Approaches for evaluating Young's and shear moduli in terms of a single SAW velocity via the SAM technique

In ultrasonic material investigations Young's modulus, E, and shear modulus, G, conventionally expressed in terms of the velocities of longitudinal (V_L,) and transverse (V_T) modes, are usually difficult to determine from a single measurement, in particular for scanning acoustic microscopy. Therefore, using Viktorov formula and physically acceptable approximations, we derive simple expressions for E and G in terms of the velocity, V_i, of just one propagating mode (including Rayleigh mode V_R). It was found that (E, G) = (α_i, β_i)ρV_i². The validity of these expressions is successfully tested, analytically and graphically, for a great number of materials representing a large spectrum of densities, 1000 kg/m³ < ρ < 22 000 kg/m³, and characterized by a wide interval of velocities, 1400 m/s < V_L < 12 000 m/s.     

Synthesis, structure and magnetic properties of a new iron phosphonate-oxalate with 3D framework: [Fe(O3PCH3)(C2O4)0.5(H2O)]

A new iron phosphonate-oxalate [Fe(O₃PCH₃)(C₂O₄)_0.5(H₂O)] (1), has been synthesized under hydrothermal condition. The single-crystal X-ray diffraction studies reveal that 1 consists of layers of vertex-linked FeO₆ octahedra and O₃PC tetrahedra, which are further connected by bis-chelate oxalate bridges, giving to a 3D structure with 10-membered channels. Crystal data: monoclinic, P2₁/n (no. 14), a = 4.851(2) Å, b = 16.803(7) Å, c = 7.941(4) Å, β = 107.516(6)°, V = 617.2(5) Å³, Z = 4, R₁ = 0.0337 and wR₂=0.0874 for 1251 reflections [I > 2σ(I)]. Mössbauer spectroscopy measurement confirms the existence of high-spin Fe(III) in 1. Magnetic studies show that 1 exhibits weak ferromagnetism with T_N = 30 K due to a weak spin canting.     

Absorption and emission properties of Ho doped lead-zinc-borate glasses

This paper reports on the affect of lead content on the absorption and emission spectra of the Ho³⁺ ion doped lead-zinc-borate glasses in the composition (mol%) of (20 − x)PbO-20ZnO-(59 + x)B₂O₃-1.0Ho₂O₃ where x = 0, 5,10,15 of PbO content with λ_exc = 405 nm. The experimental absorption band energies have satisfactorily been correlated with the theoretical results with an r.m.s deviation of zero with the following correction factors obtained by a least square fit analysis: ΔE¹ = 348.495936 cm^− 1, ΔE² = 1.436043 cm^− 1, ΔE³ =  46.481575 cm^− 1, Δξ_4f = − 28.512979 cm^− 1, Δα = 55.508936 cm^− 1, Δβ = − 1394.339908 cm^− 1 and Δγ = 1208.424336 cm^− 1. By applying the Judd-Ofelt intensity parameter Ω₂ has been found to be linearly decreasing with the PbO content from 5 to 10 mol% and then increasing. And also radiative (A, A_T, β, τ_r) characteristic factors of the luminescent transitions (⁵I₈ ← ⁵F_3,4,5 and ⁵S₂) of the glasses have been evaluated. Stimulated emission cross-sections (σ_p^E) of the measured emission transitions of holmium glasses have also been computed.     

Crystal structure of a new organic condensed phosphate (C6H9N3O)H2P2O7

Crystals of a new organic compound, the isonicotinic acid hydrazide dihydrogendiphosphate, (C₆H₉N₃O)H₂P₂O₇ (denoted INHDP) were prepared and grown at room temperature. The INHDP crystallizes in the triclinic system with the space group. Its unit cell dimensions are: a = 7.316(3) Å, b = 7.783(3) Å, c = 10.802(4) Å, α = 82.41(3)°, β = 75.19(3)°, γ = 72.57(3)°, with V = 566.3(4) Å³ and Z = 2. Crystal structure has been determined and refined to a reliability R factor of 0.0389. The atomic arrangement can be described as inorganic infinite ribbons of H₂P₂O₇²⁻ anions spreading parallel to the b-axis. These ribbons are themselves interconnected by the organic (C₆H₉N₃O)⁺ cations so as to build a three dimensional arrangement. In the present work, we describe the crystal structure, thermal behaviour and IR analysis of this new compound.     

Synthesis and crystal structure of [3,5-(CH3O)2C6H3NH3]4P4O12·4H2O

The chemical preparation and crystal structure are given for a new organic-cation cyclotetraphosphate. This compound is triclinic P-1 with the following unit cell parameters: a=7.857(1) Å, b=8.877(2) Å, c=17.271(3) Å, α=93.94(1)°, β=101.75(2)°, γ=103.72(1)° V=1137.0(4) Å³, Z=1 and ρ_cal=1.467 g cm⁻³. The crystal structure has been determined and refined to R=0.037, using 6291 independent reflections. The atomic arrangement can be described by inorganic layers parallel to the (0 0 1) planes, between which the organic entities are located.     

Crystal structure and physicochemical properties of a new organic condensed phosphate (C7H10NO)3P3O9·4H2O

Chemical preparation, X-ray characterization, IR spectroscopy and thermal analysis of a new cyclotriphosphate: (C₇H₁₀NO)₃P₃O₉·4H₂O abbreviated as OACTP, are reported. This mixed organo-mineral compound crystallizes in the monoclinic system with P2₁/n space group, the unit cell dimensions are: a = 6.605(3) Å, b = 26.166(3) Å, c = 18.671(8) Å, β = 91.95(3)°, Z = 4 and V = 3255(2) Å³. The structure was solved using a direct method and refined to a reliability R-factor of 0.043 using 3931 independent reflections (I > 2σI). Atomic arrangement exhibits infinite (P₃O₉·2H₂O)_n³ⁿ⁻ chains connected by organic cations. The thermal behavior and the IR spectroscopic studies of this new compound are discussed.     

Effects of annealing and deforming temperature on microstructure and deformation characteristics of Ti–Ni–V shape memory alloy

Effects of annealing temperature T_an and deforming temperature T_d on microstructure and deformation characteristics of Ti–50.8Ni–0.5V (atomic fraction, %) shape memory alloy were investigated by means of optical microscopy and tensile test. With increasing T_an, the microstructure of Ti–50.8Ni–0.5V alloy wire changes from fiber style to equiaxed grain, and the recrystallization temperature of the alloy is about 580 °C; the critical stress for stress-induced martensite σ_M of the alloy decreases first and then increases, and the minimum value 382 MPa is got at T_an = 450 °C; the residual strain ?_R first increases, then decreases, and then increases, and its maximum value 2.5% is reached at T_an = 450 °C. With increasing T_d, a transformation from shape memory effect (SME) to superelasticity (SE) occurs in the alloy annealed at different temperatures, and the SME → SE transformation temperature was affected by T_an; the σ_M of the alloy increases linearly; the ?_R of the alloy annealed at 350–600 °C decreases first and then tends to constant, while that of the alloy annealed at 650 °C and 700 °C decreases first and then increases. To get an excellent SE at room temperature for Ti–50.8Ni–0.5V alloy, T_an should be 500–600 °C.     

The first bulk synthesis of ReO3-type tungsten trioxide, WO3, from nanometric precursors

A perovskite form of WO₃ has been synthesized in bulk for the first time at 0.66 GPa and 973 K with a=3.7823(4) Å [a₀=3.7719(4) Å, at ambient conditions] from nanometric powder of WO₃ with an average crystallite size of 35 nm. Data collected during tests to determine both the likelihood of retaining the structure at room temperature and the effect of high pressure on distortion have afforded analysis of thermal expansivity and compressibility of this phase. These result in V_T=53.407(5)exp(−3.9(12)×10⁻⁶(T−298)+1.91(9)×10⁻⁸(T²−298²)) Å³ and equation of state parameters of V₀=53.67(4) Å³, K₀=41.8(19) GPa with ∂K/∂P=K′=5.6(12).     

Synthesis and crystal structure of triphosphate RbPrHP3O10

Crystals of RbPrHP₃O₁₀ have been grown by the flux technique and characterized by single-crystal X-ray diffraction. RbPrHP₃O₁₀ crystallizes in the triclinic space group with lattice parameters: a = 7.0655(5), b = 7.7791(4), c = 8.6828(6) Å, α = 74.074(3), β = 74.270(3), γ = 82.865(2)°, V = 441.09(5) ų, Z = 2. The crystal structure has been solved yielding a final R(F²) = 0.0443 and R_w(F²) = 0.1426 for 1955 independent reflections (F_o² ≥ 2σ(F_o²)). The structure of RbPrHP₃O₁₀ consists of PrO₈ polyhedra and P₃O₁₀⁵⁻ groups sharing oxygen atoms to form a two-dimensional framework; the PrO₈ polyhedra form infinite chains by edge-sharing. Each Rb⁺ ion is bonded to 10 oxygen atoms, these ions are located between chains formed of (HP₃O₁₀)⁴⁻. The energies of the vibrational modes of the crystal were obtained from measurements of the infrared spectrum.     

Synthesis and characterization of a new monophosphate (5-Cl-2,4-(OCH3)2C6H2NH3)H2PO4

Chemical preparation, crystal structure and NMR spectroscopy of a new organic cation 5-chloro(2,4-dimethoxy)anilinium monophosphate H₂PO₄ are given. This new compound crystallizes in the monoclinic system, with the space group P2₁/c and the following parameters: a = 5.524(2) Å, b = 9.303(2) Å, c = 23.388(2) Å, β = 90.66(4), V = 1201.8(2) Å³, Z = 4 and D_x = 1.573 g cm⁻³. Crystal structure has been determined and refined to R = 0.031 and R_w = 0.080 using 1702 independent reflections. Structure can be described as an infinite (H₂PO₄)_nⁿ⁻ corrugated chains in the a-direction. The organic groups (5-Cl-2,4-(OCH₃)₂C₆H₂NH₃)⁺ are anchored between adjacent polyanions through multiple hydrogen bonds. This compound is also investigated by IR, thermal, and solid-state, ¹³C, ³¹P MAS NMR spectroscopies.     

Nonlinear optical activity in Bridgman growth layered compounds

Layered semiconductor compound CdI₂ has been grown with the Bridgman technique and studied by nonlinear transmittance spectroscopy. The optical absorption in CdI₂ shows a nonlinear transmission of the incident laser power (P₀) within a lower power limit. The transmission, however, is found to saturate at high powers, giving a clamped output. The value of the incident power (P_0C) at which clamping starts is also found to depend on the crystal temperature (T_L). The values of P_OC ranges from 55 to 65 MW cm⁻² for T_L = 4.2–180 K. The dynamic range (D_R) as a function of T_L is calculated and the values are found to range from D_R = 2 to 1.6. The optical limiting mechanisms are discussed. The two-photon absorption (TPA) coefficient (β) of the optical nonlinear process in CdI₂ is estimated. The values are found to be within a range from β = 47 to 25 cm GW⁻¹ and be decreasing with increasing T_L. As expected for the TPA process, the experimental data within a certain range follows the linear relation: log (P₀/P_T) = A_G + Ω(P₀ − P_T), where P_T is the transmitted power, A_G is the absorbance of the ground state and Ω is a constant depending on the absorption cross-section and the relaxation time. The values of A_G and Ω estimated from the fits to the measured data vary with T_L. The findings resulting from this investigation might have potential applications in optical sensors protection.     

Fatigue crack growth behavior of silica particulate reinforced epoxy resin composite

In the present work, fatigue crack growth tests of epoxy resin composite reinforced with silica particle under various R-ratios were carried out to investigate the effect of R-ratio on crack growth behavior and to discuss fatigue crack growth mechanism. Crack growth curves arranged by ΔK showed clear R-ratio dependence even under no crack closure, where the values of ΔK_th were 0.82 and 0.33 MPa √m for R = 0.1 and 0.7 respectively. However, crack growth curves arranged by K_max merged into almost one curve regardless of R-ratio, which indicated that crack growth behavior of the present composite was time-dependent. The value of K_max,th were in the range from 0.78 to 1.12 MPa √m. In situ crack growth observation revealed the crack growth mechanism: micro-cracking near the interface between silica particle and resin matrix occurs ahead of a main crack and then micro-cracks coalesce with a main crack to grow. The crack path was in the epoxy matrix, which was consistent with the time-dependent crack growth.     

Synthesis and characterization of a new organic dihydrogen phosphate-arsenate: [H2(C4H10N2)][H2(As, P)O4]2

Chemical preparation, crystal structure, calorimetric and spectroscopic investigations (IR and RMN) are given for a new non-centrosymmetric organic-cation dihydrogen phosphate-arsenate [H₂(C₄H₁₀N₂)][H₂(As, P)O₄]₂. This compound is triclinic P1 with the following unit-cell parameters: a = 7.082(2) Å, b = 7.796(1) Å, c = 12.05(3) Å, α = 95.37(2)°, β = 98.38(3)°, γ = 62.98(1)°, Z = 2, V = 586.2(1) Å³ and D_x = 1.836 g cm⁻³. The crystal structure has been solved and refined to R = 0.03 using 2328 independent reflections. The structure can be described as infinite (H₂XO)_n chains spreading parallel to the b direction. These chains are themselves interconnected by a set of NH?O hydrogen bonds generated by the organic entities, alternating with the chains. Solid-state ¹³C, ¹⁵N and ³¹P MAS NMR spectroscopies are in agreement with the X-ray structure.     

Studies on the effect of solvents on self-assembly of thioctic acid and Mercaptohexanol on gold

In this article we investigated the effect of solvents (CCl₄, CH₃CN, DMF, ethanol, ethanol-H₂O and H₂O) on self-assembly of Thioctic acid (TA) and Mercaptohexanol (MCH) on gold by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Electrochemical characteristics of TA and MCH self-assembled monolayers (SAMs) formed in different solvents were evaluated by inspecting the ions permeability (interfacial capacitance C and phase angle Ф_1 Hz) and electron transfer capability (current density difference Δi and charge transfer resistance R_ct). Experimental results indicated that the ability of solvents availing the ordering of SAMs was: for TA, CCl₄ > ethanol > CH₃CN > ethanol-H₂O > DMF; for MCH, H₂O > ethanol-H₂O ≈ CCl₄ > ethanol ≈ CH₃CN > DMF. Through relating the C, Ф_1 Hz, Δi and R_ct of SAMs (TA and MCH) with parameters of solvent (polarity E_T^N, solubility parameter δ and octanol/water partition coefficients logP_ow), it was found that solvents with bigger logP_ow (smaller E_T^N and δ) availed the ordering of TA-SAMs but the effect of solvents on MCH self-assembly was complex and MCH-SAMs formed in H₂O (the biggest E_T^N, δ and the smallest logP_ow) and CCl₄ (the smallest E_T^N, δ and the biggest logP_ow) were more ordered than in other solvents.     

Effect of doping with Nd ions on the structural and ferroelectric properties of Ca0.28Ba0.72Nb2O6 single crystal

The crystal structure of Ca_0.28Ba_0.72Nb₂O₆ (CBN-28) crystal with Nd-doping has been determined from X-ray single crystal diffraction data, in the tetragonal system with space group P4bm and the following parameters: a = b = 12.458 Å, c = 3.954 Å, V = 613.688 Å³, and Z = 5. X-ray diffraction results on a Nd-doped CBN-28 single crystal also have demonstrated that Nd³⁺ and Ca²⁺ occupy the same site in the crystal structure. Dielectric and ferroelectric measurements have been performed. Transition from ferroelectric to paraelectric at around 223 °C has been observed. The Nd-doped crystal has a lower Curie temperature (T_m) than that of undoped CBN-28 crystal. The spontaneous polarization (P_s) and coercive electric field (E_c) also decrease compared with their values in the undoped CBN-28 crystal.     

R3Mn1.5CuV0.5O9 (R = Y, Ho, Er, Tm, Yb and Lu) and Lu3Mn3−3xCu2xVxO9: New noncentrosymmetric oxides related to YMnO3

We report formation of new noncentrosymmetric oxides of the formula, R₃Mn_1.5CuV_0.5O₉ for R = Y, Ho, Er, Tm, Yb and Lu, possessing the hexagonal RMnO₃ (space group P6₃cm) structure. These oxides could be regarded as the x = 0.5 members of a general series R₃Mn_3−3xCu_2xV_xO₉. Investigation of the Lu-Mn-Cu-V-O system reveals the existence of isostructural solid solution series, Lu₃Mn_3−3xCu_2xV_xO₉ for 0 < x ≤ 0.75. Magnetic and dielectric properties of the oxides are consistent with a random distribution of Mn³⁺, Cu²⁺ and V⁵⁺ atoms that preserve the noncentrosymmetric RMnO₃ structure.     

Crystal structure and aggregation behavior in water of ionic liquid 1-hexadecyl-3-methylimidazolium Bromide

A large-transparent single crystal of 1-hexadecyl-3-methylimidazolium bromide monohydrate ([C₁₆mim]Br·H₂O) with 4-mm length was firstly obtained in the water-trichloromethane-toluene growth system (V_water:V_{trichloromethane}:V_toluene = 0.1:1:2). The crystal structure was determined by single crystal X-ray diffraction method. It crystallizes in the triclinic system, space group P-1, with unit cell parameters a = 5.4962(15) Å, b = 7.839(2) Å, c = 27.279(8) Å, α = 94.375°(4), β = 91.500°(5), γ = 101.999°(4), Z = 2, V = 1145.2(5)ų, Dc = 1.176 Mg/m³, μ = 1.804 mm^− 1, F(000) = 436, the final R1 = 0.0497, wR2 = 0.1154. The 3D supramolecular structure is constructed through the weak interactions between imidazolium cations, Br⁻ anions and lattice water molecules. The long alkyl chain to imidazolium ring and lattice water molecules play an important role in the self-assembled process. Moreover, it is proposed that [C₁₆mim]Br has the aggregation behavior in water at the higher concentration and the possible self-assembled structure is the interdigitated pattern.     

Study of GeYSi1 − Y:H films deposited by low frequency plasma

In this work, we report a study of the optical properties measured through spectral transmission and spectroscopic ellipsometry in Ge:H and Ge_YSi_1 − Y:H (Y ≈ 0.97) films deposited by low frequency (LF) PE CVD with hydrogen (H) dilution. The dilution was varied in the range of R = 20 to 80. It was observed that H-dilution influences in a different way on the interface and bulk optical properties, which also depend on incorporation of silicon. The films with low band tail characterized by its Urbach energy, E_U, and defect absorption, α_D, have been obtained in Ge:H films for R = 50 with E_U = 0.040 eV and α_D = 2 × 10³ cm^− 1 (hν ≈ 1.04 eV), and in Ge_YSi_1 − Y:H films for R=75 with E_U = 0.030 eV and α_D = 5 × 10² cm^− 1 (hν ≈ 1.04 eV).     

Crystal structure and ionic conductivity of ruthenium diphosphate ARu2(P2O7)2, A=Li, Na, and Ag, with a tunnel structure

Crystal structure and ionic conductivity of ruthenium diphosphates, ARu₂(P₂O₇)₂ A=Li, Na, and Ag, were investigated. The structure of the Ag compound was determined by single crystal X-ray diffraction techniques. It crystallized in the triclinic space group P−1 with a=4.759(2) Å, b=6.843(2) Å, c=8.063(1) Å, α=90.44(2)°, β=92.80(2)°, γ=104.88(2)°, V=253.4(1) Å³. The host structure of it was composed of RuO₆ and P₂O₇ groups and formed tunnels running along the a-axis, in which Ag⁺ ions were situated. The ionic conductivities have been measured on pellets of the polycrystalline powders. The Li and Ag compounds showed the conductivities of 1.0×10⁻⁴ and 3.5×10⁻⁵ S cm⁻¹ at 150 °C, respectively. Magnetic susceptibility measurement of the Ag compound showed that it did not obey the Curie-Weiss law and the effective magnetic moment decreased as temperature decreased due to the large spin-orbital coupling effect of Ru⁴⁺ ions.     

Vanadium dioxide nanobelts: Hydrothermal synthesis and magnetic properties

VO₂ (B) nanobelts were prepared by a hydrothermal method at 180 °C using V₂O₅·nH₂O sol and H₂C₂O₄·2H₂O as starting agents. The obtained nanobelts have diameters ranging from 50 to 100 nm in width, 20-30 nm in thickness with lengths up to 1.5 μm. Measurements of the static magnetic susceptibility provide evidence for two phase transitions at T₁ = 225 K and T₂ = 290 K, respectively. Below T₁, the data suggest the presence quasi-free as well as of strongly antiferromagnetic correlated spins associated to V⁴⁺-ions.