Thickness Dependent Physical Properties of Thermally Evaporated Nanocrystalline CdSe Thin Films

This paper presents a study on thickness dependent physical properties of cadmium selenide thin films. The films of thickness 445, 631 and 810 nm were deposited employing thermal evaporation technique on glass and ITO-coated glass substrates followed by thermal annealing in air atmosphere at 200 °C. These films were subjected to X-ray diffractometer, UV–Vis spectrophotometer, scanning electron microscopy(SEM) and electrometer for structural, optical,surface morphological and electrical analysis respectively. The structural analysis reveals that the films are nanocrystalline in nature with cubic phase and preferred orientation(111). The crystallographic parameters such as lattice constant, interplanar spacing, grain size, internal strain, dislocation density, number of crystallites per unit area and texture coefficient are calculated and discussed. The optical band gap is found in the range 1.75–1.92 e V and observed to increase with thickness.The SEM study shows that the annealed films are uniform, fully covered and well defined. The electrical analysis shows that the conductivity is varied with film thickness and found within the order of semiconductor behavior.     

Growth of ω inclusions in Ti alloys: An X-ray diffraction study

We investigated the size and crystal structure of nanometer-sized ω inclusions in single crystals of β-Ti alloys by X-ray diffraction pole-figure measurements and reciprocal space mapping. We studied the topotactical relation of the β and ω crystal lattices, and from the positions and shapes of the diffraction maxima of the ω lattice determined the mean size of the ω inclusions and the misfit of the inclusion lattice with respect to the host lattice, as well as their changes during ageing. The lattice of the ω inclusions exhibits a large positive misfit already before ageing and the misfit is subsequently reduced during the ageing process. Using the theories of elasticity and X-ray scattering we simulated diffuse X-ray scattering around the β diffraction maxima and demonstrated that the diffuse scattering is caused mainly by local elastic strains in the β host phase around the ω inclusions.     

Sub-microsecond X-ray crystallography: techniques,challenges, and applications for materials science

Dynamics of crystals is a subject of recent interest in solid-state physics and a challenge for modern X-ray crystallography. Time-dependent response of solids to an external perturbation on atomic and microstructural length scales is the key to understanding many physical properties. This paper reviews the challenges and opportunities for probing of sub-micro-, micro-, and millisecond dynamics of solids using the methods of X-ray crystallography. It starts with an overview of recent time-resolved X-ray diffraction techniques. It then focuses on the processes that are important for understanding functional materials: dynamics of ferroelectric and ferroelastic domain patterns, texture in piezoelectric ceramics, mechanical resonances in solids, and dynamics of structural disorder. Knowledge available from macroscopic experiments is summarized, and opportunities for X-ray crystallography to resolve existing controversies are presented. This paper suggests the possible synergy of macroscopic and X-ray crystallographic experimental techniques.     

Off-axis texture in nanostructured Ti1 − xAlxN thin films

Standard θ-2θ and pole figure X-ray diffraction techniques were used to study structural properties and preferred orientation of nanostructured TiAlN thin films prepared using cathodic arc deposition. Systematic collection of reflections from lattice planes {111}, {200}, {220}, and {311} showed that the in-plane orientation of crystallites exhibits cylindrical symmetry with random distribution of crystallites, while the out-of-plane growth presents strong texture which is inclined with respect to the surface normal. This brings the crystallographic orientation of fibre texture towards high indices lattice planes (113) and (115) contrary to traditionally grown films that develop a preferred orientation following to low indices close-packed planes (111) and (200). The origin of inclined growth is discussed taking into account the role of crystallographic defects in particular twin faults that develop in the lattice of growing crystal and change the stacking sequences of atom layers.     

Total scattering and the pair distribution function in crystallography

The importance of total scattering and its Fourier transform, the pair distribution function, in crystallography was understood soon after it was shown that crystals diffract X-rays. However for the next fifty years or so other techniques based more firmly on the crystal lattice came to the fore and total scattering measurements were largely the domain of those studying liquid and amorphous structure. In the late 1980s it was ‘rediscovered’ as a way to uncover disorder within crystal structures and since then the combination of improved instrumentation and analysis has led to a resurgence of the total scattering method. This review sets out this journey, highlighting both the early origins and – more importantly – the ways that total scattering and pair distribution functions are routinely used within crystallography today.     

A guide to the crystallographic analysis of icosahedral viruses

Determining the structure of an icosahedral virus crystal by X-ray diffraction follows very much the same course as conventional protein crystallography. The major differences arise from the relatively large sizes of the particles, which significantly affect the data collection process, data processing and management, and later, the refinement of a model. Most of the other differences are due to the high 5 3 2 point group symmetry of icosahedral viruses. This alters dramatically the means by which initial phases are obtained by molecular substitution, extended to higher resolution by electron density averaging and density modification, and the refinement of the structure in the light of high non-crystallographic symmetry. In this review, we attempt to lead the investigator through the various steps involved in solving the structure of a virus crystal. These steps include the purification of viruses, their crystallization, the recording of X-ray diffraction data, and its reduction to structure amplitudes. It further addresses the problems attending phase determination and ultimately the refinement of a model. Finally, we describe the unique properties of virus crystals and the factors that influence their physical and diffraction properties.     

Protein crystallography from the perspective of technology developments

Early on, crystallography was a domain of mineralogy and mathematics and dealt mostly with symmetry properties and imaginary crystal lattices. This changed when Wilhelm Conrad Röntgen discovered X-rays in 1895, and in 1912, Max von Laue and his associates discovered that X-ray irradiated salt crystals would produce diffraction patterns that could reveal the internal atomic periodicity of the crystals. In the same year, the father-and-son team, Henry and Lawrence Bragg successfully solved the first crystal structure of sodium chloride and the era of modern crystallography began. Protein crystallography (PX) started some 20 years later with the pioneering work of British crystallographers. In the past 50–60 years, the achievements of modern crystallography and particularly those in PX have been due to breakthroughs in theoretical and technical advancements such as phasing and direct methods; to more powerful X-ray sources such as synchrotron radiation; to more sensitive and efficient X-ray detectors; to ever faster computers and to improvements in software. The exponential development of PX has been accelerated by the invention and applications of recombinant DNA technology that can yield nearly any protein of interest in large amounts and with relative ease. Novel methods, informatics platforms and technologies for automation and high-throughput have allowed the development of large-scale, high-efficiency macromolecular crystallography efforts in the field of structural genomics. Very recently, the X-ray free-electron laser sources and its applications in PX have shown great potential for revolutionizing the whole field again in the near future.     

Structural transformations in quenched Fe–Ga alloys

It has been speculated that the large increase in magnetostriction in Fe–Ga alloys results from local short-range ordering of the Ga atoms along specific crystallographic directions in the disordered Fe structure. The structural transitions associated with different cooling rates from the high temperature disordered state were investigated with X-ray diffraction of oriented single crystals of Fe–19 at% Ga. Results are presented for long-range ordering during slow cooling and indirect evidence of local short-range ordering of Ga atoms in the disordered state when the alloys are quenched is also presented. In the latter case, the short-range ordering of Ga atoms leads to a tetragonal distortion of the lattice. The dependence of the magnetostrictive response of Fe–Ga alloys on thermal history has been found to be directly related to these structural transformations in Fe–19 at% Ga alloys and experimental support for the proposed magnetostriction model based on Ga–Ga pairing along [100] crystallographic directions is presented.     

Determination of the structure of UFe2Al10 compound

The atomic structure of a new ternary phase UFe₂Al₁₀ appearing in the U–Fe–Al system was determined using direct methods applied to X-ray powder diffraction data. High resolution electron microscopy combined with the methods of crystallographic image processing was used for the verification of the structural model. The UFe₂Al₁₀ phase is orthorhombic and belongs to Cmcm space group, its unit cell contains 40 Al, eight Fe, and four U atoms. The lattice parameters obtained after Rietveld refinement are: a=8.919 Å, b=10.208 Å, and c=9.018 Å. The reliability factors characterizing the Rietveld refinement procedure are: R_p=5.9%, R_wp=8.1%, and R_b=2.9%.     

Electron diffraction and three-dimensional crystallography for structural biology

Electron crystallography is increasingly becoming a viable alternative for structure elucidation of three-dimensional, multi-nanometre sized crystals of beam-sensitive organics and macromolecules. Because electrons interact with matter strongly, crystals cannot be much more than 200?nm thick. Diffracted volumes are therefore small, leading to a poor signal-to-noise ratio (SNR) as beam damage limits the total electron dose. Data can be collected in diffraction – and imaging mode. Imaging has the advantage of providing spatial phase information but comes at a substantial cost in SNR. Highly sensitive hybrid pixel detectors push the limits of high-quality diffraction data acquisition even further. Data integration, structure solution and refinement are feasible with existing software after minor adaptations. We review the current state of electron diffraction for structural biology, including instrumentation, data acquisition and structure determination.     

The crystal structure of (Nb0.75Cu0.25)Sn2 in the Cu-Nb-Sn system

During the processing of superconducting Nb₃Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg₂ type with a proposed composition of about (Nb_0.75Cu_0.25)Sn₂. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg₂ type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn₂ by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg₂ type for NbSn₂ to the NiMg₂ type for (Nb_0.75Cu_0.25)Sn₂. In the previous literature the (Nb_0.75Cu_0.25)Sn₂ phase described here has occasionally been referred to as Nausite.     

Microstructure and magnetic properties of HVOF thermally sprayed Fe75Si15B10 coatings

Partially amorphous Fe₇₅Si₁₅B₁₀ coatings were prepared from nanostructured feedstock powders by using high velocity oxy-fuel spraying. Scanning electron microscopy, X-ray diffraction, Vickers indenter and magnetic measurements were used to investigate microstructural, structural, microhardness and magnetic properties of the coatings. The Rietveld refinement of the X-ray diffraction patterns reveals the presence of an amorphous phase, nanocrystalline α-Fe(Si,B) structure having a lattice parameter close to 0.2841 nm and an average crystallite size of about 78-83 nm in addition to small amounts of Fe₃O₄ oxide (104 nm) and Fe₂B boride (151 nm), which disappear completely with increasing coating thickness. Coercivity and microhardness values are 15.5 Oe and 478 Hv, respectively, for 84 μm thickness.     

电子背散射衍射（EBSD）及其在材料研究中的应用

论述了电子背散射衍射（EBSD）的形成原理、花样包含的物理意义，并给出了EBSD在测定晶体取向、织构、取向关系、物相鉴定、应变分布、晶格常数及晶界性质研究等方面的应用实例。     

Comparative study of microwave and conventional methods for the preparation and optical properties of novel MgO-micro and nano-structures

Magnesium oxide (MgO) was synthesised by a simple microwave-assisted combustion route without using any template, catalyst or surfactant. For the purpose of comparison, it was also prepared using conventional method. The as-synthesized MgO was characterized by powder X-ray diffraction (XRD), Fourier Transform infrared spectra (FT-IR), high resolution scanning electron microscopy (HR-SEM), transmission electron microscopy (TEM), Energy Dispersive X-ray analysis (EDX), diffuse reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The XRD results confirmed the formation of cubic phase MgO. FT-IR was used to investigate the adsorption of water and CO₂ on MgO surface and confirm the formation of Mg-O phase. The formation of MgO micro cubes structures was confirmed by HR-SEM. The formation of MgO nanosheets was confirmed by HR-SEM and TEM and their possible formation mechanisms were also proposed. The optical absorption and photoluminescence emissions were determined by DRS and PL spectra respectively. An attempt has been made to compare the lattice parameter and the PL intensity.     

Effect of crystallite size on structural and luminescent properties of nanostructured Eu:KGdF4 synthesised by co-precipitation method

The Eu³⁺:KGdF₄ powders with average crystallite size of 20 and 25 nm have been obtained from solution by co-precipitation method. Morphology of the as-received powders was examined by XRD and TEM methods. Behaviour of these two powdered batches, characterised by different size of nanocrystallites, versus thermal treatment has been studied by X-ray powder diffraction, thermogravimetric, infrared spectroscopy and emission spectroscopy methods. The phase transitions between low-temperature cubic, orthorhombic, trigonal and high-temperature cubic modifications of KGdF₄ were detected for both samples heated in 300–790 °C temperature range. Abundance of the particular polymorphic form observed at given temperature differs considerably for samples of different initial crystallite size. Besides, significant differences in number of lattice defects, water contents and emission properties were observed for these two samples. The properties of material precipitated from solution are also compared with structural and optical properties of the Eu³⁺:KGdF₄ fluoride synthesised by a solid-state reaction.     

钢中残余奥氏体测定的异常散射修正问题

研究了异常散射校正支Ｘ射线测定钢中残余奥氏体含量的影响，指出了一些文献中对异常散射校正提法上的混乱和所附数表中的错误。     

Crystallography and the liquid crystal phase: a new approach to structural studies on a thermo-tropic smectic Schiff base

In spite of the apparent contradiction between ‘liquid crystals’ (LC, materials exhibiting some degree of disorder) and ‘crystallography’ (a paradigmatic ordered kingdom), X-ray diffraction (XRD) studies make a substantial contribution to the field of LC. Focusing this review on smectic (Sm, lamellar) LC, we first describe how extremely careful XRD studies performed on mono-domain samples in the LC phase helped to elucidate the molecular structure of ordered Sm phases. Then, we describe selected examples in which single-crystal (SC) XRD on the solid-state phase of the mesogens provided information about their supra-molecular organization in the Sm phase. Finally, we present a different approach to this problem in the case of a thermo-tropic Schiff base (SB) which undergoes crystal???LC???isotropic liquid phase transformations. By combined SC and variable-temperature powder XRD, we show that the SB LC is a hexatic smectic B phase that derives from the crystal phase by relatively small topological changes promoted by the set-in of thermal rotational disorder around the long SB molecular axis.     

Lattice misfit during ageing of a polycrystalline nickel-base superalloy

The temporal evolution of the lattice parameters and lattice misfit of an advanced polycrystalline nickel-base superalloy have been studied in situ during an ageing heat treatment using synchrotron X-ray diffraction. During ageing, the γ and γ′ lattice parameters were both observed to decrease, a trend that cannot be attributed to a loss of coherency alone. Phase-extracted γ′ replicated this behaviour. Atom probe tomography was used to measure the compositional changes between the start and end of the ageing heat treatment. Using these data, a thermodynamic assessment was made using the software ThermoCalc of the structural change across the interface between γ and γ′. Subsequently, the unconstrained lattice parameters were estimated and were shown to be in good agreement with the X-ray diffraction measurements. Thus, the observed anomalous lattice misfit behaviour was concluded to be dominated by elemental exchange between the γ and γ′ phases during ageing.     

Phase transformations after long-time annealing in metastable Fe–Cr alloy films prepared by pulsed laser deposition

Metastable Fe–Cr alloy films of various composition prepared by cross-beam pulsed laser deposition using two different procedures are investigated by wide-angle X-ray scattering. Depending on the Fe–Cr composition of the samples in an extended range, a body-centered cubic (bcc) phase or metastable phases with body-centered tetragonal (bct), face-centered orthorhombic (fco) or primitive orthorhombic (po) and primitive cubic (pc) lattices are formed in the films prepared by simultaneous co-deposition of Fe and Cr. In the films produced by layer-by-layer deposition of thin separate Fe and Cr layers (thickness of about 1 nm), only bcc and bct Fe–Cr phases were observed. A long-time annealing (50 h) at a temperature of 425 °C near the low-temperature existence limit of the σ-phase under equilibrium conditions followed by slow cooling (rate 0.5 °C/min) has been performed and various phase transformations were observed. In addition to known equilibrium and metastable Fe–Cr crystalline phases (mainly bcc and bct phases in the films prepared by layer-by-layer technique and bcc, bct and σ-FeCr phases in co-deposited films), a new metastable Fe–Cr superstructure characterised by a primitive tetragonal lattice with parameters a and c of about 0.57 and 0.63 nm, respectively, has been identified. It is shown that the formation of ″-crystallites with preferred orientation in the metastable Fe–Cr alloy films during dedicated long-time annealing gives rise to a spatially periodic modulation of chemical composition resulting in the formation of multilayers with periods of one or a few atomic monolayers of individual Fe and Cr components.