Flame spray deposition of nanocrystalline dense Ce0.8Gd0.2O2 − δ thin films: Deposition mechanism and microstructural characterization

Nanocrystalline dense sub-micron thin films of Ce_0.8Gd_0.2O_2 − δ have been successfully deposited by flame spray deposition. The deposition mechanism has been identified as droplet deposition. The deposition temperature of the substrate was as low as 200 °C and the deposition rate ∼ 30 nm/min. Under these conditions the droplets have a very limited residence time in the hot zone of the flame and are deposited as liquid, forming smooth films free of particles. They exhibited a dense and crack-free microstructure. Grain growth, lattice constant, crystallographic density and surface roughness have been investigated as a function of annealing temperature. The good quality of the films, in association with the high deposition rates at low deposition temperatures shows the preeminence of the flame spray method for depositing thin films for micro-solid oxide fuel cells.     

ZrO2-based thin films synthesized by electrostatic spray deposition: Effect of post-deposition thermal treatments

Cubic and tetragonal Y₂O₃-doped ZrO₂ thin films were deposited with a dense surface morphology by electrostatic spray deposition. Four dependent process parameters – substrate temperature, precursor solution flow rate, nozzle to substrate distance and the deposition time – have been used to control the process. Temperature dependent Raman spectroscopy and X-ray diffraction were performed in order to investigate the crystallization behavior and structural properties.     

Structural,optical and electrical properties of tin oxide thin films by electrostatic spray deposition

Tin oxide (SnO₂) thin films were deposited by electrostatic spray deposition (ESD). The structural, optical and electrical properties of the films for different solvents were studied. The morphology of the deposited thin films was investigated by scanning electron microscopy. The optical transmission spectra of the films showed 66–75% transmittance in the visible region of spectrum. The electrical resistivity of thin films deposited using the different solvents ranged 1.08 × 10^?3–1.34 × 10^?3 Ω-cm. Overall, EG and PG were good solvents for depositing SnO₂ thin films by the ESD technique with stable cone jet.     

Preparation and characterization of alkyl sulfate and alkylbenzene sulfonate surfactants/TiO2 hybrid thin films by the liquid phase deposition (LPD) method

Hybrid titanium oxide thin films containing surfactants, sodium dodecyl benzylsulfonate and sodium dodecyl sulfate, have been prepared by a novel liquid-phase deposition method. It is a new attempt to prepare organic–inorganic hybrid thin film by this method which usually be applied in preparing metal oxide thin film before. The two kinds of surfactants/TiO₂ hybrid thin films were characterized by means of FT-IR, SEM, XRD, fluorescence X-ray, ICP–AES and Raman spectroscopy, and showed noticeable differences in surface top view and particle diameter, cross-section image and thickness, deposited amount of Ti, XRD patterns and Raman shift. The reasons giving rise to above differences of the two kinds composite thin films has been discussed. The deposition mechanism of organic–inorganic hybrid thin film has been also presumed. The use of this processing parameter may open up a new way to the preparing of the organic–inorganic hybrid thin film.     

Electrospray of fine droplets of ceramic suspensions for thin-film preparation

An electrostatic atomization technique has been developed to generate ultra-fine spray of ZrO₂ and SiC ceramic suspensions in a range of 4–5 μm with a narrow size distribution (1–9 μm). The aim of this work is to generate fine spray of ceramic suspensions for the preparation of uniform thin films of these ceramic materials on substrates. Thin-film formation using electrostatic atomization process allows one to tightly control the process while meeting the economics in comparison with some other competing process technologies such as chemical vapour deposition, physical vapour deposition and plasma spray, etc. Preliminary results have shown that for low through put atomization, the cone-jet is the most suitable method to produce a fine charged aerosol with a narrow size distribution. It was found that the droplet size of the spray is in the range of a few micrometers with a narrow size distribution and that droplet size and spray current obey theoretical prediction of scaling law. As prepared ZrO₂ and SiC thin films were observed to be homogenous with a particle size of less than 10 μm.     

Investigations of the hydrophobic and scratch resistance behavior of polystyrene films deposited on bell metal using RF-PACVD process

Polystyrene films are deposited on bell metal substrates using radiofrequency plasma assisted chemical vapor deposition (RF-PACVD) process. The deposition of polystyrene film is carried out at working pressure of 1.6 × 10⁻¹ mbar and in the RF power range of 20-110 W. The hydrophobic and mechanical behaviors of the polystyrene films are studied as a function of RF power. The chemical compositions and surface chemistry of the polystyrene films are investigated using Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It is revealed that enhanced cross-linked chemical structure and higher loss of oxygen by peroxy polystyryl radical with increasing RF power results in the formation of polystyrene films with more hydrophobic and scratch resistance behavior. However, extensive destruction of cross-linked chemical structure due to high energetic ion bombardment tends to decrease the hydrophobic and scratch resistance behavior of the polystyrene film deposited at RF power of 110 W. Atomic force microscopy (AFM) images show quite uniform and crack free surfaces of the polystyrene films having rms roughness in the range of 0.35-0.87 nm. Attempts are made to correlate the characterization results with the parameters that are used for thin film depositions.     

A study of structural, compositional and optical properties of spray-deposited non-stoichiometric (Zn,Fe)S thin films

Non-stoichiometric ternary chalcogenides (Zn,Fe)S were prepared in the film form by pyrolytic spray deposition technique, using air/nitrogen as the carrier gas. The precursor solution comprised of ZnCl₂, FeCl₂ and thiourea. The depositions were carried out under optimum conditions of experimental parameters viz. carrier gas (air/nitrogen) flow rate, concentration of precursor constituents, nozzle substrate distance and temperature of quartz substrate. The deposited thin films were later sintered in argon at 1073 K for 120 min.The structural, compositional and optical properties of the sintered thin films were studied. X-ray diffraction studies of the thin films indicated the presence of (Zn,Fe)S solid solution with prominent cubic sphalerite phase while surface morphology as determined by scanning electron microscopy (SEM) revealed a granular structure.The chemical composition of the resulting thin films as analyzed by energy dispersive X-ray analysis (EDAX) reflected the composition of the precursor solutions from which the depositions were carried out with Fe at% values ranging from 0.4 up to 33.SEM micrographs of thin films reveal that the grain sizes of the thin films prepared using air as carrier gas and N₂ as carrier gas are in the vicinity of 300 and 150 nm, respectively.The diffuse transmittance measurements for thin films, as a function of wavelength reveal the dependence of direct optical band gap on Fe content and type of phase.     

Electrostatic spray deposited zinc oxide films for gas sensor applications

In this work, thin films of zinc oxide (ZnO) for gas-sensor applications were deposited on platinum coated alumina substrate, using electrostatic spray deposition (ESD) technique. As precursor solution zinc acetate in ethanol was used. Scanning electron microscopy (SEM) evaluation showed a porous and homogeneous film morphology and the energy dispersive X-ray analysis (EDX) confirmed the composition of the films with no presence of other impurities. The microstructure studied with X-ray diffraction (XRD) and Raman spectroscopy indicated that the ZnO oxide films are crystallized in a hexagonal wurtzite phase. The films showed good sensitivity to 1 ppm nitrogen dioxide (NO₂) at 300 °C while a much lower sensitivity to 12 ppm hydrogen sulphide (H₂S).     

Electrostatic spray deposition of Gd0.1Ce0.9O1.95 and La0.9Sr0.1Ga0.8Mg0.2O2.87 thin films

The deposition of gadolinia-doped ceria (CGO, Gd_0.1Ce_0.9O_1.95) and LaGaO₃-based perovskite oxides (LSGM, La_0.9Sr_0.1Ga_0.8Mg_0.2O_2.87) thin films on a stainless steel substrate was studied using the electrostatic spray deposition (EDS) technique. The effect of process conditions, such as deposition temperature, deposition time and liquid flow rate, on the surface morphology and microstructure of thin films was examined with scanning electron microscopy (SEM) and powder X-ray diffraction (XRD). The deposited CGO films with a highly porous and three-dimensional interconnected structure were obtained at a liquid flow rate of 0.5 ml/h, a deposition temperature of 503 K and a deposition time ranging from 0.5 to 1 h. On the other hand, the deposited LSGM thin films with porous microstructure were also obtained at the deposition time of 1 h, the deposition temperature of 533 K and the liquid flow rate of 0.5 ml/h. The deposited CGO and LSGM thin films were amorphous at the used deposition temperature. Subsequently, the samples were annealed at 1173 K for 2 h and the desired crystal structures were obtained. The chemical analysis of the thin films was investigated by energy dispersive X-ray (EDX) analysis. The observed chemical compositions of the samples were in a fair agreement with those of the starting solutions.     

Study on SiN and SiCN film production using PE-ALD process with high-density multi-ICP source at low temperature

SiN and SiCN film production using plasma-enhanced atomic layer deposition (PE-ALD) is investigated in this study. A developed high-power and high-density multiple inductively coupled plasma (multi-ICP) source is used for a low temperature PE-ALD process. High plasma density and good uniformity are obtained by high power N₂ plasma discharge. Silicon nitride films are deposited on a 300-mm wafer using the PE-ALD method at low temperature. To analyze the quality of the SiN and SiCN films, the wet etch rate, refractive index, and growth rate of the thin films are measured. Experiments are performed by changing the applied power and the process temperature (300–500 °C).     

Optimization of spray parameters in the fabrication of SnO2 layers using electrostatic assisted deposition technique

Tin oxide (SnO₂) thin films for gas sensing applications were prepared using electrostatic spray deposition method under optimum deposition conditions. It is shown in the paper that desired film morphology can be obtained by controlling different spray parameters (liquid properties, applied voltage, nozzle-substrate distance and substrate temperature). The spray parameters were optimized with respect to droplet diameter and applied voltage. An empirical relationship between critical voltage and different spray parameters was established for optimization. The morphology of the films prepared using these optimized spray parameters were investigated using X-Ray Diffraction (XRD) and Scanning Electron Microscope (SEM).     

高活性氧化亚铜薄膜材料的绿色合成研究

本文采用一步脉冲雾化化学气相沉积法在250℃下制备了氧化亚铜薄膜催化剂.实验研究了前驱体中掺杂水对氧化铜薄膜表面形貌、拓扑结构、表面成分和光学特性的影响规律.结果表明所制得的催化剂为纯相的氧化亚铜.前驱体溶液中掺杂水会导致氧化亚铜的晶粒变小,从而使得共光学能隙从2.16 eV降至2.04 eV.原子力显微镜结果表明随着水的加入,氧化亚铜的表面粗糙度降低,表面更加均匀.此外,利用密度泛函理论计算得到了水和乙醇在氧化亚铜薄膜表面的吸附和反应特性,并提出了氧化亚铜的形成机理.本文开发了一种低成本且实际可行的薄膜制造方法,该方法在太阳能电池和半导体等领域具有潜在应用.     

Chemical bath deposition of hausmannite Mn3O4 thin films

A low-temperature chemical bath deposition (CBD) technique has been used for the preparation of Mn₃O₄ thin films onto glass substrates. The kinetic behavior and the formation mechanism of the solid thin films from the aqueous solution have been investigated. Structure (X-ray diffraction and Raman), morphological (atom force microscope), and optical (UV-vis-NIR) characterizations of the deposited films are presented. The results indicated that the deposited Mn₃O₄ thin films of smooth surface with nanosized grains were well crystalline and the optical bandgap of the film was estimated to be 2.54 eV.     

Fast electrochromic response of porous-structured cobalt oxide (Co<Subscript>3</Subscript>O<Subscript>4</Subscript>) thin films by novel nebulizer spray pyrolysis technique

Electrochromic effect of cobalt oxide thin films was studied as a function of substrate temperature (573–673 K). Tricobalt tetraoxide (Co₃O₄) thin films were deposited on glass and fluorine-doped tin oxide (FTO) substrates by nebulized spray technique using cobalt nitrate as precursor material. The XRD patterns indicated (311) plane was dominant for all the films irrespective of the deposition temperature. Williamson-Hall (W-H) analysis was made to understand the strain variation in the prepared Co₃O₄ films under different deposition temperature by employing uniform deformation model (UDM). Scanning electron microscopy images revealed porous morphology for the film prepared at 623 K. The optical parameters such as refractive index (n), extinction coefficient (k), and band gap were derived from UV-visible spectra of Co₃O₄ films. The electrochromic performance of the deposited Co₃O₄ films was analyzed through cyclic voltammetry, chronocoulometry, chronoamperometry, and iono-optical studies.     

Liquids microprinting through a novel film-free femtosecond laser based technique

Laser-induced forward transfer (LIFT) is a high resolution microprinting technique in which small amounts of material are transferred from a previously prepared donor thin film to a receptor substrate. The application of LIFT to liquid donor films allows depositing complex and fragile materials in solution or suspension without compromising the integrity of the deposited material. However, the main drawback of LIFT is the preparation of the donor material in thin film form, being difficult to obtain reproducible thin films with thickness uniformity and good stability.In this work we present a laser microprinting technique that is able to overcome the drawbacks associated with the preparation of the liquid film, allowing the deposition of well-defined uniform microdroplets with high reproducibility and resolution. The droplet transfer mechanism relies on the highly localized absorption of strongly focused femtosecond laser pulses underneath the free surface of the liquid contained in a reservoir.An analysis of the influence of laser pulse energy on the morphology of the printed droplets is carried out, revealing a clear correlation between the printed droplet dimensions and the laser pulse energy. Such correlation is interpreted in terms of the dynamics of the liquid displaced by a laser-generated cavitation bubble close to the free surface of the liquid. Finally, the feasibility of the technique for the production of miniaturized biosensors is tested.     

Bioactive glass and hydroxyapatite thin films obtained by pulsed laser deposition

Bioactive glass (BG), calcium hydroxyapatite (HA), and ZrO₂ doped HA thin films were grown by pulsed laser deposition on Ti substrates. An UV KrF^* (λ = 248 nm, τ ≥ 7 ns) excimer laser was used for the multi-pulse irradiation of the targets. The substrates were kept at room temperature or heated during the film deposition at values within the (400-550 °C) range. The depositions were performed in oxygen and water vapor atmospheres, at pressure values in the range (5-40 Pa). The HA coatings were heat post-treated for 6 h in a flux of hot water vapors at the same temperature as applied during deposition. The surface morphology, chemical composition, and crystalline quality of the obtained thin films were studied by scanning electron microscopy, atomic force microscopy, and X-ray diffractometry. The films were seeded for in vitro tests with Hek293 (human embryonic kidney) cells that revealed a good adherence on the deposited layers. Biocompatibility tests showed that cell growth was better on HA than on BG thin films.     

Optimization of plasma parameters for high rate deposition of titanium nitride films as protective coating on bell-metal by reactive sputtering in cylindrical magnetron device

Nano-structured titanium nitride (TiN) thin film coating is deposited by reactive sputtering in cylindrical magnetron device in argon and nitrogen gas mixtures at low temperature. This method of deposition using DC cylindrical magnetron configuration provides high uniform yield of film coating over large substrate area of different shapes desirous for various technological applications. The influence of nitrogen gas on the properties of TiN thin film as suitable surface protective coating on bell-metal has been studied. Structural morphological study of the deposited thin film carried out by employing X-ray diffraction exhibits a strong (2 0 0) lattice texture corresponding to TiN in single phase. The surface morphology of the film coating is studied using scanning electron microscope and atomic force microscope techniques. The optimized condition for the deposition of good quality TiN film coating is found to be at Ar:N₂ gas partial pressure ratio of 1:1. This coating of TiN serves a dual purpose of providing an anti-corrosive and hard protective layer over the bell-metal surface which is used for various commercial applications. The TiN film's radiant golden colour at proper deposition condition makes it a very suitable candidate for decorative applications.     

BC2N薄膜的柱状生长及生长机理

应用热丝辅助等离子体化学气相沉积法(CVD)合成了表面呈柱状的BC₂N薄膜,X射线、红外及X射线电子能谱分析表明,薄膜的化学组分主要为BC₂N,B,C和N原子间互相结合成键.扫描电镜观察到,薄膜表面形貌呈排列整齐、取向一致的柱体,并且发现这种生长方式与沉积参数密切相关.最后从结合能方面讨论了柱状BC₂N的生长机理. 关键词： 2N')" href="#">BC₂N 柱状生长 CVD法     

The effect of oxygen rf discharge on pulsed laser deposition of oxide films

In this work final results on TiO₂ film deposition by Plasma Assisted Pulsed Laser Deposition (PAPLD) with an rf biased substrate are presented. In previous work it has been shown that PAPLD is an improvement over conventional PLD for the elimination of particulates in high refractive index thin film deposition. This paper will give a comparison between conventional PLD and PAPLD on the stoichiometry, morphology, and optical properties of deposited TiO₂ films. It will be demonstrated that oxygen rf discharge during the PLD process makes incorporation of oxygen into the depositing films extremely effective. This effect of the rf discharge allows operation of the PLD process at a lower oxygen background pressure while enhancing the deposition rate. Also, the production of a good quality TiO₂ film by PAPLD using a pure metal titanium target will be shown. PACS 79.20.Ds; 52.80.Pi     

Properties of NiO thin films deposited by intermittent spray pyrolysis process

NiO thin films have been grown on glass substrates by intermittent spray pyrolysis deposition of NiCl₂·6H₂O diluted in distilled water, using a simple “perfume atomizer”. The effect of the solution molarity on their properties was studied and compared to those of NiO thin films deposited with a classical spray system. It is shown that NiO thin films crystallized in the NiO structure are achieved after deposition. Whatever the precursor molarity, the grain size is around 25-30 nm. The crystallites are preferentially oriented along the (1 1 1) direction. All the films are p-type. However, the thickness and the conductivity of the NiO films depend on the precursor contraction. By comparison with the properties of films deposited by classical spray technique, it is shown that the critical precursor concentration, which induces strong thin films properties perturbations, is higher when a perfume atomizer is used. This broader stability domain can be attributed to better chlorides decomposition during the rest time used in the perfume atomizer technique.