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Register a new userX-Ray diffraction on large single crystals using a powder diffractometer
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Information on the lattice parameter of single crystals with known crystallographic structure allows for estimations of sample quality and composition. In many cases it is suffcient to determine one lattice parameter or the lattice spacing along a certain, high-symmetry direction, e.g. in order to determine the composition in a substitution series by taking advantage of Vegards rule. Here we present a guide to accurate measurements of single crystals with dimensions ranging from 200 $mu$m up to several millimeter using a standard powder diffractometer in Bragg-Brentano geometry. The correction of the error introduced by the sample height and the optimization of the alignment are discussed in detail. In particular for single crystals with a plate-like habit, the described procedure allows for measurement of the lattice spacings normal to the plates with high accuracy on a timescale of minutes.
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NeXus is an international standard data format intended to reduce the need for redundant software development efforts in the neutron and x-ray scattering communities. As the NeXus standard matures it is starting to be used at laboratories for storing raw data. The Manuel Lujan Jr. Neutron Scattering Center (MLNSC) at Los Alamos National Laboratory and the Intense Pulsed Neutron Source (IPNS) at Argonne National Laboratory have been working with NeXus in an effort to share data and software. MLNSC is now writing files compliant with NeXus and the Integrated Spectral Analysis Workbench (ISAW) software from IPNS is being used with this data. Problems can arise if the standard is interpreted in different ways and information that belongs in the file is not accounted for in the standard. This paper will discuss an inter-laboratory collaboration in relation to a maturing data standard.
Lithium doped sodium niobate is an ecofriendly piezoelectric material that exhibits a variety of structural phase transitions with composition and temperature. We have investigated the phase stabilities of an important composition Li0.12Na0.88NbO3 (LNN12) using a combination of powder x-ray and neutron diffraction techniques in the temperature range 300 - 1100 K. Detailed Rietveld analyses of thermo-diffractograms show a variety of structural phase transitions ranging from non-polar antiferrodistortive to ferroelectric in nature. In the temperature range of 525 K to 675 K, unambiguous experimental evidence is shown for phase coexistence of orthorhombic paraelectric O1 phase (space group Cmcm) and orthorhombic ferroelectric O2 phase (space group Pmc21). The bp primitive lattice parameter of the ferroelectric orthorhombic phase (O2 phase) decreases, while the ap and cp primitive lattice parameters show normal increase with increase in temperature. Above 675 K, in the O1 phase, all lattice parameters come close to each other and increase continuously with increase of temperature, and around 925 K, ap parameter approaches bp parameter and thus the sample undergoes an orthorhombic to tetragonal phase transition. Further as temperature increases, the cp lattice parameter decreases, and finally approaches to ap parameter, and the sample transform into the cubic phase. The continuous change in the lattice parameters reveals that the successive phase transformations from orthorhombic O1 to high temperature tetragonal phase and finally to the cubic phase are not of a strong first order type in nature. We argue that application of chemical pressure as a result of Li substitution in NaNbO3 matrix, favours the freezing of zone centre phonons over the zone boundary phonons that are known to freeze in pure NaNbO3 as function of temperature.
The diffraction technique is widely used in the determination of crystal structures and is one of the bases for the modern science and technology. All related structure determination methods are based on the assumption that perfect single crystal X-ray diffraction (SXRD) can determine a structure uniquely. But as the structure factor phases are lost in SXRD and even more information is lost in powder X-ray diffraction (PXRD), this assumption is still questionable. In this work, we found that structures with certain characteristic can have its sister structure with exactly the same PXRD or even SXRD pattern. A computer program is developed to search the ICSD database, and about 1000 structures were identified to have this characteristic. The original structure and its sister structures can have different space groups, topologies, crystal systems etc. and some may even have multiple sisters. Our studies indicate that special caution is needed since a structure with reasonable atomic positions and perfect match of experimental diffraction intensities could still be wrong.
The equations for calculating diffraction profiles for bent crystals are revisited for both meridional and sagittal bending. Two approximated methods for computing diffraction profiles are treated: multilamellar and Penning-Polder. A common treatment of crystal anisotropy is included in these models. The formulation presented is implemented into the XOP package, completing and updating the crystal module that simulates diffraction profiles for perfect, mosaic and now distorted crystals by elastic bending.
Enhancement of second harmonic generation (SHG) efficiency and the correlation between crystalline perfection and SHG with urea doping on tristhioureazinc(II) sulphate (ZTS) single crystals have been investigated. ZTS is a potential semiorganic nonlinear optical (NLO) material. Pure and urea doped single crystals of ZTS have been successfully grown by slow evaporation solution technique (SEST). Presence of dopants has been confirmed and analyzed by Fourier transform infrared (FTIR) spectrometer. The influence of urea doping at different concentrations on the crystalline perfection has been thoroughly assessed by high resolution X-ray diffractometry (HRXRD). HRXRD studies revealed that the crystals could accomodate urea in ZTS up to some critical concentration without any deterioration in the crystalline perfection. Above this concentration, very low angle structural grain boundaries were developed and it seems, the excess urea above the critical concentration was segregated along the grain boundaries. At very high doping concentrations, the crystals were found to contain mosaic blocks. The SHG effeiciency has been studied by using Kurtz powder technique. The relative SHG efficiency of the crystals was found to be increased substantially with the increase of urea concentration. The correlation found between the crystalline perfection and SHG efficiency was discussed.
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