Cross-linking density and distribution are decisive for the mechanical and other properties of stimuli-sensitive poly(N-isopropylacrylamide) microgels. Here we investigate the structure of ultra-low cross-linked microgels by static light scattering and scanning force microscopy, and show that they have an inverted cross-linking structure with respect to conventional microgels, contrary to what has been assumed previously. The conventional microgels have the largest polymer volume fraction in the core from where the particle density decays radially outwards, whereas ultra-low cross-linked particles have the highest polymer volume fraction close to the surface. On a solid substrate these particles form buckled shapes at high surface coverage, as shown by scanning force micrographs. The special structure of ultra-low cross-linked microgels is attributed to cross-linking of the particle surface, which is exposed to hydrogen abstraction by radicals generated from persulfate initiators during and after polymerization. The particle core, which is less accessible to the diffusion of radicals, has consequently a lower polymer volume fraction in the swollen state. By systematic variation of the cross-linker concentration it is shown that the cross-linking contribution from peroxide under typical synthesis conditions is weaker than that from the use of 1 mol% N,N'-methylenebisacrylamide. Soft deformable hydrogel particles are of interest because they emulate biological tissues, and understanding the underlying synthesis principle enables tailoring the microgel structure for biomimetic applications. Deformability of microgels is usually controlled by the amount of added cross-linker; here we however highlight an alternative approach through structural softness.
A study of the conductance and capacitance associated with traps in Schottky barriers is described. A sample calculation of these two quantities is developed and compared with experimental data obtained in GaP VPE saples. It is shown that traps introduce peaks on the conductance-vs-temperatures curves; from them the concentration of each trap can be calculated. A study at different frequencies permits the determination of the characteristics of the traps. In GaP we have observed trapping effects in donor levels at Ec−Et?100 and 86 meV, the emission rates were found, respectively, to equal 2×1011 and 2×109 s−1 for these two levels. It is also shown that photoconductance effects occur at the oxygen deep levels.
We describe a semi-analytical method for the fast calculation of secondary fluorescence in electron probe microanalysis of material couples. The calculation includes contributions from primary K-, Land M-shell characteristic x-rays and bremsstrahlung photons. The required physical interaction parameters (subshell partial cross sections, attenuation coefficients, etc) are extracted from the database of the Monte Carlo simulation code system PENELOPE. The calculation makes use of the intensities of primary photons released in interactions of beam electrons and secondary electrons. Since these intensities are not readily available and do not allow analytical calculation, they are generated from short Monte Carlo simulation runs. The reliability of the proposed calculation method has been assessed by comparing calculated, distance-dependent k-ratios with experimental data available in the literature and with results from simulations with PENELOPE. Numerical results are found to be in close agreement with both simulated and experimental data.
Electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) measurements are combined to characterize an industrial produced dual-phase steel containing some bainite fraction. High-resolution carbon mappings acquired on a field emission electron microprobe are utilized to validate and improve the identification of the constituents (ferrite, martensite, and bainite) performed by EBSD using the image quality and kernel average misorientation. The combination eliminates the ambiguity between the identification of bainite and transformation-induced dislocation zones, encountered if only the kernel average misorientation is considered. The detection of carbon in high misorientation regions confirms the presence of bainite. These results are corroborated by secondary electron images after nital etching. Limitations of this combined method due to differences between the spatial resolution of EBSD and EPMA are assessed. Moreover, a quantification procedure adapted to carbon analysis is presented and used to measure the carbon concentration in martensite and bainite on a submicrometer scale. From measurements on reference materials, this method gives an accuracy of 0.02 wt% C and a precision better than 0.05 wt% C despite unavoidable effects of hydrocarbon contamination.
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