CO and NH3 sensor properties and paramagnetic centers of nanocrystalline SnO2 modified by Pd and Ru

Nanocrystalline gas sensitive materials based on tin dioxide modified by Pd or Ru were synthesized via wet chemical route. The interaction of modified materials with CO and ammonia was studied by in situ DC-conductivity measurements and ex situ EPR spectroscopy. Modification by Pd yields the material highly sensitive to CO in low temperature region, while Ru-modified SnO₂ is very sensitive to NH₃ at raised temperature. We have detected that O₂⁻ and OH radicals are the main spin centers in unmodified nanocrystalline tin dioxide. The modification of tin dioxide by Pd and Ru is accompanied by formation of new spin centers in the samples: Pd^+ 3 and Ru^+ 3. The concentration of these paramagnetic species on the materials interacting with CO and ammonia gases decreased because of their transition to the diamagnetic state Pd^+ 2, Pd⁰ and Ru^+ 4, respectively.     

Study on the homogeneity of hydrogenation for LaFe11.5Si1.5 intermetallic compound

The homogeneity of hydrogen absorption for LaFe_11.5Si_1.5 intermetallic compound was investigated. The hydrides remained NaZn₁₃-type structure when the hydrogenation temperature varied from 423 K to 923 K under 1 atm hydrogen atmosphere. The Differential Scanning calorimetric (DSC) measurements revealed slightly inhomogeneous distribution of hydrogen atoms in the hydrides hydrogenated at a low temperature. The activation before hydrogenating at a higher temperature could improve the homogeneity of hydrogen absorption. Uniform magnetic transition temperature, corresponding to the homogeneous hydrogen absorption, was observed by hydrogenating the compound at 823 K, or at 523 K after activation. The maximum magnetic entropy change ΔS_M (ΔH = 2 T) for the compound hydrogenated at 823 K is about 15.5 J/kg K with the latent heat of 5.12 × 10³ J/kg during the phase transition.     

Liquid petroleum gas sensor based on SnO2/Pd composite films deposited on Si/SiO2 substrates

SnO₂/Pd composite films were synthesized by d.c. sputtering of a SnO₂ target followed by thermal evaporation of a thin layer of Pd on top of it. This structure, deposited on Si wafer with 300 μm SiO₂ on the top, was subjected to rapid thermal annealing at 573 K for 5 min for the incorporation of Pd in SnO₂. The films were characterized by microstructural, optical, FTIR and Raman studies. Liquid petroleum gas (LPG) sensing measurements were carried out on these films. Sensitivity of 72% was obtained at an operating temperature of ∼573 K. The response time for these sensors was found to be ∼27 s. Sensitivity was found to increase with grain growth at higher sensing temperatures. It could be observed that the selectivity for LPG is extremely good as compared to that of methane, hydrogen, CO₂ and C₂H₅OH.     

Microstructure and mechanical properties of ZA62 Mg alloy by equal-channel angular pressing

The Mg-6Zn-2Al alloy was processed by ECAP and microstructure and mechanical properties of the alloy before and after ECAP were studied. The results revealed that the microstructure of the ZA62 alloy was successfully refined after two-step ECAP (2 passes at 473 K and 2-8 passes at 423 K). The course bulk interphase of Mg₅₁Zn₂₀ was crushed into fine particles and mixed with fine matrix grains forming “stripes” in the microstructure after the second step of ECAP extrusion. A bimodal microstructure of small grains of the matrix with size of ∼0.5 μm in the stripes and large grains of the matrix with size of ∼2 μm out of stripes was observed in the microstructure of samples after 4-8 passes of ECAP extrusion at the second step. The mechanical properties of the alloy studied were significantly improved after ECAP and the highest yield strength and elongation at room temperature were obtained at the samples after 4 and 8 ECAP passes at the second step, respectively. Tensile tests carried out at temperature of 473 K to 573 K and strain rate of 1 × 10⁻³ s⁻¹ to 3 × 10⁻² s⁻¹ revealed that the alloy after 8 ECAP passes at the second step showed superplasticity and the highest elongation and strain rate sensitivity (m-value) reached 520% and 0.45, respectively.     

Synthesis and spectroscopic investigations of Mn3O4 nanoparticles

Trimanganese tetraoxide (Mn₃O₄) nanoparticles have been synthesized via hydrothermal process. Nevertheless, homogeneous nanoparticles of Mn₃O₄ with platelet lozange shape were obtained. The crystallite size ranged from 40 to 70 nm. The Mn₃O₄ product was investigated by X-ray diffraction, transmission electron microscopy (MET), and impedance spectroscopy. Electrical conductivity measurements showed that the as-synthesized Mn₃O₄ nanomaterial has a conductivity value which goes from 1.8 10⁻⁷ Ω⁻¹ cm⁻¹ at 298 K, to 23 10⁻⁵ Ω⁻¹ cm⁻¹ at 493 K. The temperature dependence of the conductivity between 298 and 493 K obeys to Arrhenius law with an activation energy of 0.48 eV.     

Photoconductive properties of organic-inorganic hybrid perovskite (C6H13NH3)2(CH3NH3)m − 1PbmI3m + 1:TiO2 nanocomposites device structure

Photoconductive devices, with remarkable photoconductive performance, of fluorine doped tin oxide/TiO₂/(C₆H₁₃NH₃)₂(CH₃NH₃)_m − 1Pb_mI_3m + 1 (m = 1, 2):TiO₂/Pt were fabricated. An electron injection mechanism from the (C₆H₁₃NH₃)₂(CH₃NH₃)_m − 1Pb_mI_3m + 1 (m = 1, 2) to TiO₂ was proposed for the photoconductive effects, where organic-inorganic hybrid perovskite (C₆H₁₃NH₃)₂(CH₃NH₃)_m − 1Pb_mI_3m + 1 (m = 1, 2), self-organized into mesoscopic TiO₂ films from solution directly, served as the electron donor. The photoconductive performance of the devices can be adjusted by the inorganic sheet thickness (tuned by m) of the hybrid perovskite. The photocurrent value increased as m value increased at the same illumination. Further, when bias voltage was 1.0 V, the ratio of photocurrent and dark current for (C₆H₁₃NH₃)₂(CH₃NH₃)_2⁻ Pb₂I₇:TiO₂ reached as high as 7.05 × 10³. The devices could be potentially used as light detectors and light-controlled switch.     

Ar assisted carbidization of TiO2 (1 1 0) supported Mo nanoparticles by decomposition of C2H4

Ar⁺ assisted carbidization of Mo nanoparticles supported on TiO₂ (1 1 0) is studied by scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS). In order to activate the diffusion of carbon into the bulk of Mo nanoparticles we applied Ar ions (1 keV) during the exposure of C₂H₄. XPS exhibited that the decomposition of C₂H₄ at 850 K accompanied by ion bombardment results in an almost complete carbidization of nanocrystalline Mo while this treatment performed without ion bombardment results only in the carbidization of the particle surface. The modification of the crystallinity of the Mo-carbide particles was deduced from STM measurements.     

Deposition temperature effect on the electric and dielectric properties of InSbSe3 thin films

Thin films of InSbSe₃ compound were obtained by thermal evaporation on to clean glass substrates maintained at various deposition temperatures from 423 to 593 K. At deposition temperature T_d?473 K, the films have an amorphous structure, while those prepared at T_d>473 K have a polycrystalline structure identified by X-ray diffraction analysis. The DC electrical conductivity of the films increases as T_d increases, whereas activation energy decreases with increasing T_d, which reflects a change in the degree of disorder. AC conductivity was studied as a function of frequency in the range (10²-10⁵ Hz) and as a function of deposition temperature. The dependence of T_d on the frequency exponent s in the conductivity-frequency relation confirmed that the mechanism of AC conductivity is correlated barrier hopping with a single polaron hopping mechanism. The discrepancy between DC and AC activation energies was studied as a function of deposition temperature. The maximum barrier height W_m and the density of defect states N were also determined. Finally, the dependence of dielectric constant and dielectric loss on T_d were studied. A Debye-like relaxation of dielectric behavior was observed for crystalline films and is found to be a thermally activated process. The position of maximum dielectric loss is shifted towards higher temperature with T_d treatment and there by reduces the relaxation time.     

Effect of P on crystallization behavior and soft-magnetic properties of Fe83.3Si4Cu0.7B12 − xPx nanocrystalline soft-magnetic alloys

The P content dependences of the crystallization behavior, thermal stability and soft-magnetic properties of high Fe content Fe_83.3Si₄Cu_0.7B_12 − xP_x (x = 0 to 8) nanocrystalline soft-magnetic alloys were investigated. P addition is very effective in widening the optimum annealing temperature range and refining of bcc-Fe grain size in addition to the increasing of nanocrystalline grain density. Uniform nanocrystalline bcc-Fe grains with average size of about 20 nm and number density of 10²³-10²⁴ /m³ were prepared at around x = 6-8 for the annealed Fe_83.3Si₄Cu_0.7B_12 − xP_x alloys. The coercivity H_c markedly decreases with increasing x and exhibits a minimum at around x = 6-8, while the saturation magnetic flux density B_s shows a slight decrease. Fe_83.3Si₄Cu_0.7B₆P₆ nanocrystalline alloy exhibits excellent soft-magnetic properties with a high saturation magnetic flux density B_s of 1.77 T, low coercivity H_c of 4.2 A/m and high effective permeability μ_e of 11,600 at 1 kHz.     

Mechanical and thermal properties of LaMgAl11O19

Lanthanum magnesium hexaaluminate (LaMgAl₁₁O₁₉) powders were synthesized successfully at 1300 °C for 4 h by solid-state reaction, and LaMgAl₁₁O₁₉ ceramic was prepared at 1700 °C for 6 h by pressureless sintering. Phase composition, microstructure, mechanical and thermophysical properties of LaMgAl₁₁O₁₉ ceramic were investigated. Results show that the flexural strength and fracture toughness of LaMgAl₁₁O₁₉ ceramic are 353.3 ± 12.5 MPa and 4.60 ± 0.46 MPa m^1/2. Young's Modulus and Poisson ratio is 295 GPa and 0.23, respectively. The linear thermal expansion coefficient of LaMgAl₁₁O₁₉ ceramic from 473 K to 1473 K is 9.17 × 10⁻⁶/K, and thermal conductivity at 1273 K is 2.55 W/m K.     

Tribological behavior of radio-frequency sputtering WS2 thin films with vacuum annealing

Thin films of tungsten disulfide (WS₂) were deposited on 3Cr13 martensitic stain less steel substrate by radio-frequency (RF) sputtering. The as-deposited films were annealed at 473, 673 and 873 K respectively for 2 h in 5 × 10^− 4 Pa vacuum. Composition of the films was inspected by energy dispersive spectroscopy. Surface morphology and structure properties were studied by scanning electron microscopy and X-ray diffraction techniques. Tribological behavior was also examined using tribometer. At 473 K, the films exhibited low crystallization structure and no significant improvement in the tribological performance. At 673 K, the tribological performance was improved and a transition from non-crystalline to hexagonal structure took in place. When the annealing temperature rose up to 873 K, the films cracked and fell off from the substrate. The results suggested that with suitable technical parameters vacuum annealing could promote crystallization and improve tribological performance of RF sputtering WS₂ films.     

Synthesis of Bi2Fe4O9 via PVA sol-gel route

Bi₂Fe₄O₉ powders were synthesized by a sol-gel process using polyvinyl alcohol (PVA) as a complexing agent. Differential scanning calorimetry (DSC), thermogravimetric (TG), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and Field emission scanning electron microscope (FSEM) techniques were used to characterize precursor and derived oxide powders. The effect of the ratios of positively charged valences to hydroxyl groups of PVA (Mⁿ⁺/-OH) on the formation of Bi₂Fe₄O₉ was investigated. XRD analysis showed that single-phase Bi₂Fe₄O₉ was obtained from the Mⁿ⁺/-OH = 2:1 and Mⁿ⁺/-OH = 1:1 precursors at the temperature of 700 °C. For the precursor with Mⁿ⁺/-OH = 4:1, pure Bi₂Fe₄O₉ formed at the temperature of 800 °C. Bi₂Fe₄O₉ powders clacined at 700 °C from Mⁿ⁺/-OH = 2:1 precursor shows weak ferromagnetism.     

Excitons in organic-inorganic hybrid compounds (CnH2n + 1NH3)2PbBr4 (n = 4, 5, 7 and 12)

Thin films of microcrystalline (C_nH_2n + 1NH₃)₂PbBr₄ (n = 4, 5, 7 and 12) have been prepared by a modified spin-coating method, and the effect of the number of carbon atoms of the alkyl chain length (n) on optical properties has been investigated. Absorption spectra reveal that (C_nH_2n + 1NH₃)₂PbBr₄ films show stable excitons with a binding energy of a few hundred meV. The excitonic structure of (C_nH_2n + 1NH₃)₂PbBr₄ varies with the number of carbon atoms. The lowest-energy exciton splits into a few fine-structure levels at low temperature. (C_nH_2n + 1NH₃)₂PbBr₄ films (n = 5, 7 and 12) show not only singlet excitons but also triplet excitons at low temperature, while (C₄H₉NH₃)₂PbBr₄ films show only singlet excitons. The intersystem crossing from excited singlet state to triplet state plays an important role in the relaxation process of excitons.     

Quasi-single scattering of low-energy Ne ions from the Fe3O4 surfaces

The energy spectra of positive and negative ions emitted from single-crystalline Fe₃O₄ (0 0 1) and (1 1 1) surfaces under low-energy Ne⁺ ion bombardments were investigated in the temperature range from 85 to 300 K. The characteristics of the LEIS spectra of the two surfaces are very similar. The positive-charged-ion spectra have revealed the O⁺-recoil and the quasi-single scattering Ne⁺-Fe peak, while a large broad O⁻¹ recoil signal was observed in the negative-charged-ion ones. No change of the peak shape and of the energy position have revealed for the (0 0 1) surface, whereas the (1 1 1) one implies an appearance of a small peak around 150 K attributed to recoil-oxygen ions from the double-collisions.     

Hygroscopicity and bulk thermal expansion in Y2W3O12

Negative thermal expansion material, Y₂W₃O₁₂ has been synthesized by the solid-state method and bulk thermal expansion of the material has been investigated from 300 to 1100 K. The material reversibly forms a trihydrate composition whose X-ray diffraction pattern can be indexed to an orthorhombic unit cell with a = 10.098(1) Å, b = 13.315(3) Å, c = 9.691(4) Å. The cell volume of the hydrated pattern is 7% smaller than the unhydrated cell volume. According to the dilatometric studies, the material shows a 3-6% increase in the linear strain at about 400 K, which can be attributed to the removal of water. Sintering the material at 1473 K leads to large grain size of >100 μm, which results in a large hysteresis in the bulk thermal expansion behavior. Hot pressing at 1273 K under a uniaxial pressure of 25 MPa results in a fine-grained (2-5 μm) ceramic. Glazing the ceramic prevents moisture pick up and a linear thermal expansion over the entire temperature range 1100-300 K and an average linear thermal expansion co-efficient of −9.65 × 10⁻⁶/K is observed. The effect of water on the thermal expansion behavior of this system is discussed.     

Synthesis and Li ion conductivity of Li2O-Nb2O5-P2O5 glasses and glass-ceramics

Glasses with the compositions of xLi₂O-(70 − x)Nb₂O₅-30P₂O₅, x = 30-60, and their glass-ceramics are synthesized using a conventional melt-quenching method and heat treatments in an electric furnace, and Li⁺ ion conductivities of glasses and glass-ceramics are examined to clarify whether the glasses and glass-ceramics prepared have a potential as Li⁺ conductive electrolytes or not. The electrical conductivity (σ) of the glasses increases monotonously with increasing Li₂O content, and the glass of 60Li₂O-10Nb₂O₅-30P₂O₅ shows the value of σ = 2.35 × 10⁻⁶ S/cm at room temperature and the activation energy (E_a) of 0.48 eV for Li⁺ ion mobility in the temperature range of 25-200 °C. It is found that two kinds of the crystalline phases of Li₃PO₄ and NbPO₅ are formed in the crystallization of the glasses and the crystallization results in the decrease in Li⁺ ion conductivity in all samples, indicating that any high Li⁺ ion conducting crystalline phases have not been formed in the present glasses. 60Li₂O-10Nb₂O₅-30P₂O₅ glass shows a bulk nanocrystallization (Li₃PO₄ nanocrystals with a diameter of ∼70 nm) and the glass-ceramic obtained by a heat treatment at 544 °C for 3 h in air exhibits the values of σ = 1.23 × 10⁻⁷ S/cm at room temperature and E_a = 0.49 eV.     

Physical properties of flash evaporated In2O3 films prepared at different substrate temperatures

Indium oxide (In₂O₃) thin films were prepared by flash evaporated technique under various substrate temperatures in the range of 303-673 K and systematically studied the structural, electrical and optical properties of the deposited films. The films formed at substrate temperatures of < 373 K were amorphous while those deposited at higher substrate temperatures (≥ 373 K) were polycrystalline in nature. The optical band gap of the films decreased from 3.71 eV to 2.86 eV with the increase of substrate temperature from 303 K to 673 K. Figure of merit of the films increased from 2.8 × 10³ Ω^− 1 cm^− 1 to 4.2 × 10³ Ω^− 1 cm^− 1 with increasing substrate temperature from 303 K to 573 K, thereafter decreased to 2.2 × 10³ Ω^− 1 cm^− 1 at higher temperature of 673 K.     

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.     

Mobility of holes in a Si/Si0.8Ge0.2/Si metal oxide semiconductor field effect transistor

Using all standard scattering mechanisms the hole mobility in a metal oxide semiconductor field effect transistor SiGe conduction channel at 17 K and room temperature was calculated. The mobility measurements were performed at different bath temperatures in the range of 4-300 K. The 4 K peak mobility at a sheet carrier concentration, n_h, of 2.1 × 10¹¹ cm^− 2 is 5100 cm² V⁻¹ s^− 1 while the 300 K mobility has a peak value of 350 cm² V⁻¹ s^− 1. By comparing between theory and measurements it is shown that the interface impurities and surface roughness more strongly limit the mobility than alloy scattering does.     

Nanoindentation behavior of bulk metastable Al65Cu20Ti15 alloy prepared by consolidation of the ball milled powder

Present study concerns assessment of nanomechanical property in the bulk Al₆₅Cu₂₀Ti₁₅ alloy with varying microstructure synthesized by consolidation of mechanically alloyed powder at different temperature. The microstructure after consolidation at room temperature and 500 °C exhibits completely amorphous and nanocrystalline states respectively. Nanoindentation experiments suggest that the maximum strength and hardness values are achieved in the sample sintered at 450 °C. The corresponding microstructure revealed dispersion of nanocrystalline intermetallic phase (<50 nm) in the amorphous matrix.