Characterization of the porosity of thin zirconium oxide coatings prepared at low temperatures

In this work we investigated the possibilities to reduce the porosity of thin protective zirconium oxide films deposited with the sol-gel technique at low temperatures. Electrochemical investigations showed that the concentration of the stabilizing agent acetylacetone is a crucial parameter for the protection performance of the zirconium oxide films and that it is possible to run the deposition process at much lower temperatures with the optimum stabilizer concentration. This allows the application of the process to sensitive substrates that cannot be treated at high temperatures and reduces energy costs as well. Characterization of the film structure with secondary ion mass spectrometry revealed that the stabilizing agent is responsible for the formation of a mixed oxide layer at the interface of substrate and coating. The thickness of this layer can be tuned with the concentration of the stabilizing agent.     

Synthesis and structure characterization of low dielectric constant MSQ films by using octamethyl cyclotetrasiloxane (D4) as a porosity promotion agent

Low dielectric methylsilsesquioxane (MSQ) film can be synthesized by spin-coating on P–Si (100) wafer. Octamethyl cyclotetrasiloxane (D4) was used as a porosity promotion agent to MSQ film. Seven samples with different treatment were prepared. The dielectric constants of these MSQ films significantly lowered from 3.0 to 2.1. Fourier transform infrared spectroscopy was used to identify the Si–O–Si network structure, Si–O–Si cage structure and other bonds. The change of structure resulted in significant lowering of the dielectric constant (k). The capacitance–voltage (C–V) characteristic by HP4294A was used to determine the dielectric constant. Current–voltage (I–V) measurement by Keithley6517A was used to determine the breakdown electric field.     

Electrochemical preparation and characterization of three-dimensional nanostructured Sn2S3 semiconductor films with nanorod network

Three-dimensional (3D) nanostructured Sn₂S₃ semiconductor films have been prepared on ITO-coated glass substrates by potentiostatic electrodeposition at −0.80 V (vs. SCE) from a novel plating bath containing K₄P₂O₃ as a complexing agent and Na₂SO₃ as a stabilizing agent and by subsequent annealing. Results showed that the annealing drove the as-deposited Sn₂S₃ films to grow from a granular structure into a nanorod network structure. The nanorods were around 50-100 nm in diameter and 1000 nm in length. The band gap of the annealed film was 1.65 eV and the conductivity was n type. The carrier mobility achieved up to 20.5 cm² V⁻¹ s⁻¹ due to the direct electrical pathways provided by the nanorod network.     

Silicon for thin-film transistors

We are standing at the beginning of the industrialization of flexible thin-film transistor (TFT) backplanes. The two important research directions for the TFTs are (i) processability on flexible substrates and (ii) sufficient field-effect mobilities of electrons and holes to support complementary metal insulator semiconductor operation. The most important group of TFT capable semiconductors are the several modifications of silicon films: amorphous, nanocrystalline and microcrystalline. We summarize their TFT properties and their compatibility with foil substrate materials.     

Electrochemical performance of diamond-like carbon thin films

Diamond-like carbon (DLC) thin films used in this study were intended for their electrochemical properties. The DLC films were deposited by a filtered cathodic vacuum arc (FCVA) process on p-type silicon (100) substrates biased at different pulse voltages (0-2000 V). The chemical bonding structures of the DLC films were characterized with micro-Raman spectroscopy and the electrochemical properties were evaluated by means of electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization. The DLC films showed high impedance, high polarization resistance and high breakdown potential in a 0.5 M H₂SO₄ aqueous solution, which were attributed to the high sp³ content and uniformity of the films. The excellent chemical inertness of the DLC films made them promising corrosion resistant coating materials.     

Spectroscopic ellipsometry analyses of thin films in different environments: An innovative “reverse side” approach allowing multi angle measurements

An innovative ellipsometer sample holder has been designed and tested in order to measure thin films optical properties under different environments and so infer the porosity through effective medium approximation models. Compared to commercial cells that require a fixed angle of incidence or a cell with a cylindrical geometry, we present a simple cell in which the sample is mounted in “reverse side”, allowing multiple angle analyses without the need for cell windows. Standard ellipsometry measurements are compared to the “reverse side” approach in order to confirm the feasibility of this new procedure, obtaining the same refractive index dispersion curves in both cases. Then different samples have been tested in “reverse side” under different environments to measure porosity. The multiangle approach has been found useful to improve the fitting of the experimental data by reducing both the fitting error and the correlation between parameters.     

Combined kinetic and X-ray electron probe microanalysis characterization of local porosity variation and pore shape across anodic alumina films

Porous anodic alumina films on Al were prepared by anodic oxidation of Al in H₂SO₄ electrolyte at a constant temperature and current density and different thicknesses, up to ≈ 41 μm. Their cross section was examined by EPMA for revealing the variation of local porosity across the films and shape of pores while a kinetic model for film growth was developed describing the variation of pore diameter. It was found that the pores open, and local porosity increases, towards the film surface, predicting a conical pore shape, while the results coincided with those obtained by kinetic study. The EPMA analysis combined with kinetic results emerges as a promising tool for studying structural features of these films.     

Comparative Study of LiMn2O4 Thin Films Heat-treated by Conventional and Rapid Thermal Annealing

Cathode material LiMn2O4 thin films were prepared by solution deposition followed by conventional thermal annealing (CTA) and rapid thermal annealing (RTA) using lithium acetate and manganese acetate as starting materials. The phase and surface morphology identification was done by X-ray diffraction and scanning electron microscopy. The electrochemical properties of the thin films were carried out by cyclic voltammetry, charge-discharge experiments, electrochemical impedance spectroscopy and potential step technique. The results show that both thin films are homogeneous and crack-free. Compared with the CTA derived thin films, the RTA derived ones with smaller grain size are more smooth and dense. The CTA and RTA derived LiMn2O4 thin films deliver the capacity of 34.5 μAh/(cm2 ·μm) and 38 μAh/(cm2 ·μm) and show the capacity loss of 0.050% and 0.037% per cycle after being cycled 100 times, respectively. The diffusion coefficient of lithium ion in the CTA derived LiMn2O4 thin-film electrode is 4.59×10-11 cm2/s, and that of lithium ion in the RTA derived one is 3.86×10-11 cm2/s.     

化学镀镀层孔隙率对电化学行为的影响及其量化评价

通过调整镀层厚度得到了具有不同孔隙率的Ni-P化学镀层。使用图形分析软件辅助贴滤纸法测得了镀层孔隙率,并研究了孔隙率对镀层电化学行为的影响,探讨了利用电化学测试对镀层孔隙率进行量化评价的方法。结果表明,图形分析软件可以提高贴滤纸法的准确性和可重复性,而电化学方法在测量镀层微小孔隙方面具有明显优势。极化曲线测试表明,孔隙率较小的镀层具有较高的腐蚀电位和较低的腐蚀电流密度,可根据所测曲线精确计算出镀层孔隙率。交流阻抗测试可进一步揭示孔隙率对镀层腐蚀机理的影响,存在孔隙的镀层其交流阻抗谱会表现双时间常数的特征,通过拟合所得电化学参数可以用来评价镀层孔隙率大小。     

Preparation and characterization of ultra-thin sol-gel films

The formation and characterization of nanometer thick sol-gel films are reported. The films were prepared by spin-coating of a diluted solution of a silane precursor on a number of different substrates. The effect of dilution, rotation speed and nature of substrate on the thickness and homogeneity of the films was examined. Characterization of the films was carried out by profilometry, reflectance spectroscopy, atomic force microscopy, adhesion test and electrochemistry. We find that the dilution factor has a pronounced effect on the film thickness. Moreover, the time of dilution, namely, whether dilution was carried out before or after a period of hydrolysis, has a noticeable effect on the thickness as well as on the permeability of embedded species.     

Pulsed laser deposition of alumina coating for corrosion protection against liquid uranium

Alumina coatings find wide applications as tribological coatings and as corrosion protective coatings for structural materials against chemical attack. We have investigated alumina coatings deposited on Stainless Steel (SS) substrates via pulsed laser deposition (PLD) technique. Characterization tests performed on these coatings including their compatibility with liquid uranium suggests alumina to be a potential candidate as a coating material for handling and containment of liquid uranium. We present here results of our detailed parametric study including dependence of average mass removal rate on laser fluence and ablation geometry and average deposition efficiency during PLD. These measurements provide vital inputs facilitating proper choice of process parameters for PLD runs. Deposited coatings have been characterized in terms of their microstructure, surface profile, adhesion to substrate, crystalline phase and corrosion resistance against liquid uranium. Our PLD based alumina coatings have shown a high degree of compaction and excellent corrosion resistance to molten uranium even upto a temperature of 1165 °C.     

Electrochemical characterization of carbon nanotube forests grown on copper foil using transition metal catalysts

Growth of vertical, multiwalled carbon nanotubes (CNTs) on bulk copper foil substrates can be achieved by sputtering either Ni or Inconel thin films on Cu substrates followed by thermal chemical vapor deposition using a xylene and ferrocene mixture. During CVD growth, Fe nanoparticles from the ferrocene act as a vapor phase delivered catalyst in addition to the transition metal thin film, which breaks up into islands. Both the thin film and iron are needed for dense and uniform growth of CNTs on the copper substrates. The benefits of this relatively simple and cost effective method of directly integrating CNTs with highly conductive copper substrates are the resulting high density of nanotubes that do not require the use of additional binders and the potential for low contact resistance between the nanotubes and the substrate. This method is therefore of interest for charge storage applications such as double layer capacitors. Inconel thin films in conjunction with Fe from ferrocene appear to work better in comparison to Ni thin films in terms of CNT density and charge storage capability. We report here the power density and specific capacitance values of the double layer capacitors developed from the CNTs grown directly on copper substrates.     

Electrochromic and morphological investigation of dry-lithiated nanostructured tungsten trioxide thin films

Electrochromic properties of porous nanostructured thin films of tungsten trioxide were investigated. Films were fabricated at normal and high vapor incidence angles with the technique of glancing angle deposition in a thermal evaporation chamber. A dry lithiation method was subsequently used to intercalate films with lithium atoms. Coloration in both visible and near-infrared regions was observed with lithium insertion. We report on the morphology, porosity, and optical properties of as-deposited and lithiated films, and discuss the role of substrate tilt in comparing the coloration efficiency of these films.     

A three-dimensional electrode for photoelectrochemical cell: TiO2 coated ITO mesoporous film

In this letter, TiO₂ coated ITO mesoporous film was prepared by dipping doctor-blade ITO mesoporous film in TiO₂ sol, followed by sintering at 500 °C for 30 min. The CdS quantum dots (QDs) were deposited on TiO₂ coated ITO mesoporous film using sequential chemical bath deposition (S-CBD) method to form a three-dimensional (3D) electrode. The photo-activity of ITO mesoporous film/TiO₂/CdS electrode was investigated by forming a photoelectrochemical cell, which indicated that the ITO mesoporous film/TiO₂/CdS electrode was efficient in photoelectrochemical cell as a working electrode. The 3D electrode showed lower performance than the conventional electrode of TiO₂ mesoporous film/CdS, and more works are needed to improve the performance of 3D electrode.     

In-situ hydrothermal crystallization Mg(OH)2 films on magnesium alloy AZ91 and their corrosion resistance properties

Mg(OH)₂ films have been fabricated on magnesium alloy AZ91 substrates by an in-situ hydrothermal method. AZ91 alloy substrates act as both the source of Mg²⁺ ion and the support for the Mg(OH)₂ film in synthetic process. The effect of pH value and hydrothermal treatment time on the morphologies and corrosion resisting properties of Mg(OH)₂ film is studied. The obtained Mg(OH)₂ films are uniform and compact. The adhesion between the films and the substrate is strong due to the in-situ growth process, which enhances their potential for practical applications. Potentiodynamic polarization measurements showed that the Mg(OH)₂ films obtained at pH 10, 3 h exhibits the highest increase in corrosion potential at −0.7097 V and lowest i_corr, which suggests that it is the best effective film in improving the corrosion resistance of AZ91in all obtained films.     

Aluminum scandium nitride thin-film bulk acoustic resonators for wide band applications

Piezoelectric c-textured Al_(1−x)Sc_xN thin films, where the Sc relative concentration, x, varies in the range 0-0.15 have been studied in view of radio frequency (RF) electro-acoustic applications. Thin film bulk acoustic wave resonators (FBARs) employing these films were fabricated and characterized as a function of the Sc concentration for the first time. The measured electromechanical coupling is found to increase by as much as 100% in the above concentration range. The results from this work underline the potential of the c-textured Al_(1−x)Sc_xN based FBARs for wide band RF applications.     

Electrochemical preparation and characterization of thin deposits of Pd-noble metal alloys

The procedures of Pd-noble metal alloy (Pd-Au, Pd-Pt, Pd-Rh, Pd-Pt-Rh) preparation by electrochemical deposition from chloride solutions are described. The influence of deposition conditions on alloy composition is presented. The deposits were characterized electrochemically in acidic solutions (H₂SO₄ aq) by cyclic voltammetry. The surface morphology of the alloys was examined by scanning electron microscopy and scanning tunneling microscopy. The alloy surface composition was investigated in situ by the electrochemical method and ex situ by Auger electron spectroscopy, while the bulk composition was determined by energy dispersive analysis of X-rays and atomic absorption spectroscopy. The electrochemical methods of the real surface area determination were compared and discussed.     

Application of nano-cutting for mechanical characterization of materials

A novel technique for the mechanical characterization of materials near the surface using a nano-cutting process is proposed. In this technique a cutting machine cuts a layer of the specimen material, and the stresses on the shear plane and the shear angle deduced from the measured components of the cutting force are used for the characterization. The usefulness of this method is demonstrated by a cutting of poly methyl-methacrylate (PMMA) surface with a nano-cutting machine SAICAS.     

Transport of Caesium ions through thin poly-p-xylylene films

We describe an experimental setup for investigating the transport of alkali ions through poly(p-xylylene) membranes. It consists of an ion source where a continuous beam of alkali ions is generated from a surface emitter. Via ion-optics the ions are guided to the main chamber where the interaction with the free-standing membranes of variable thickness is investigated as a function of the impact energy. For a cesium ion beam the transmission of ions exhibits a maximum at an impact energy of several hundred volts, depending on the membrane thickness. The transport of the ions most likely proceeds through pores or porosities in the membrane. At the highest impact energies employed (around 2000 eV) the transmission of electrons is observed, most likely due to collision processes causing kinetic electron emission.