Hydrogen evolution from aqueous methanol solution on mesoporous titania prepared by a process combining evaporation induced self-assembly and spray pyrolysis

Mesoporous TiO₂ powders were prepared in 1 min from an aqueous mixture of chelated complex titanium precursor and tri-block copolymer by using a process combining evaporation induced self-assembly (EISA) and spray pyrolysis. Photocatalytic activity was evaluated by measuring the rate of hydrogen evolution from methanol solution. The prepared powders were mainly anatase phase and had worm-like pores. Crystallite size was in the range from 7.8 to 18.6 nm in diameter. The mesoporous TiO₂ powders calcined at 823 K had surface area of 144 m² g⁻¹ and high pore volume of 0.33 cm³ g⁻¹. Pore size distribution was also narrow. In addition, it had high light absorption intensity below 350 nm. The rate of hydrogen evolution was by a factor of six higher than the rate measured with commercial nano-sized TiO₂ powder (Degussa P-25). Unique structural and optical properties, which were mainly originated from our new combined process of EISA and spray pyrolysis, contributed to the enhanced rate of hydrogen evolution.     

Magnetic properties and microstructure of La-substituted BaCr-ferrite powders

A combustion process was used to synthesize crystalline powders of La-substituted barium chromium hexaferrites Ba_1 − xLa_xFe_11.5Cr_0.5O₁₉ (x = 0-0.25). The structures, morphologies and ferromagnetic properties of La³⁺ substituted nanocomposites were characterized by powder X-ray diffractometer (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). XRD results showed that single-phase barium chromium ferrite powders was found at La content x ≤ 0.2. From the SEM, it was observed that the particles calcined at 1100 °C had a plate-like hexagonal shape. The results of magnetic mensuration revealed that both M_S and H_C of barium hexaferrite increased up to x = 0.1, and then decreased with the increasing of La content.     

Pulsed laser deposition of p-type α-AgGaO2 thin films

Polycrystalline α-AgGaO₂ powders were prepared by the hydrothermal conversion of β-AgGaO₂. The β-AgGaO₂ was synthesized by the ion exchange reaction between NaGaO₂ and molten AgNO₃ under nitrogen atmosphere. The α-AgGaO₂ thus synthesized was used as the target for pulsed laser ablation. The films grown on α-Al₂O₃ (0001) single crystal substrates are crystalline and are 50% transparent in the visible region. The temperature dependence of conductivity shows a semiconducting behaviour with room temperature conductivity 3 × 10^− 4 Scm^− 1. The positive sign of Seebeck coefficient (+ 70 μVK^− 1) demonstrated the p-type conduction in the films. Transparent p-n heterojunctions on a glass substrate were fabricated. The structure of the device was glass/ITO/n-ZnO/p-AgGaO₂. The ratio of forward to reverse current was more than 100 in the range of − 1.5 V to + 1.5 V.     

Low-resistance and highly transparent Ag/IZO ohmic contact to p-type GaN

The electrical, structural, and optical characteristics of Ag/ZnO-doped In₂O₃ (IZO) ohmic contacts to p-type GaN:Mg (2.5 × 10¹⁷ cm^− 3) were investigated. The Ag and IZO (10 nm/50 nm) layers were prepared by thermal evaporation and linear facing target sputtering, respectively. Although the as-deposited and 400 °C annealed samples showed rectifying behavior, the 500 and 600 °C annealed samples showed linear I-V characteristics indicative of the formation of an ohmic contact. The annealing of the contact at 600 °C for 3 min in a vacuum (~ 10^− 3 Torr) resulted in the lowest specific contact resistivity of 1.8 × 10^− 4 Ω·cm² and high transparency of 78% at a wavelength of 470 nm. Using Auger electron spectroscopy, depth profiling and synchrotron X-ray scattering analysis, we suggested a possible mechanism to explain the annealing dependence of the electrical properties of the Ag/IZO contacts.     

Polymer-assisted hydrothermal synthesis of single crystal Pb1 − xLaxTiO3 nanorods

Single-crystal Pb_xLa_1 − xTiO₃ (PLT) nanorods of various La concentrations have been synthesized by polymer-assisted hydrothermal method. The nanorods have diameters of 25-60 nm and average lengths of 3 μm. With tetragonal lattices structures, the PLT nanorods grow along the (001) direction. As La concentration increasing, the tetragonality c/a decreases and the Raman mode E(1TO) becomes softening. PLT nanorods with various lengths and diameters have been prepared by using different polymer additives. To fabricate well-crystallized nanorods, an annealing process after the hydrothermal treatment is proved to be necessary.     

Preparation and characterization of La-doped Ba(1 − x)SrxTiO3 powders and thin films

Ba_(1 − x)Sr_xTiO₃ powders with different Ba/Sr ratios (x = 0.10, 0.25, 0.40, 0.55, 0.70) and La-doped Ba_0.9Sr_0.1TiO₃·yLa powders (y = 0.002, 0.004, 0.006, 0.008, 0.010) have been prepared by sol-gel technology using dehydrated barium-acetate, strontium-carbonate, lanthanum-nitrate, and titanium-isopropoxide as raw materials. The experimental results show that the dielectric properties of Ba_(1 − x)Sr_xTiO₃ powders depend on the Ba/Sr ratios. When the Sr fraction is 0.10, the dielectric constant is relatively higher and the dielectric loss is relatively lower, which are more than 2000 and less than 2.0 × 10^− 2 at 1000 Hz, respectively, the most important is that this kind of powder has better frequency stability. La-doping can increase the dielectric constant distinctly, but the dielectric loss can also be increased. Their dielectric properties at 1.0 × 10³ Hz are better than those at 1.0 × 10⁵ Hz. At 1.0 × 10³ Hz the dielectric constant is much higher, while the dielectric loss is much lower. The dielectric constant of different La-doping contents is nearly 3.5 × 10⁴ and the dielectric loss is less than 0.20 when La fraction is 0.008. The La-doped BST sample also has better frequency stability, especially at high frequency. La-doped BST thin films are successfully deposited on mild steel substrates by using plasma spray system with suspension precursors of Ba_0.90Sr_0.10TiO₃·0.8La powders. The XRD patterns of Ba_0.90Sr_0.10TiO₃ and Ba_0.90Sr_0.10TiO₃·0.8La powders are almost the same. No new peaks appear after La-doping, but the peaks move slightly to a larger degree, which indicates that the element La has entered the lattice of the Ba_0.90Sr_0.10TiO₃ and has made the constant of the crystal cell reduce. The XRD pattern of the thin films is just like that of the Ba_0.90Sr_0.10TiO₃·0.8La powders except a peak corresponding to Fe substrate. The SEM results show that the thin films have a uniform and smooth surface. The morphology of cross-section shows a columnar grain structure indicating smooth surface and uniform thickness of the film. The thickness of the film is about 15 um. The thin films obtained are expected to be prospective material for applications in tunable microwave devices.     

The effect of sodium doping to CuInSe2 monograin powder properties

The effect of sodium doping to the electrical and photoluminescence properties of CuInSe₂ monograin powders was studied. Sodium was added in controlled amounts from 5 × 10¹⁶ cm^− 3 to 1 × 10²⁰ cm^− 3. The photoluminescence spectra of Na-doped stoichiometric CuInSe₂ powders had two bands with peak positions at 0.97 and 0.99 eV. The photoluminescence bands showed the shift of peak positions depending on the Na doping level. Peak positions with maximum energy were observed if added sodium concentration was 1 × 10¹⁹ cm^− 3. This material had the highest carrier concentration 2 × 10¹⁷ cm^− 3. In the case of stoichiometric CuInSe₂ (Cu:In:Se = 25.7:25.3:49.0), Na doping at concentrations of 3 × 10¹⁷ cm^− 3 and higher avoided the precipitation of Cu-Se phase. Solar cells output parameters were dependent on the Na doping level. Sodium concentration 3 × 10¹⁸ cm^− 3 resulted in the best open-circuit voltage.     

Preparation of LiFePO4/C composite powders by ultrasonic spray pyrolysis followed by heat treatment and their electrochemical properties

LiFePO₄ powders could be successfully prepared from a precursor solution, which was composed of Li(HCOO)·H₂O, FeCl₂·4H₂O and H₃PO₄ stoichiometrically dissolved in distilled water, by ultrasonic spray pyrolysis at 500 °C followed by heat treatment at sintering temperatures ranging from 500 to 800 °C in N₂ + 3% H₂ gas atmosphere. Raman spectroscopy revealed that α-Fe₂O₃ thin layers were formed on the surface of as-prepared LiFePO₄ powders during spray pyrolysis, and they disappeared after sintering above 600 °C. The LiFePO₄ powders prepared at 500 °C and then sintered at 600 °C exhibited a first discharge capacity of 100 mAh g⁻¹ at a 0.1 C charge-discharge rate. To improve the electrochemical properties of the LiFePO₄ powders, LiFePO₄/C composite powders with various amounts of citric acid added were prepared by the present method. The LiFePO₄/C (1.87 wt.%) composite powders prepared at 500 °C and then sintered at 800 °C exhibited first-discharge capacities of 140 mAh g⁻¹ at 0.1 C and 84 mAh g⁻¹ at 5 C with excellent cycle performance. In this study, the optimum amount of carbon for the LiFePO₄/C composite powders was 1.87 wt.%. From the cyclic voltammetry (CV) and AC impedance spectroscopy measurements, the effects of carbon addition on the electrochemical properties of LiFePO₄ powders were also discussed.     

Preparation and electrochemical performance of LiFePO4/C composite with carbon core structure

LiFePO₄/C composite with carbon core structure was successfully prepared by using araldite as carbon source. The microstructure and morphology of LiFePO₄/C composite were confirmed by X-ray diffraction and transmission electron microscopic observation. The experimental results show that this structure is entirely different from carbon coating. The LiFePO₄/C composite forms a common core structure in which carbon is used as line core and carbon core is covered by nano-LiFePO₄ grains. Moreover, the LiFePO₄/C composite exhibits higher tap density of 1.66 g cm^− 3, shows higher capacity about 162 mAhg^− 1 applied 30 mAg^− 1 current, excellent cyclic ability and rate capability about 139 mAhg^− 1 applied 700 mAg^− 1 current at room temperature.     

Potentiodynamical co-deposited manganese oxide/carbon composite for high capacitance electrochemical capacitors

Manganese oxide/carbon composite materials were prepared by introducing the carbon powders into the potentiodynamical anodic co-deposited manganese oxide in 0.5 mol L^− 1 MnSO₄ and 0.5 mol L^− 1 H₂SO₄ mixed solution at 40 °C. The surface morphology and structure of the composite material were examined by scanning electron microscope and X-ray diffraction. Cyclic voltammetry tests and electrochemical impedance measurements were applied to investigate the performance of the composite electrodes with different ratios of manganese oxide and carbon. These composite materials with rough surface, which consisted of approximately amorphous manganese oxide, were confirmed to possess the ideal capacitive property. The highest specific capacitance of manganese oxide/carbon composite electrode was up to 410 F g^− 1 in 1.0 mol L^− 1 Na₂SO₄ electrolyte at the scan rate 10 mV s^− 1. The synthesized composite materials exhibited ideal capacitive behavior indicating a promising electrode material for electrochemical supercapacitors.     

Structural and optical properties of amorphous and crystalline antimony sulfide thin-films

Smooth and compact thin films of amorphous and crystalline antimony sulfide (Sb₂S₃) were prepared by radio frequency sputtering of an Sb₂S₃ target. As-deposited films are amorphous. Polycrystalline antimony sulfide films composed of ∼ 500 nm grains are obtained by annealing the as-deposited films at 400 °C in sulfur vapors. Both amorphous and crystalline antimony sulfide have strong absorption coefficients of 1.8 × 10⁵ cm^− 1 at 450 nm and 7.5 × 10⁴ cm^− 1 at 550 nm, and have direct bandgaps with band energies of 2.24 eV and 1.73 eV, respectively. These results suggest the potential use of both amorphous and crystalline antimony sulfide films in various solid state devices.     

Electrical, optical and morphological properties of nanoparticle indium-tin-oxide layers

Porous layers were prepared from DEGUSSA's ITO (In₂O₃:Sn) nanoparticle dispersion by doctor blading followed by annealing in air. We investigated the influence of various annealing parameters on electrical, optical and morphological thin film properties.Conductance rises with increasing annealing temperature and time by more than three orders of magnitude up to 44 Ω^− 1cm^− 1. Besides this we found an abrupt decrease in free charge carrier concentration above a critical annealing temperature of 250 °C, which leads to a step in conductance curve. In spite of particle growing during annealing no decrease in porosity was observed and in opposite to compact material, nanoparticle layers do not exhibit an appreciable shrinkage below recrystallisation temperature. These both indicate a densification hindering particle pinning effect, which is believed to be currently the main obstruction to achieve higher electrical conductivities.     

Characterization and photocatalytic activity of nanostructured indium tin oxide thin-film electrode for azo-dye degradation

Photocatalytically active indium tin oxide thin film electrodes were prepared by electron beam evaporation technique onto a glass substrate having thickness 120 nm. Degradation of reactive dye yellow direct 42 has been performed using photoeletrocatalysis. A biased potential is applied across indium tin oxide photoelectrode illuminated by UV light. The best experimental conditions were found to be dye concentration 1.0 × 10^− 5 mol L^− 1, pH 5.25 and 0.5 mol L^− 1 NaCl as supporting electrolyte when the photoelectrode was biased at + 0.5 V versus saturated calomel electrode. The effects of other electrolytes, dye concentration, pH solution, electrode annealing temperature and applied potentials have been also investigated and are discussed. Several common inorganic salts Na₂SO₄, Na₂CO₃, NaNO₃ and NaCl were chosen to act as supporting electrolytes, which was added into the dye solution. It is shown that the charge-transfer resistance of photoanode can be calculated by the analysis of its electrochemical impedance spectroscopy, and the photoelectrocatalytic degradation rate of yellow direct 42 was inversely proportional to the value of charge-transfer resistance of photoelectrodes at different pH. The value of charge-transfer resistance is smaller, the higher its photoelectro-activity is.     

Comparative study of sputtered and electrodeposited CI(S,Se) and CIGSe thin films

Copper indium disulphide CuInS₂ (CIS) and diselenide CuInSe₂ (CISe) and their alloys with gallium CuIn_1 − xGa_xSe₂ (CIGSe) thin films have been prepared using both high- and non-vacuum processes. The well known two-stage process consisting in a sequential sputtering of Cu and In thin layers and a subsequent sulfurisation has led to the formation of good quality CuInS₂ ternary compound. The films exhibit the well known chalcopyrite structure with a preferential orientation in the (112) plane suitable for the production of the efficient solar cells. The absorption coefficient of the films is higher than 10⁴ cm^− 1 and the band gap value is about 1.43 eV. A non-vacuum technique was also used. It consists on a one step electrodeposition of Cu, In and Se and in a second time Cu, In, Se and Ga. From the morphological and structural point of view, the films obtained are similar to those prepared by the first technique. The band gap value increases up from 1 eV for the CIS films to 1.26 eV for the CuIn_1 − xGa_xSe₂ with 0 < x < 0.23. The resistivity at room temperature of the films was adjusted to 10 Ωcm after annealing. The films exhibit an absorption coefficient more than 10⁵ cm^− 1. The most important conclusion of this study is the interesting potential of electrodeposition as a promising option in low-cost CISe and CIGSe thin film based solar cells processing.     

Electrical, optical, and structural properties of InZnSnO electrode films grown by unbalanced radio frequency magnetron sputtering

We have investigated the electrical, optical, structural, and annealing properties of indium zinc tin oxide (IZTO) films prepared by an unbalanced radio frequency (RF) magnetron sputtering at room temperature, in a pure Ar ambient environment. It was found that the electrical and optical properties of unbalanced RF sputter grown IZTO films at room temperature were influenced by RF power and working pressure. At optimized growth condition, we could obtain the IZTO film with the low resistivity of 3.77 × 10^− 4 Ω cm, high transparency of ~ 87% and figure of merit value of 21.2 × 10^− 3Ω^− 1, without the post annealing process, even though it was completely an amorphous structure due to low substrate temperature. In addition, the field emission scanning electron microscope analysis results showed that all IZTO films are amorphous structures with very smooth surfaces regardless of the RF power and working pressure. However, the rapid thermal annealing process above the temperature of 400 °C lead to an abrupt increase in resistivity and sheet resistance due to the transition of film structure from amorphous to crystalline, which was confirmed by X-ray diffraction examination.     

Ultra-thin zinc oxide film on Mo(100)

Zinc oxide films on a single crystal Mo(100) substrate were fabricated by annealing the pre-deposited metal Zn films in 10^− 5-10^− 4 Pa O₂ ambience at 300-525 K, and were characterized by in situ Auger electron spectroscopy, electron energy loss spectroscopy, low energy electron diffraction and high-resolution electron energy loss spectroscopy. The results show that the atomic ratio of oxygen to zinc in zinc oxide film is significantly dependent on sample annealing temperature and O₂ pressure. A stoichiometric zinc oxide film has been obtained under ∼10^− 4 Pa O₂ at about 400 K. A redshift of Fuchs-Kliewer phonon energy correlated with surface oxygen deficiency is observed.     

The effect of nitrogen on the properties of zinc nitride thin films and their conversion into p-ZnO:N films

Zinc nitride thin films were deposited by magnetron sputtering using ZnN target in plasma containing either N₂ or Ar gases. The rf-power was 100 W and the pressure was 5 mTorr. The properties of the films were examined with thermal treatments up to 550 °C in N₂ and O₂ environments. Films deposited in Ar plasma were opaque and conductive (ρ ∼ 10^− 1 to 10^− 2 Ω cm, N_D ∼ 10¹⁸ to 10²⁰ cm^− 3) due to excess of Zn in the structure. After annealing at 400 °C, the films became more stoichiometric, Zn₃N₂, and transparent, but further annealing up to 550 °C deteriorated the electrical properties. Films deposited in N₂ plasma were transparent but very resistive even after annealing. Both types of films were converted into p-type ZnO upon oxidation at 400 °C. All thermally treated zinc nitride films exhibited a shoulder in transmittance at around 345 nm which was more profound for the Ar-deposited films and particularly for the oxidized films. Zinc nitride has been found to be a wide band gap material which makes it a potential candidate for transparent optoelectronic devices.     

Luminescent properties of YAG:Ce phosphor powders prepared by hydrothermal-homogeneous precipitation method

Y_3 − xCe_xAl₅O₁₂ (YAG:Ce³⁺) phosphor powders were successfully prepared by hydrothermal-homogenous precipitation (HHP) method, under mild conditions with inexpensive aluminum and yttrium nitrates as the starting materials and urea as homogenous precipitant. The pure YAG crystalline phase could be formed after hydrothermal treatment at 100 °C for 4 h and 240 °C for 20 h and postannealing process at 1200 °C for 2 h. All of the as-prepared YAG:Ce³⁺ powders did not have the CeO₂ phase. The photoluminescence spectrum of crystalline YAG:Ce³⁺ phosphors showed the emission intensity of phosphor increased with increasing the annealed temperature and reached its maximum as the molar fraction of cerium ion was 0.10, and also showed the maximum emission wavelength nearly unchanged with the calcination temperature and cerium doping concentration.     

Synthesis of LiNi0.9Co0.1O2 cathode material for lithium secondary battery by a novel route

The cathode material, LiNi_0.9Co_0.1O₂ was prepared using a rheological phase reaction method with LiOH·H₂O, home-made Ni(OH)₂, and Co₂O₃ as starting materials. At first, the mixture of reactants and a proper amount of water reacted to form a rheological precursor. Then the dried precursor was heated at 730 °C in one step to yield the product. The effects of calcination time (between 0.5 and 10 h) on the structural, morphological and electrochemical properties were investigated. All obtained powders show a single phase with α-NaFeO₂ structure (R-3m space group). The sample prepared in 2.5 h delivers the largest initial discharge capacity of 218 mA h g^− 1 (3.0-4.35 V, 25 mA g^− 1) and still remains 192 mA h g^− 1 after 15 cycles. The method is simple, economical and effective and is promising for practical application.     

Effects of heat treatment on properties of ITO films prepared by rf magnetron sputtering

Indium tin oxide (ITO) films were deposited on glass substrates by rf magnetron sputtering using a ceramic target (In₂O₃-SnO₂, 90-10 wt%) without extra heating. The post annealing was done in air and in vacuum, respectively. The effects of annealing on the structure, surface morphology, optical and electrical properties of the ITO films were studied. The results show that the increase of the annealing temperature improves the crystallinity of the films, increases the surface roughness, and improves the optical and electrical properties. The transmittance of the films in visible region is increased over 90% after the annealing process in air or in vacuum. The resistivity of the films deposited is about 8.125×10⁻⁴ Ω cm and falls down to 2.34×10⁻⁴ Ω cm as the annealing temperature is increased to 500°C in vacuum. Compared with the results of the ITO films annealed in air, the properties of the films annealed in vacuum is better.