On the thermal stability of the cobalt nanostructure formed under severe plastic deformation

The results of the investigations of the temperature dependence of thermal expansion of nanostructured cobalt have been presented. It has been shown that deformation nanostructuring results in the nonlinear behavior of the cobalt thermal expansion curve, and the manifestation of a stepwise sample elongation in the phase transformation temperature range in this curve disappears. It has been found that the sample length at room temperature changes after cycles of heating to various temperatures. Based on the results obtained and X-ray diffraction data, it has been demonstrated that there is a correlation of these changes with recovery and recrystallization processes.     

High temperature relaxation in metals and alloys

The characteristics of elastic lag and internal friction in metals at high temperatures are investigated using data from the literature and by theoretical analysis. It is shown that there is a connection between the elementary mechanisms of relaxation and recrystallization, and methods are discussed for determining the activation energy of these processes from internal friction recovery kinetics. Experimental data are presented for high temperature internal friction of tungsten before and after recrystallization.Paper presented at a conference on energy dissipation of low and high amplitude vibrations in metals and alloys, Tula, 1964.     

Dislocation emission in A1 during recrystallization

Summary The dislocation structure evolution during isothermal recrystallization of Al has been followed by means of internal friction, modulus defect and X-ray diffraction analyses accompanying the microscopical observations. Many peaks ofQ ⁻¹ and of modulus defect and X-ray diffraction line width have been found, both in nucleation and grain growth, all referable to dislocations. The first of these peaks, at the beginning of recrystallization, presents recovery characteristics, different from those shown by the subsequent, secondary peaks. Secondary peaks are interpreted in terms of dislocation emission from grain boundaries, whereas the first peak appears connected with subboundaries, walls present in the initial stages of recrystallization. To speed up publication, the authors of this paper have agreed to not receive the proofs for correction.     

磷对冷轧纯铜再结晶的影响

本文研究了微量磷对冷轧纯铜再结晶的影响。当磷原子主要是溶解在铜中时,大大提高了再结晶温度,增加了再结晶激活能,阻止了立方结构的形成,改变了再结晶结构;但出氧化磷状态存在于铜中时,对以上各方面的影响就不很明显。所有样品的再结晶结构,都与加工结构中的某一种取向相同或接近,并且与主要加工结构间存在着沿<111>相差20—45°的几何关系。分析从金相及X光研究后得到的结果,认为在这种情况下,同位再结晶和选择性生长是再结晶结构形成的过程。 关键词：     

Changes in the diffusion properties of nonequilibrium grain boundaries upon recrystallization and superplastic deformation of submicrocrystalline metals and alloys

The effect of an increase in the coefficient of the grain-boundary diffusion upon recrystallization and superplastic deformation of submicrocrystalline (SMC) materials prepared by severe plastic deformation has been studied. It is shown that the coefficient of the grain-boundary diffusion of the SMC materials is dependent on the intensity of the lattice dislocation flow whose value is proportional to the rate of the grain boundary migration upon annealing of SMC metals or the rate of the intragrain deformation under conditions of superplastic deformation of SMC alloys. It is found that, at a high rate of grain boundary migrations and high rates of superplastic deformation, the intensity of the lattice dislocation flow bombarding grain boundaries of SMC materials is higher than the intensity of their diffusion accommodation, which leads to an increase in the coefficient of the grain-boundary diffusion and a decrease in the activation energy. The results of the numerical calculations agree well with the experimental data.     

Thermodynamics of a phase transition of silicon nanoparticles at the annealing and carbonization of porous silicon

The formation of SiC nanocrystals of the cubic modification in the process of high-temperature carbonization of porous silicon has been analyzed. A thermodynamic model has been proposed to describe the experimental data obtained by atomic-force microscopy, Raman scattering, spectral analysis, Auger spectroscopy, and X-ray diffraction spectroscopy. It has been shown that the surface energy of silicon nanoparticles and quantum filaments is released in the process of annealing and carbonization. The Monte Carlo simulation has shown that the released energy makes it possible to overcome the nucleation barrier and to form SiC nanocrystals. The processes of laser annealing and electron irradiation of carbonized porous silicon have been analyzed.     

硫化温度对ZnS薄膜生长质量的影响

采用热反应法对玻璃衬底上以磁控溅射制备的Zn薄膜进行硫化,制备出ZnS薄膜。薄膜的微观结构、物相结构和表面形貌分别采用正电子湮没技术（PAT）、X射线衍射仪（XRD）、扫描电子显微镜（SEM）进行分析和表征。利用慢正电子湮没多普勒展宽对四个不同硫化温度下得到的ZnS薄膜样品中膜层结构缺陷进行研究,测量了薄膜中的空位型微观缺陷的相对浓度,指出445℃硫化样品中正电子注入能量在1.5~4.5 keV后S参数最小,说明该硫化温度下反应生成的ZnS薄膜结构缺陷浓度最小,膜的致密度最高。XRD结果显示薄膜在445℃以上硫化后,呈（111）择优生长趋势。从扫描电镜的结果也可以看出,在445℃硫化后,薄膜的晶粒明显地变得更大、更致密,这是因为ZnS晶胞比Zn晶胞大以及硫化过程中ZnS固相再结晶的缘故。ZnS thin films have been prepared by sulfurizing zinc thin films deposited on glass substrate by magnetron sputtering for two hours. The microstructure defects, crystallizations and surface morphology of zinc films sulfurized at different temperature were analyzed by PAT (positron annihilation technique), XRD(X-ray diffraction) and SEM (Scanning electron microscopy), respectively. For analyzing the structure defect of four samples with different sulfurization temperature, PAT has been used to obtain the relative concentration of defects. With the positron energy range of 1.5~4.5 keV, the S parameter of ZnS films is minimum. It demonstrates that ZnS films produced at 445℃ have the minimum structural defect concentration and the highest density. XRD results show that films are blende structure with the preference of (111) orientation above 445℃. And from the result of SEM, because of ZnS films recrystallization, the crystal grains obviously become large and dense at 445℃.     

Influence of sintering conditions and laser radiation on the surface microstructure,chemical composition,and electrical conductivity of CuO/Ag ceramics

The influence of the third harmonic radiation of a YAG: Nd³⁺ laser on the microstructure, chemical composition, and electrical conductivity of CuO and CuO/Ag ceramic samples subjected to heat treatment under different conditions has been investigated. It has been found that the surface morphology is almost identical for all the samples sintered at the same temperatures. According to the X-ray microanalysis, the ratio of the copper and oxygen concentrations (Cu/O) increases with an increase in the sintering temperature and upon quenching cooling of the samples. It has been shown that laser irradiation changes the micro-structure of the samples, increases the concentration ratio Cu/O, and leads to the inclusion of silver atoms into the lattice of copper oxides. It has been revealed that the temperature dependence of electrical resistance of all the studied samples in the temperature range of 80–300 K has a semiconducting character, and the activation energy of electrical resistance varies in the range from 0.19 to 0.48 eV. The activation energy of electrical resistance decreases with an increase in the sintering temperature of the samples and increases upon their quenching, whereas the laser treatment leads to a weakening of the dependence of the activation energy on the sintering temperature. The deposition of a silver layer before the laser treatment has no noticeable influence on the activation energy. The obtained data can be used to purposefully change the physical properties of compounds formed in the Cu-O-Ag system.     

Amorphization and recrystallization of ion implanted Si nanocrystals probed through their luminescence properties

In this paper the amorphization of Si nanocrystals (nc) by ion beam irradiation and the subsequent recrystallization are investigated in detail. The luminescence properties of Si nanocrystals embedded within a SiO₂ matrix are used as a probe of the damaging effects generated by high-energy ion beam irradiation. Samples have been irradiated with 2 MeV Si⁺ ions at different doses, in the range between 1×10⁹ and 1×10¹⁶ cm⁻². By increasing the ion dose, the nc-related photoluminescence (PL) strongly decreases after a critical dose value. It is shown that the lifetime quenching alone cannot quantitatively explain the much stronger PL drop, but the total number of emitting centers has to diminish too. Moreover, we studied the recovery of the amorphized Si nc by performing thermal annealings. It is demonstrated that the recovery of the PL properties of completely amorphized Si nc is characterized by a single activation energy, whose value is 3.4 eV. Actually, this energy is associated to the transition between the amorphous and the crystalline phases of each Si grain. The recrystallization kinetics of Si nanostructures is demonstrated to be very different from that of a bulk system.     

In-situ and ex-situ study of crystallization behaviour of magnetron sputtered Ni63Zr37 amorphous thin film

ABSTRACT

The stages of crystallization of magnetron sputter-deposited Ni₆₃Zr₃₇ film with mostly amorphous structure have been investigated by differential scanning calorimetry (DSC) and in-situ annealing at 300°C by use of heating stage on a high-resolution transmission electron microscope (HRTEM). These results have been further confirmed by grazing incidence X-ray diffraction analyses of thin film specimens annealed ex-situ at 300°C for various durations. The temperature for crystallization found by DSC has been found to increase from 371°C to 434°C with an increase in heating rate from 3°C/min to 10°C/min, and the apparent activation energy for amorphous to crystalline transformation has been found as ～260.2?kJ/mol from the Kissinger plot. Studies on HRTEM using in-situ heating stage have shown the crystallization to occur on annealing at 300°C for ～10?min. Crystallization at a temperature lower than that found by DSC is attributed to structural relaxation with reduction of free volume due to thermal activation. It has been observed that Ni₃Zr forms first due to its large negative enthalpy of formation, and is followed by the formation of Ni-rich solid solution (Ni_ss) grains. HRTEM studies have shown grain rotation with the formation of partial dislocations at Ni₃Zr-Ni_ss interfaces as well as twinning followed by detwinning with dislocation formation in the Ni_ss matrix possibly to reduce the interfacial energy.     

Structural,thermal, electrical and magnetic properties of pure and 50% La doped BiFeO3 ceramics

Polycrystalline ceramic samples of pure and 50% La substituted BiFeO₃ have been prepared by standard solid state reaction method using high purity oxides and carbonates. The formation of the single phase compound as well as its chemical analysis has been checked by X-ray diffraction and energy dispersive X-ray microanalysis (EDAX) techniques. A better agreement between observed and calculated X-ray powder diffraction patterns was obtained by performing the Rietveld refinement with a structural model using the non-centrosymmetric space group R3c. The lattice parameters in both the cases have been refined but the over-all structure remains the same. The microstructural studies have been carried out using scanning electron microscopy (SEM). Modulated differential scanning calorimetry (MDSC) has been used to detect the Neel/transition temperature in the compounds. The activation energies calculated from log σ vs 1/T curve are 0.81 eV and 1.13 eV respectively. Vibrating sample magnetometer (VSM) has been used to study the magnetic behaviour of the compounds. It has been observed that by 50% La substitution the insulating behaviour of the material has been improved and showing the antiferromagnetic to weak ferromagnetic behaviour.     

Zum Einfluß der Versetzungsdichte auf die Primärrekristallisation von Kupfer und Silber nach extrem hoher plastischer Verformung

The isochronal and isothermal recovery of the electrical resistivity after large homogeneous compression of copper and silver was measured with a low frequency eddy current method. Two relations between the recovery data and the flow stress were found: 1. For high purity copper and silver the recovery of the electrical resistivity with recrystallization is proportional to the square of the flow stress. 2. The temperature at which half of the resistivity decrease with recrystallization is reached may be related to the flow stressσ by the equation \(\sigma ^2 e^{ - a/T_R } = const\) . The present experiments indicate that a simple relation between the quantitya and the activation energy for recrystallization cannot be given.     

In situ transmission electron microscopy observations of?the?crystallization of?amorphous?Ge?films

The crystallization of amorphous Ge films has been studied as a function of annealing temperature between 400 and 700°C by in situ transmission electron microscopy (TEM). It is found that crystallization does not occur until the annealing temperature reaches 650°C, which is nearly 250°C higher than the crystallization temperature in previous reports. The high crystallization temperature and average crystal size obtained by in situ TEM are in agreement with those from Raman spectroscopy and X-ray diffraction measurement. The kinetics analysis indicates that homogeneous nucleation is the dominant crystallization mode and the activation energy is up to about 3.1 eV.     

Microstructural characterization and recrystallization kinetics of cold rolled copper

The recrystallization kinetics in pure copper deformed by cold rolling is mainly investigated by differential scanning calorimetry (DSC) under non-isothermal conditions. DSC curves show exothermic peaks corresponding to the stored energy released during recrystallization process. Variation of the heating rate and application of different methods allowed us to calculate two kinetic parameters of recrystallization: (i) the activation energy of the process was calculated using three different methods and (ii) the Avrami exponent was estimated using the Matusita method. On other hand, the microstructural evolution during recrystallization and grain growth of cold rolled copper were investigated at a temperature of 450 °C by scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD).     

Effect of post-deformation ageing on the recrystallization of KCl-SrCl2 crystals

Room-temperature recrystallization of KCl single crystals, both pure and doped with 0.02 and 0.06 wt % Sr, deformed preliminarily at 250°C is studied. It is found that annealing of the original single crystals at 650°C results in the precipitation of the SrCl₂ phase from the solid solution. X-ray diffraction studies reveal that the deformed crystals undergo ageing at room temperature, which is accompanied by a change in the phase composition. In the first place, particles of the KSr₂Cl₅ phase are formed instead of the phase SrCl₂ observed in the original and deformed crystals. These particles, which are located at the boundaries of growing recrystallized grains (twins of the original single crystal) occupying not more than 8% of the volume, impede the motion of grain boundaries and hamper further recrystallization. Second, it is shown that post-deformation ageing occurring in the remaining 92% of the deformed crystal region that has not undergone recrystallization lends stability to the strain-hardened state of alkali halide crystals over a period of at least two years at room temperature.     

Rapid treatment of CIGS particles by intense pulsed light

Intense pulsed light (IPL) technique has been proposed to make large grains Cu(In_0.7Ga_0.3)Se₂ (CIGS) film using CIGS particles. The proposed process is non-vacuum based and performed at room temperature without selenization treatment. Melting and recrystallization of CIGS particles to larger grains without structural deformation and phase transformation are proved with adequate characterization evidences. X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion analysis (EDS) were used to characterize the prepared films. Melting of the CIGS particles and recrystallization to larger grains by light energy in 20 ms short reaction time could be the reason for no structural deformation and secondary phase generation during the process. The CIGS film prepared from its constituent nanoparticles by IPL treatment has great potential for use as absorber layer for solar cell application and is expected to have large impact on cell fabrication process in terms of cost reduction and simplified processing.     

A structural study of promethium metal under pressure

Abstract

The structural behaviour of Pm metal has been investigated up to 60 GPa of pressure using a Diamond Anvil Cell (DAC) and the energy dispersive X-ray diffraction technique. The room temperature/pressure structural form of Pm is dhcp and it transforms to a fcc phase by 10 GPa. This cubic phase of the metal converts by 18 GPa to a third phase, which has frequently been referred to as representing a distorted fcc structure. This latter form of Pm was retained up to 60 GPa, the maximum pressure studied, but subtle changes in the X-ray spectra between 50 and 60 GPa hinted that an additional structural change could be forthcoming at higher pressures. From the experimental data a bulk modulus (B₀) of 38 GPa and a B₀′ constant of 1.5 were calculated using the Birch equation. This modulus for Pm is in accord with the moduli reported for the neighboring lanthanide metals.     

Activation energy of self-diffusion along symmetric tilt grain boundaries 〈111〉 in the Ni3Al intermetallic compound

Activation energy of self-diffusion along symmetric tilt grain boundaries 〈111〉 in the Ni₃Al inter-metallic compound has been calculated depending on the temperature and misorientation angle. For comparison, two types of potentials of interatomic interaction have been used: pair Morse potentials and multi-particle Cleri-Rosato potentials. It has been shown that the activation energy of grain-boundary diffusion increases with temperature on applying the additional diffusion mechanisms. Three temperature ranges with various activation energies have been found.     

Crystal growth,structural and photoluminescence studies of L-tyrosine hydrobromide semi organic single crystal

Nearly perfect single crystal of L-tyrosine hydrobromide (LTHB) has been grown at room temperature from the saturated solution prepared from the solvent with optimised normality (2N) using slow evaporation solution growth technique. Crystal system and lattice parameters have been estimated by single crystal X-ray diffraction analysis. Prominent peeks of powder X-ray diffraction pattern have been indexed and diffraction data have been presented. The presence of various functional groups in LTHB has been identified by vibrational and Nuclear Magnetic Resonance spectral study. The crystalline nature and defect during the growth has been studied by obtaining high resolution X-ray diffraction curve (rocking curve) for the title crystal and detailed explanation is given in this paper. Cyclic voltammetric behaviour and photoluminescence properties of LTHB have also been investigated.