Chemical solution deposition of CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> thin film

CaCu₃Ti₄O₁₂ (CCTO) thin film was successfully deposited on boron doped silica substrate by chemical solution deposition and rapid thermal processing. The phase and microstructure of the deposited films were studied as a function of sintering temperature, employing X-ray diffractometry and scanning electron microscopy. Dielectric properties of the films were measured at room temperature using impedance spectroscopy. Polycrystalline pure phase CCTO thin films with (220) preferential orientation was obtained at a sintering temperature of 750°C. There was a bimodal size distribution of grains. The dielectric constant and loss factor at 1 kHz obtained for a film sintered at 750°C was k ∼ 2000 and tan δ ∼ 0.05.     

Fast response detection of H2S by CuO-doped SnO2 films prepared by electrodeposition and oxidization at low temperature

Fast response detection of H₂S by CuO-doped SnO₂ films prepared was prepared by a simple two-step process: electrodeposition from aqueous solutions of SnCl₂ and CuCl₂, and oxidization at 600 °C. The phase constitution and morphology of the CuO-doped SnO₂ films were characterized by X-ray diffraction and scanning electron microscopy. In all cases, a polycrystalline porous film of SnO₂ was the product, with the CuO deposited on the individual SnO₂ particles. Two types of CuO-doped SnO₂ films with different microstructures were obtained via control of oxidation time: nanosized CuO dotted island doped SnO₂ and ultra-uniform, porous, and thin CuO film coated SnO₂. The sensor response of the CuO doped SnO₂ films to H₂S gas at 50–300 ppm was investigated within the temperature range of 25–125 °C. Both of the CuO-doped SnO₂ films show fast response and recovery properties. The response time of the ultra-uniform, porous, and thin CuO coated SnO₂ to H₂S gas at 50 ppm was 34 s at 100 °C, and its corresponding recovery time was about 1/3 of the response time.     

Chemical synthesis and characterization of hydrous tin oxide (SnO<Subscript><Emphasis Type="Bold">2</Emphasis></Subscript>:H<Subscript><Emphasis Type="Bold">2</Emphasis></Subscript>O) thin films

In the present investigation, we report chemical synthesis of hydrous tin oxide (SnO ₂ :H ₂ O) thin films by successive ionic layer adsorption and reaction (SILAR) method at room temperature ( \thicksim \thicksim 300 K). The films are characterized for their structural and surface morphological properties. The formation of nanocrystalline SnO ₂ with porous and agglomerated particle morphology is revealed from X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies, respectively. The Fourier transform infrared spectroscopy (FTIR) study confirmed the formation of Sn–O phase and hydrous nature of the deposited film. Static water contact angle studies showed the hydrophilic nature of SnO ₂ :H ₂ O thin film. Electrical resistivity showed the semiconducting behaviour with room temperature electrical resistivity of 10 ⁵  W\boldsymbol\Omega cm. The electrochemical properties studied in 0·5 M Na ₂ SO ₄ electrolyte showed a specific capacitance of 25 F g ^− 1 at 5 mVs ^− 1 scan rate.     

On the synthesis,characterization and photocatalytic applications of nanostructured TiO<Subscript>2</Subscript>

Nanocrystalline semiconducting materials are attracting much attention due to their potential applications in solar energy conversion, nonlinear optics, and heterogeneous photocatalysis. In the present investigation, we have synthesized nanostructured TiO₂ photocatalysts, which have been used in the photocatalytic degradation of phenol (one of the most common water pollutants). These catalysts have been prepared through sol-gel technique using titanium tetra-isopropoxide as a raw material for synthesis. Characterization techniques such as XRD, SEM and TEM have been employed for structural/microstructural investigations. XRD results show that the as synthesized TiO₂ nanopowder exhibit anatase phase, TiO₂. The average sizes of the TiO₂ nanopowders are ∼ 5–10 nm. The optical properties of the samples were investigated through UV-visible and fluorescence techniques. It has been observed that absorption edge corresponds to ∼ 410 nm (bandgap, ∼ 3.02 eV). The emission peak in the fluorescence spectrum at ∼ 418 nm corresponds to the bandgap energy of ∼ 2.97 eV. Concentration of phenol (initial concentration, ∼ 100 ppm) with illumination time was monitored by measuring the absorbance of pure and illuminated phenol through UV-visible spectrophotometer. Salient feature of this study relates to the fact that the present sol-gel synthesized TiO₂ nanopowders have been found to be better photocatalysts for phenol degradation than the presently employed commercial TiO₂ (P-25, Degussa) photocatalyst. Thus, whereas phenol concentration, with the presently synthesized TiO₂ nanopowders, the concentration of phenol decreases up to ∼ 32% but for commercial TiO₂ nanopowder (P-25, Degussa), it decreased only up to ∼ 25%. The improved surface area is considered as an important factor for the aforesaid decrease in phenol concentration.     

Ethanol and LPG sensing characteristics of SnO<Subscript>2</Subscript> activated Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> thick film sensor

The sensing response of pure and SnO₂ activated Cr₂O₃ to ethanol vapours and liquefied petroleum gas (LPG) has been investigated. Fine particles of commercial chromium oxide powder were selected and deposited as thick film to act as a gas sensor. The sensor surface has been activated by tin dioxide, on surface oxidation of tin chloride. The concentration of tin chloride solution, used as activator, was varied from 0 to 5% and its effect on gas response, selectivity and operating temperature has been studied. It was found that response to ethanol vapours significantly improved, whereas response to LPG remained unaffected. Moreover, operating temperature remains unchanged both for LPG and ethanol vapours.     

Superconducting YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−δ</Subscript> thick film (T<Subscript>c</Subscript>(0) = 92 K) on a newly developed perovskite ceramic substrate

A complex perovskite oxide, YbBa₂NbO₆, as a non-reacting substrate for YBa₂Cu₃O_7-° super-conducting film has been developed. The dielectric constant and loss factor values of the material are in the range suitable for its use as substrate for microwave applications. A YBa₂Cu₃O_7−δ superconducting thick film dip coated on YbBa₂NbO₆ substrate gave a T_c (0) of 92 K and current density of ∼ 1.3 × 10⁴ A cm⁻².     

Gas sensing properties of nano SnO<Subscript>2</Subscript> based thick films prepared by dip coating method with effect of molarity of PtCl<Subscript>2</Subscript> solution

Synthesized nanophase SnO₂ powder was used as a functional material along with optimized 15 wt% of glass, fired at 550 °C for better adhesion, to fabricate thick films using screen printing on alumina substrate. Their surface was modified by dip coating in platinum chloride solution (PtCl₂) of different molarities (0.05–0.2 M). A subsequent thermal treatment to these thick films was carried out at an optimized temperature of 750 °C in air atmosphere. The films were tested for 400 ppm concentration of H₂, CO and LPG. Sensors dip coated with 0.15 M solution of PtCl₂ show the highest sensitivity towards the test gases which is ten times higher than undoped SnO₂ sensors.XRD, EDX and SEM measurements showed that the behavior could be associated with the spatial distribution of the platinum within the tin oxide film. The sensors have fast response time of 10 s to all the three gases with a minimum detection limit of 10 ppm.     

(Cu, Fe, Co, or Ni)-doped tin dioxide films deposited by spray pyrolysis: doping influence on film morphology

The results of structural characterization of SnO₂ films doped by impurities such as Fe, Cu, Ni, and Co during spray pyrolysis deposition from 0.2 M SnCl₄–water solutions are presented. The change of parameters such as film morphology, the grain size, texture, and the intensity of X-ray diffraction peaks were controlled. For structural analysis of tested films, we used X-ray Diffraction, Scanning Electron Microscopy, and Atomic Force Microscopy techniques. It was shown that the doping promoted the change of the film morphology and the decrease of the SnO₂ grain size; however, these changes were not great. The doping influence becomes apparent more obviously for thin films and the films deposited at low temperatures (T _pyr ∼ 350 °C). At higher pyrolysis temperatures (T _pyr ∼ 450 °C), the influence of the doping on both the grain size and the film morphology was weakened. We concluded that used additives had dominant influence on the structural properties of SnO₂ at the initial stages of the film growth, as well as at the stages of twinning and agglomeration of the SnO₂ crystallites. It was shown that the increase in the contents of the fine dispersion phase in as-deposited film is an important consequence of the SnO₂ doping.     

Effect of N<Subscript>2</Subscript> gas annealing and SiO<Subscript>2</Subscript> barrier on the optical transmittance and electrical resistivity of a transparent Sb-doped SnO<Subscript>2</Subscript> conducting film

During the fabrication process of transparent conducting thin films of ATO (antimony-doped tin oxide) on a soda lime glass substrate by a sol-gel dip coating method, the effects of the SiO₂ buffer layer formed on the substrate and N₂ annealing treatment were investigated quantitatively. The deposited ATO thin film was identified as a crystalline SnO₂ phase and the film thickness was about 100 nm/layer at a withdrawal speed of 50 mm/min. Optical transmittance and electrical resistivity of the 400 nm-thick ATO thin film that was deposited on SiO₂ buffer layer/soda lime glass and then annealed under nitrogen atmosphere were 84% and 5.0 × 10^–3cm, respectively. The XPS analysis confirmed that a SiO₂ buffer layer inhibited Na ion diffusion from the substrate, preventing the formation of a secondary phase such as Na₂SnO₃ and SnO and increasing Sb ion concentration and ratio of Sb⁵⁺/Sb³⁺ in the film. It was found that N₂ annealing treatment leads to the reduction of Sn⁴⁺ as well as Sb⁵⁺, however the reduction of Sn⁴⁺ is more effective, and consequently results in a decrease in the electrical resistivity to produce excellent electrical properties in the film. © Springer Science + Business Media, Inc.     

Synthesis and Optical Studies of Superconducting MgB<Subscript>2</Subscript> Thin Films

Synthesis and optical transmission of MgB₂ thin films on optically transparent glass are reported. In the 400–1000 nm regime as deposited films show high metallic reflectivity and very little transmission. After deposition, the films were annealedex situ and rendered superconducting withT _c of 38 K, approaching that of the bulk material. The reaction conditions where quite soft ∼ 10 min at 550°C. The optical absorption coefficient,α and photon energy,E followed a Tauc-type behavior, (αE)^1/2=β _T(E −E _g). The band gap (E _g) was observed to peak at 2.5 eV; but, the slope parameterβ _Tbehaved monotonically with reaction temperature. Our results indicate that an intermediate semiconducting phase is produced before the formation of the superconducting phase; also optical measurements provide valuable information in monitoring the synthesis of MgB₂ from its metallic constituents. In addition these films have interesting optical properties that may be integrated into optoelectronics.     

Piezoelectric and optical properties of ZnO thin films deposited using various O<Subscript>2</Subscript>/(Ar+O<Subscript>2</Subscript>) gas ratios

In this study, ZnO thin films were fabricated on a Pt(111)/TiO_x/SiO₂/Si substrate using the RF magnetron sputtering method. Then, the effect of the crystallization orientation and microstructure on the piezoelectric and optical properties of the ZnO thin film was investigated for various O₂/(Ar+O₂) gas ratios. When the O₂/(Ar+O₂) gas ratio was 50%, the intensity of the (002) peak corresponding to the preferred orientation of the ZnO thin film was a maximum and the minimum FWHM value of 0.56° was observed. The surface roughness of the ZnO thin film measured using AFM also had a minimum value of 16.43 °C at an O₂/(Ar+O₂) gas ratio of 50%. The piezoelectric characteristics of the ZnO thin film were measured using the pneumatic loading method (PLM) and the corresponding constant had the largest value of 11.9 pC/N at an O₂/(Ar+O₂) gas ratio of 50%. The transmittance of the ZnO thin film obtained from the transmittance curve using a spectrophotometer was slightly greater than 80% in the human visible light region at an O₂/(Ar+O₂) gas ratio of 50%. By using the refractive index data obtained from the transmittance curve and the Sellmeir dispersion relation, we can also predict the refractive index at a wavelength of 400 nm. When the O₂/(Ar+O₂) gas ratio was 50%, the refractive index was 2.043 and, at other gas ratios, the corresponding refractive indices were 2.004∼2.006. The band gap energies of the ZnO thin film were 3.27∼3.33 eV depending on the O₂/(Ar+O₂) gas ratio and were little affected by the variation of the oxygen inflow volume.     

Synthesis,characterization and gas sensing performance of SnO<Subscript>2</Subscript> thin films prepared by spray pyrolysis

In this work, SnO₂ thin films were deposited onto alumina substrates at 350°C by spray pyrolysis technique. The films were studied after annealing in air at temperatures 550°C, 750°C and 950°C for 30 min. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and optical absorption spectroscopy technique. The grain size was observed to increase with the increase in annealing temperature. Absorbance spectra were taken to examine the optical properties and bandgap energy was observed to decrease with the increase in annealing temperature. These films were tested in various gases at different operating temperatures ranging from 50–450°C. The film showed maximum sensitivity to H ₂S gas. The H₂S sensing properties of the SnO₂ films were investigated with different annealing temperatures and H ₂S gas concentrations. It was found that the annealing temperature significantly affects the sensitivity of the SnO₂ to the H ₂S. The sensitivity was found to be maximum for the film annealed at temperature 950°C at an operating temperature of 100°C. The quick response and fast recovery are the main features of this film. The effect of annealing temperature on the optical, structural, morphological and gas sensing properties of the films were studied and discussed.     

Characterization and photocatalytic activity of boron-doped TiO<Subscript>2</Subscript> thin films prepared by liquid phase deposition technique

Boron doped TiO₂ thin films have been successfully deposited on glass substrate and silicon wafer at 30°C from an aqueous solution of ammonium hexa-fluoro titanate and boron trifluoride by liquid phase deposition technique. The boric acid was used as an F ⁻ scavenger. The resultant films were characterized by XRD, EDAX, UV and microstructures by SEM. The result shows the deposited film to be amorphous which becomes crystalline between 400 and 500°C. The EDAX and XRD data confirm the existence of boron atom in TiO₂ matrix and a small peak corresponding to rutile phase was also found. Boron doped TiO₂ thin films can be used as photocatalyst for the photodegradation of chlorobenzene which is a great environmental hazard. It was found that chlorobenzene undergoes degradation efficiently in presence of boron doped TiO₂ thin films by exposing its aqueous solution to visible light. The photocatalytic activity increases with increase in the concentration of boron.     

Temperature dependent growth and optical properties of SnO<Subscript>2</Subscript> nanowires and nanobelts

SnO₂ nanowires and nanobelts have been grown by the thermal evaporation of Sn powders. The growth of nanowires and nanobelts has been investigated at different temperatures (750–1000°C). The field emission scanning electron microscopic and transmission electron microscopic studies revealed the growth of nanowires and nano-belts at different growth temperatures. The growth mechanisms of the formation of the nanostructures have also been discussed. X-ray diffraction patterns showed that the nanowires and nanobelts are highly crystalline with tetragonal rutile phase. UV-visible absorption spectrum showed the bulk bandgap value (∼ 3–6 eV) of SnO₂. Photoluminescence spectra demonstrated a Stokes-shifted emission in the wavelength range 558–588 nm. The Raman and Fourier transform infrared spectra revealed the formation of stoichiometric SnO₂ at different growth temperatures.     

Synthesis of nanocrystalline SnO<Subscript>2</Subscript> powder at 100°C

A simple gel to crystal conversion route has been followed for the preparation of nanocrystalline SnO₂ at 80–100°C under refluxing conditions. Freshly prepared stannic hydroxide gel is allowed to crystallize under refluxing and stirring conditions for 4–6 h. Formation of nano crystallites of SnO₂ is confirmed by X-ray diffraction (XRD) study. Transmission electron microscopic (TEM) investigations revealed that the average particle size is 30 nm for these powders.     

Effects of Ni doping on photocatalytic activity of TiO<Subscript>2</Subscript> thin films prepared by liquid phase deposition technique

The TiO₂ thin films doped by Ni uniformly and non-uniformly were prepared on glass substrate from an aqueous solution of ammonium hexa-fluoro titanate and NiF₂ by liquid phase deposition technique. The addition of boric acid as an F ⁻ scavenger will shift the equilibrium to one side and thereby deposition of the film is progressed. The rate of the reaction and the nature of deposition depend on growing time and temperature. The resultant films were characterized by XRD, EDAX, UV and SEM. The result shows that the deposited films have amorphous background, which becomes crystalline at 500°C. The EDAX data confirms the existence of Ni atoms in TiO₂ matrix. XRD analysis reveals the peaks corresponding to Ni but no peak of crystalline NiO was found. The transmittance spectra of Ni uniformly and non-uniformly doped TiO₂ thin films show ‘blue shift and red shift’, respectively. Ni-doped TiO₂ thin films can be used as photocatalyst for the photodegradation of methyl orange dye. It was found that, organic dye undergoes degradation efficiently in presence of non-uniformly Ni-doped TiO₂ thin films when compared to uniformly doped films and pure TiO₂ films under visible light. The photocatalytic activity increases with increase in the concentration of Ni in case of nonuniformly doped thin films but decreases with the concentration when uniformly doped thin films were used.     

Synthesis and characterization of nanostructured SnO<Subscript>2</Subscript> film

Nanostructured tin dioxide (SnO₂) film was deposited on glass substrate by thermal evaporation of tin metal followed by thermal oxidation at 600 °C for 2 h. XRD investigation confirms that grown film is crystalline tetragonal rutile. The average optical transmittance of the film was as high as 90%. The optical band gap of the nanostructured SnO₂ was estimated from transmittance data and found to be 3.4 eV. The variation of electrical conductivity with temperature was investigated. The root mean square (RMS) roughness and topography of the film were investigated by atomic force microscopy and found to be 2 nm with grain size of 17 nm.     

Highly Transparent and Conductive Zn<Subscript>0.86</Subscript>Cd<Subscript>0.11</Subscript>In<Subscript>0.03</Subscript>O Thin Film Prepared by Pulsed Laser Deposition

Zn_0.86Cd_0.11In_0.03O alloy semiconductor film was deposited on quartz substrate by pulsed laser deposition technique. Cd is used to change the optical band gap and In is used to increase the carrier concentration of the ZnO film. XRD studies confirm that the structure of Zn_0.86Cd_0.11In_0.03O is hexagonal wurtzite structure without CdO phase appeared. FE-SEM shows that the grain size of Zn_0.86Cd_0.11In_0.03O film is smaller than that of ZnO. These films are highly transparent (∼85%) in visible region. Most importantly, the electrical properties of Zn_0.86Cd_0.11In_0.03O film highly improved with In doped. It has low resistivity (4.42×10⁻³ Ω cm) and high carrier concentration (5.50×10¹⁹ cm⁻³) that enable this film a promising candidate for window layer in solar cells and other possible optoelectronic applications.     

Electrodeposition and electrocatalytic characteristics of porous crystalline SnO2 thin film using butyl-rhodamine B as a structure-directing agent

Porous crystalline SnO₂ thin films were electrodeposited from an oxygen-saturated acid aqueous solution of SnCl₂ containing different amounts of butyl rhodamine B (BRhB) at 70 °C. BRhB can not only be dissolved in the acid deposition solution due to its amidocyanogen substitute, where HCl was added to suppress hydrolysis of SnCl₂, but also be adsorbed on the surface of SnO₂ through its carbonate substitute. Therefore, it was used as a structure-directing agent to control the growth of SnO₂ crystals and then the crystalline structure and surface morphology of the deposited film. The electrodeposited thin films show porous morphology and rutile-type SnO₂ crystalline structure due to the effects of BRhB on the growth, and these structural features can be adjusted by changing the added amount of BRhB. The SnO₂ thin film electrodeposited with addition of BRhB exhibits electrocatalytic characteristic enhancement on oxidation of phenol due to its porous structure.     

Characterization of spray deposited CoWO<Subscript>4</Subscript> thin films for photovoltaic electrochemical studies

Preparation of Cobalt tungstate (CoWO₄) thin film by spray pyrolysis with ammonical solution as a precursor is presented. The phase and surface morphology characterizations have been carried out by XRD and SEM analysis. The study of optical absorption spectrum in the wavelength range 350 – 850 nm shows direct as well as indirect optical transitions in the thin film material. The d. c. electrical conductivity measurements in the temperature range 310–500 K indicate semiconducting behavior of the thin film. The thin films deposited on fluorine doped tin oxide (FTO) coated conducting glass substrates were used as a photoanode in photovoltaic electrochemical (PVEC) cell with configuration: CoWO₄ | Ce⁴⁺, Ce³⁺ | Pt; 0.1 M in 0.1 N H₂SO₄. The PVEC characterization reveals the fill factor and power conversion efficiency to be 0.36 and 0.62%, respectively. The flat band potential is found to be −0.18 V (SCE).