Tailoring the morphology of self-assembled block copolymer hollow fiber membranes

Isoporous asymmetric polystyrene-block-poly(4-vinylpyridine) (PS-b-P4VP) hollow fiber membranes were successfully made by a dry-jet wet spinning process. Well-defined nanometer-scale pores around 20–40 nm in diameter were tailored on the top surface of the fiber above a non-ordered macroporous layer by combining block copolymer self-assembly and non-solvent induced phase separation (SNIPS). Uniformity of the surface-assembled pores and fiber cross-section morphology was improved by adjusting the solution concentration, solvent composition as well as some important spinning parameters such as bore fluid flow rate, polymer solution flow rate and air gap distance between the spinneret and the precipitation bath. The formation of the well-organized self-assembled pores is a result of the interplay of fast relaxation of the shear-induced oriented block copolymer chains, the rapid evaporation of the solvent mixture on the outer surface and solvent extraction into the bore liquid on the lumen side, and gravity force during spinning. Structural features of the block copolymer solutions were investigated by small-angle X-ray scattering (SAXS) and rheological properties of the solutions were examined as well. The scattering patterns of the optimal solutions for membrane formation indicate a disordered phase which is very close to the disorder-order transition. The nanostructured surface and cross-section morphology of the membranes were characterized by scanning electron microscopy (SEM). The water flux of the membranes was measured and gas permeation was examined to test the pressure stability of the hollow fibers.     

Nanoscale Analysis of a Hierarchical Hybrid Solar Cell in 3D

A quantitative method for the characterization of nanoscale 3D morphology is applied to the investigation of a hybrid solar cell based on a novel hierarchical nanostructured photoanode. A cross section of the solar cell device is prepared by focused ion beam milling in a micropillar geometry, which allows a detailed 3D reconstruction of the titania photoanode by electron tomography. It is found that the hierarchical titania nanostructure facilitates polymer infiltration, thus favoring intermixing of the two semiconducting phases, essential for charge separation. The 3D nanoparticle network is analyzed with tools from stochastic geometry to extract information related to the charge transport in the hierarchical solar cell. In particular, the experimental dataset allows direct visualization of the percolation pathways that contribute to the photocurrent.     

Quantitative matrix-assisted laser desorption ionization-time-of-flight mass spectrometry analysis of synthetic polymers and peptides

Matrix-assisted laser desorption ionization (MALDI) is a very powerful and widely used mass spectrometric technique to ionize high molecular weight compounds. The most commonly used dried droplet (DD) technique can lead to a concentration distribution of the analyte on the target and is therefore often not suitable for reproducible analyses. We developed a new solvent-free deposition technique, called compressed sample (CS), to prevent the distribution of the analytes caused by the crystallization of the compounds. The CS technique presented in this work allows the quantitative analysis of synthetic polymers such as derivatized maltosides with correlation coefficients of 0.999 and peptides up to 3500 Da with correlation coefficients of at least 0.982 without the use of stable-isotope-labeled standards.     

Detailed performance modeling of a pulsed high-power single-frequency Ti:sapphire laser

Differential absorption lidar (DIAL) is a unique technique for profiling water vapor from the ground up to the lower stratosphere. For accurate measurements, the DIAL laser transmitter has to meet stringent requirements. These include high average power (up to 10 W) and high single-shot pulse energy, a spectral purity >99.9%, a frequency instability <60 MHz rms, and narrow spectral bandwidth (single-mode, <160 MHz). We describe extensive modeling efforts to optimize the resonator design of a Ti:sapphire ring laser in these respects. The simulations were made for the wavelength range of 820 nm, which is optimum for ground-based observations, and for both stable and unstable resonator configurations. The simulator consists of four modules: (1) a thermal module for determining the thermal lensing of the Brewster-cut Ti:sapphire crystal collinear pumped from both ends with a high-power, frequency-doubled Nd:YAG laser; (2) a module for calculating the in-cavity beam propagations for stable and unstable resonators; (3) a performance module for simulating the pumping efficiency and the laser pulse energy; and (4) a spectral module for simulating injection seeding and the spectral properties of the laser radiation including spectral impurity. Both a stable and an unstable Ti:sapphire laser resonator were designed for delivering an average power of 10 W at a pulse repetition frequency of 250 Hz with a pulse length of approximately 40 ns, satisfying all spectral requirements. Although the unstable resonator design is more complex to align and has a higher lasing threshold, it yields similar efficiency and higher spectral purity at higher overall mode volume, which is promising for long-term routine operations.     

Boundary effect on the softening curve of concrete

The apparent fracture energy of concrete experimentally determined on the basis of the work of fracture in bending or wedge splitting tests becomes larger with increasing specimen dimensions. This experimental observation may be attributed to the varying local fracture energy along the crack path. When the crack tip approaches the specimen boundary, the size of the fracture process zone will be reduced and, consequently, only a portion of the fracture energy is activated; i.e., the local fracture energy is getting smaller. The influence of this boundary effect diminishes with increasing specimen size resulting in the size dependence of the apparent fracture energy determined by the work-of-fracture method as an average value in the ligament. With varying local fracture energy, the local softening curve will also show variations. The latter are subject of the present study. Wedge splitting tests with different specimen sizes as well as inverse analyses of these experiments were carried out. For the inverse analyses, the cohesive crack model was adopted and an evolutionary optimization algorithm has been used. The boundary effect on the local fracture properties was taken into account and, as a result, the variation of the softening curve along the crack path could be determined. It was found that the tail of the softening curve is shortened and lowered due to the boundary effect whereas the initial slope of this curve appears to be not affected.     

Powder Injection Molding – An innovative manufacturing method for He-cooled DEMO divertor components

At Karlsruhe Institute of Technology (KIT), a He-cooled divertor design for future fusion power plants has been developed. This concept is based on the use of modular cooling fingers made from tungsten and tungsten alloy, which are presently considered the most promising divertor materials to withstand the specific heat load of 10 MW/m². Since a large number of the finger modules (n > 250,000) are needed for the whole reactor, developing a mass-oriented manufacturing method is indispensable. In this regard, an innovative manufacturing technology, Powder Injection Molding (PIM), has been adapted to W processing at KIT since a couple of years. This production method is deemed promising in view of large-scale production of tungsten parts with high near-net-shape precision, hence, offering an advantage of cost-saving process compared to conventional machining.The complete technological PIM process for tungsten materials and its application on manufacturing of real divertor components, including the design of a new PIM tool is outlined and, results of the examination of the finished product after heat-treatment are discussed. A binary tungsten powder feedstock with a solid load of 50 vol.% was developed and successfully tested in molding experiments. After design, simulation and manufacturing of a new PIM tool, real divertor parts are produced. After heat-treatment (pre-sintering and HIP) the successful finished samples showed a sintered density of approximately 99%, a hardness of 457 HV0.1, a grain size of approximately 5 μm and a microstructure without cracks and porosity.     

Morphology and mechanical properties of bisphenol A polycarbonate/poly (styrene-co-acrylonitrile) blends based clay nanocomposites

Two organic modified clays (Cloisite®30B (CL30B) and PCL/Cloisite®30B masterbatch (MB30B)) were used to improve the mechanical properties of polycarbonate (PC)/poly (styrene-co-acrylonitrile) (SAN) blends. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) measurements of the melt blended nanocomposites revealed that partially exfoliated and partially degraded structure was obtained and the clay platelets were located mostly in the SAN phase and at the two-phase boundary. Dispersion of the clay platelets is better when MB30B were used. The mechanical properties of the clays filled nanocomposites vary accordingly and when MB30B is used better mechanical properties can be achieved. Tensile strength increases 41% at maximum as the CL30B loading is 5 wt.%, while elongation at break decreases dramatically. Impact strength can be improved up to 430% compared to the pure blend when 1 wt.% MB30B was used.