Study of hyperfine interactions in Fe–Co nanocomposite films by Mössbauer spectroscopy and NMR

Nanogranular magnetic films were produced by the specially designed UHV plasma-jet system with DC hollow-cathode discharge. We investigated the properties of these ferromagnetic FeCo-AlN films. The samples were studied by nuclear magnetic resonance, Mössbauer spectroscopy, and transmission electron microscopy. The films are composed of nanoparticles of cubic FeCo, 2–10 nm in size, embedded in amorphous matrix containing Al, N and O. The Mössbauer spectra indicate that the orientation of local magnetic moments on the surface is random for the sample with 1:1 Fe/Co ratio, while the magnetization lays in the plane of the layer for samples with Fe/Co smaller than 1 (0.91–0.95).     

Study of the Phase Situation in 4-n-pentylphenyl-4′-n-heptyloxythiobenzoate (7S5)

Results of measurements of the specific heat of 4-n-pentylphenyl-4′-n-heptyloxythiobenzoate in the temperature range from about 90 K to about 370 K are presented. They were carried out with an adiabatic calorimeter, a differential scanning calorimeter and a polarizing microscope. Adiabatic calorimetry revealed four anomalies in the specific heat vs. temperature curve viz., two associated with transitions in the solid phase, one with melting and one with the liquid-crystalline nematic-to-isotropic phase transition. Also, two modifications of the solid, stable and metastable, were found to exist. In addition, the DSC method applied in the 285 K to 370 K range revealed a smectic C phase, but only when the sample is being cooled. The polarizing microscope showed the structural polymorphism of the solid phase in the 297 K to 327 K range to be more complex than would stem from adiabatic calorimetry and DSC measurements alone. It also confirmed the occurence of the S_c phase on cooling as ascertained by the DSC method.     

Study of the sulfur atom as hydrogen bond acceptor in N(2)-pyridylmethyl-N′-arylthioureas

The hydrogen acceptor capability of the sulfur atom in the biologically relevant N-2-pyridylmethyl-N-arilthioureas was explored. N-2-Pyridylmethyl thioreas were selected to avoid the formation of intramolecular six-membered hydrogen-bonded ring. The compounds studied were N-2-pyridylmethyl-N-phenylthiourea (1), N-2-pyridylmethyl-N-2-methoxythiourea (2), N-2-pyridylmethyl-N-4-methoxyphenylthiourea (3), and N-2-pyridylmethyl-N-4-bromophenylthiourea (4). 1 crystallizes in the monoclinic space group P2₁/c, with a = 7.419(1) Å, b = 18.437(2) Å, c = 9.656(1) Å, = 106.277(6)°, V = 1267.8(3) ų, Z = 4. 2 crystallizes in the monoclinic space group P2₁/c, with a = 8.064(2) Å, b = 18.382(7) Å, c = 9.865(5) Å, = 97.81(3)°, V = 1448.8(11) ų, Z = 4. 3 crystallizes in the monoclinic space group P2₁/c, with a = 11.472(1) Å, b = 13.520(1) Å, c = 10.088(1) Å, = 112.60(1)°, V = 1444.5(2) ų, Z = 4. 4 crystallizes in the triclinic space group P-1, with a = 4.583(3) Å, b = 10.263(3) Å, c = 14.396(3) Å, = 77.92(2)°, = 88.55(4)°, = 80.02(4)°, V = 652.1(5) ų, Z = 2. Both thiourea N–H groups form intermolecular hydrogen bonds, one with the thione sulfur atom and the other with the pyridine nitrogen atom but the H-bonding schemes are not the same maybe due to the flexibility of the molecules.     

Band gap determination by absorption spectrum fitting method (ASF) and structural properties of different compositions of (60−x) V2O5–40TeO2–xSb2O3 glasses

Glasses with compositions (60?x) V₂O₅–40TeO₂–xSb₂O₃ with 0 ? x ? 10 (in mol%) have been prepared using usual melt quenching method. The position of the absorption edge and hence the values of the optical band gap was found to depend on the glass composition. Using the Tauc model, the absorption spectrum fitting method (ASF) was employed to obtain the optical band gap. This method requires only the measurement of the absorbance spectrum of the sample. For each sample, the width of the band tail was determined. Also, the density and glass transition temperature values indicate that the rigidity and packing of the samples increase with increase in Sb₂O₃ concentration.     

Study of the Fracture Toughness of K2NixCo(1 – x)(SO4)2 · 6H2O Crystals in Dependence of the Growth Direction and Rate

Crystallography Reports - K2Ni(SO4)2 · 6H2O (KNSH), K2Co(SO4)2 · 6H2O (KCSH), and K2NixCo(1 – x)(SO4)2 · 6H2O (KCNSH) crystals have been grown by traditional...     

The Electron Diffraction Investigation of the Phase Structures in the Systems MF2–RF3 (CaF2–ErF3, SrF2–LaF3)

Crystallography Reports - The electron diffraction investigation of two-component phases in the systems MF2–RF3 (CaF2–ErF3, SrF2–LaF3) and components of the systems CaF2, SrF2,...     

Dielectric Study on the Alignment or Orientation of N(4-n-heptyloxy benzylidene)4´-n-butylaniline and the Anomalous Dielectric Behavior in the Smectic G Phase

The present article reports on the alignment or orientation of a particular compound N(4-n-heptyloxy benzylidene)4´-n-butylaniline through dielectric study. The effect of using two different alignment layers (for homogenous alignment) and doping silver nanoparticles (0.25% by weight) on the behavior in dielectric property with varying temperature and biasing electric field was studied in terms of liquid crystal alignment or orientation using the mechanism proposed by earlier workers. The study includes the anomalous dielectric behavior in SmG phase by presenting a technique for the analysis of the absorption process, which exists only in SmG phase at fixed frequency while varying temperature, is also presented.     

Growth of KR3F10 (R = Tb–Er) Crystals by the Vertical Directional Crystallization Technique. I: Optimization of the Melt Composition for the Growth of KTb3F10 and Correction of the Phase Diagram of the KF–TbF3 System

Crystallography Reports - KTb3F10 crystals have been grown from the melt by the vertical directional crystallization. The incongruent character of melting of this compound is confirmed...     

Antimicrobial Activity of Composite Hydrogels in the Poly(N-vinylpyrrolidone)–RE(NO3)3 · xH2O (RE Are Rare-Earth Ions) System

Crystallography Reports - The bactericidal and bacteriostatic properties (in darkness) of salts RE(NO3)3 · xH2O (RE = La, Ce, Gd, Yb, Y) and composite hydrogels with poly(N-vinylpyrrolidone)...     

Incorporation of group III,IV and V elements in 3C–SiC(1 1 1) layers grown by the vapour–liquid–solid mechanism

We report on a comparative investigation of the incorporation of group III, IV and V impurities in 3C–SiC heteroepitaxial layers grown by the vapour–liquid–solid (VLS) mechanism on on-axis α-SiC substrates. To this end, various Si-based melts have been used with addition of Al, Ga, Ge and Sn species. Homoepitaxial α-SiC layers grown using Al-based melts were used for comparison purposed for Al incorporation. Nitrogen incorporation depth profile systematically displays an overshoot at the substrate/epilayer interface for all the layers. Ga and Al incorporations follow the same distribution shape as N whereas this is not the case for the isoelectronic impurities Ge and Sn. This suggests some interaction between Ga/Al and N coming from the high bonding energy between the group III and V elements, which does not exist with Ge and Sn. This is why both incorporate as a cluster. A model of incorporation is proposed taking into account metal-N and metal-C bonding energies together with the solid solubility of the corresponding nitrides.     

Fabrication of Multilayer Films on the Basis of Lysozyme Protein and Precipitant (Iodide and Potassium) Ions on a Silicon Substrate by the Modified Langmuir–Schaefer Method

Multilayer structures, consisting of successive lysozyme layers and layers of iodide and potassium ions, have been formed on a silicon substrate by the modified Langmuir–Schaefer method; the use of this technique implies preliminary preparation of a crystallization protein solution containing an oligomeric phase. The multilayer structure has been characterized by methods of X-ray reflectivity and total external reflection X-ray standing waves (TER XSW). The data obtained indicate the formation of a dense lysozyme film (3 nm thick) and layers of potassium and iodide ions, adjacent to this film.     

Mössbauer Study of the Effect of Cation Substitutions on the Magnetic Phase Transitions in BiFe1 – xCrxO3 and (1 – x)BiFeO3–xPbFe0.5Sb0.5O3 Solid Solutions

Crystallography Reports - The concentration dependences of the magnetic phase transition temperature TN, determined based on the changes in Mössbauer spectra, were investigated for a BiFeO3...     

Growth of Crystals of Solid Solutions with Tysonite Structure in the PbF2–RF3 Systems (R = Pr,Nd)

Crystallography Reports - Crystals of the R1 – yPbyF3 – y (R = Pr (0 ≤ y ≤ 0.09) or Nd (0 ≤ y ≤ 0.10)) solid solutions with a...     

Production of Complex Hydrosulphates in the K3H(SO4)2–Rb3H(SO4)2 Series: Part I

Crystallography Reports - The phase equilibria in the K3H(SO4)2–Rb3H(SO4)2–H2O cross section have been investigated under isothermal conditions at 25°C. The concentration limits of...     

Hydrogen Bonding and Sulfur–Sulfur Interactions in the Crystal Structure of the Radical-Cation Salt (BPDT-TTF)2[W6O19]

Abstract  The synthesis and crystal structure of the salt (BPDT-TTF)₂[W₆O₁₉] is described. The compound crystallizes in the triclinic space group P − 1 with a = 10.927(2) ?, b = 11.904(2) ?, c = 12.660(2) ?, α = 101.261(5)°, β = 115.174(5)°, and γ = 114.434(5)°. The bond length of the central C=C bond in BPDT-TTF is 1.384(17) ?, in accord with an oxidation state of +1 for the BPDT-TTF radical-cations and the observed stoichiometry between BPDT-TTF and [W₆O₁₉]²⁻ which is 2:1. Index Abstract  The X-ray crystallographic structure of the radical cation salt (BPDT-TTF)₂[W₆O₁₉] has been determined and its structural features, including examples of interatomic interactions, as well as its synthetic preparation are discussed.      

Diphosphine ligand substitution in H4Ru4(CO)12: X-ray diffraction structures and reactivity studies of the cluster compounds H4Ru4(CO)10(P–P) [where P–P–(Z)–Ph2PCH–CHPPh2, bpcd]

The tetraruthenium cluster H₄Ru₄(CO)₁₂ (1) has been studied for its reactivity with the unsaturated diphosphine ligands (Z)–Ph₂PCH–CHPPh₂ and 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) under thermal, near-UV photolysis, and Me₃NO-assisted activation. All three cluster activation methods promote loss of CO and furnish the anticipated substitution products H₄Ru₄(CO)₁₀[(Z)–Ph₂PCH–CHPPh₂] (2) and H₄Ru₄(CO)₁₀(bpcd) (3) that possess a chelating diphosphine ligand. Clusters 2 and 3 have been characterized in solution by IR and NMR spectroscopies, and these data are discussed with respect to the crystallographically determined structure for both new cluster compounds. The ³¹P NMR spectral data and the solid-state structures confirm the presence of a chelating diphosphine ligand in clusters 2 and 3. Cluster 2 crystallizes in the monoclinic space P2₁/c, a=11.768(6) ?, b=18.521(9) ?, c=20.48(1) ?, β=102.291(8)°, V=4361(4) A³, Z=4, and d _calc=1.726 Mg/m³; R=0.0225, R _w=0.0491 for 6798 reflections with I > 2σ(I). The four bridging hydrides were located in H₄Ru₄(CO)₁₀[(Z)–Ph₂PCH–CHPPh₂] and their adopted positions are discussed relative to the solution ¹H NMR spectrum. H₄Ru₄(CO)₁₀(bpcd) crystallizes in the orthorhombic space Pbca, a=19.072(3) ?, b=20.169(3) ?, c=22.774(3) ?, V=8760(2) A³, Z=8, and d _calc=1.870 Mg/m³; R=0.0428, R _w=0.0896 for 10296 reflections with I > 2σ(I). Sealed NMR tubes containing clusters 2 and 3 were found to be exceeding stable towards near-UV light and temperatures up to ca. 125 °C. The surprisingly robust behavior of 2 and 3 is contrasted with the related cluster Ru₃(CO)₁₀(bpcd) that undergoes fragmentation to the donor-acceptor compound Ru₂(CO)₆(bpcd) and the phosphido-bridged compound Ru₂(CO)₆(μ–PPh₂)[μ–C–C(PPh₂)C(O)CH₂C(O)] under mild conditions. The electrochemical properties of each substituted cluster have been investigated by cyclic voltammetry, and our findings are discussed with respect to the reported electrochemical data on the parent cluster H₄Ru₄(CO)₁₂.

The Crystal-Chemical Features of Phases and the Nature of the Coordination Bond in the System [CuxNi(1 – x){N(CH2PO3)3}]Na4 · nH2O (x = 0–1)

Crystallography Reports - The structural features of the phases formed during crystallization of mixed copper and nickel complexes with nitrilotris(methylenephosphonic acid)...     

Production of Complex Hydrosulphates in the K3H(SO4)2–Rb3H(SO4)2 Series: II. Phase Equilibria in the K2SO4–Rb2SO4–H2SO4–H2O System

Crystallography Reports - The phase equilibria in the K2SO4–Rb2SO4–H2SO4–H2O system have been investigated under isothermal conditions at 25°C. The concentration limits of...