscopic level. High laser power in combination with the hull-core build strategy was used to increase the build-up rate without impairing the part accuracy. The influences of high laser power, laser diameter and scan speed on the melt pool were studied by using a thermal simulation of single laser tracks. Based on the simulation results the process window could be derived and was tested on a laser beam melting (LBM) system. The achieved reduction of the build time of up to 31 % without loss in part accuracy proved the novel approach for the prediction of the required process window as an efficient method to reduce costly and time-consuming experimental work.     

Additive Manufacturing of Hard Magnetic Passive Shims to Increase Field Homogeneity of a Halbach Magnet

Obtaining a highly homogeneous magnetic field is desired for field-controlled applications. For example, the resolution of magnetic analysis methods can be improved by generating a stronger and more homogeneous field over the region of interest (ROI). A set of 3D-printed passive shims is fabricated using additive manufacturing to improve the magnetic field homogeneity of a Halbach magnet assembly. The feedstock is a custom acrylonitrile butadiene styrene (ABS)-hard magnet composite filament filled with 60% wt. isotropic NdFeB. Additionally, a method for investigating the remanence is developed and validated. The result reveals a good agreement between the new method and existing measurement techniques for the remanence of permanent magnets. It is also shown that the additive manufacturing procedure has negligible effects on the magnetic properties. Performing a parametric study over a rectangular ROI, an optimized shim configuration is achieved. In the optimized and 3D-printed configuration, the average norm of the magnetic flux density, B_norm, is increased by 13% and, more importantly, a 43% increase in the magnetic uniformity is obtained. These results highlight the great potential of freeform manufacturing, namely, additive manufacturing, to tailor the properties of magnet structures.     

Isothermal Hybridization Kinetics of DNA Assembly of Two‐Dimensional DNA Origami

The Watson–Crick base‐pairing with specificity and predictability makes DNA molecules suitable for building versatile nanoscale structures and devices, and the DNA origami method enables researchers to incorporate more complexities into DNA‐based devices. Thermally controlled atomic force microscopy in combination with nanomechanical spectroscopy with forces controlled in the pico Newton (pN) range as a novel technique is introduced to directly investigate the kinetics of multistrand DNA hybridization events on DNA origami nanopores under defined isothermal conditions. For the synthesis of DNA nanostructures under isothermal conditions at 60 °C, a higher hybridization rate, fewer defects, and a higher stability are achieved compared to room‐temperature studies. By quantifying the assembly times for filling pores in origami structures at several constant temperatures, the fill factors show a consistent exponential increase over time. Furthermore, the local hybridization rate can be accelerated by adding a higher concentration of the staples. The new insight gained on the kinetics of staple‐scaffold hybridization on the synthesis of two dimensional DNA origami structures may open up new routes and ideas for designing DNA assembly systems with increased potential for their application.     

Effect of chemical termination of self-assembled organic monolayers on the tip induced local anodic oxidation of silicon(100)

We evaluated the scanning probe microscope based anodization process of silicon(100) terminated by organic monolayers of the same thickness but with different surface properties. The surface energy of these monolayers with its dispersive and polar component was determined by contact angle measurements. We discovered that the anodization oxide characteristics depend ceteris paribus clearly on the surface properties of the sample. With an increased polar component, and therefore hydrophilic character of the surface, the formed oxide structures became broader and thinner. On the other hand a hydrophilic surface allowed the generation of oxide structures at higher tip velocities and lower applied voltages. The absolute amount of formed oxide is independent of the monolayer indicating a dominating influence of initially formed oxide on the following oxidation process.     

Ferromagnetism in Ga0.90Mn0.10As1 − yPy: From the metallic to the impurity band conduction regime

The magnetic properties of low temperature MBE grown Ga_0.90Mn_0.10As_1 − yP_y films with 0 < y < 0.20 have been studied as a function of the phosphorous content. The films are ferromagnetic for all phosphorous compositions. For y < 0.15 the conductivity type is metallic but above y > 0.15 it changes to impurity band conduction (IBC). In the IBC regime the main magnetic properties are profoundly modified: the saturation magnetization decreases from typically 50 emu/cm³ to 35 emu/cm³, the critical temperature drops sharply from 130 K to 45 K and the uniaxial magnetic anisotropy spectroscopy is strongly reduced.