Characterization on pulsed laser deposited nanocrystalline ZnO thin films

Nanocrystalline zinc oxide thin films were deposited on glass and silicon substrates by using pulsed laser deposition at different laser energy densities (1.5, 2, and 3 J/cm²). The film thickness, surface roughness, composition, optical and structural properties of the deposited films were studied using an α-step surface profilometer, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), optical transmittance, and X-ray diffraction (XRD), respectively. The film thickness was calculated as 244 nm. AFM analysis shows that the root-mean-square roughness increases with increasing laser energy density. XPS analysis shows that the interaction of zinc with oxygen atoms is greatly increased at high laser energy density. In the optical transmittance spectra, a shift of the absorption edge towards higher wavelength region confirms that the optical band gap increases with an increase in laser energy density. The particle size of the deposited films was measured by XRD, it is found to be in the range from 7.87 to 11.81 nm. It reveals that the particle size increases with an increase in laser energy density.     

Surface morphology of AlN films synthesized by pulsed laser deposition

Surface morphology of AlN films, synthesized on Si substrates by pulsed laser deposition, has been examined by recording atomic-force-microscopy (AFM) images. The influence of N₂ ambient pressure, ranging from 5 × 10⁻⁴ Pa to 10 Pa, is reflected well in the alteration of the surface roughness and size of crystallites of the AlN films. A tendency of a decrease in the surface roughness with increasing N₂ pressure was observed, which also correlates with the polycrystalline structure of the films. Deposition in vacuum resulted in the highest surface roughness due to the large size of crystallites emerging from the surface, while increasing the nitrogen pressure yielded smaller crystallites and a smoother film surface. The presented results could be useful for applications of pulsed laser deposited AlN in different optical and acoustic devices, where the crystalline quality of the AlN films and the surface is very important.     

The properties of transparent semiconductor Zn1 − xTixO thin films prepared by the sol-gel method

Transparent semiconductor thin films of Zn_1 − xTi_xO (0 ≦ x ≦ 0.12) were deposited on alkali-free glass substrates by the sol-gel method. The effects of Ti addition on the crystallization, microstructure, optical properties and resistivity of ZnO thin films were investigated. The as-coated films were preheated at 300 °C, and then annealed at 500 °C in air ambiance. X-ray diffraction results showed all polycrystalline Zn_1 − xTi_xO thin films with preferred orientation along the (002) plane. Ti incorporated within the ZnO thin films not only decreased surface roughness but also increased optical transmittance and electrical resistivity. In the present study, the Zn_0.88Ti_0.12O film exhibited the best properties, namely an average transmittance of 91.0% (an increase of ~ 12% over the pure ZnO film) and an RMS roughness value of 1.04 nm.     

Synthesis of aluminum nitride thin films by filtered arc ion plating deposition

Thin films of aluminum nitride (AlN) were deposited on stainless steel and glass substrates by a modified deposition technique, filtered arc ion plating, at an enhanced deposition rate. X-ray diffraction spectra confirmed the exclusive presence of AlN hexagonal wurtzite phase. Under a mixed gas (Ar + N₂) pressure of 0.90 Pa and a bias voltage of − 400 V, the deposited films exhibited a fairly low surface roughness of 2.23 nm. The thin films were proved higher than 75% transparent in the visible spectral region. The bonding strength between the film and substrate was verified higher than 20 N. Thus high performance of such AlN thin films can be expected in applications.     

The role of the Zn buffer layers in the structural and photoluminescence properties of ZnO films on Zn buffer layers deposited by RF magnetron sputtering

Highly c-axis oriented ZnO thin films were grown on Si (100) substrates with Zn buffer layers. Effects of the Zn buffer layer thickness on the structural and optical qualities of ZnO thin films were investigated for the ZnO films with the buffer layers 90, 110, and 130 nm thick using X-ray diffraction (XRD), photoluminescence (PL) and atomic force microscopy (AFM) analysis techniques. It was confirmed that the quality of a ZnO thin film deposited by RF magnetron sputtering was substantially improved by using a Zn buffer layer. The highest ZnO film quality was obtained with a Zn buffer layer 110 nm thick. The surface roughness of the ZnO thin film increases as the Zn buffer layer thickness increases.     

High roughness Ag back reflector on a metal underlayer for thin film solar cell applications

The roughness development of Ag film was investigated for potential as a back reflector material in thin film solar cells on flexible stainless steel (STS) substrates. The influence of metal underlayers was evaluated in order to obtain a rough Ag film at a low deposition temperature (≤400 °C). By depositing Ag on a 100 nm Al underlayer to induce Ag–Al alloying, the film roughness was increased three times more than that of Ag films on bare STS at 400 °C. The Ag film deposited on an Al underlayer at 350 °C exhibited 75 nm roughness and uniformly distributed crystallites, which was effective for visible light scattering. The Ag–Al alloy phase was also controlled using the thickness ratio of Ag and Al. The present work clearly demonstrated that an Ag back reflector film with a higher roughness could be fabricated through inserting a metal underlayer at a deposition temperature much lower than the 500 °C that has been reported in earlier works.     

Effect of annealing temperature on growth of Ce-ZnO nanocomposite thin films: X-ray photoelectron spectroscopy study

Ce-doped ZnO nanocomposite thin films with Ce/Zn ratio fixed at optimum value (10 at.%) have been prepared via sol-gel method at different annealing temperatures varied from 180 to 500 °C. The synthesized samples were characterized employing atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) techniques. According to AFM analysis, the average grain size increased from about 70 nm to 150 nm by increasing the annealing temperature from 300 to 500 °C. Moreover, based on the XPS data analysis, it was found that three major metal ions namely Ce³⁺, Ce⁴⁺, and Zn²⁺ coexist on the surface of the nanocomposite films. XPS data analysis also revealed that Ce³⁺ ion is oxidized to Ce⁴⁺ ion with increasing annealing temperature. Due to oxidation, the ratio of [Ce^3±]/[Ce total] changed from 68.8 to 38.1% by increasing the annealing temperature from 180 to 500 °C. In addition, the Ce/Zn ratio increased from 0.21 to 0.42 when increasing the annealing temperature from 180 to 500 °C indicating migration of Ce ions toward the surface at higher temperatures. Finally, the XRD measurements determined that the ZnO thin films have a hexagonal wurtzite structure and CeO₂ crystallites are formed at 500 °C in the Ce-doped ZnO nanocomposite thin films.     

Morphology and growth of e-beam deposited YSZ thin films

Yttria-stabilized zirconium (YSZ) thin films were grown from the tetragonal phase of ZrO₂ stabilized by 8 wt% of Y₂O₃ (8% of YSZ) ceramic powders using e-beam deposition technique (EB-PVD). The influence of the type of substrate on the microstructure of deposited YSZ thin films was analysed. YSZ thin films (2-3 μm of thickness) were deposited on three different types of substrates: optical quartz (SiO₂), porous Ni-YSZ substrates and Alloy 600 (Fe-Ni-Cr). The dependence of the substrate temperature (from 20 to 600 °C) on the thin film structure and the surface morphology were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). It was found that (i) the substrate temperature has an influence on the crystallite size, which varied between 12 and 50 nm, (ii) the substrate type has an influence on the growth mechanism of YSZ thin films, and (iii) a bias voltage applied to the substrate during the deposition of thin films has an influence on the densification of YSZ layers.     

Poly-silicon thin films by aluminium induced crystallisation of microcrystalline silicon

Al-induced crystallisation of microcrystalline Si thin films prepared by electron cyclotron resonance plasma-enhanced chemical vapour deposition (ECR-PECVD) on glass and SiO₂ coated Si wafers has been studied. The starting structure was substrate/μc-Si/Al. Annealing this structure in the temperature range 370-520 °C, immediately following deposition of the Al layer, resulted in successful layer exchange and the formation of a substrate/Al+Si layer/poly-Si geometry. The top poly-Si layer exhibited grain sizes generally in the range ∼2-6 μm, although larger grains were also sparsely present. The films did not exhibit any appreciable degree of preferred orientation. The surface roughness was relatively high with a R_a value of ∼20 nm.     

Preparation of anatase TiO2 thin films for dye-sensitized solar cells by DC reactive magnetron sputtering technique

Anatase titanium dioxide (TiO₂) thin films are prepared by DC reactive magnetron sputtering using Ti target as the source material. In this work argon and oxygen are used as sputtering and reactive gas respectively. DC power is used at 100 W per 1 h. The distance between the target and substrate is fixed at 4 cm. The glass substrate temperature value varies from room temperature to 400 °C. The crystalline structure of the films is determined by X-ray diffraction analysis. All the films deposited at temperatures lower than 300 °C were amorphous, whereas films obtained at higher temperature grew in crystalline anatase phase. Phase transition from amorphous to anatase is observed at 400 °C annealing temperature. Transmittances of the TiO₂ thin films were measured using UV-visible NIR spectrophotometer. The direct and indirect optical band gap for room temperature and substrate temperature at 400 °C is found to be 3.50, 3.41 eV and 3.50, 3.54 eV respectively. The transmittance of TiO₂ thin films is noted higher than 75%. A comparison among all the films obtained at room temperature showed a transmittance value higher for films obtained at substrate temperature of 400 °C. The morphology of the films and the identification of the surface chemical stoichiometry of the deposited film at 400 °C were studied respectively, scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The surface roughness and the grain size are measured using AFM.     

Transparent conductive titanium-doped indium oxide films prepared by a magnetic null discharge sputter source

Titanium-doped indium oxide (ITiO) films were prepared on soda-lime glass substrate using a magnetic null discharge (MND) sputter source. The ITiO thin films containing 10 wt.% Ti showed the minimum resistivity of ρ = 5.5 × 10⁻³ Ω cm. The optical transmittance increases from 70% at 450 nm to 80% at 700 nm in visible spectrum. Photoelectron peaks for In 3d, Ti 2p, O 1s and C 1s were detected for the ITiO film in the binding energy range of 0-1100 eV. The surface roughness of the sample showed a change from 10 nm to 50 nm. The ITiO film used for TCO layer of DSCs exhibited an energy conversion efficiency of about 3.8% at light intensity of 100 mW/cm².     

Influence of high temperature processing of sol-gel derived barium titanate thin films deposited on platinum and strontium ruthenate coated silicon wafers

Thin films of barium titanate (BTO) of 200 nm thickness, derived from an alkoxide-carboxylate sol-gel process, were deposited on Pt/Ti and SrRuO₃/ZrO₂-8%Y₂O₃ coated Si wafers. Films with a dense columnar microstructure were obtained by repeated deposition of thin amorphous layers from low-concentrated sols, and crystallization at 800 °C. This method added 10 nm thickness to the crystalline BTO film in each deposition step. The harsh processing conditions had a negative impact on the platinized silicon wafers, where Pt-Si silicides were formed. This led to diffusion of Si into BTO and interfacial silicate formation. The interfacial silicate layer was the cause of deteriorated dielectric and ferroelectric properties of the BTO layer. Use of SrRuO₃/ZrO₂-8%Y₂O₃/Si substrates solved the problem. No diffusion of Si was observed, and BTO films with good dielectric and ferroelectric properties were obtained.     

Direct ion beam deposited carbon films and clusters

Carbon films and clusters have been formed by direct ion beam deposition. In all experiments crystalline n-Si 〈1 0 0〉 wafers with the 300 nm thermal SiO₂ film have been used as substrates. Effects of thermally microstructured Ni and substrate temperature were studied. Chemical structure of the carbon films was investigated using Raman spectroscopy. Surface morphology was studied by atomic force microscopy (AFM). Supplemental research on sheet resistance of the films has been performed. Rough diamond-like carbon film was grown onto the catalytic layer at 400 K temperature, and surface of the diamond-like carbon film deposited directly onto the SiO₂ layer at 400 K temperature was very smooth. At 750 K growth of the array of cylindrically shaped clusters was observed by AFM in the case of catalytically assisted deposition. Raman spectra of deposited films were typical for glassy carbon and/or carbon nanotubes with the carbonaceous deposits. Catalyticless deposition at 750 K temperature resulted in the formation of the conductive polymer-like carbon film with the graphite clusters in it.     

Influence of annealing on the structure and stoichiometry of europium-doped titanium dioxide thin films

This work presents the influence of annealing on the structure and stoichiometry of europium (Eu)-doped titanium dioxide (TiO₂). Thin films were fabricated by magnetron sputtering from a metallic Ti-Eu target in oxygen atmosphere and deposited on silicon and SiO₂ substrates. After deposition the selected samples were additionally annealed in air up to 1070 K.Film properties were examined by means of X-ray diffraction (XRD), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) and the results were analyzed together with the undoped TiO₂ thin films prepared under similar technological conditions.XRD results showed that depending on the Eu content, as-deposited thin films consisted of the TiO₂-anatase or TiO₂-rutile.An additional annealing will result in the growth of anatase crystals up to 35 nm, but anatase to rutile phase transformation has not been recorded. AFM images display high quality and a dense nanocrystalline structure. From the XPS Ti2p spectra the 4+oxidation state of Ti was confirmed. The O1s XPS spectra displayed the presence of an O²⁻ photoelectron peak accompanied by an additional broader peak that originates from hydroxyl species chemisorbed at the sample surface. It has been found that Eu dopant increases the OH⁻ content on the surface of prepared TiO₂:Eu thin films. The calculated O/Ti ratio was in the range of 1.85-2.04 depending on the sample.     

Biomimetic formation of titania thin films: effect of amino acids on the deposition process

Different types of amino acids have been used as additives to control the aqueous deposition of titanium dioxide thin films on single-crystal Si wafers. Thin titania films can be obtained through a chemical bath deposition (CBD) process using TiCl? as a precursor in an aqueous solution at temperatures below 100 °C. The addition of amino acids to the deposition solution was shown to reduce the thickness and roughness of the films and to increase their density. These protein building blocks were employed to modify the deposition rate as well as the size of aggregates that form the film. The thickness, crystallinity, morphology and composition of the grown films were characterized by a variety of techniques, including XRD, XPS, AFM and SEM. The consequences of the type of the amino acid additive (and its concentration in the solution) on the microstructural evolutions of the deposed films are thus revealed and discussed on the basis of the organic-inorganic interactions in solution and at the film surface.     

Deposition and structural properties of RF magnetron-sputtered ZnO thin films on Pt/Ti/SiNx/Si substrate for FBAR device

This work investigates high-quality bottom electrode and piezoelectric film used in a thin-film bulk acoustic resonator (TFBAR) device. The titanium (Ti) seeding layer and platinum (Pt) bottom electrode were deposited on silicon substrates by DC sputtering using a dual-gun system. Zinc oxide (ZnO) was then deposited onto the Pt bottom electrode by RF magnetron sputtering. Field-emission scanning electron microscopy (SEM), atom force microscopy (AFM) and the four-point probe method showed that the Pt bottom electrode deposited on the Ti seeding layer exhibited favorable characteristics, such as a crystallite size of less than 10 nm, a surface roughness of 0.69 nm and a sheet resistance of 2.27 Ω/□. The ZnO thin film with a highly c-axis-preferred orientation (FWHM = 0.28°) and a roughness of 6.22 nm was investigated by X-ray diffraction (XRD) and AFM analysis, respectively. The bottom electrode with a low resistance and the highly crystalline ZnO thin film will contribute significantly to the favorable characteristics of the FBAR devices.     

Synthesis of epitaxial BaZrO3 thin films by chemical solution deposition

This work reports on the low temperature preparation and characterization of BaZrO₃ (BZO) epitaxial thin films by chemical solution deposition (CSD). The X-ray θ-2θ scan and φ-scan measurements have demonstrated that the BZO films exhibit cube-on-cube epitaxy on (100) MgO substrates, with the full width at half maximum (FWHM) for the ω-scan and φ-scan of 0.35° and 0.46°, respectively. The SEM and AFM analyses revealed that the morphology of the films is strongly correlated with annealing temperature. The root mean square roughness for the film annealed at 600 °C is 3.63 nm, while for the film grown at 1000 °C is 5.25 nm.     

Synthesis of thermally evaporated ZnSe thin film at room temperature

Zinc selenide (ZnSe) thin film on glass substrates were prepared by thermal evaporation under high vacuum using the quasi-closed volume technique at room temperature (300 ± 2 K). The deposited ZnSe properties were assessed via X-ray diffraction, atomic force microscope (AFM), UV-Vis specrophotometry, Raman spectroscopy, photo-luminescence, Fourier transform infrared spectroscopy (FT-IR) and spectroscopic ellipsometry. The X-ray diffraction patterns of the film exhibited reflection corresponding to the cubic (111) phase (2θ = 27.20°). This analysis indicated that the sample is polycrystalline and have cubic (Zinc blende) structure. The crystallites were preferentially oriented with the (111) planes parallel to the substrates. The AFM images showed that the ZnSe films have smooth morphology with roughness 6.74 nm. The transmittance spectrum revealed a high transmission of 89% in the infrared region (≥ 600 nm) and a low transmission of 40% at 450 nm. The maximum transmission of 89.6% was observed at 640 nm. Optical band-gap was calculated from the transmission data of specrophotometry, photo-luminescence and ellipsometry and was 2.76, 2.74 and 2.82 eV respectively. Raman spectroscopic studies revealed two longitudinal optical phonon modes at 252 cm ^-1 and 500 cm ^-1. In photoluminescence study, the luminescence peaks was observed at 452 nm corresponding to band to band emission. FT-IR study illustrated the existence of Zn-Se bonding in ZnSe thin film. The optical constants were calculated using spectroscopic ellipsometry and were determined from the best fit ellipsometric data in the wavelength regime of interest from 370-1000 nm. These results manifested excellent room temperature ZnSe synthesis and characteristics for opto-electronics technologies.     

Characteristics and mechanical properties of titanium-containing diamond like carbon films deposited by cathodic arc evaporation

Depositions of titanium-containing diamond-like carbon (Ti-DLC) films were conducted by mixing C+ and Ti+ plasma streams originated from cathodic arc plasma sources in argon (Ar). The deposition was processed at Ti target current ranging from 20 Amp to 70 Amp. Film characteristics were investigated using Raman spectroscopy, X-ray photoelectron spectroscopy (XPS). Film microstructures were evaluated using field emission scanning electron microscopy (FEGSEM), an atomic force microscope (AFM), X-ray diffractometry (XRD) and high-resolution transmission electron microscopy (HRTEM). Mechanical properties were investigated by using a nanoindentation tester and ball on disc wear test. Results shows that surface roughness (Ra) of the films ranged between 2.4 and 7.2 nm and roughness increased relative to the increase in Ti target current. The FESEM studies showed that the surface micrographs of Ti-DLC films revealed a cauliflower-like microstructure and the cross-sectional micrograph revealed a snake-skin like structure. HRTEM studies showed that the Ti-DLC films consisted of nano scale TiC particles which were comparable with low angle XRD and XPS results. XPS analysis established that the Ti2p spectrum is present when the Ti target current reaches 30 Amp or higher. Ti concentration increased as the Ti target current was increased. An extremely thin TiO2 layer exists on the top of the Ti-DLC films which was comparable with the AES results. The film thickness which could be deposited for Ti-DLC is much higher than that of conventional DLC films. Nanoindentation tests show that the nanohardness of the films ranging 15-22 GPa, with Er values ranging from 145 to 175 GPa. The wear test demonstrates the friction coefficient of the 420SS substrate, DLC and Ti-DLC films were about 0.8, 0.3 and 0.2, respectively. Obviously, the friction coefficients of the Ti-DLC films were lower than that of the DLC films.     

Influence of 150 MeV Ni swift heavy ion irradiation on CuFe2O4 thin films prepared by radio frequency magnetron sputtering: Modification on structure and surface morphology

The bulk copper ferrite nanomaterials are synthesized by co-precipitation technique. The vibrating sample magnetometer measurement for bulk CuFe₂O₄ reveals its unsaturated superparamagnetic behavior. The crystallites of the synthesized nanomaterial are in cubic form having an average size of ~ 100 Å and are used as target to prepare thin films of various thicknesses (600, 900 and 1100 nm) by radio frequency magnetron sputtering technique. X-ray peaks arise only when films are annealed at 1200 °C and also they are found to be in tetragonal structure. The magnetic characteristics of 900 nm unirradiated CuFe₂O₄ thin film exhibit superparamagnetic behavior and have an unsaturated magnetic moment at high field. Magnetic force microscopy images of unirradiated CuFe₂O₄ thin films confirm the soft nature of the magnetic materials. The 150 MeV Ni¹¹⁺ swift heavy ion irradiation on these thin films at the fluence of 1 × 10¹⁴ ions/cm² modifies the polycrystalline nature due to electron-phonon coupling. Atomic force microscopy image shows that the swift heavy ion irradiation induces agglomeration of particles in 600 and 900 nm thin films and increases rms surface roughness from 33.43 to 39.65 and 69.7 to 102.46 nm respectively. However, in 1100 nm film, holes are created and channel-like structures are observed along with a decrease in the rms surface roughness from 75.12 to 24.46 nm. Magnetic force microscopy images of 900 nm irradiated thin film explain the formation of domains on irradiation and are also supported by the ferromagnetic hysteresis observed using vibrating sample magnetometer.