Orientation selective growth of MgO films on Si (100) by pulsed laser deposition

Selective growth of single-oriented (110), (100) and (111) MgO films on Si (100) substrates without buffer layers was obtained via a two-step method by pulsed laser deposition. It was found that the orientation of the films was determined at the initial deposition stage by the substrate temperature only. The ambient pressure during deposition, the laser fluence and the etching of the Si substrates have no apparent effect on the orientation of the films, but affect their crystalline quality. Under the present deposition conditions, the surfaces of all three different single-oriented films were very smooth and devoid of any particulates. Received: 23 January 2001 / Accepted: 6 June 2001 / Published online: 2 October 2001     

Growth of completely (110)-oriented Pt film on Si (100) by using MgO as a buffer by pulsed laser deposition

(110)-textured MgO films were grown on Si (100) with etching and without etching by pulsed laser deposition. The deposited MgO films were shown to be droplets-free. The MgO film was used as a buffer layer to further grow Pt film on Si (100). A completely (110)-oriented Pt film was obtained on such a buffer layer and its surface is very smooth with a roughness of about 7.5 nm over 5×5 μm. This can be used as a new oriented Pt electrode on silicon for devices. Received: 23 January 2001 / Accepted: 27 April 2001 / Published online: 27 June 2001     

Growth of a textured quasicrystalline phase in Ti-Ni-Zr films prepared by pulsed laser deposition

The preparation in thin film form of the known icosahedral phase in Ti-Ni-Zr bulk alloys has been investigated as a function of substrate temperature. Films were deposited by pulsed laser deposition on sapphire substrates at temperatures ranging from room temperature to 350 °C. Morphological and structural modifications have been followed by grazing-incidence and θ–2θ X-ray diffraction, transmission electron diffraction and imaging. Chemical composition has been analyzed by electron probe microanalysis. The in-depth variation of composition has been studied by secondary neutral mass spectroscopy. We show that pulsed laser deposition at 275 °C makes the formation of a 1-μm-thick film of Ti-Ni-Zr quasicrystalline textured nanocrystallites possible. Received: 7 June 2001 / Accepted: 18 February 2002 / Published online: 3 June 2002 RID="*" ID="*"Corresponding author. Fax: +33-3/8357-6300, E-mail: brien@mines.u-nancy.fr     

Optical properties of SrTiO<Subscript>3</Subscript> thin films by pulsed laser deposition

SrTiO₃ thin films were prepared on a fused-quartz substrate by pulsed laser deposition (PLD). Dense and homogeneous films with a thickness of 260 nm were prepared. Optical constants (refractive index n and extinction coefficient k) were determined from the transmittance spectra using the envelope method. The optical band gap energy of the films was found to be 3.58 eV, higher than the 3.22 eV for bulk SrTiO₃, attributable to the film stress exerted by the substrate. The dispersion relation of the refractive index vs. wavelength follows the single electronic oscillator model. The refractive index and the packing density for the PLD-prepared SrTiO₃ thin films are higher than those for the SrTiO₃ films prepared by physical vapor deposition, sol–gel and RF sputtering. Received: 18 March 2002 / Accepted: 7 October 2002 / Published online: 8 January 2003 RID="*" ID="*"Corresponding author. Fax: +86-25/359-5535, E-mail: mszhang@nju.edu.cn     

Dependence of the sp3 bond fraction on the laser wavelength in thin carbon films prepared by pulsed laser deposition

3 bonds in the carbon films prepared by pulsed laser deposition of carbon obtained from graphite was investigated by electron energy loss spectroscopy (EELS) and X-ray photoelectron spectroscopy (XPS). The fraction of sp³ bonds increased with a decreasing laser wavelength. Energetic C⁺ ion species were effectively produced by using a short-wavelength laser. The sp³ bond fraction increased with an increasing amount of energetic C⁺ ion species. The fractions of sp³ bonds in the carbon film were 80%, 42%, 26% and 15% at wavelengths of 193, 248, 532 and 1064 nm, respectively. Received: 28 October 1997/Accepted:29 October 1997     

Growth of stoichiometric and textured LiNbO3 films on Si by pulsed laser deposition

Laser ablation of single-crystal LiNbO₃ in a gas environment is used to grow films on (100) Si substrates heated to 650 °C. The film composition and crystallinity are studied as a function of the nature (reactive, O₂, or inert, Ar) and pressure of the gas environment applied during deposition and cooling-down processes, the laser energy density and the target–substrate distance. Experimental results show that a gas pressure close to 1 mbar is required to produce stoichiometric films in either O₂ or Ar. The modification of the laser energy density and the target–substrate distance allows us to improve the crystallinity of the films that become textured along the (006) direction. The influence of the experimental parameters on the film properties is discussed in the frame of the formation of a blast wave, that leads to the focusing of the expanding Li species and thus, to the increase of the Li content in the films. Received: 8 February 2001 / Accepted: 9 February 2001 / Published online: 3 May 2001     

Production of biologically inert Teflon thin layers on the surface of allergenic metal objects by pulsed laser deposition technology

Allergic-type diseases are current nowadays, and they are frequently caused by certain metals. We demonstrated that the metal objects can be covered by Teflon protective thin layers using a pulsed laser deposition procedure. An ArF excimer laser beam was focused onto the surface of pressed PTFE powder pellets; the applied fluences were 7.5–7.7 J/cm². Teflon films were deposited on fourteen-carat gold, silver and titanium plates. The number of ablating pulses was 10000. Post-annealing of the films was carried out in atmospheric air at oven temperatures between 320 and 500 °C. The thickness of the thin layers was around 5 μm. The prepared films were granular without heat treatment or after annealing at a temperature below 340 °C. At 360 °C a crystalline, contiguous, smooth, very compact and pinhole-free thin layer was produced; a melted and re-solidified morphology was observed above 420 °C. The adhesion strength between the Teflon films and the metal substrates was determined. This could exceed 1–4 MPa depending on the treatment temperature. It was proved that the prepared Teflon layers can be suitable for prevention of contact between the human body and allergen metals and so for avoidance of metal allergy. Received: 12 June 2002 / Accepted: 13 June 2002 / Published online: 4 November 2002 RID="*" ID="*"Corresponding author. E-mail: bhopp@physx.u-szeged.hu     

Diamond-like-carbon films produced by magnetically guided pulsed laser deposition

We have compared the quality of carbon films deposited with magnetically guided pulsed laser deposition (MGPLD) and conventional pulsed laser deposition (PLD). In MGPLD, a curved magnetic field is used to guide the plasma but not the neutral species to the substrate to deposit the films while, in conventional PLD, the film is deposited with a mixture of ions, neutral species and clusters. A KrF laser pulse (248 nm) was focused to intensities of 10 GW/cm² on a carbon source target and a magnetic field strength of 0.3 T was used to steer the plasma around a curved arc to the deposition substrate. Electron energy loss spectroscopy was used in order to measure the fraction of sp³ bonding in the films produced. It is shown that the sp³ fraction, and hence the diamond-like character of the films, increased when deposited only with the pure ion component by MGPLD compared with films produced by the conventional PLD technique. The dependence of film quality on the laser intensity is also discussed. Received: 7 December 2000 / Accepted: 20 August 2001 / Published online: 2 October 2001     

ZnO thin films on Si(1 1 1) grown by pulsed laser deposition from metallic Zn target

ZnO thin films with highly c-axis orientation have been fabricated on p-type Si(1 1 1) substrates at 400 °C by pulsed laser deposition (PLD) from a metallic Zn target with oxygen pressures between 0.1 and 0.7 mbar. Experimental results indicate that the films deposited at 0.3 and 0.5 mbar have better crystalline and optical quality and flatter surfaces than the films prepared at other pressures. The full width at half maximum (FWHM) of (0 0 0 2) diffraction peak decreases remarkably from 0.46 to 0.19° with increasing annealing temperature for the film prepared at 0.3 mbar. In photoluminescence (PL) spectra at room temperature, the annealed film at 700 °C exhibits a smaller ultraviolet (UV) peak FWHM of 108 meV than the as-grown film (119 meV). However, an enhanced deep-level emission is observed. Possible origins to above results are discussed.     

Characterization of defect type and dislocation density in double oxide heteroepitaxial CeO2/YSZ/Si(001) films

In order to qualitatively and quantitatively analyze the structural defects including the defect types and their concentrations in oxide heteroepitaxial films, a new X-ray rocking-curve width-fitting method was used in the case of doubleCeO₂/YSZ/Si (YSZ=yttria-stabilized ZrO₂) films that were prepared by pulsed laser deposition. Two main defect types, angular rotation and oriented curvature, were found in both CeO₂ and YSZ. Dislocation densities of CeO₂ and YSZ, which were obtained from the angular rotations, are functions of the YSZ thickness. A distinct two-step correlation between dislocation densities of CeO₂ and YSZ was found that as the dislocation density of YSZ is higher than 2.4×10¹¹ cm^-2, the dislocation density of CeO₂ shows a high sensitivity with that of YSZ compared with the low relativity in lower dislocation density (<2.4×10¹¹ cm^-2). In addition, YSZ always has higher dislocation densities and oriented curvatures than CeO₂ in each specimen, which can be attributed to the smaller mosaic domain sizes in YSZ than in CeO₂ as observed by high-resolution transmission electron microscopy. Received: 12 August 2002 / Accepted: 14 August 2002 / Published online: 4 December 2002 RID="*" ID="*"Corresponding author. Fax: +81-3/5734-3369, E-mail: chun_hua_chen@hotmail.com     

Epitaxial growth of yttria-stabilised zirconia buffer layers on X-cut LiNbO3 for superconducting electrodes

We report on the epitaxial growth of yttria-stabilised zirconia (YSZ) buffer layers on X-cut LiNbO₃ (LNO) single crystals by pulsed laser deposition. Despite the low chemical stability of the substrates at high temperature, high quality fully reproducible films were obtained over a relatively broad range of processing conditions. The films were (00h) out-of-plane single oriented and the in-plane edge of the YSZ unit cell was aligned with the polar axis of the LNO. However, the YSZ deposition also promoted the formation of the compound LiNb₃O₈. This compound is epitaxial and located at the interface. The homogeneous YSZ film presents a uniform surface, free of outgrowths and with a low roughness. These characteristics are suitable for the epitaxial growth of other oxides, as has been demonstrated with the preparation of YBa₂Cu₃O₇/CeO₂/YSZ/LNO heterostructures. The superconducting YBa₂Cu₃O₇ films were epitaxial, with the c axis perpendicular to the surface and single in-plane orientation, and presented good transport properties (critical temperatures around 86 K and critical current densities close to 10⁶ A/cm² at 77 K). Received: 5 April 2001 / Accepted: 30 July 2001 / Published online: 30 October 2001     

Laser–MBE growth of high-quality ZnO thin films on Al2O3(0001) and SiO2/Si(100) using the third harmonics of a Nd:YAG laser

High-quality ZnO thin films were grown on single-crystalline Al₂O₃(0001) and amorphous SiO₂/Si(100) substrates at 400–640 °C using laser molecular beam epitaxy. For film growth, the third harmonics of a pulsed Nd:YAG laser were illuminated on a ZnO target. The ZnO films were epitaxially grown on Al₂O₃(0001) with the narrow X-ray diffraction full width at half maximum (FWHM) of 0.04° and the films on SiO₂/Si(100) exhibited a preferred c-axis orientation. Furthermore, the films exhibited excellent optical properties in photoluminescence (PL) measurements with very sharp excitonic and weak deep-level emission peaks. At 15 K, PL FWHM values of the films grown on Al₂O₃(0001) and SiO₂/Si(100) were 3 and 18 meV, respectively. Received: 8 May 2001 / Accepted: 18 September 2001 / Published online: 20 December 2001     

Microstructures and dielectric properties of compositionally graded (Ba1-xSrx) TiO3 thin films prepared by pulsed laser deposition

Compositionally graded (Ba_1-xSr_x)TiO₃ (BST) (x:0.0∼0.25) thin films were grown on Pt (111)/TiO₂/SiO₂/Si (100) substrates using layer-by-layer pulsed laser deposition in the temperature range 550–650 °C. Both downgraded (Ba/Sr ratio varying from 100/0 at the bottom surface to 75/25 at the top surface) and upgraded (Ba/Sr ratio varying from 75/25 at the bottom surface to 100/0 at the top surface) BST films were prepared. Their microstructures were systematically studied by X-ray diffractometry and scanning electron microscopy. A grain morphology transition from large ‘rosettes’ (>0.30 μm) to small compact grains (70–110 nm) was observed in the downgraded BST films as the deposition temperature was increased from 550 to 650 °C. No such grain morphology transition was detected in the upgraded BST films. Dielectric measurements with metal electrodes revealed an enhanced dielectric behavior in the downgraded films. This enhancement is mainly attributed to the large compressive stress field built up near the interface between the downgraded film and substrate. Furthermore, the BaTiO₃ layer in the downgraded BST films not only serves as a bottom layer but also as an excellent seeding layer for enhancing the crystallization of the subsequent film layers in the downgraded films. Received: 10 December 2001 / Accepted: 12 March 2002 / Published online: 19 July 2002 RID="*" ID="*"Corresponding author. Fax: 86-25/359-5535, E-mail: xhzhu@public1.ptt.js.cn     

Distinct correlation between CeO2 and YSZ in out-of-plane and in-plane mosaic dispersions of heteroepitaxial CeO2/YSZ/Si(001) films

The structural correlations including the lattice constants and the mosaic dispersions between CeO₂ and yttria-stabilized ZrO₂ (YSZ) in CeO₂/YSZ/Si(001) heteroepitaxial films have been investigated by out-of-plane and in-plane X-ray-diffraction techniques. The distinct linear correlations of the full width at half-maximum (FWHM) of the ω scan between CeO₂ and YSZ have been found in both directions. CeO₂ always has a 0.7° lower FWHM of the ω scan than YSZ in the out-of-plane direction, but has a 2.6° higher FWHM in the in-plane direction. A possible relationship between the out-of-plane and in-plane FWHMs of the ω scans has been demonstrated with a lattice-rotation model. Besides, the lattice constants of CeO₂ are dependent on the FWHMs of the YSZ ω scans: as the FWHM is below 3.5°, CeO₂ has a tetragonal distortion, and as the FWHM is higher than 3.5°, CeO₂ exhibits a cubic structure without distortion. The results are of great interest, both for the fundamental understanding of the film-growth mechanisms and for potential applications. Received: 11 September 2000 / Accepted: 5 June 2001 / Published online: 30 August 2001     

Influence of inert gas pressure on deposition rate during pulsed laser deposition

The deposition rates of permalloy and Ag are monitored during pulsed laser deposition in different inert gas atmospheres. Under ultrahigh vacuum conditions, resputtering from the film surface occurs due to the presence of energetic particles in the plasma plume. With increasing gas pressure, a reduction of the particle energy is accompanied with a decrease of resputtering and a rise in the deposition rate for materials with high sputtering yield. In contrast, at higher gas pressures, scattering of ablated material out of the deposition path between target and substrate is observed, leading to a decrease in the deposition rate. While in the case of Xe and Ar these processes strongly overlap, they are best separated in He. A He pressure of about 0.4 mbar should be used to reduce the kinetic energy of the deposited particles, to reach the maximum deposition rate and to avoid implantation of the particles. This is helpful for the preparation of stoichiometric metallic alloy films and multilayers with sharp interfaces. Received: 27 March 2002 / Accepted: 3 April 2002 / Published online: 5 July 2002     

Characterization of ablation plumes and carbon nitride films produced by reactive pulsed laser deposition in the presence of a magnetic field

x ) films in a nitrogen atmosphere within the range 5×10^-4–4×10^-1 Torr. In the presence of a magnetic field, the emission intensities of N₂ (second positive system) and CN species in the graphite ablation plumes were altered significantly, depending on the pressure of the N₂ environment. Corresponding to an intense CN emission, a magnetic field-induced enhancement of N incorporation – for example, up to 37% at an N₂ pressure of 300 mTorr – and the formation of sp³ tetrahedral CN bonding were both observed in the films. This suggests that the arrival of CN species at the substrate surface with kinetic energies is important for film deposition. Received: 27 August 1997/Accepted: 8 September 1997     

Growth of InN films on spinel substrates by pulsed laser deposition

We have grown InN films on MgAl₂O₄(111) substrates with atomically flat surfaces using pulsed laser deposition (PLD) and compared their structural properties with those grown on (Mn,Zn)Fe₂O₄(111) substrates. It has been revealed that InN(0001) films grow on MgAl₂O₄(111) with an in‐plane epitaxial relationship of InN[1 00] // MgAl₂O₄[1 0], achieving a lattice mismatch minimum. The InN films exhibited a clear sixfold rotational symmetry, without 30° rotational domains and with a full width at half maximum value of the InN 0002 rocking curve being 17.5 arcmin. Comparison between InN films grown on MgAl₂O₄ and those on (Mn,Zn)Fe₂O₄ led us to conclude that suppression of the interfacial reactions between the InN films and the substrate is inherently important to obtain high quality InN on substrates with a spinel structure. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Studies of interface structures of W films grown on patterned and bare Si(100) by TEM

+ Si(100) and bare Si(100) wafers by low pressure chemical vapour deposition (LPCVD) at 230–280 °C. The films were investigated by transmission electron microscopy (TEM). The cross-sectional TEM samples of W/Si(100) exhibited a fine scale interface roughness, which was attributed to the surface preparation. Irregular W plug structures were observed depending on the predeposition procedures. It was observed that an insufficient deposition of W films on the contact surface leads to the presence of aluminium around and underneath the plugs. This was observed by energy dispersive X-ray spectrometry (EDX). A study, using conventional electron diffraction, confirmed that no silicides formed at the interfaces of W-bare Si(l00) wafers. Received: 16 December 1996/Accepted: 6 May 1997     

Raman characteristics of carbon nitride synthesized by nitrogen-ion-beam-assisted pulsed laser deposition

Raman characteristics of carbon nitride films synthesized by nitrogen-ion-beam-assisted pulsed laser deposition were investigated. In addition to the D (disorder) band and G (graphitic) band commonly observed in carbon nitride films, two Raman bands located at 1080–1100 and 1465–1480 cm^-1 were found from our carbon nitride films. These two bands were well matched with the predicted Raman frequencies for βC₃N₄ and the observed Raman bands reported for carbon nitride films, indicating their relation to carbon-nitrogen stretching vibrations. Furthermore, the relative intensity ratio of the two Raman bands to the D and G bands increased linearly with increasing nitrogen content of the carbon nitride films. Received: 30 October 2000 / Accepted: 5 February 2001 / Published online: 2 October 2001     

Resonant infrared pulsed laser deposition of thin biodegradable polymer films

Thin films of the biodegradable polymer poly(DL-lactide-co-glycolide) (PLGA) were deposited using resonant infrared pulsed laser deposition (RIR-PLD). The output of a free-electron laser was focused onto a solid target of the polymer, and the films were deposited using 2.90 (resonant with O-H stretch) and 3.40 (C-H) μm light at macropulse fluences of 7.8 and 6.7 J/cm², respectively. Under these conditions, a 0.5-μm thick film can be grown in less than 5 min. Film structure was determined from infrared absorbance measurements and gel permeation chromatography (GPC). While the infrared absorbance spectrum of the films is nearly identical with that of the native polymer, the average molecular weight of the films is a little less than half that of the starting material. Potential strategies for defeating this mass change are discussed. Received: 22 August 2001 / Accepted: 23 August 2001 / Published online: 17 October 2001