Characteristics of pulse electrodeposited PbS thin films

PbS thin films were deposited for the first time using the pulse electrodeposition technique at different duty cycles in the range of 9 to 50% and at room temperature using lead nitrate and sodium thiosulphate. The thickness of the films increased from 0.5 to 1.0 μm with increase of duty cycle. The films were polycrystalline and exhibited cubic structure. The band gap of the films deposited at 50% duty cycle is 0.42 eV. The resistivities of the films decreased from 0.9 to 0.5 × 10⁵ ohm cm as the duty cycle increased. Films with grain size in the range of 20 to 35 nm were deposited. Films with refractive index varying in the range of 4.45–3.75 with increase of wavelength were obtained. Films with higher photosensitivity and higher detectivity compared to earlier reports were obtained.     

Photoelectrochemical behaviour of pulse plated CdS films

Cadmium sulphide (CdS) films were deposited by the pulse plating technique at room temperature and at different duty cycles in the range of 6–50% using AR grade 0.25 M cadmium sulphate and 0.30 M sodium thiosulphate at a deposition potential of −0.75 V (SCE). The total deposition time was kept constant at 1 h. The thickness of the films were around 2.0 μm. X-ray diffraction (XRD) studies indicate the formation of polycrystalline films with the cubic structure. The crystallite size increased from 23.0 to 27.5 nm as the duty cycle increased from 10 to 50%. Optical absorption studies indicated a direct band gap in the range of 2.40–2.80 eV as the duty cycle is decreased. XPS studies indicated the formation of CdS. Photoelectrochemical (PEC) cell measurements made with the photoelectrodes deposited at 50% duty cycle have exhibited higher conversion efficiency compared to earlier reports.     

Properties of GaAs films deposited by pulse periodic technique

GaAs is a III-V compound possessing high mobility and a direct band gap of 1.43 eV , making it a very suitable candidate for photovoltaic applications. Thin GaAs films were prepared at room temperature by plating an aqueous solution containing GaCl₃ and As₂O₃ at a pH of 2. The current density was kept as 50 mA cm⁻² and the duty cycle was varied in the range 10–50%. The films were deposited on titanium and tin oxide coated glass substrates. Films exhibited polycrystalline nature with peaks corresponding to single phase GaAs. Optical absorption measurements indicated a direct band gap of 1.40 eV. The surface roughness of the films varied from 3 nm to 6 nm as the duty cycle increased. Raman spectra indicated both the LO and TO phonons for the films deposited at duty cycles above 25%. Photoelectrochemical studies indicated that the current and voltage output are higher than earlier reports on thin film electrodes.     

Pulse plated zinc sulphide films and their characteristics

Zinc sulphide thin films were deposited by the pulse plating technique using AR grade Zinc sulphate and sodium thiosulphate precursors. The pH of the deposition bath was adjusted to 2. The duty cycle was varied in the range of 20–60%. Total deposition time was kept constant as 60 min in all the cases. X-ray diffraction studies indicated the formation of single phase cubic zinc sulphide films. After heat treatment the crystal structure transformed to hexagonal structure. Optical absorption measurements indicated a band gap values in the range of 3.6–4.0 eV as the duty cycle decreased. EDAX studies yielded a composition of the films deposited at 50% duty cycle is Zn = 48%, S = 52%. XPS studies indicated the formation of ZnS. The Zn 2p and S 3p peaks are observed. AFM studies indicated a rms value of surface roughness of 55 nm for the films deposited at a duty cycle of 60%.     

Structural,optical, electrical and morphological properties of ZnTe films deposited by electron beam evaporation

ZnTe films were deposited on glass substrates at different substrate temperatures in the range 30–300 °C. The thickness of the films was about 200 nm. The films exhibited cubic structure with preferential orientation in the (111) direction. Band gap values in the range 2.34–2.26 eV are observed with increase of the substrate temperature. The refractive index values are in the range of 2.55–2.92 for the films deposited at different substrate temperatures. It is observed that the conductivity increases continuously with temperature. Laser Raman studies indicated the presence of peaks at 206.9 and 412.2 cm⁻¹corresponding to the first order and second order LO phonon.     

ZnO nanocrystalline thin films: a correlation of microstructural,optoelectronic properties

The compositional, structural, microstructural, dc electrical conductivity and optical properties of undoped zinc oxide films prepared by the sol–gel process using a spin-coating technique were investigated. The ZnO films were obtained by 5 cycle spin-coated and dried zinc oxide films followed by annealing in air at 600 °C. The films deposited on the platinum coated silicon substrate were crystallized in a hexagonal wurtzite form. The energy-dispersive X-ray (EDX) spectrometry shows Zn and O elements in the products with an approximate molar ratio. TEM image of ZnO thin film shows that a grain of about 60–80 nm in size is really an aggregate of many small crystallites of around 10–20 nm. Electron diffraction pattern shows that the ZnO films exhibited hexagonal structure. The SEM micrograph showed that the films consist in nanocrystalline grains randomly distributed with voids in different regions. The dc conductivity found in the range of 10⁻⁵–10⁻⁶ (Ω cm)⁻¹. The optical study showed that the spectra for all samples give the transparency in the visible range.     

Properties of pulse electrodeposited copper gallium sulphide films

Copper gallium sulphide films were deposited for the first time by the pulse electrodeposition technique at different duty cycles in the range of 6–50 % at room temperature and at a constant current density of 1.0 mA cm^?2. The films exhibited single phase copper gallium sulphide. The grain size increased from 30 to 70 nm with increase of duty cycle. Optical band gap of the films varied in the range of 2.30–2.36 eV. The resistivity increased from 0.10 to 1.70 ohm cm with increase of duty cycle from 6 to 50 %. Preliminary studies on solar cells with p-CuGaS₂/n-CuInS₂ junction yielded an efficiency of 4.14 %. This is the first report on solar cells using CuGaS₂ with CuInS₂.     

Properties of pulse electrodeposited copper indium selenide films

Copper Indium Selenide films were deposited by the pulse plating technique at different bath temperatures in the range of 30–80 °C and at 50 % duty cycle (15 s ON and 15 s OFF). X-ray diffraction studies indicated the formation of single phase chalcopyrite copper indium selenide films. The band gap of the films decreased from 1.17 to 1.05 eV with decrease of duty cycle. Atomic force microscope studies indicated that the surface roughness and grain size increased with duty cycle. Room temperature resistivity of the films is in the range of 0.01–2.0 ohm cm. Films deposited at 50 % duty cycle have exhibited a V_oc of 0.59 V, J_sc of 15 mA cm^?2, FF of 0.75 and efficiency of 6.64 %.     

Characteristics of pulse electrodeposited AgGaSe2 films

In this work, the pulse electrodeposition technique has been employed for the first time to deposit AgGaSe₂ films. The films were deposited at room temperature from a bath containing Analar grade 10 mM silver nitrate, 10 mM gallium nitrate and 10 mM SeO₂. The deposition potential was maintained as—0.68 V (SCE). Tin oxide coated glass substrates (5.0 ohms/sq) was used as the substrate. The duty cycle was varied in the range of 6–50 %. The XRD profile of the thin films deposited at different duty cycles indicate the peaks corresponding to AgGaSe₂. Atomic force microscopy studies indicated that the surface roughness increased from 0.95 to 1.25 nm with duty cycle. The transmission spectra exhibited interference fringes. Refractive index of 2.71 was observed in the wavelength range 600–1,000 nm. Electrochemical Impedance studies indicated a single semicircle. The grain boundary resistance decreased with increase of duty cycle.     

Water-based sol–gel nanocrystalline barium titanate: controlling the crystal structure and phase transformation by Ba:Ti atomic ratio

Highly stable, water-based barium titanate (BaTiO₃) sols were developed by a low cost and straightforward sol–gel process. Nanocrystalline barium titanate thin films and powders with various Ba:Ti atomic ratios were produced from the aqueous sols. The prepared sols had a narrow particle size distribution in the range 21–23 nm and they were stable over 5 months. X-ray diffraction pattern revealed that powders contained mixture of hexagonal- or perovskite-BaTiO₃ as well as a trace of Ba₂Ti₁₃O₂₂ and Ba₄Ti₂O₂₇ phases, depending on annealing temperature and Ba:Ti atomic ratio. Highly pure barium titanate with cubic perovskite structure achieved with Ba:Ti = 50:50 atomic ratio at the high temperature of 800 °C, whereas pure barium titanate with hexagonal structure obtained for the same atomic ratio at the low temperature of 500 °C. Transmission electron microscope revealed that the crystallite size of both hexagonal- and perovskite-BaTiO₃ phases reduced with increasing the Ba:Ti atomic ratio, being in the range 2–3 nm. Scanning electron microscope analysis revealed that the average grain size of barium titanate thin films decreased with an increase in the Ba:Ti atomic ratio, being in the range 28–35 nm. Moreover, based on atomic force microscope images, BaTiO₃ thin films had a columnar-like morphology with high roughness. One of the highest specific surface area reported in the literature was obtained for annealed powders at 550 °C in the range 257–353 m²g⁻¹.     

Novel process for low temperature crystallization of a-SiC:H for optoelectronic applications

Metal-induced crystallization (MIC) process was employed to crystallize hydrogenated amorphous silicon carbide (a-SiC:H) films deposited by PECVD on n-type Si substrate. To optimize the crystallization process, Aluminum thin films of different thicknesses were deposited on a-SiC:H films which were then annealed at 600 °C in N₂ environment for 1 h. UV–visible spectrophotometer, atomic force microscopy (AFM) and hall measurement system were used to characterize the films. It was observed from the UV–visible spectrum that the films crystallized using higher Al thickness show absorption in the visible range whereas the samples crystallized with lower Al thickness did not show absorption in the visible range but shows large absorption above the bandgap of the material. Considering UV–visible and Hall measurement data it can be concluded that the sample crystallized with 50 nm of Al can be a good candidate for SiC–Si hetero-junction solar cells.     

P-type semiconducting Cu2O–NiO thin films prepared by magnetron sputtering

P-type semiconducting thin films consisting of a new multicomponent oxide composed of Cu₂O and NiO were deposited on glass substrates by r.f. magnetron sputtering using Cu₂O–NiO mixed powder targets. The multicomponent oxide thin films deposited in an Ar atmosphere with a Ni content (Ni/(Cu + Ni) atomic ratio) in the range from 0 to 100 at.% were found to be p-type semiconductors. As the Ni content was increased in the range from 0 to about 30 at.%, the energy bandgap of the resulting films gradually increased as well as the obtained resistivity increased from 70 to 4 × 10⁴ Ω cm, a consequence of decreases in both the Hall mobility and the hole concentration. The films prepared with a Ni content of about 30–50 at.% exhibited a relatively constant resistivity and energy bandgap. The resistivity and the energy bandgap of films prepared with a Ni content above about 60 at.% considerably increased as the Ni content was increased. Furthermore, a pn thin-film heterojunction prepared by depositing undoped n-ZnO and p-multicomponent oxide (Ni content of 50 at.%) thin films exhibited a rectifying I–V characteristic.     

Characterization of Tin disulphide thin films prepared at different substrate temperature using spray pyrolysis technique

Thin films of tin disulphide on glass substrates were prepared by spray pyrolysis technique using precursor solutions of SnCl₂·2H₂O and n–n dimethyl thiourea at different substrate temperatures varied in the range 348–423 K. Using the hot probe technique the type of conductivity is found to be n type. X ray diffraction analysis revealed the polycrystalline nature with increasing crystallinity with respect to substrate temperature. The preferential orientation growth of SnS₂ compound having hexagonal structure along (002) plane increased with the substrate temperature. The size of the tin disulphide crystallites with nano dimension were determined using the Full Width Half Maximum values of the Bragg peaks and found to increase with the substrate temperature. The surface morphology had been observed on the surface of these films using scanning electron microscope. The optical absorption and transmittance spectra have been recorded for these films in the wavelength range 400–800 nm. Thickness of these films was found using surface roughness profilometer. The absorption coefficient (α) was determined for all the films. Direct band gap values were found to exist in all the films deposited at different substrate temperatures. The value of room temperature resistivity in dark decreased from 5.95 × 10³ Ω cm for the amorphous film deposited at low temperature (348 K) to 2.22 × 10³ Ω cm for the polycrystalline film deposited at high temperature (423 K) whereas the resistivity values in light decreased from 1.48 × 10³ to 0.55 × 10³ Ω cm respectively, which is determined using the four probe method. Activation energy of these thin films was determined by Arrhenius plot.     

Effect of formaldehyde gas adsorption on the electrical conductivity of Pd-doped TiO<Subscript>2</Subscript> thin films

0.5 wt% Pd-doped titanium oxide thin films were obtained by dip-coating on silicon substrates. The films were compacted by annealing in air at 300 and 500 °C. Temperature dependent electrical conductivity measurements were performed in the temperature range 373–623 K, in different environments (air, methane, acetone, ethanol, formaldehyde and liquefied petroleum gas), to test the films sensing gas properties. Formaldehyde was found to be the test gas that produces the most significant changes in the electrical conductivity of the studied films. This was the reason why it was chosen to investigate its effect on their electrical conductivity. A model was proposed, the model of the potential fluctuations at grain boundaries. A comparison between some parameters obtained in the proposed model was performed as a function of annealing temperature, and as a function of gas atmosphere. The values of the mean barrier height and the standard deviation were estimated to range between 0.336–0.588 eV and 0.175–0.199 eV, respectively. It was found that formaldehyde leads to a rather sharp decrease in the values of the barrier height and the standard deviation, and to an increase in the conductivity. We have observed the best sensing gas performance for the films annealed at 300 °C, comparing to their counterparts annealed at 500 °C, explained by the lowest values of the barrier energy height and the standard deviation.     

Power and gas pressure effects on properties of amorphous In–Ga–ZnO films by magnetron sputtering

Amorphous In–Ga–ZnO thin films were deposited on quartz glass substrate at room temperature utilizing radio frequency magnetron sputtering technique. Sputtering power and oxygen flow rate effects on the physical properties of the In–Ga–ZnO films were systematically investigated. It is shown the film deposition rate and the conductivity of the In–Ga–ZnO films increased with the sputtering power. The as-grown In–Ga–ZnO films deposited at 500 W exhibited the Hall mobility of 17.7 cm²/Vs. Average optical transmittance of the In–Ga–ZnO films is greater than 80% in the visible wavelength. The extracted optical band gap of the In–Ga–ZnO films increased from 3.06 to 3.46 eV with increasing the sputtering power. The electrical properties of the In–Ga–ZnO films are greatly dependent on the O₂/Ar gas flow ratio and post-growth annealing process. Increasing oxygen flow rate converted the In–Ga–ZnO films from semiconducting to semi-insulating, but the resistivity of the films was significantly reduced after being annealed in vacuum. Both the as-grown and annealed In–Ga–ZnO films show n-type electrical conductivity.     

Effects of substrate temperatures on the thermal stability of Al-doped ZnO thin films grown by DC magnetron sputtering

In this work, Al-doped (4 at%) ZnO(AZO) thin films were prepared by DC magnetron sputtering using a home-made ceramic target at different substrate temperatures. The microstructure, optical, electrical and thermal stability properties of these thin films were characterized systematically using scanning electron microscopy, UV–Vis-NIR spectrometry, X-ray diffraction, and Hall measurements. It was observed that the AZO thin films deposited at 350 °C exhibited the lowest resistivity of 5.76 × 10⁻⁴ Ω cm, high average visible transmittance (400–800 nm) of 92%, and the best thermal stability. Comparing with the AZO thin films deposited at low substrate temperatures, the AZO thin films deposited at 350 °C had the highest compact surface morphology which could hinder the chemisorbed and diffused oxygen. This was considered to be the main mechanism which was responsible for the thermal degradation of AZO thin films.     

Fabrication and ferroelectric properties of sol–gel derived 1–1 intergrowth-superlattice-structured Bi<Subscript>3</Subscript>TiNbO<Subscript>9</Subscript>-Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films

1–1 intergrowth-superlattice-structured Bi₃TiNbO₉–Bi₄Ti₃O₁₂ (BTN–BIT) ferroelectric thin films have been prepared on p-Si substrates by sol-gel processing. The precursor films are crystallized in the desired intergrown BTN–BIT superlattice structures by optimizing the processing conditions. Synthesized BTN–BIT thin films annealed below 750 °C are polycrystalline, uniform and crack-free, no pyrochlore phase or other second phase, and exhibited good ferroelectric properties. As the annealing temperature increases from 600 to 700 °C, both remanent polarization P _r and coercive electric field E _c of BTN–BIT thin films increase, but the pyrochlore phase in BTN–BIT films annealed above 750 °C will impair the ferroelectric properties. The BTN–BIT thin films annealed at 700 °C have a P _r value ~19.1μC/cm² and an E _c value ~135 kV/cm.     

Nanocrystalline TiO2 thin films for NH3 monitoring: microstructural and physical characterization

Nanocrystalline titanium oxide thin films have been deposited by spin coating technique and then have been analyzed to test their application in NH₃ gas-sensing technology. In particular, spectrophotometric and conductivity measurements have been performed in order to determine the optical and electrical properties of titanium oxide thin films. The structure and the morphology of such material have been investigated by X ray diffraction, Scanning microscopy, high resolution electron microscopy and selected area electron diffraction. The X-ray diffraction measurements confirmed that the films grown by this technique have good crystalline tetragonal mixed anatase and rutile phase structure. The HRTEM image of TiO₂ thin film showed grains of about 50–60 nm in size with aggregation of 10–15 nm crystallites. Selected area electron diffraction pattern shows that the TiO₂ films exhibited tetragonal structure. The surface morphology (SEM) of the TiO₂ film showed that the nanoparticles are fine with an average grain size of about 50–60 nm. The optical band gap of TiO₂ film is 3.26 eV. Gas sensing properties showed that TiO₂ films were sensitive as well as fast in responding to NH₃. A high sensitivity for ammonia indicates that the TiO₂ films are selective for this gas.     

Effect of microstructural evolution on magnetic properties of Ni thin films

The magnetic properties of Ni thin films, in the range 20–500 nm, at the crystalline-nanocrystalline interface are reported. The effect of thickness, substrate and substrate temperature has been studied. For the films deposited at ambient temperatures on borosilicate glass substrates, the crystallite size, coercive field and magnetization energy density first increase and achieve a maximum at a critical value of thickness and decrease thereafter. At a thickness of 50 nm, the films deposited at ambient temperature onto borosilicate glass, MgO and silicon do not exhibit long-range order but are magnetic as is evident from the non-zero coercive field and magnetization energy. Phase contrast microscopy revealed that the grain sizes increase from a value of 30–50 nm at ambient temperature to 120–150 nm at 503 K and remain approximately constant in this range up to 593 K. The existence of grain boundary walls of width 30–50 nm is demonstrated using phase contrast images. The grain boundary area also stagnates at higher substrate temperature. There is pronounced shape anisotropy as evidenced by the increased aspect ratio of the grains as a function of substrate temperature. Nickel thin films of 50 nm show the absence of long-range crystalline order at ambient temperature growth conditions and a preferred [111] orientation at higher substrate temperatures. Thin films are found to be thermally relaxed at elevated deposition temperature and having large compressive strain at ambient temperature. This transition from nanocrystalline to crystalline order causes a peak in the coercive field in the region of transition as a function of thickness and substrate temperature. The saturation magnetization on the other hand increases with increase in substrate temperature.     

Conversion of copper and manganese metallic films to spinel coating

Oxidation of copper + manganese metallic thin films on UNS 430 stainless steel was studied at temperatures of 600–950 °C. The Cu–Mn metallic films were converted to Cu–Mn spinel coating in the temperature range of 600–950 °C as confirmed by X-ray diffraction. Conversion mechanisms of metals to the spinel were investigated. Examination by SEM showed that negligible oxidation of the substrate alloy occurred in the coated samples at temperatures up to 750 °C; a transition layer formed between the substrate and spinel coating at higher temperatures. Cu–Mn spinel coating can provide protection to the metallic substrate at temperatures up to 850 °C. Formation of the spinel coating was due to reactions of CuO, which formed through outward diffusion of copper, with manganese oxides, which formed through inward diffusion of oxygen.