0000000001225152
AUTHOR
Luc Imhoff
Flash annealing influence on structural and electrical properties of TiO2/TiO/Ti periodic multilayers
Abstract Multilayered structures with a 40 nm period composed of titanium and two different titanium oxides, TiO and TiO 2 , were accurately produced by DC magnetron sputtering using the reactive gas pulsing process. These multilayers were sputtered onto Al 2 O 3 sapphire to avoid substrate compound diffusion during flash annealing (ranging from 350 °C to 550 °C). Structure and composition of these periodic TiO 2 /TiO/Ti stacks were investigated by X-ray diffraction, X-ray photoemission spectroscopy and transmission electronic microscopy techniques. Two crystalline phases α-Ti and fcc-TiO were identified in the metallic-rich sub-layers whereas the oxygen-rich ones were composed of a mixture…
Chemical and structural characterization of periodic metal/oxide nanometric layers using STEM-EELS
Chemical and structural characterization of periodic metal/oxide nanometric layers using STEM-EELS
Structuration of nanometric tungsten/tungsten oxide periodic films combining gas pulsing and glancing angle deposition
Structuration of nanometric tungsten/tungsten oxide periodic films combining gas pulsing and glancing angle deposition
Development of dark Ti(C,O,N) coatings prepared by reactive sputtering
Accepted manuscript
Structural and electrical properties of magnetron sputtered Ti(ON) thin films:The case of TiN doped in situ with oxygen.
International audience; Incorporation of oxygen into TiN lattice results in formation of titanium oxynitrides, TiOxNy that have become particularly interesting for photocatalytic applications. Elaboration as well as characterization of TiN and in situ oxygen-doped thin films is the subject of this paper. Thin films, 250–320nm in thickness, have been deposited by dc-pulsed magnetron reactive sputtering from Ti target under controllable gas flows of Ar, N2 and O2. Optical monitoring of Ti plasma emission line at = 500nm has been implemented in order to stabilize the sputtering rate. Scanning electron microscopy (SEM), X-ray diffraction in grazing incidence (GIXRD), micro-Raman spectroscopy, X…
Nitrogen plasma pressure influence on the composition of TiNxOy sputtered films
Thin films of TiNxOy were deposited by d.c. magnetron sputtering on glass substrates using an (Ar+,N2) plasma and Ti target. The N2 partial pressure was changed from 2.3 × 10−4 mbar to 4.6 × 10−3 mbar in order to obtain films with increasing nitrogen contents. X-ray photoelectron spectroscopy was used to determine the as-deposited composition. The presence of oxygen, which is probably due to contamination from the residual atmosphere in the vacuum chamber, is always detected, both in the surface layers and in the bulk of the films, confirming the formation of TiNxOy. When the nitrogen partial pressure was increased, a maximum for the nitrogen content in the films was reached, corresponding …
Structure and chemical bonds in reactively sputtered black Ti–C–N–O thin films
The evolution of the nanoscale structure and the chemical bonds formed in Ti–C–N–O films grown by reactive sputtering were studied as a function of the composition of the reactive atmosphere by increasing the partial pressure of an O2+N2 gas mixture from 0 up to 0.4 Pa, while that of acetylene (carbon source) was constant. The amorphisation of the films observed by transmission electron microscopy was confirmed by micro- Raman spectroscopy, but it was not the only effect associated to the increase of the O2+N2 partial pressure. The chemical environment of titanium and carbon, analysed by X-ray photoemission spectroscopy, also changes due to the higher affinity of Ti towards oxygen and nitro…
Chemical characterization of gallium droplets grown by LP-MOCVD.
International audience; This study is concerned with the chemical characterization of metallic gallium droplets, obtained on silicon (1 0 0) substrates with a single growth step, by the LP-MOCVD technique with TMGa like precursor. These structures are characterized by SIMS, XPS and TEM. The analyses results lead to a structure proposition for the droplets. The core is composed of metastable metallic gallium with a non-negligible carbon quantity probably coming from incomplete precursor decomposition. The outer part, composed of gallium oxide maintains the structure stability. Covering of the substrate by a thin gallium layer of gallium compounds is observed.
Interdependence of structural and electrical properties in tantalum/tantalum oxide multilayers
International audience; Dc reactive sputtering was used to deposit tantalum metal/oxide periodic nanometric multilayers using the innovative technique namely, the reactive gas pulsing process (RGPP). Different pulsing periods were used for each deposition to produce metal-oxide periodic alternations included between 5 and 80 nm. Structure, crystallinity and chemical composition of these films were systematically investigated by Transmission Electron Microscopy (TEM) and Energy-dispersive X-ray (EDX) spectroscopy techniques. Moreover, electrical properties were also studied by the Van der Pauw technique.
Pulsed Direct liquid Injection ALD of TiO2 Films Using Titanium Tetraisopropoxide Precursor
Abstract TiO 2 thin films are grown by pulsed direct liquid injection atomic layer deposition with rapid thermal heating using titanium tetraisopropoxide and water vapor as precursors. The ALD growth rate is constant in the saturation zone range 35-47 ms at the temperature deposition of 280 °C. The TiO 2 growth rate of 0.018 nm/cycle was achieved in a self-limited ALD mode. SEM and AFM analysis showed the as-deposited films have a smooth surface with a low roughness. XPS analysis exhibited the stoichiometry of TiO 2 in the homogenous depth composition.
CVD elaboration and in situ characterization of barium silicate thin films.
International audience; This study is concerned with the elaboration of barium silicate thin films by metal organic chemical vapor deposition (MOCVD) and in situ characterization by X-ray photoemission spectroscopy (XPS) with an apparatus connected to the deposition reactor. The difficulty to find an efficient metal organic precursor for barium is described. After characterizations of the selected reactant, Ba(TMHD)2tetraglyme, the development of an original specific vapor delivering source which allows reactant sublimation in the CVD reactor was performed. In the most optimized cases, including use of oxygen introduction during the deposition, barium silicate films were obtained. Moreover,…
Structural characterization of original 3D gallium structures grown by LP‐MOCVD
This study is concerned with the growth and characterization of metallic gallium 3D structures, obtained with a single growth step, by the LP-MOCVD technique on various substrates. Commercial organo-metallic is used as gallium precursor and nitrogen as carrier gas. The growth temperature and the reactor pressure are ranking between 500 and 700 °C, and between 150 and 700 torr, respectively. Depending on the elaboration conditions, different 3D structures are obtained such as droplets, cauliflowers, aggregates or thin stems, with micrometer sizes. The morphology, substrate surface density and thermal stability are studied by optical and scanning electron microscopy. At last, X-ray microanaly…
Surface preparation influence on the initial stages of MOCVD growth of TiO2 thin films
In situ chemical surface analyses using X-ray photoelectron spectroscopy (XPS), completed by ex situ atomic force microscopy (AFM) analyses, were performed in order to compare the initial stages of MOCVD growth of TiO 2 thin films on two different surface types. The first type was a silicon native oxide free hydrogen terminated surface and the second one was a silicon dioxide surface corresponding to a thin layer of 3.5 nm thick in situ thermally grown on silicon substrate. Si(100) was used as substrate, and the growths of TiO 2 thin films were achieved with titanium tetraisopropoxide (TTIP) as precursor under a temperature of 675 °C, a pressure of 0.3 Pa and a deposition time of 1 h. Whate…
MOVPE growth of Ga 3D structures for fabrication of GaN materials
Abstract This paper presents the growth and characterization of metallic gallium three-dimensional (3D) structures and preliminary results of their transformation into GaN-like structures. The structures were grown by metal-organic vapour phase epitaxy (MOVPE), using trimethyl gallium as gallium precursor on silicon (1 0 0). The growth temperature was between 550°C and 750°C. Interesting and new metallic structures were obtained with our growth parameters: balloon (montgolfier-like structure) and cauliflower-like. These metallic structures can grow up perpendicular to the substrate surface and have diameters between 0.1 and 5 μm, depending on the growth conditions. Moreover, selective metal…
Structural and in depth characterization of newly designed conducting/insulating TiN O /TiO2 multilayers obtained by one step LP-MOCVD growth
Abstract TiNxOy/TiO2 multilayers have been grown by LP-MOCVD using titanium isopropoxide (TIP) precursor during the whole growth, but with an ammonia flow interrupted for the TiO2 layers. The one step growth process used to grow these structures allowed to stack the conducting and insulating layers without any growth breakdown. SIMS and TEM analyses showed the presence of an alternated insulating/conducting layers structure. Moreover, electrical measurements allowed to measure the dielectric part of insulating TiO2 stacked in these structures, whose permittivity was found to be about 80 for a MOS structure. Thus, such multilayers may lead to very promising applications in the microelectroni…
Redox reactions in the Pt/TiO2–WO3/SiO2 planar system
Abstract The thermal behavior of the titanium–tungsten adhesive layer (30–70 at.%) deposited on a SiO2 substrate followed by a thicker Pt layer was investigated. The resulting Pt/TiW/SiO2 planar system was annealed under air or vacuum. Morphological and chemical characterizations at different stages of the annealing, as a function of several parameters such as treatment atmosphere, annealing temperature and thickness of the Pt film were performed through surface science analyses. When annealing under air, even at mild temperature (773 K), the whole interlayer oxidizes while a low amount of tungsten diffuses through platinum film. This phenomenon is related to tungsten oxidation which acts a…
Structural characterization of TiNxOy/TiO2 single crystalline and nanometric multilayers grown by LP-MOCVD on (110)TiO2
TiO2/TiNxOy superlattices were grown by Low Pressure-Metal-Organic Vapor Phase Epitaxy (LP-MOVPE) technique at deposition temperatures ranking from 650 to 750°C. The growth was performed on top of TiO2(110) rutile substrates. Intense peaks observed in the X-rays rocking curves and θ-2θ diffraction patterns show the presence of crystalline epilayers. The TiNxOy layers were grown in a (200) cubic structure on the (110) quadratic TiO2 epilayer structure. Transmission electron microscopy confirmed the XRD results and showed the formation of periodic and well structured epilayers.
Curvature radius measurement by optical profiler and determination of the residual stress in thin films
Abstract The Stoney formula, based on the measurement of the substrate curvature, is often used for the determination of the thin films' residual stress. In this study, titanium nitride coatings were deposited by DC reactive magnetron sputtering on silicon substrates. An optical profiler was used to determine the curvature of the surface before and after coating. Two radii were then obtained, along the principal perpendicular directions of the surface curvature. A simple and efficient method to determine the experimental error on the stress calculation was developed taking into account the film thickness dispersion and the radii dispersion. Using constant deposition parameters, some samples…
Conductimetry and impedance spectroscopy study of low pressure metal organic chemical vapor deposition TiN O films as a function of the growth temperature: a percolation approach
Abstract Titanium oxinitride thin films have been grown by low pressure metal organic chemical vapor deposition (LP-MOCVD) using titanium isopropoxide, Ti(OCH(CH 3 ) 2 ) 4 (TIP) and NH 3 precursors in a growth temperature range from 450 to 750°C on sapphire substrates. The electrical behaviour of these films was studied between 400 and 173 K, revealing three different behaviours, ranking from a hopping conductivity (450–500°C) to a conducting one (700–750°C), with a dual behaviour for the intermediate growth temperatures. Moreover, at room temperature, both conductimetry and impedance spectroscopy highlighted a percolation behaviour, interpreted in terms of continuum percolation. The effect…
MOCVD growth of porous cerium oxide thin films on silicon substrate
Abstract Porous cerium oxide thin films were grown by pulsed direct liquid injection metal organic chemical vapor deposition (DLI-MOCVD) on silicon substrate, using cerium tetrakis (1-methoxy-2-methyl-2-propanolate) dissolved in cyclohexane as precursor as well as oxygen as oxidant agent. The chemical and morphological characteristics of the films were investigated by XPS, SEM and TEM. The influence of the growth conditions on the morphological features of the thin films and the cerium chemical states are reported and discussed. The decrease of the oxygen and/or alkoxide flow rate induces the decrease of both the film thickness and the porosity of the layer. Moreover, the growth of silicate…
Structural characterization of TiO2/TiN O (δ-doping) heterostructures on (1 1 0)TiO2 substrates
Abstract TiO2/TiNxOy δ-doping structures were grown on the top of (1 1 0)TiO2 rutile substrates by low pressure metal-organic vapor phase epitaxy (LP-MOVPE) technique at 750 °C. The samples were analyzed by high resolution transmission electron microscopy (HRTEM), electron energy loss spectroscopy (EELS) and X-ray diffraction techniques (rocking curves and φ-scans). The presence of satellites in the (1 1 0)TiO2 rocking curve revealed the epitaxial growth of 10 period δ-doping structures. The thickness of the TiO2 layers, 84 nm, was deduced from the satellites period. HRTEM observations showed around 1.5 nm thick δ-doping layers, where the presence of nitrogen was detected by EELS. The analy…
Temperature and substrate influence on the structure of TiN O thin films grown by low pressure metal organic chemical vapour deposition
Abstract This paper presents the growth and characterization of titanium oxinitride (TiN x O y ) films grown by low pressure metal organic chemical vapour deposition (LP-MOCVD). The film nitrogen content, obtained by Rutherford backscattering spectroscopy (RBS), increases as the growth temperature increases (from 23 at.% at 450°C to 46 at.% at 750°C). Below 550°C, the films do not show any X-ray diffraction pattern. Above 550°C, the deposited films present the (111) and (200) TiN textures. Films deposited on (100) Si exhibit a 2 θ shift to higher Bragg angles, depending on the N/O ratio. These shifts are explained by using a substitutional oxygen model. Moreover, the atomic structure of suc…
Dynamics of molybdenum nano structure formation on the TiO2(110) surface: A kinetic Monte Carlo approach
Abstract The rutile TiO 2 (1 1 0) surface is a highly anisotropic surface exhibiting “channels” delimited by oxygen rows. In previous experimental and theoretical DFT works we could identify the molybdenum adsorption sites. They are located inside the channels. Moreover, experimental studies have shown that during subsequent annealing after deposition, special molybdenum nano structures can be formed, especially two monolayer high pyramidal chains of atoms. In order to better understand the dynamics of nano structure formation, we present a kinetic Monte Carlo study on diffusion and adsorption of molybdenum atoms on a TiO 2 (1 1 0) surface. A quasi one-dimensional lattice gas model has been…
Interfacial reaction during MOCVD growth revealed by in situ ARXPS.
International audience; Angle-resolved X-ray photoelectron spectroscopy (ARXPS) experiments were performed to study in situ the reaction at the film–substrate interface during metal organic chemical vapor deposition (MOCVD) growth of TiO2 thin films deposited on the silicon substrate. The in-depth distribution of chemical species was determined using several ARXPS thickness calculation models considering either single or bilayer systems. By the comparison of two single-layermodels, the presence of a second layer composed of silicon oxidewas evidenced. High-resolution transmission electron microscopy (HRTEM) observations confirmed the stratification of the film in two layers, as well as the …
Alumina particle reinforced TiO2 composite films grown by direct liquid injection MOCVD
Abstract The use of a liquid injection delivery system to form composite films containing nanoparticles was investigated. Al 2 O 3 –TiO 2 films were grown on silicon substrates by direct liquid injection MOCVD (DLI-MOCVD) at 400 °C. The α-Al 2 O 3 nanoparticles (α-Al 2 O 3 NPs) dispersed in TiO 2 films resulted from co-deposition using colloidal α-Al 2 O 3 solution and titanium tetraisopropoxide as titanium precursor. Scanning electron microscopy coupled with EDS as well as Raman spectroscopy confirmed the presence of α-Al 2 O 3 NPs aggregates embedded in the TiO 2 matrix. The liquid injection system coupled with CVD technique can be promising to form composite films containing preformed na…
Angle resolved X-ray photoemission spectroscopy double layer model for in situ characterization of metal organic chemical vapour deposition nanometric films.
International audience; In situ Angle Resolved X-ray Photoemission Spectroscopy (ARXPS) characterizations of TiO2 thin films grown on silicon by Metal Organic Chemical Vapour Deposition were performed in order to get information on interfacial reactions at the first stages of the growth, one of the aims being to understand the influence of deposition conditions. Thickness measurements were also carried out from ARXPS analyses. As the real structure of the films was shown to be a double layer system such as TiO2/SiO2/Si, an ARXPS model of thickness and surface coverage determination was applied to each layer independently. However, the application of this model to very thin films underestima…
Nanostructured Pt–TiO2 composite thin films obtained by direct liquid injection metal organic chemical vapor deposition: Control of chemical state by X-ray photoelectron spectroscopy
Abstract Nanostructured Pt–TiO 2 composite thin films were synthesized by direct liquid injection metal organic chemical vapor deposition process, using trimethyl(methylcyclopentadienyl)platinum and titanium isopropoxide as precursors. Surface and cross-sectional morphologies obtained by scanning electron microscopy and transmission electron microscopy evidenced the uniform distribution of platinum nanoparticles in the TiO 2 matrix. At higher Pt content, the X-ray diffraction analysis showed that the face-centered cubic phase of platinum appeared together with an anatase TiO 2 structure. In addition, as far as the platinum chemical state is concerned, the co-deposition of TiO 2 and Pt allow…
Elaboration and characterization of barium silicate thin films.
International audience; Room temperature depositions of barium on a thermal silicon oxide layer were performed in ultra high vacuum (UHV). In-situ X-ray photoelectron spectroscopy (XPS) analyses were carried out as well after exposure to air as after subsequent annealings. These analyses were ex-situ completed by secondary ion mass spectrometry (SIMS) profiles and transmission electron microscopy (TEM) cross-sectional images. The results showed that after air exposure, the barium went carbonated. Annealing at sufficient temperature permitted to decompose the carbonate to benefit of a barium silicate. The silicate layer was formed by interdiffusion of barium with the initial SiO2 layer.
Phase mixture in MOCVD and reactive sputtering TiOxNy thin films revealed and quantified by XPS spectra factorial analysis
International audience
TiO2 anatase films obtained by direct liquid injection atomic layer deposition at low temperature
International audience; TiO2 thin films were grown by direct liquid injection atomic layer deposition (DLI-ALD) with infrared rapid thermal heating using titanium tetraisopropoxide and water as precursors. This titanium tetraisopropoxide/water process exhibited a growth rate of 0.018 nm/cycle in a self-limited ALD growth mode at 280 degrees C. Scanning electron microscopy and atomic force microscopy analyses have shown a smooth surface with a low roughness. XPS results demonstrated that the films were pure and close to the TiO2 stoichiometric composition in depth. Raman spectroscopy revealed that the films were crystallized to the anatase structure in the as-deposited state at low temperatu…
Growth of WC–Cr–N and WC–Al–N coatings in a RF-magnetron sputtering process
Tungsten carbide-based coatings have been used in a wide variety of industrial applications such as high speed cutting tools, extrusion dies, drills, aerospace industries, and more. A few reports on ternary and quaternary coatings of WC with other elements indicate good prospects for these material systems. The present study focuses on the formation of quaternary WCeCreN and WCeAleN coatings during the simultaneous reactive RF-magnetron sputtering of tungsten carbide and Al or Cr targets in an argon/nitrogen gas mixture. The resulting coatings, with thicknesses of 3.5 mme8.2 mm, were characterized by using several analytical techniques including X-ray diffraction, SEM/EDS, AFM, and X-ray ph…
Initial stages of TiO2 thin films MOCVD growth studied by in situ surface analyses
Abstract In situ chemical surface analyses using X-ray photoelectron spectroscopy (XPS) were performed to understand the initial stages of TiO 2 thin-film MOCVD growth. Deposits on Si (1 0 0), a few nanometres thick, were obtained at a fixed temperature of 650 °C and for two different pressures, 2.9 and 0.05 mbar, using titanium tetraisopropoxide (TTIP) as precursor. Pressure lowering led to a higher deposit growth rate. Reduction of titanium with respect to stoichiometric titanium dioxide and oxidation of the wet-cleaned silicon substrate are observed from decomposition of the Ti 2p and Si 2p peaks. The formation of a TiSi x O y mixed oxide is also pointed out and confirmed by the presence…
The interdependence of structural and electrical properties in TiO2/TiO/Ti periodic multilayers
International audience; Multilayered structures with 14-50 nm periods composed of titanium and two different titanium oxides, TiO and TiO2, were accurately produced by DC magnetron sputtering using the reactive gas pulsing process. The structure and composition of these periodic TiO2/TiO/Ti stacks were investigated by X-ray diffraction and transmission electronic microscopy techniques. Two crystalline phases, hexagonal close packed Ti and face centred cubic TiO, were identified in the metallic-rich sub-layers, whereas the oxygen-rich ones comprised a mixture of amorphous TiO2 and rutile phase. DC electrical resistivity rho measured for temperatures ranging from 300 to 500 K exhibited a meta…
Structural and electrical properties in tungsten/tungsten oxide multilayers
International audience; Tungsten and tungsten oxide periodic nanometric multilayers have been deposited by DC reactive sputtering using the reactive gas pulsing process. Different pulsing periods have been used for each deposition to produce metal-oxide periodic alternations ranging from 3.3 to 71.5 nm. The morphology, crystallinity and chemical composition of these films have been investigated by transmission electron microscopy and energy-dispersive X-ray spectroscopy techniques. The produced multilayers exhibited an amorphous structure and the composition stability of WO3 sub-layers has been pointed out. Moreover, electrical properties have also been studied by the van der Pauw technique…
Structure and properties of GaNxOy films grown by nitridation of GaAs (100) substrates
GaAs (100) substrates have been heat-treated in a metal-organic chemical vapor deposition reactor under flows of NH 3 and an oxygen organo-metallic precursor at temperatures between 650°C and 750°C. Yellowish films formed at the surface of all the samples. Gallium, nitrogen and oxygen were detected by EDX analysis of the films. The oxygen content was estimated in the range of at 5-10 at% depending on the heat-treatment temperature. X-ray diffraction and HRTEM results indicate that the structure of the films corresponds to the hexagonal wurtzite phase of GaN with an expanded unit cell. Raman spectra show hands corresponding to the Raman active GaN modes as well as disorder-activated broad ba…
Photoemission study of the reactivity of barium towards SiOx thermal films
Abstract Barium was deposited at room temperature on a thermal silicon oxide layer and the interfacial reaction was monitored by synchrotron induced photoemission (both core level and valence band). The first step of the growth consists of an interfacial reaction which leads to the formation of an interfacial silicate layer. The next step consists in formation of barium oxide while metallic barium occurs subsequently. The deposit can be also homogenized by annealing above 575 K. This results in the formation of several layers of silicate by consumption of silicon oxide. In the case of fractional coverage, subsequent annealing at 975 K induces the decomposition of barium silicate. However, s…
Thermal effects on the growth by metal organic chemical vapour deposition of TiO2 thin films on (100) GaAs substrates
Abstract TiO 2 thin films were deposited on (100) GaAs substrates by LP-MOCVD with deposition temperatures ( T d ) ranking from 450 to 750 °C. The structure of these layers was studied by X-ray diffraction (XRD) and Raman spectroscopy. The growth of the TiO 2 anatase phase was observed for T d T d >600 °C. Finally, X-ray photoelectron spectrometry (XPS) and secondary ion mass spectroscopy (SIMS) experiments showed the presence of small quantities of Ga and As through the whole film thickness, slightly increasing at the surface of the layers. This result was related to the SEM observations and explained by considering the growth conditions.
Phase mixture in MOCVD and reactive sputtering TiOxNy thin films revealed and quantified by XPS factorial analysis.
Abstract Titanium oxynitride thin films have been deposited by low-pressure metalorganic chemical vapour deposition and reactive sputtering. The growth temperature for chemical vapour-deposited films and water vapour partial pressure for sputter-deposited films have been used to modulate the chemical composition. Both series have been analysed using X-ray photoelectron spectroscopy (XPS) in order to describe the structure of the materials using a factorial analysis approach. Titanium and metalloid concentrations have also been determined and compared to an elemental analysis performed using Rutherford backscattering spectroscopy and nuclear reaction analysis. The two deposition methods led …
Structural analysis of W3O/WO3 and TiO/TiO2 periodic multilayer thin films sputter deposited by the reactive gas pulsing process
International audience; DC reactive sputtering was used to deposit titanium and tungsten-based metal/oxide periodic nanometric multilayers using pure metallic targets and Ar + O-2 gas mixture as reactive atmosphere. The innovative technique namely, the reactive gas pulsing process allows switching between the metal and oxide to prepare a periodic multilayered structure with various metalloid concentrations and nanometric dimensions. The same pulsing period was used for each deposition to produce metal-oxide periodic alternations close to 10 nm. Structure, crystallinity and chemical composition of these films were systematically investigated by Raman spectroscopy, X-ray diffraction and Energ…
Influence of flash annealing on structure and electrical properties of multilayered TiO2/TiO/Ti thin films
Influence of flash annealing on structure and electrical properties of multilayered TiO2/TiO/Ti thin films
Correlation Between the Electrical Properties and the Morphology of Low-Pressure MOCVD Titanium Oxynitride Thin Films Grown at Various Temperatures
Titanium oxynitride (TiN x O y ) thin films were deposited by low-pressure metal-organic CVD (LP-MOCVD) on (100) silicon, sapphire, and polycrystalline alumina substrates. Titanium isopropoxide (TIP) and ammonia were used as precursors. The influence of the growth temperature, ranking from 450°C to 750°C, was investigated by scanning electron microscopy (SEM), and electrical DC measurements. Rutherford back-scattering (RBS) measurements were used to determine the N/O ratio in the films. The surface observations of the deposited films showed two morphological transitions. The resistivity decreased with the growth temperature, while the nitrogen content increased. Moreover, for the highest de…
Amorphous TiO2 in LP-OMCVD TiNxOy thin films revealed by XPS
Abstract TiN(O)–TiO 2 thin films were prepared on Si(1 0 0) by the low pressure organo metallic chemical vapor deposition (LP-OMCVD) method, using ammonia and titanium isopropoxide as precursors. In order to complete previous characterizations, an Ar + bombardment/XPS coupled study was carried out. This method is based on the fact that the behavior of a compound towards an ion bombardment is a function of its composition. In particular, Ar + bombardment of TiO 2 (whatever its form) leads to a preferential sputtering of oxygen atoms with subsequent reduction of titanium and formation of Ti 3+ and Ti 2+ easily detectable by XPS from a significant broadening of the Ti 2p lines. In the opposite…
Pulsed laser growth and characterization of thin films on titanium substrates
Abstract Colored layers were obtained by laser surface treatment of Ti substrates with a pulsed Nd:YAG Q-switched laser. The changes in the morphology, structure and chemical composition of the layers were studied by SEM, EDS, XPS, SIMS and Raman spectroscopy as a function of the laser fluence in the 4–60 J cm −2 . For laser fluences lower than 25 J cm −2 , the layers are colorless or yellow. Their surface is smooth, but they display cracks which increase when the fluence increases. The O/Ti ratio, determined by XPS analysis, varies from 0.7 (colorless layers) to 1.3 (yellow layer). Moreover, XPS spectra evidence non-negligible amounts of nitrogen and carbon in these layers. Raman spectra s…
Thermal stability of Au–TiO2 nanocomposite films prepared by direct liquid injection CVD
Abstract Nanocomposite films composed of gold nanoparticles (AuNPs) embedded in a TiO 2 matrix have been prepared by direct liquid injection chemical vapor deposition process, using preformed nanoparticles and titanium isopropoxide as precursors. The spherical AuNPs about 4.1 nm in diameter were synthesized by using gold (III) chloride trihydrate and stabilized by thiol ligands. The depositions were carried out by performing at first oxide deposition, then gold nanoparticle one and capping with oxide. The morphology, structure; the chemical state and optical properties of nanocomposite films were characterized by scanning electron microscopy, Raman, X-ray photoelectron and UV–Vis absorption…