Changes of structural properties of tobermorite in autoclaved aerated concrete (AAC) for various compositions were characterized and the disadvantages of SEM analysis in this context are discussed. The influence of variations in the chemical composition of raw materials on lattice parameters, morphology and domain sizes of tobermorite was investigated by XRD and for comparison by SEM analysis. Particularly the effect of substitution by Al3+ and (SO4)2− in tobermorite structure was examined. The dimensions of coherently scattering domains were calculated based on the refinement of anisotropic peak broadening of tobermorite in XRD diffractograms using a Rietveld compatible approach. No effect of (SO4)2− on the domain sizes and lattice parameters of tobermorite could be observed. The amount of anhydrite detected by quantitative XRD analysis indicates that all of the available (SO4)2− is present as anhydrite. Lath-like shapes of domains and a larger c parameter are calculated whenever Al3+ is incorporated in a considerable amount. Formation of katoite can be observed very clearly in SEM micrographs whenever the amount of available Al3+ exceeds a distinct value in the dry mix. The effect of Al3+ and (SO4)2− on tobermorite morphology could not be observed clearly by SEM analysis in AAC samples.

In spite of the wide availability of automated diffractometers and advanced data reduction software, numerous traditional problems still exist that make highly precise and accurate quantitative analyses of complex mixtures difficult. The problems include particle statistics, primary extinction, microabsorption, preferred orientation, overlapping and broad reflections, variation in standard data with composition, availability of pure standards, and detection of amorphous and trace phases. Our analyses of rocks use the matrix flushing method on < 5μm particle-size material mixed with a 1.0-μm corundum internal standard to minimize the first four effects. Integrated intensities are used, and we employ several peaks from each phase whenever possible. We overcame overlap problems through iterative calculations using integral, multiple peaks or with profile refinement. Use of observed and calculated diffraction patterns for every phase enables us to predict the effects of composition and preferred orientation on RIRs. This allows us to correct for these effects if reference intensity ratios (RIRs) are known as a function of composition and orientation. Detection of amorphous phases is a significant problem, and standard mixtures reveal that amounts of amorphous components below 30% are difficult to detect. The poor detection limit and the nature of the diffraction band from amorphous phases make internal standard or spiking methods the best approach for analyzing samples containing amorphous materials. The Rietveld method of quantitative analysis has the potential to minimize all of the above problems. This method requires a knowledge of the crystal structures of all component crystalline phases, but no calibration data are necessary, structural and cell parameters can be varied during the refinement process, so that compositional effects can be accommodated and precise cell parameters can be obtained for every phase. Since this method fits the entire diffraction pattern and explicitly uses all reflections from every phase, complex, overlapped patterns can be easily analysed. In addition, this method presents the opportunity to correct for preferred orientation and microabsorption during data analysis.

The importance of software continues to grow for all areas of scientific research, no less for powder diffraction. Knowing how to program a computer is a basic and useful skill for scientists. This paper explains the three approaches for programming languages and why scripting languages are preferred for non-expert programmers. The Python-scripting language is extremely efficient for science and its use by scientists is growing. Python is also one of the easiest languages to learn. The language is introduced, as well as a few of the many add-on packages available that extend its capabilities, for example, for numerical computations, scientific graphics, and graphical user interface programming. Resources for learning Python are also provided.

A mathematical model for interpreting the anisotropical broadening of the powder diffraction lines by an average crystallite in the form of a triaxial ellipsoid is developed. The model covers satisfactorily a broad range of averaged crystallite shapes in polycrystalline samples of all crystal symmetries and provides simple formulas for use in powder pattern fitting routines. When ra, rb, rc are the principal ellipsoid radii, and ca, cb, cc direction cosines of diffraction vector related to the principal axes of ellipsoid, the average dimension of crystallites along the diffraction vector (Dhkl) is: Dhkl=K/ca2/ra2+cb2/rb2+cc2/rc2. The coefficient K has the value 3/2 if Dhkl is the volume average dimension of crystallites along the diffraction vector, or 4/3 in the case of the surface average dimension. The appropriate expression for use in whole pattern fitting routines is: b11h2+b22k2+b33l2+2b12hk+2b13hl+2b23kl=K2/Lhkl2dhkl2, where bij are the elements of a second-rank symmetric tensor. Finding eigenvalues and vectors of tensor b gives dimensions and orientations of the principal ellipsoid radii in reciprocal lattice values.

Without experimental or predicted literature crystal structures for succinonitrile at low temperature, structure solution was attempted from powder diffraction data taken at 173 and 90 K from a solid sample. Its room-temperature plastic-crystal state makes production of a sample with good particle statistics and random orientation almost impossible. Combining constrained models, simulated annealing, and careful application of second-order spherical harmonic corrections nevertheless produced viable-looking structures at 90 and 173 K, yielding two distinct structure models with the same projection down c. VASP optimization of atom coordinates in the experimental cell agreed well with the 90 K model but poorly with the model derived from the 173 K data. The refined 90 K structure changed little on optimization and fitted all datasets from 85 to 225 K. Plots of cell data, torsion angles, and isotropic displacement parameters against temperature suggest possible phase transitions around 100, 120, and 180 K. Cell data at 90 K: monoclinic P21/a, a=9.0851(5) Å, b=8.5617(5) Å, c=5.8343(3) Å, β=79.295(2)°, and Z=4. Succinonitrile has gauche conformation, in agreement with literature spectroscopy data.

Ba(3−x)Srx(PO4)2 orthophosphates (0≤x≤3) have been prepared by solid state reaction. The final temperature was 1000°C. The X-ray diffraction analyses show the existence of a continuous solid solution. Ba(3−x)Srx(PO4)2 orthophosphates (0≤x≤3) crystallize in the hexagonal system with the space group R3m. Their structure is based on a three-dimensional framework constructed of infinite layers of Ba1/Sr1O12 linked and parallel to infinite layers of Ba2/Sr2O10 polyhedra and PO4 tetrahedra.

Amino acids often cocrystallize with water molecules, which make them pseudopolymorphs of their anhydrous forms. In this work, we discuss in detail the hydrogen bond patterns in anhydrous L-proline and DL-proline and its pseudopolymorphic forms: L-proline monohydrate and DL-proline monohydrate. For this propose, the crystal structure of L-proline anhydrous was determined from synchrotron X-ray powder diffraction data and refined using the Rietveld method. Special emphasis is given to the role played by the water molecule in the hydrogen bond network observed in the crystalline structures.

A computer program is presented that allows for the merging of diffraction patterns collected at multiple positions on the Powder Diffraction beamline of the Australian Synchrotron. It is also generally applicable to detector systems based on other modular detectors. The program allows for the interpolation of data to a constant 2θ step size and to normalise intensities to beam current and/or monitor count rate.

The residual stress left on the fracture surface is one of the important parameters in X-ray fractography and has been used to analyse fracture mechanisms in fracture toughness, stress corrosion cracking and fatigue tests especially of high strength steels.

In this study, the distribution of residual stress near fatigue fracture surfaces made in air and in 3.5% NaCl solution was measured by the X-ray diffraction method. The effect of aqueous environment on the plastic deformation near fatigue fracture surfaces was discussed on the basis of the residual stress distribution.

ZnGa2Te4 was found to crystallize in a defect tetrahedral structure with possible space group I4(82) with Z=2. Complete X-ray powder diffraction data were obtained and the unit cell parameters a and c and X-ray density were calculated. These were a=0.5930(1) nm, c=1.1859(3) nm, and Dx=5.7×103 kg/m3.

Optimized vacuum spectrographic measurement of low-energy fluorescence has been found to yield counting rates and peak-to-background ratios which are enough to permit the extension of fluorescence analysis for elementary chemistry into the light-element range—sodium through boron. This is accomplished with an efficient, demountable ultrasoft X-ray source, with close coupling among source, crystal, and detector, with KAP and multilayered stearate analyzers, and with, optimized flow-propordonal counting. Specific methods for achieving peak-to-background ratios on practical samples containing these light elements are presented. The extension of these methods of light-element analysis with the use of curved long-spaced crystals for X-Ray macroprobe and electron microprobe measurements is discussed. The design and construction of multilayered soap film “crystals” for long-wavelength X-ray analysis is described.

Synchrotron X-ray diffraction was used to monitor the hydrothermal precipitation of akaganeite (β-FeOOH) and its transformation to hematite (Fe2O3) in situ. Akaganeite was the first phase to form and hematite was the final phase in our experiments with temperatures between 150 and 200 °C. Akaganeite was the only phase that formed at 100 °C. Rietveld analyses revealed that the akaganeite unit-cell volume contracted until the onset of dissolution, and subsequently expanded. This reversal at the onset of dissolution was associated with a substantial and rapid increase in occupancy of the Cl site, perhaps by OH− or Fe3+. Rietveld analyses supported the incipient formation of an OH-rich, Fe-deficient hematite phase in experiments between 150 and 200 °C. The inferred H concentrations of the first crystals were consistent with “hydrohematite.” With continued crystal growth, the Fe occupancies increased. Contraction in both a- and c-axes signaled the loss of hydroxyl groups and formation of a nearly stoichiometric hematite.

The study presents the results of the influence of high-energy ball-milling time on the structure of the new β-type Ti–Ta–Nb–Zr alloys for biomedical applications. Initial elemental powders were mechanically alloyed in a planetary high-energy ball mill at different milling times (from 10 to 90 h). Observation of the powder morphology after various stages of milling leads to the conclusion that with the increase of the milling time the size of the powder particles as well as the degree of aggregation change. Clear tendency of crystalline size reduction at every stage of the grinding process is clearly observed. The X-ray diffraction results confirmed the formation of β phase during high-energy ball milling of the precursor mixture of Ti, Ta, Nb, and Zr. The Rietveld refinement method has shown that both the production method and the atomic radii of the elements used in the mechanical synthesis have influence on the structure. Furthermore, it was found that a broadening of the diffraction peaks with increase of the milling time results from an increase in the crystallites dispersion and an enlargement in the lattice distortion. The results indicate that this technique is a powerful and high productive process for preparing new β-titanium alloys with nanocrystalline structure and appropriate morphology.

The purpose of this paper is to give a rapid overview of the recent developments in the field of X-ray diffraction on polycrystalline materials from the viewpoint of the instruments. After a brief historical report, the main types of laboratory diffractometers are presented. At the end of the twentieth century the apparition of position sensitive detectors and artificial crystal monochromators have induced the conception of new diffractometer often based on old geometrical arrangements. Those modern diffractometers are described with respect to the more conventional ones. Among the experimental parameters which can characterize a given diffractometer, the instrumental resolution function and the acquisition time of the pattern are of primary importance. The different apparatus are compared with respect to those two parameters.

Bright apple green millimeter-sized crystals of tavorite from the Tip Top pegmatite, near Custer, South Dakota are triclinic, space group , with refined unit-cell parameters a = 5.340(2), b = 7.283(2), c = 5.110(2)Å, α = 109.29(2)°, β = 97.86(3)°, γ = 106.32(3)°, V = 174.1(3)Å3, a:b:c = 0.7332:1:0.7016, Z = 2, D(m) (suspension in methylene iodide) = 3.32(1) and D(x) = 3.33 g/cm3 (for the theoretical formula). A fully indexed X-ray powder pattern is presented. Semiquantitative electron microprobe and secondary ion mass spectroscopic analyses indicate a formula near end-member LiFe + 3(PO4)(OH). The Tip Top tavorite is biaxial positive, α = 1.795(5), β = 1.81(1), γ = 1.86(1), 2V(meas.) = 50(2)°, 2V(calc.) = 59°, XΛa ≃ 15°, YΛb ≃ 0°, and ZΛc ≃ 38°. There is no evidence for optical absorption, pleochroism or dispersion.

The crystal structures of some nickel hexacyanoferrates (II, III), including mixed compositions containing Na+, K+ and Cs+, were resolved and refined from XRD powder patterns. Data from infrared, Mössbauer and adsorption techniques provided complementary structural information. The crystal structures of Ni3[Fe(CN)6]2⋅16H2O and NiCs2[Fe(CN)6] were refined in space group Fm3m. NiNa2[Fe(CN)6]⋅2H2O and NiK2[Fe(CN)6]⋅2H2O were found to be orthorhombic (space group Pmn21). This structure (Pmn21) results from a distortion around the alkali ion, which appears as a monohydrated interstitial species. On ionic exchange in an aqueous solution containing Cs+, the orthorhombic distortion disappears and the cubic cell is obtained. Cs+ is a large cation and space is not available for interstitial water molecules. This orthorhombic model is also supported by the Mössbauer spectra of the ferrous analogs, FeK2[Fe(CN)6]⋅xH2O and Fe[Pt(CN)6]. © 2004 International Centre for Diffraction Data.

The crystal structures of calcium citrate hexahydrate, calcium citrate tetrahydrate, and anhydrous calcium citrate have been solved using laboratory and synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Both the hexahydrate and tetrahydrate structures are characterized by layers of edge-sharing Ca coordination polyhedra, including triply chelated Ca. An additional isolated Ca is coordinated by water molecules, and two uncoordinated water molecules occur in the hexahydrate structure. The previously reported polymorph of the tetrahydrate contains the same layers, but only two H2O coordinated to the isolated Ca and two uncoordinated water molecules. Anhydrous calcium citrate has a three-dimensional network structure of Ca coordination polyhedra. The new polymorph of calcium citrate tetrahydrate is the major crystalline phase in several commercial calcium supplements.

Detailed structural properties of La1−xBaxCoO3 (LBCO) have been investigated by means of X-ray powder diffraction and Rietveld analysis. A structural phase transformation from R3c to Pm3m at x=0.30–0.35 has been detected based on a comparison between the refinements of R3c and Pm3m. The Co–O bond length of the CoO6 octahedron expanded rapidly with increasing Ba content when x<0.1, and then it leveled off and kept constant at 0.1⩽x⩾0.35, where the Co–O–Co bond angle reaches 180°. The Co–O bond length expansion resumed with increasing Ba content beyond x=0.35.

XLENS is a traditional direct methods program working exclusively in reciprocal space. The distinctive feature of XLENS is the use of the modulus sum function as target function for the phase refinement. Due to its efficiency, robustness, and no need of weighting schemes, this function is specially well suited for treating powder diffraction data. The mathematical basis as well as the significance of the most important control parameters of the program will be described here. To illustrate how XLENS works, three different examples will be shown. Due to its simplicity, the modulus sum function can be easily combined with real-space filtering procedures to produce even more efficient crystal structure solving strategies.

Total scattering data of nanocrystalline gahnite (ZnAl2O4, 2–3 nm) have been collected with three of the most commonly used instruments: (i) ID31 high-resolution diffractometer at the European Synchrotron Radiation Facility (ESRF) (Q max = 22 Å−1); (ii) ID11 high-energy beamline at the ESRF (Q max = 26.6 Å−1); and (iii) Empyrean laboratory diffractometer by PANalytical with molybdenum anode X-ray tube (Q max = 17.1 Å−1). Pair distribution functions (PDFs) for each instrument data-set have been obtained, changing some of the parameters, by PDFgetX3 software, with the aim of testing the software in the treatment of different total scattering data. The material under analysis has been chosen for its nanometric (and possibly disordered) nature, to give rise to a challenge for all the diffractometers involved. None of the latter should have a clear advantage. The PDF and F(Q) functions have been visually compared, and then the three PDF sets have been used for refinements by means of PDFgui suite. All the refinements have been made exactly in the same way for the sake of a fair comparison. Small differences could be observed in the experimental PDFs and the derived results, but none of them seemed to be significant.