The structural response of BCC Fe lattice loaded in [110] direction

The structural response of BCC Fe lattice loaded in [110] direction has been investigated with MAEAM. The results show that, even if an orthorhombic path (b₂≠b₃) is applied, the deformation is spontaneous along the tetragonal path (b₂≡b₃) while b₁ is less than 0.3449nm in compressive region. In addition to the initial BCC phase, a BCT phase and the other BCC phase appear also at stress‐free states. The BCT phase with the local maximum internal energy of ‐4.227eV is unstable and would slip spontaneously into the appeared BCC phase with the same minimum internal energy of ‐4.280eV as the initial BCC phase. The stable region ranges from ‐43.87eV/nm³ to 44.06eV/nm³ in the theoretical strength or from ‐7.34% to 6.49% in the strain correspondingly. Furthermore, the relations B₁₁=B₂₂, B₁₃=B₂₃ and B₄₄=B₅₅ occur at the initial state. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal data and some physical properties of Tl2InGaTe4 crystals

The room temperature crystal data, Debye temperature, dark and photoelectrical properties of the Bridgman method grown Tl₂InGaTe₄ crystals are reported for the first time. The X‐ray diffraction technique has revealed that Tl₂InGaTe₄ is a single phase crystal of tetragonal body‐centered structure belonging to the space group. A Debye temperature of 124 K is calculated from the results of the X‐ray data. The current‐voltage measurements have shown the existence of the switching property of the crystals at a critical voltage of 80 V. The dark electrical resistivity and Hall effect measurements indicated the n ‐type conduction with an electrical resistivity, electron density and Hall mobility of 2.49×10³ Ω cm, 4.76×10¹² cm^–3 and 527 cm²V^–1s^–1, respectively. The photosensitivity measurements on the crystal revealed that, the variation of photocurrent with illumination intensity is linear, indicating the domination of monomolecular recombination at room temperature. Moreover, the spectral distribution of the photocurrent allowed the determination of the energy band gap of the crystal studied as 0.88 eV. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

High resolution neutron and X‐ray diffraction studies as a function of temperature and electric field of the ferroelectric phase transition of RDP

Neutron and high resolution X‐ray diffraction investigations on perfect single crystals of RbH₂PO₄ (RDP), a hydrogen bonded ferroelectric of KDP type are reported. The results of crystal structure analysis from diffraction data, below and above the paraelectric ‐ ferroelectric phase transition, support a disorder ‐ order character of [PO₄H₂]^‐‐groups. The tetragonal symmetry of the paraelectric phase with the double well potential of the hydrogen atoms obtained by diffraction, results simply from a time‐space average of orthorhombic symmetry. According to the group ‐ subgroup relation between the tetragonal space group I42d and the orthorhombic Fdd2 a short range order of ferroelectric clusters in the tetragonal phase is observed. With decreasing temperature the ferroelectric clusters increase and the long range interaction between their local polarisation vectors leads to the formation of lamellar ferroelectric domains with alternating polarisation directions at T_C = 147 K. From the high resolution X‐ray data it is concluded that below T_C the ferroelastic strain in the (a,b)‐plane leads to micro‐angle grain boundaries at the domain walls. The tilt angle is enhanced by an applied electric field parallel to the ferroelectric axis. The resulting dislocations at the domain walls persist in the paraelectric phase leading to a memory effect for the arrangement of twin lamellae. With increased electric field the phase transition temperature T_C is decreased. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical properties of pure and metal ions doped ammonium sulfate single crystals

A study of the optical properties of pure‐and some metal ions doped ammonium sulfate crystals (AS) were made. Optical constants of AS crystals were calculated at room temperature. The optical absorption coefficient (α ) was analyzed and interpreted to be in the allowed direct transition. The introduction of Rb⁺ or Cs⁺ ions gives rise to an intense charge transfer band with a maximum at λ= 310 nm in the optical spectrum. In case of Cr³⁺ ‐doping, the absorption shows a shoulder just before the onset band to band transition. The values of the allowed direct energy gap E_g for undoped and doped crystals were calculated. It was found that E_g values were decreased with metal ions doping. The refractive index, the extinction coefficient and both the real and imaginary parts of the dielectric permittivity were calculated as a function of photon energy. The validity of Cauchy‐Sellimeier equation was checked in the wavelength range 4.9 ‐ 5.6 eV and its parameters were calculated. Applying the Single‐Effective‐Oscillator model, the moments of ε (E ) could be estimated. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Data,Electrical Resisitivity and Mobility in Cu3In5Se9 and Cu3In5Te9 Single Crystals

X-ray powder diffraction data were obtained for Cu₃In₅Se₉ and Cu₃Te₉, which were found to crystallize in orthorhombic and tetragonal systems, respectively. The electrical resistivities and Hall mobilities of these compounds were investigated in the temperature range 35–475 K. Cu₃In₅Se₉, was identified to be n-type with a room temperature resistivity of 3 × 10³ Ω·cm which decreases with increasing temperature. For T < 65 K impurity activation energy of 0.03 eV and for T > 350 K onset of intrinsic conduction yielding a band gap energy of 0.99eV were detected. The neutral impurity scattering was found to dominate at low temperatures, while in the high temperature region thermally activated mobility was observed. Cu₃In₅Te₉ exhibits p-type conduction with a room temperature resistivity of 8.5 × 10⁻³ Ω·cm decreasing sharply above 400 K and yielding an impurity ionization energy of 0.13 eV. The temperature dependence of mobility indicates the presence of lattice and ionized impuritiy scattering mechanisms above and below 160 K, respectively.     

X‐ray powder diffraction structural characterization of Ba1‐xEuxTiO3 ternary oxides

The single‐phase Ba_1‐xEu_xTiO₃ (0.1≤x≤0.4) samples have been synthesized by solid state reaction under high pressure and ‐temperature. X‐ray powder diffraction data was determined by MS Modeling using Reflex Powder Indexing technique. The Ba_1‐xEu_xTiO₃ series exhibited an interesting orthorhombic‐tetragonal‐cubic structural transformation as Eu composition increases, the distinct change of the X‐ray diffraction peak profile in the vicinity of 45.5º is characteristic of structural transformation. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural Characterization of Y2Pd14B5

Y₂Pd₁₄B₅ is the major phase in as‐cast and annealed multiphase alloys with nominal compositions near YPd₅B₃C_0.3. Its crystal structure determined the first time here by single crystal X‐ray diffraction is body‐centered tetragonal (space group I4₁/amd). Transmission electron microscopy (TEM) reveals that in as‐cast specimens the tetragonal phase has a modulated structure and is oriented intergrown with a face‐centered cubic phase of similar composition, namely YPd₇B₂. According to Rietveld analyses of the multiphase system the structure of this phase can be well‐described by space group Fm m. Annealing the sample for 150 hrs at 973 K results in a coarsening and enrichment of the tetragonal phase as well as a disappearance of the modulations allowing a detailed structure analysis by single crystal diffractometry.     

On the capability of revealing the pseudosymmetry of the chalcopyrite‐type crystal structure

The tetragonal crystal‐structure type of chalcopyrites (chemical formula A^IB^IIIC^VI₂) is a superstructure of sphalerite type. The c /a ratio differs generally from the ideal value 2, i.e., the crystal structure is pseudocubically distorted. For CuInSe₂ and CuGaSe₂ thin films, simulations demonstrate that it is theoretically possible to reveal the tetragonality in electron backscatter‐diffraction (EBSD) patterns for CuGaSe₂, whereas it may not be possible for CuInSe₂. EBSD experiments on CuGaSe₂ thin films using the ”Advanced Fit” band‐detection method show that it is possible to extract accurate misorientation‐angle distributions from the CuGaSe₂ thin film. Pole figures revealing the texture of the CuGaSe₂ thin film are shown, which agree well with X‐ray texture measurements from the same layer. (© 2008 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure,dielectric properties of (K0.5Na0.5)NbO3 single crystal grown by flux method using B2O3 flux

Lead free piezoelectric single crystals of sodium potassium niobate (K_0.5Na_0.5)NbO₃ (KNN) were grown by high‐temperature solution method using two different fluxes; one with a mixture of NaF and KF and other with addition of B₂O₃ along with the mixture. In the present study, the growth of KNN crystals without B₂O₃ flux and the same with B₂O₃ flux were compared. It was found that additions of small amounts of B₂O₃ lowered the melting temperature of the solid solution and enabled better dielectric properties. Phase analysis showed that all samples were crystallized in pure orthorhombic perovskite phase. AFM morphological studies showed that the addition of B₂O₃ flux increased the roughness of the grown crystal. Further, addition of B₂O₃ flux slightly decreased the orthorhombic to tetragonal phase transition temperature T_(O—T) and the Curie temperature T_C. The ferroelectric behaviour of KNN single crystal has been investigated at room temperature. The crystal grown using B₂O₃ flux exhibited a remanent polarization (P_r) ∼ 32 μC/cm² and coercive field (Ec) of ∼11.8 kV/cm whereas the crystal grown without the use of B₂O₃ flux had a remanent polarization (P_r) ∼ 36 μC/cm² and coercive field (Ec) of ∼14.6 kV/cm.     

Flux growth and low temperature dielectric relaxation in piezoelectric Pb[(Zn1/3Nb2/3)0.91Ti0.09]O3 single crystals

Single crystals of Pb[(Zn_1/3Nb_2/3)_0.91Ti_0.09]O₃ (PZNT 91/9) have been grown by flux method after modifications in temperature profile, flux ratio and addition of excess ZnO/B₂O₃ which resulted in enhanced perovskite yield (more than 95%). Only a few crystals showed the presence of pyrochlore phase/variation in composition. A comparative characterization of these crystals were carried out in respect of piezoelectric charge coefficient d₃₃, dielectric constant, ac conductivity and hysteresis loop after cutting and poling the crystals along [001] direction. The total activation energy for conduction has been found to increase with Ti‐content in the sample. The effect of ZnO on growth behavior has been analyzed. A detailed analysis of PZNT (91:9) has been carried out at low temperature in respect of the various thermodynamic parameters related to the dielectric relaxation mechanism, like optical dielectric constant, static dielectric constant, free energy of activation for dipole relaxation, enthalpy of activation and relaxation time, have been calculated in the vicinity of transition temperature in the lower temperature region. The activation energy for relaxation at ‐10 and ‐49 °C have been found to be 0.09 and 0.02 eV respectively. The results were analyzed and a detailed dielectric analysis and low temperature relaxation behavior of PZNT crystals were interpreted. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and X‐ray powder diffraction studies of semiconducting alloys in the system AgCd2‐xZnxGaS4

X‐ray powder technique was used in the investigation of AgCd₂GaS_4–'AgZn₂GaS₄' section to determine the region of AgCd₂GaS₄‐based solubility. It was established that the solid solution forms up to 75 mol.% 'AgZn₂GaS₄'. The refinement of AgCd_0.5Zn_1.5GaS₄ structure was performed. This alloy crystallizes in orthorhombic structure (space group Pmn2₁ ) with unit cell parameters a =0.78772(2), b =0.67221(2), c =0.64019(2) nm, V =0.33899(3) nm³. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Zur Bestimmung der Gitterkonstanten und der Orientierung nichtkubischer Kristalle mit der Pseudo-Kossel-Technik

Pseudo-Kossel-patterns are very usefull for the study of small monocrystalline regions. This paper deals with a method, which permits the evaluation of transmission patterns without knowledge of the distance between the X-ray source and the film. The center of a Pseudo-Kossel-Diagramm is determined during the procedure of evaluation, and the crystal can be oriented with respect to the film in any desired way. By the method presented here it is possible to determine the reciprocal lattice of cubic, tetragonal, hexagonal and orthorhombic crystals and their orientation. To know the lattice parameters is not necessary. The method permits the estimation of lattice parameters with an inaccuracy λa/a ≈ ± 1 · 10⁻⁴ even for relatively small Bragg-angles. To demonstrate the procedure tetragonal ZnSiP₂ is used.     

Crystallization and structural studies of n‐benzyloxycarbonyl‐L‐tyrosine‐L‐glycine‐ethyl ester (Z‐Tyr‐Gly‐OEt)

It is axiomatic that efficient crystal production reflects upon the quality of structure. An empirical relation for mass proportions of two solvents in crystallization of Z‐Tyr‐Gly‐OEt shows a linear relationship. The dipeptide crystallizes in orthorhombic space group P2₁2₁2_1, with cell parameters a = 5.0680(1) Å, b = 13.8650(1) Å and c = 28.2630(1) Å, Z = 4, D_calc= 1.339Mg/m³, μ=0.820mm^‐1, F₀₀₀=848, CuKα = 1.5418 Å. The structure was solved by direct methods and final R1 and wR2 are 0.444 and 0.1276, respectively. The structure analysis reveals the trans conformation of the peptide unit with ω = ‐178.2(5)°, implying only a slight deviation from planarity. The torsion angles at glycine [ϕ, ψ = ‐84.4(7)°, 179.9(5)°] are characteristic of left‐handed poly glycine II helices. A number of N‐H…O, O‐H…O and C‐H…O hydrogen bondings play a role in stabilizing the molecules within unit cell. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

An optical microscopy study of the biaxial ‐ calamitic nematic lyotropic phase transition

Lyotropic nematic textures are investigated, using optical microscopy, near the reentrant isotropic (I_RE) ‐ discotic nematic (N_D^‐) ‐ biaxial nematic (N_B) ‐ calamitic nematic (N_C⁺) ‐ isotropic (I) phase transitions in a lyotropic mixture of potassium laurate, decanol and D₂O. The N_B, intermediate phase between the two uniaxial nematic ones, is characterized by optical birefringence measurements. In this way, using a polarizing microscope and a colour CCD digital camera, the N_B – N_C⁺ phase transition is identified as well as the domain of the N_B phase and N_D^‐ – N_B transition point in accordance with optical birefringence data (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Transport Properties of (NH4)2 CuCl4.2H2O Low Dimensional Single Crystals

The X‐ray diffraction and Infrared (IR) spectral studies of (NH₄)₂ CuCl₄.2H₂O single crystals reveals that these crystals contains tetragonal crystal structure with the unit cell dimensions of a = 7.58Å, c = 7.95Å, z= 2, β =90° and two water molecules in the unit cell. The temperature dependence of thermally stimulated depolarization current (TSDC) and dc electrical conductivity (σ) studies of this two‐dimensional (NH₄)₂ CuCl₄.2H₂O single crystal have been carried out in 77K–300K temperature region. The TSDC thermograph shows only one sharp peak at 248K with a peak current of 130nA, which is attributed to the Maxwell‐Wagner peak. The activation energy (U), relaxation time (τ) are calculated as 0.78eV and 3.44×10^‐15 s respectively. Dc electrical conductivity studies of these crystals show a first order phase transition at about 248K.     

High temperature x‐ray diffraction studies of zirconia thin films prepared by reactive pulsed laser deposition

Zirconium oxide thin films have been deposited on Si (100) substrates at room temperature at an optimized oxygen partial pressure of 3x10^‐2 mbar by reactive pulsed laser deposition. High temperature x‐ray diffraction (HTXRD) studies of the film in the temperature range room temperature‐1473 K revealed that the film contained only monoclinic phase at temperatures ≤ 673 K and both monoclinic and tetragonal phases were present at temperatures ≥ 773 K. The tetragonal phase content was significantly dominating over monoclinic phase with the increase of temperature. The phase evolution was accompanied with the increase in the crystallite size from 20 to 40 nm for the tetragonal phase. The mean thermal expansion coefficients for the tetragonal phase have been found to be 10.58x10^‐6 K^‐1 and 20.92x10^‐6K^‐1 along a and c‐axes, respectively. The mean volume thermal expansion coefficient is 42.34x10^‐6 K^‐1 in the temperature range 773‐1473 K. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Temperature variation of the structural and thermal characteristics of YBa2Cu3O7−x in the range from 90 to 400 K

The X-ray studies of the tetragonal YBa₂Cu₃O_7−x compound are performed at different temperatures from 400 to 90 K and the temperature variation of the thermal expansion coefficients and the Debye characteristic temperature is determined. The anisotropy of thermal expansion is investigated. It is found that the two dynamical characteristics monotonously decrease with temperature lowering whereas for the superconducting orthorhombic modification their temperature dependences are anomalous. The mean thermal expansion coefficient as well as the overall Debye temperature for the tetragonal phase are smaller than those for the orthorhombic one.     

In‐situ investigation of the temperature dependent structural phase transition in CuInSe2 by synchrotron radiation

The temperature dependent structural phase transition from the tetragonal chalcopyrite like structure to the cubic sphalerite like structure in CuInSe₂ was investigated by in‐situ high temperature synchrotron radiation X‐ray diffraction. The data were collected in 1K steps during heating and cooling cycles (rate 38 K/h). The Rietveld analysis of the diffractograms led us to determine the temperature dependence of the lattice parameters, including the tetragonal deformation, |1‐η|, and distortion |u‐¼| (η=c/2a, a and c are the tetragonal lattice constant; u is the anion x‐coordinate). The thermal expansion coefficients α_a and α_c of the tetragonal lattice constant which are related to the linear thermal expansion coefficient α_L were obtained, as were α_a of the cubic lattice constant, also α_u and α_η. The transition temperature is clearly identified via a strong anomaly in α_L. The temperature dependence of the anion position parameter was found to be rather weak, nearly α_u∼0, whereas α_η increases slightly. However, both increase strongly when approaching to within 10 K of the transition temperature (the critical region) and |1‐η| as well as |u‐¼| go to zero with |T‐T_trans|^0.2 approaching the phase transition. The cation occupancy values, derived from the Rietveld analysis, remain constant below the critical region. Close to the transition temperature, the number of electrons at the Cu site increases with a dercrease in the number of electrons at the In site with increasing temperature, indicating a Cu‐In anti site occupancy, which is assumed to be the driving force of the phase transition. At the transition temperature 67% of Cu⁺ were found to occupy the Me1 site with a corresponding 67% of In³⁺ at the Me2 site. Although full disorder is reached with 50%, this level seems to be high enough that the phase transition takes place. The order parameter of the phase transition, goes with |T‐T_trans|^β to zero with the critical exponent β=0.35(7) which is in good agreement to the critical exponent β=0.332 calculated for order‐disorder transitions according to the Ising model. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Kinetics of crystallization of FeB-based amorphous alloys studied by neutron thermo-diffractometry

Kinetics of crystallization of two amorphous alloys, Fe₇₀Cr₁₀B₂₀ and Fe₈₀Zr₁₀B₁₀, have been followed up by neutron thermo-diffractometry experiments performed in the two axis diffractometer D20 (Institut Laue-Langevin, Grenoble). The structural changes are directly correlated with the temperature dependence of the magnetization. Fe₇₀Cr₁₀B₂₀ crystallizes following a two-step process: an eutectic crystallization of α-Fe (BCC) and the metastable tetragonal phase (Fe_0.8Cr_0.2)₃B followed by another eutectic transformation to the stable phase (Fe_0.75Cr_0.25)₂B and more segregation of α-Fe. These tetragonal phases are magnetically anisotropic, giving rise to a large increase of the coercivity. This behavior is similar to that of Fe₈₀B₂₀ alloys, with Cr atoms replacing the Fe positions in both crystalline phases. Fe₈₀Zr₁₀B₁₀ shows also a two-step process in which two polymorphic transformations take place.     

Identification of crystal symmetry in Kramers and non‐Kramers ions by optical absorption: Divalent copper and nickel ions in diamagnetic lattices

The optical absorption spectra of Ni(II) doped hexaimidazole zinc(II) dichloride tetrahydrate (HZDT) and Cu(II) doped magnesium potassium phosphate hexahydrate (MPPH) have been studied at room temperature. Ni(II)/HZDT spectrum consists of three strong and one weak band. The calculated value of Dq is 1051 cm^‐1 and the interelectron repulsion parameters B and C are 854 and 3626 cm^‐1 respectively. The correlation of optical work with EPR has yielded the spin‐orbit interaction parameters λ and ξ as –225 and –450 cm^‐1 respectively. The symmetry around the Ni(II) ion is distorted octahedral, as suggested by EPR results. The estimated percentage covalency of the nickel‐nitrogen bond is around 30%. The optical absorption studies of Cu(II)/MPPH show three bands, which are identified as ²B_1g → ²A_1g, ²B_1g → ²B_2g and ²B_1g → ²E_g transitions. The octahedral field parameter Dq and the tetragonal field parameters have been evaluated from the observed adsorption bands. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)