Mössbauer effect studies and X-ray diffraction analysis of cobalt ferrite prepared in powder form by thermal decomposition method

Cobalt ferrite (Co_xFe_3?xO₄) is prepared in powder form by thermal decomposition of iron and cobalt salts and is analysed by X-ray diffraction and Mössbauer spectroscopic techniques. The variation of Mössbauer parameters, lattice parameters and crystallite size of the products formed with variation in the composition of Fe and Co ratios are studied. The studies confirm the formation of nano-size cobalt ferrite particles with defect structure and it is found to be maximum for the Fe : Co = 60 : 40 ratio of the initial precursor oxides.     

Elastic properties of polycrystalline gold thin films: Simulation and X-ray diffraction experiments

The elastic behavior of supported gold thin films has been studied using a framework in which the elastic interaction between grains and the actual structure of the film (i.e. preferential grain orientation and grain shape) are taken into account. Experiments were carried out using synchrotron X-ray diffraction combined with in-situ tensile testing and thereafter, no assumptions on the residual stress state and on the stress-free lattice parameter a₀ have to be made. Modeling of grain elastic interactions is based on the extension of Eshelby-Kröner model, which allows for estimating the elastic behavior of polycrystals considering the texture and the shape of the crystallites. Flat-disc shaped grains arrangement is shown to yield the best representation of the elastic behavior of the fiber-textured gold thin films composed of columnar grains. This non-intuitive representation results from free-surface effect.     

Thermogravimetry and wide angle X-ray diffraction study on the structure of irradiated and thermally treated kodar film

The degradation behaviour of Kodar [poly(1,4-cyclohexylene dimethyl-eneterephthalate)] was investigated in air using thermogravimetry, differential thermal analysis and wide angle X-ray diffraction studies. The rates of crystallization and degradation were influenced by thermal exposure and polychromatic irradiation (Λ > 290 nm) for different time intervals. The crystallinity changes (X_c%) and activation energies (ΔE) for the systems have been determined.     

多相物质粉末衍射的物相检索

讨论了多相物质粉末衍射的物相检索问题，介绍了XRDS的物相检索软件。这是一种智能型的物相检索程序，考虑了测试数据的不确定度，以及粉末样品和块状样品衍射图谱各自的特点，不仅注意到实际样品中微量物相存在的可能，也注意到块状样品结构有序性的可能。XRDS能够帮助材料工作者同时检出样品中所含的多种物相及其含量，操作简单、结果可靠。     

Investigation of the Correlation between Texture and Microstructure on a Submicrometer Scale in the TEM

In recent years the investigation of local texture and microstructure by analysis of electron backscatter diffraction patterns (EBSP) in the SEM has become a very powerful and popular method. With the introduction of SEM with field emission guns (FEG) the spatial resolution of EBSP measurements could be enhanced from 500 nm with a tungsten emitter to better than 50 nm. This evolution of SEM techniques raises the question whether transmission electron microscopy (TEM) still has fields of application in texture research. The present article answers this question with a clear “yes” and presents three examples of investigations where TEM is indispensable. The three examples comprise the investigation of the correlation between dislocation structure and deformation texture, a study on nucleation mechanisms of recrystallization in highly deformed metals and the investigation of microtexture and microstructure in nanocrystalline materials. Together with the presentation of these cases some of the necessary measurement techniques are described briefly. It is shown that TEM has to be applied when highest spatial resolution of orientation determination and imaging and high accuracy of orientation determination are to be reached, when the three‐dimensional and quantitative characterization of lattice defects is required or when materials with a high density of lattice defects are to be investigated.     

Formation reactions of chalcopyrite compounds and the role of sodium doping

The selenisation of the thin film precursors indium, Cu-In and Cu-In-Ga has been studied by in-situ X-ray diffraction. The influence of sodium doping on the kinetics of the solid-state reactions observed agrees with the predictions derived from a phenomenological model presented earlier. In this model a layer of sodium polyselenide is assumed to form at the surface of the precursor, or around each crystal grain. This layer might be responsible for impeded ion exchange in certain solid-state reactions.     

Fabrication and characterization of Cu2ZnSnS4 thin films deposited by spray pyrolysis technique

We have investigated synthesis conditions and some properties of sprayed Cu₂ZnSnS₄ (CZTS) thin films in order to determine the best preparation conditions for the realization of CZTS based photovoltaic solar cells. The thin films are made by means of spraying of aqueous solutions containing copper chloride, zinc chloride, tin chloride and thiourea on heated glass substrates at various temperatures. In order to optimize the synthesis conditions of the CZTS films, two series of experiments are performed. In the first series the sprayed duration was fixed at 30 min and in the second it is fixed at 60 min. In each series, the substrate temperature was changed from 553°K to 633°K. The X-ray diffraction shows, on one hand, that the best crystallinity was obtained for 613°K as substrate temperature and 60 min as sprayed duration. On the other hand, these CZTS films exhibit the kesterite structure with preferential orientation along the [112] direction. Atomical Force Microscopy was used to determine the grain sizes and the roughness of these CZTS thin film. After the annealing treatment, we estimated the optical band-gap energy of the CZTS thin film exhibiting the best crystallinity as 1.5 eV which is quite close to the optimum value for a solar cell.     

Characterization of supported Pd-Pt catalysts by chemical probes

The temperature programmed (palladium) hydride decomposition appeared very effective method for diagnosing the extent of alloying in Pd-Pt/SiO₂ catalysts. Introduction of Pt to Pd catalysts moves the TPHD peak gradually towards lower temperatures and the shift in hydride decomposition peak is accompanied by a decrease in the amount of released hydrogen. The catalysts prepared the direct redox method showed much better alloy homogeneity than the samples prepared by coimpregnation. The results of probing with other techniques, i.e. catalytic probing with hydrodechlorination of CCl₂F₂ and XRD, were in line with TPHD data. The catalytic probing showed the presence of synergistic effect, a clear indication of Pd-Pt mixing. XRD data of post-reaction samples showed carbon incorporation into Pd-rich phase, whereas separate Pt-rich phase did not experience any bulk carbiding.     

T(x) phase diagram of the Cu2Se-Al2Se3 system

Twenty alloys of various compositions in the Cu₂Se-Al₂Se₃ system were prepared and investigated. The T(x) phase diagram of the Cu₂Se-Al₂Se₃ system was obtained from x-ray diffraction, differential thermal analysis, and microstructure investigation for the first time. The homogeneity region of the CuAlSe₂ semiconducting compound was established. Previous articles by this author were presented with the spelling of his name as B.V. Korzun.