Ultrafine 5 nm ceria isotropic nanoparticles were prepared using the rapid chemical precipitation approach from cerium(III) nitrate and ammonium hydroxide aqueous solutions. The as-prepared nanoparticles were shown to contain predominantly Ce(IV) species. The solubility of nanocrystalline CeO 2 at several pH values was determined using ICP-MS and radioactive tracer methods. Phase composition of the ceria samples remained unchanged upon partial dissolution, while the shape of the particles changed dramatically, yielding nanorods under neutral pH conditions. According to X-ray absorption spectroscopy investigation of the supernatant, Ce(III) was the main cerium species in solution at pH < 4. Based on the results obtained, a reductive dissolution model was used for data interpretation. According to this model, the solubility product for ceria nanoparticles was determined to be logK sp =-59.3 ± 0.3 in 0.01M NaClO 4. Taken together, our results show that the pH-dependence of ceria anti-and pro-oxidant activity can be related to the dissolution of CeO 2 in aqueous media.
In the first part of this article we experimentally show that contrast between the very thin layers of La and B enables close to theoretical reflectance. The reflectivity at 6.8 nm wavelength was measured from La/B multilayer mirrors with period thicknesses ranging from 3.5 to 7.2 nm at the appropriate angle for constructive interference. The difference between the measured reflectance and the reflectance calculated for a perfect multilayer structure decreases with increasing multilayer period. The reflectance of the multilayer with the largest period approaches the theoretical value, showing that the optical contrast between the very thin layers of these structures allows to experimentally access close to theoretical reflectance. In the second part of the article we discuss the structure of La/B and LaN/B multilayers. This set of multilayers is probed by hard X-rays (λ = 0.154 nm) and EUV radiation (λ = 6.8 nm). The structure is reconstructed based on a simultaneous fit of the grazing incidence hard X-ray reflectivity and the EUV reflectivity curves. The reflectivity analysis of the La/B and LaN/B multilayer mirrors shows that the lower reflectance of La/B mirrors compared to LaN/B mirrors can be explained by the presence of 5% of La atoms in the B layer and 63% of B in La layer. After multi-parametrical optimization of the LaN/B system, including the nitridation of La, the highest near normal incidence reflectivity of 57.3% at 6.6 nm wavelength has been measured from a multilayer mirror, containing 175 bi-layers. This is the highest value reported so far.
Silicene, a 2D honeycomb lattice of Si atoms similar to graphene, is expected to be a platform for nanoelectronics and home to novel quantum phenomena. Unlike graphene, free-standing silicene is notoriously difficult to stabilize, while strong hybridization of silicene with substrates destroys its desirable properties. On the other hand, Dirac cones of silicene are effectively realized in a bulk - stoichiometric ionic multilayer silicene intercalation compound CaSi2. Besides, a number of new 2D silicene-based materials are synthesized employing CaSi2 as a precursor. However, the rather complex atomic structure of CaSi2 and fresh opportunities of physical and chemical breakthroughs drive the search for alternative compounds with silicene networks. Here, a new polymorph of SrSi2 is synthesized, enjoying both the structure of intercalated multilayer silicene and the simplest possible stacking of silicene sheets. The MBE-quality synthesis accomplished on Si(001) and Si(111) surfaces leads to epitaxial films of SrSi2 with orientation controlled by the substrate, as revealed by XRD, RHEED and electron microscopy studies. The structural SrSi2/Si relation is mirrored in the transport properties of the films.
We present a way to analyze the chemical composition of periodical multilayer structures using the simultaneous analysis of grazing incidence hard X-Ray reflectivity (GIXR) and normal incidence extreme ultraviolet reflectance (EUVR). This allows to combine the high sensitivity of GIXR data to layer and interface thicknesses with the sensitivity of EUVR to the layer densities and atomic compositions. This method was applied to the reconstruction of the layered structure of a LaN/B multilayer mirror with 3.5 nm periodicity. We have compared profiles obtained by simultaneous EUVR and GIXR and GIXR-only data analysis, both reconstructed profiles result in a similar description of the layered structure. However, the simultaneous analysis of both EUVR and GIXR by a single algorithm lead to a ∼ 2x increased accuracy of the reconstructed layered model, or a more narrow range of solutions, as compared to the GIXR analysis only. It also explains the inherent difficulty of accurately predicting EUV reflectivity from a GIXR-only analysis.
Correspondence email: a.zameshin@utwente.nl Synopsis A custom free-form approach is used for reconstruction of GIXRR from periodic multilayers, simulated and experimental data fits are presented.Abstract Grazing Incidence X-ray Reflectivity (GIXRR) is a widely used analysis method for thin films and multilayer structures. However, conventional so-called model-based approaches of structural reconstruction from GIXRR data are lacking analytical power when dealing with very thin structures (down to the nm scale), because a priori assumptions have to be made about the interface composition and structure. This makes it very difficult to reliably analyse such structures. In this work custom freeform approach is presented which solves this task without the need for a priori assumptions on layer or interface parameters. As a proof of principle, a perfect optical constant profile reconstruction and GIXRR curve matching for the simulated data are demonstrated. The developed approach is used to analyse structures of multilayer LaN/B Bragg reflectors designed for the Extreme UV range. Performed analysis allowed to reveal the difference in optical constant profiles of these structures produced with different processes. The uncertainties of structural reconstruction are also discussed.
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