Effect of oxygen partial pressure on microstructural and optical properties of titanium oxide thin films prepared by pulsed laser deposition

Nanocrystalline titanium oxide (TiO₂) thin films were deposited on silicon (1 0 0) and quartz substrates at various oxygen partial pressures (1 × 10⁻⁵ to 3.5 × 10⁻¹ mbar) with a substrate temperature of 973 K by pulsed laser deposition. The microstructural and optical properties were characterized using Grazing incidence X-ray diffraction, atomic force microscopy, UV–visible spectroscopy and photoluminescence. The X-ray diffraction studies indicated the formation of mixed phases (anatase and rutile) at higher oxygen partial pressures (3.5 × 10⁻² to 3.5 × 10⁻¹ mbar) and strong rutile phase at lower oxygen partial pressures (1 × 10⁻⁵ to 3.5 × 10⁻³ mbar). The atomic force microscopy studies showed the dense and uniform distribution of nanocrystallites. The root mean square surface roughness of the films increased with increasing oxygen partial pressures. The UV–visible studies showed that the bandgap of the films increased from 3.20 eV to 3.60 eV with the increase of oxygen partial pressures. The refractive index was found to decrease from 2.73 to 2.06 (at 550 nm) as the oxygen partial pressure increased from 1.5 × 10⁻⁴ mbar to 3.5 × 10⁻¹ mbar. The photoluminescence peaks were fitted to Gaussian function and the bandgap was found to be in the range ∼3.28–3.40 eV for anatase and 2.98–3.13 eV for rutile phases with increasing oxygen partial pressure from 1 × 10⁻⁵ to 3.5 × 10⁻¹ mbar.     

Rietveld X-ray diffraction analysis of nanostructured rutile films of titania prepared by pulsed laser deposition

Rietveld powder X-ray diffraction analysis of the rutile films of titanium oxide prepared by pulsed laser deposition was carried out. The crystallite size increased with increase of substrate temperature, while the strain showed a reverse trend. The films synthesized at temperature ≥573 K showed that the crystal structure was almost close to that of bulk rutile structure. The influence of the substrate temperature on the lattice parameters and oxygen coordinates were also studied in the present work.     

Cold laser machining of nickel-yttrium stabilised zirconia cermets: Composition dependence

Cold laser micromachining efficiency in nickel-yttrium stabilised zirconia cermets was studied as a function of cermet composition. Nickel oxide-yttrium stabilised zirconia ceramic plates obtained via tape casting technique were machined using 8-25 ns pulses of a Nd: YAG laser at the fixed wavelength of 1.064 μm and a frequency of 1 kHz. The morphology of the holes, etched volume, drill diameter, shape and depth were evaluated as a function of the processing parameters such as pulse irradiance and of the initial composition. The laser drilling mechanism was evaluated in terms of laser-material interaction parameters such as beam absorptivity, material spallation and the impact on the overall process discussed. By varying the nickel oxide content of the composite the optical absorption (-value is greatly modified and significantly affected the drilling efficiency of the green state ceramic substrates and the morphology of the holes. Higher depth values and improved drilled volume upto 0.2 mm³ per pulse were obtained for substrates with higher optical transparency (lower optical absorption value). In addition, a laser beam self-focussing effect is observed for the compositions with less nickel oxide content. Holes with average diameter from 60 μm to 110 μm and upto 1 mm in depth were drilled with a high rate of 40 ms per hole while the final microstructure of the cermet obtained by reduction of the nickel oxide-yttrium stabilised zirconia composites remained unchanged.     

Characterization of ZnO-In2O3 transparent conducting films by pulsed laser deposition

Transparent conducting oxide (TCO) films in the ZnO-In₂O₃ system were prepared by a pulsed laser deposition method. A target that consists of the mixture of ZnO and In₂O₃ powders was used. Influences of the target composition x (x = [Zn]/([Zn] + [In])) and heater temperature on structural, electrical and optical properties of the TCO films were examined. Introduction of oxygen gas into the chamber during the deposition was necessary for improvement in the transparency of the deposited films. The amorphous phase was observed for a wide range of x = 0.20-0.60 at 110 °C. Minimum resistivity was 2.65 × 10⁻⁴ Ω cm at x = 0.20. The films that showed the minimum resistivity had an amorphous structure and the composition shifted toward larger x, as the substrate temperature increased. The films were enriched in indium compared to the target composition and the cationic In/Zn ratio increased as the substrate temperature was increased.     

Properties of amorphous Si thin film anodes prepared by pulsed laser deposition

Amorphous Si (a-Si) thin film anodes were prepared by pulsed laser deposition (PLD) at room temperature. Structures and properties of the thin films were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and electrochemical measurements. Galvanostatic charge/discharge tests of half cells using lithium counter electrode were conducted at a constant current density of 100 μA/cm² in different voltage windows. Cyclic voltammetry (CV) was obtained between 0 and 1.5 V at various scan rates from 0.1 to 2 mV/s. The apparent diffusion coefficient (D_Li) calculated from the CV measurements was about ∼10⁻¹³ cm²/s. The Si thin film anode was also successfully coupled with LiCoO₂ thin film cathode. The a-Si/LiCoO₂ full cell showed stable cycle performance between 1 and 4 V.     

Physical properties of (La,Sr)Ti(O,N)3 thin films grown by pulsed laser deposition

Thin films of La_xSr_1−xTiO_3+x/2 (x = 0, 0.25, 0.5, 0.75, 1) were grown by laser ablation on two different kinds of substrates (SrTiO₃ (STO) and MgO) and were subsequently ammonolysed to yield the corresponding oxynitrides La_xSr_1−xTi(O,N)₃. For both substrates all films were found to grow epitaxially to the (1 0 0) direction of the cubic perovskite structure, except for x = 0.5 that grew parallel to the (1 1 0) direction. For some of the films TiN was detected as impurity phase. Scanning electron microscopy revealed that the films are dense and homogeneous with thicknesses around 350 nm. Atomic force microscopy showed that the surface roughness of the films varied between 4.2 and 14.1 nm. The employed substrate had a strong influence on the electrical properties. Films grown on STO exhibited a metallic behaviour, in contrast to the films grown on MgO, which were insulating.     

Studies on the photoconductivity of vacuum deposited ZnTe thin films

The present paper reports the analysis of photoconductivity of vacuum deposited zinc telluride (ZnTe) thin films as a function of substrate temperature and post-deposition annealing. Detailed analyses were first carried out to understand the effect of substrate temperature and annealing on the structure, composition, optical and electrical properties of the films. The films deposited at elevated substrate temperatures showed faster and improved photoresponse. Post-deposition annealing was found to further enhance the photoresponse of the films. Attempts have been made to explain the improvement in the photoresponse on the basis of structural and compositional changes, taking place in the films, due to the substrate temperature and annealing.     

Deposition of hydroxyapatite thin films by Nd:YAG laser ablation: a microstructural study

Hydroxyapatite (HA) thin films has been successfully deposited by Nd:YAG laser ablation at λ = 532 nm. The morphology and microstructure of the deposited layers was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high resolution electron microscopy (HREM). Polycrystalline HA films were directly obtained with the substrate at 300 °C and without introducing water vapors in the deposition chamber. Electron paramagnetic resonance (EPR) measurements show that the oxygen stoichiometry in the HA films is also maintained. Depositions performed at λ = 335 nm laser wavelength and 300 °C substrate temperature resulted in polycrystalline layers of mixed composition of HA and tricalciumphosphate (TCP).     

Adhesion study of pulsed laser deposited hydroxyapatite coating on laser surface nitrided titanium

Hydroxyapatite (HA) coatings were fabricated by pulsed laser deposition (PLD) on commercially pure titanium which had been subjected to different types of pre-treatment. These include: (i) 60-grit SiC grinding, (ii) 320-grit SiC grinding, (iii) 1-µm diamond paste mirror-finishing, (iv) etching with Knoll solution, and (v) laser surface nitriding followed by selective etching. The HA coatings were pulsed laser deposited at different water-vapor pressures to determine the optimal processing conditions. The nitrided-etched specimen exhibits a three dimensional TiN dendritic network which promotes the adhesion between HA coating and titanium substrate. Among the specimens with different pre-treatments, the adhesion strength of HA is the highest for the nitrided-etched specimen, reaching about twice that for the mirror-finished specimen. Thin-film X-ray diffraction shows a high degree of crystallinity for the PLD deposited HA. According to energy-dispersive X-ray analysis, the Ca/P ratio of the deposited HA reaches an approximate value of 1.7, similar to that of the HA target. Scanning-electron microscopy reveals that the deposited HA is about 4 μm in thickness. Growth of apatite was rapidly induced on the HA coated specimens when immersed in Hanks' solution for 4 days, indicating that the PLD HA coating is highly bone bioactive. This could be partly due to the high wettability of the PLD HA surface.     

The affect of densification and dehydroxylation on the mechanical properties of stoichiometric hydroxyapatite bioceramics

This paper reports the effects of processing densification on the mechanical properties of hydroxyapatite bioceramics. Densification of synthetic hydroxyapatite is conducted in the range 1000-1300 °C. X-ray diffraction and SEM microscopy are used to check the microstructure transformations. Vickers hardness, toughness and Young's modulus are analyzed versus the density and grain size. The sintering temperature and the particle size influence strongly the densification and the resulting mechanical properties. In addition, the critical sintering temperature appears around 1200 °C and the declined strength at the temperature up to 1200 °C is found sensitive to the dehydroxylation process of hydroxyapatite.     

Preparation of hydroxyapatite rod-like crystals by protein precursor method

Hydroxyapatite (HAP) rod-like crystals were successfully prepared by thermolysis of bovine serum albumin (BSA)/calcium-phosphate (CaP) colloidal precursors. The precursors were obtained by precipitation method from Ca(H₂PO₄)₂ and Ca(OH)₂, in which BSA was added as regulation additive and ultrasound irradiation was utilized as assistant technology. The properties of the precursors, such as size distribution, morphology, thermodynamic changes, were determined by DLS, SPM and TGA-DTA. The characterization results from DLS, SPM, TG-DTA, XRD and SEM indicated that BSA interacted with CaP particles and formed about 7-130 nm BSA/CaP hybrid colloidal particles between 2 and 4 g/L of BSA concentration. With the increasing of sintering temperature, BSA disintegrated and burned out, and rod-like HAP crystals formed at about 600 °C. With the increasing of BSA concentration, the phase composition of products did not change and the HAP crystals became more uniform and smaller. The ratio of length to width ranged from 7.6 to 12 at 4 g/L BSA concentration. This method provides for a controllable bottom-up fabrication of HAP rod-like crystals.     

Cavitation erosion behavior of laser-clad Ni-Cr-Fe-WC on brass

Laser surface modification of brass with an alloy-ceramic composite powder Ni-Cr-Fe-WC was studied using a two-step process, with powder preplacement followed by laser irradiation. For preplaced coatings of a few 100 μm thick, successfully cladding/alloying was achieved at a laser (CW Nd:YAG) energy density in the range 60-100 J/mm². Under proper processing conditions, the cavitation erosion resistance was increased by a factor of 9.1. This large increase was attributed to the formation of a Ni-rich matrix reinforced by precipitated carbides and tightly bound WC particles.     

Preparation of graphene nanosheet/alumina composites by spark plasma sintering

Graphene nanosheet/alumina composite has been prepared by spark plasma sintering. A homogeneous distribution of nanosheets in an alumina matrix could be obtained by the electrostatic attraction between graphite oxide and alumina particles and their subsequent reduction. The introduction of graphene nanosheet leads to refinement of grain size of alumina after hot pressing. The experimental results have shown that the fracture toughness and conductivity of the graphene nanosheet/alumina composite are about 53% and 13 orders of magnitude higher than those of unreinforced alumina material, respectively.     

Microstructure and mechanical properties of small amounts of In2O3 reinforced Pb(ZrxTi1−x)O3 ceramics

Piezoelectric Pb(Zr_xTi_1−x)O₃ (PZT) ceramics with small amount (0.5-2.0 wt.%) of In₂O₃ are prepared by conventional sintering method. Based on X-ray diffraction analysis, the tetragonality of PZT matrix decreases with In₂O₃ content, indicating that In₂O₃ diffuses into PZT matrix. The microstructure of PZT matrix is significantly refined by doping small amounts of In₂O₃. The grain size reduction and the matrix grain boundary reinforcement are the probable mechanism responsible for the high strength and hardness in the PZT/In₂O₃ materials. The enhancement in Young’s modulus is attributed to In³⁺ substitution. The decreased tetragonality with In₂O₃ addition results in less crack energy absorption by domain switching and, hence, causes the small reduction in fracture toughness.     

Influence of cobalt phase on thermal shock resistance of Al2O3-TiC composites evaluated by indentation technique

Cobalt-coated Al₂O₃ and TiC powders were prepared using an electroless method to improve resistance to thermal shock. The mixture of cobalt-coated Al₂O₃ and TiC powders (about 70 wt.% Al₂O₃-Co + 30 wt.% TiC-Co) was hot-pressed into an Al₂O₃-TiC-Co composite. The thermal shock properties of the composite were evaluated by indentation technique and compared with the traditional Al₂O₃-TiC composite. The composites containing 3.96 vol.% cobalt exhibited better resistance to crack propagation, cyclic thermal shock and higher critical temperature difference (ΔT_c). The calculation of thermal shock resistance parameters (R parameters) shows that the incorporation of cobalt improves the resistance to thermal shock fracture and thermal shock damage. The thermal physic parameters are changed very little but the flexure strength and fracture toughness of the composites are improved greatly by introducing cobalt into Al₂O₃-TiC (AT) composites. The better thermal shock resistance of the composites should be attributed to the higher flexure strength and fracture toughness.     

Indium tin oxide films deposited by thermionic-enhanced DC magnetron sputtering on unheated polyethylene terephthalate polymer substrate

Indium tin oxide thin films were deposited onto polyethylene terephthalate substrates via thermionic enhanced DC magnetron sputtering at low substrate temperatures. The structural, optical and electrical properties of these films are methodically investigated. The results show that compared with traditional sputtering, the films deposited with thermionic emission exhibit higher crystallinity, and their optical and electrical properties are also improved. Indium tin oxide films deposited by utilizing thermionic emission exhibit an average visible transmittance of 80% and an electrical resistivity of 4.5 × 10⁻⁴ Ω cm, while films made without thermionic emission present an average visible transmittance of 74% and an electrical resistivity of 1.7 × 10⁻³ Ω cm.     

Shape deformation and texture development of consolidated Ca α-SiAlON ceramics prepared by hot-forging

Consolidated Ca α-SiAlON ceramics with gradually varying microstructure and property was prepared by hot-forging. The shape deformation as well as texture development of the sample during forging was studied in detail. It was found that the forging process promoted the growth of elongated α-SiAlON grains and enhanced their preferred orientation with the longitude perpendicular to the pressing force. The strong texture offered the hot-forged sample an increased fracture toughness of 7.9 MPa m^1/2, which was primarily attributed to the pull-out and debonding behaviors of elongated grains.     

The effect of carbon nanotubes microstructures on reinforcing properties of SWNTs/alumina composite

Alumina reinforced with 1 wt% single-wall carbon nanotubes (SWNTs) was fabricated by hot-pressing. The fracture toughness of SWNTs/Al₂O₃ composite reaches 6.40 ± 0.3 MPa m^1/2, which is twice as high as that of unreinforced alumina. Nanoindentation introduced controlled cracks and the damage were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SWNTs reinforcing mechanisms including CNT pullout, CNT fracture, CNT bridging and crack deflection were directly observed, and the relationship between carbon nanotubes microstructures in the matrix and mechanical properties was also discussed in detailed.     

Synthesis of nanostructured SiC using the pulsed laser deposition technique

We report the new results on the direct synthesis of nanostructured silicon carbide (SiC) materials using the pulsed laser deposition technique. Scanning electron microscopy images revealed that SiC nanoholes, nanosprouts, nanowires, and nanoneedles were obtained. The crystallographic structure, chemical composition, and bond structure of the nanoscale SiC materials were investigated using X-ray diffraction, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and Raman scattering spectroscopy. The transverse optical mode and longitudinal optical mode in Raman spectra were found to become sharper as the substrate temperature was increased, while the material structure evolved from amorphous to crystalline.     

Influence of oxygen pressure on elastic strain and excitonic transition energy of ZnO epilayers prepared by pulsed laser deposition

High quality ZnO epilayers (χ_min ∼ 10%) were prepared on Al₂O₃ (0 0 0 1) substrates at a temperature of 750 °C by pulsed laser deposition (PLD) with oxygen pressure of 0.015, 0.15, 1.5, and 15 Pa. The best crystalline quality and strongest intensity of UV photoluminescence were observed on ZnO layer with oxygen pressure of 15 Pa. It is probable due to the higher oxygen pressure lessens oxygen deficiency in the film. The tetragonal distortion e_T, which is caused by elastic strain in the epilayer, was determined by Rutherford backscattering/channeling. It reduces as a whole (from 0.93 to 0.65%) with the increase of oxygen pressure from 0.015 to 15 Pa and the excitonic transition energy simultaneously shows a weak blue shift.