Interface reactions in [Fe/B]<Subscript>n</Subscript> multilayers: a way to tune from crystalline/amorphous layer sequences to homogeneous amorphous Fe<Subscript>x</Subscript>B<Subscript>100-x</Subscript> films

[Fe/B]_{n ≥2} multilayers were prepared by thermal evaporation, ion-beam sputtering and laser ablation. By applying in situ electron spectroscopies (UPS, XPS) and monitoring the electrical resistance during layer growth, evidence could be provided for the occurrence of interface reactions within the range of studied deposition temperatures (77 K ≤T ≤300 K). These reactions result in amorphous Fe_xB_100-x phases, which are spatially restricted to a width of less than 3 nm at the original interface. The amorphicity of the reacted interlayers was unequivocally proven by additional high-resolution electron microscopy (HRTEM) and their characteristically changed magnetic properties. Due to the well-defined width of the interface reaction, homogeneous amorphous Fe_xB_100-x films can be obtained by reducing the individual Fe and B layer thicknesses to below the above reaction depth, while for larger thicknesses layer sequences of the crystalline/amorphous/crystalline type will result. Received: 30 January 2002 / Accepted: 31 January 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +49-731/502-2963, E-mail: hans-gerd.boyen@physik.uni-ulm.de     

Nanoscale effects in focused ion beam processing

Focused ion beams with diameters of 8 to 50 nm are used for material processing in the nanoscale regime. In this paper, effects of the ion beam–solid interaction determining the formation of small structures by ion-beam sputtering and chemically assisted material deposition and etching are investigated. In the case of decreasing feature size, angle-dependent sputtering, a non-constant sputter rate, and scattered ions play an important role. The impact on side-wall angle, aspect ratio, and shape of the bottom of the etched structures is discussed. In beam tail regions, these effects will be especially pronounced, leading to material swelling instead of material removal. Ion beam assisted etching and deposition will face additional effects. For small structures, gas depletion becomes a significant drawback. The impact on gas depletion and the competition with sputtering are discussed. Received: 21 August 2002 / Accepted: 21 August 2002 / Published online: 12 February 2003 RID="*" ID="*"Corresponding author. Fax: +49-9131/761360, E-mail: frey@iis-b.fhg.de     

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     

Formation of metal membranes by direct duplication of etched ion-track templates

A method for direct electrochemical metal duplication of pores in ion-track polymer membranes is described. It allows fabrication of metallic membranes using any metal, which is readily deposited by electroplating from aqueous solutions. The metal is deposited on one side of the template membrane, facing the anode, which is made conductive by a thin metal cladding layer. During electroplating, the lateral tapping of the pores is prevented by applying a counter-solution from the opposite non-metallized side of the plastic membrane, which increases dramatically the deposition overvoltage in the vicinity of the pore orifices. Such metallic membranes can be generated with pore diameters in the nano- and micrometer range and with densities from single pores up to 10⁶–10⁷ pores/cm². They can replace plastic filters in cases when an application of polymer material is not desirable. They could be advantageous particularly in catalysis as well as in biological science and technology. Further, they may be useful as apertures and collimators for different kinds of radiation. Received: 14 February 2002 / Accepted: 21 May 2002 / Published online: 22 November 2002 RID="*" ID="*"Corresponding author. Fax: +49-6159/712-179, E-mail: r.neumann@gsi.de     

Deposition of large-area, high-quality cubic boron nitride films by ECR-enhanced microwave-plasma CVD

Large-area, 1-μm-thick cubic boron nitride (cBN) films were deposited on (001) silicon substrates by electron-cyclotron-resonance-enhanced microwave-plasma chemical vapor deposition (ECR-MP CVD) in a mixture of He-Ar-N₂-BF₃-H₂ gases. With the assistance of fluorine chemistry in the gas phase and substrate reactions, the phase purity of the sp³-configuration was improved to over 85% at a reduced substrate bias voltage of -40 V. The grown films show clear Raman transversal optical (TO) and longitudinal optical (LO) phonon vibration modes, characteristic of cBN. Such Raman spectral characteristics are the first ever observed in cBN films prepared under ECR-MP CVD conditions. Received: 3 May 2002 / Accepted: 7 May 2002 / Published online: 22 November 2002 RID="*" ID="*"Corresponding author. Fax: +852-2788/7830, E-mail: apwjzh@cityu.edu.hk     

Pulsed laser deposition and in situ diagnostics of the process applied to shape-memory alloys

NiTi films deposited by pulsed laser ablation on Si/SiO₂ are shown to exhibit structural and functional properties related to the shape-memory effect. Film characterization suggests that relevant temperatures for the solid-to-solid transformation responsible for the shape memory are in substantial agreement with those of the bulk target material, demonstrating a good congruency of the deposition process. Besides the technological interest for this class of thin films, our findings point out the suitability of laser ablation for metal alloy deposition. An investigation based on in situ ion-mass spectroscopy and covariance mapping analysis allows us to determine the main vapor-phase processes leading to the formation of stoichiometric clusters expected to play a relevant role in assisting the growth of NiTi thin films. Received: 6 August 2001 / Accepted: 11 April 2002 / Published online: 4 November 2002 RID="*" ID="*"Corresponding author. Fax: +39-50/2214-333, E-mail: fuso@df.unipi.it     

High refractive index and transparent heavy metal oxide glassy thin films

Heavy metal oxide thin films of the ternary system Nb₂O₅–GeO₂–PbO have been prepared by pulsed laser deposition in an O₂ environment from either glassy or crystalline bulk samples. The range of ([Pb]+[Nb]) content in which the films are optically homogeneous and transparent is much broader (0.5–1.0) than that of the bulk samples considered in the present work (0.55–0.62). The imaginary part of the refractive index is very low in all cases (k<10^-3), whereas the real part increases linearly with the ([Pb]+[Nb]) content up to values as high as 2.35. The optical energy gap has been found to be strongly dependent on [Pb], whereas it is almost independent of [Nb]. This dependence is discussed in terms of the role of Pb and Nb as network modifiers or formers. Received: 5 August 2002 / Accepted: 8 August 2002 / Published online: 17 December 2002 RID="*" ID="*"Corresponding author. Fax: +34-91/564-5557, E-mail: j.gonzalo@io.cfmac.csic.es     

Three-dimensional structuring of sapphire by sequential He+ ion-beam implantation and wet chemical etching

We present a method for the selective two- and three-dimensional patterning of sapphire using light ion-beam implantation to generate severe lattice damage to depths exceeding 1 μm and subsequent selective wet chemical etching of the damaged regions by hot H₃PO₄. C-cut sapphire crystals were implanted through contact masks using ion fluences of 1×10¹⁶ to 5×10¹⁷ He⁺/cm² and energies up to 400 keV. The etching process is characterized by a high selectivity and a rate of approximately 19 nm/min. Whereas an implantation that produces a continuously damaged pathway results in complete etching from the surface, sole in-depth implantation using only high-energy ions leads to under-etching of the crystalline surface layer. By a combination of these processes we have fabricated three-dimensional structures such as channels and bridges in sapphire. Received: 14 October 2002 / Accepted: 15 October 2002 / Published online: 26 February 2003 RID="*" ID="*"Corresponding author. Fax +41-21/693-3701, E-mail: aurelian.crunteanustanescu@epfl.ch     

Hybrid pulsed laser deposition and Si-surface-micromachining process for integrated TiC coatings in moving MEMS

Titanium carbide (TiC) is one of the preferred coatings for improving the performance of macroscopic moving mechanical components due to its established wear-resistance. Pulsed laser deposition (PLD) is an excellent method for depositing TiC, because unlike any other deposition process for TiC, PLD offers the capability of producing high-quality films even at room temperature. Using a modified PLD technique, especially designed for the deposition of particulate-free films, TiC coatings have been deposited at room temperature on silicon (Si) and on several types of thin films typically employed for fabricating microelectromechanical systems (MEMS). Our results demonstrate that TiC coatings also offer a high wear-resistance to Si surfaces, which in turn has led to our application of TiC to “moving” Si MEMS devices. The performance of moving Si MEMS devices is limited by their poor operational lifetimes, which have been attributed to the excessive wear at sliding Si interfaces. The work presented here describes a hybrid process, whereby PLD is used in conjunction with a user-friendly Si surface micromachining scheme for inserting wear-resistant TiC coatings between critical sliding Si interfaces in MEMS devices. This paper describes the properties of PLD-TiC for MEMS and the hybrid PLD-surface micromachining process for the integration of TiC coatings into Si MEMS. Received: 23 January 2003 / Accepted: 8 February 2003 / Published online: 28 May 2003 RID="*" ID="*"Corresponding author. Fax: +1-310/563-7614, E-mail: gouri.radhakrishnan@aero.org     

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     

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     

Low-threshold field electron emission of Si micro-tip arrays produced by laser ablation

Low-threshold field electron emission (FEE) is reported for periodic arrays of micro-tips produced by laser ablation of Si wafers. The best samples show emission at threshold fields as low as 4–5 V/μm for n-type Si substrates and of 1–2 V/μm for p-doped Si substrates, as measured with a flat-screen technique. Auger electron spectroscopy and X-ray electron spectroscopy reveal island-like deviation of the SiO₂ stoichiometry on the tip surfaces, with lateral dimensions of less than 100 nm. Microscopic studies using a special field-emission STM show that the emission originates from well-conducting regions of sub-micron size. The experimental data suggest FEE from the tip arrays by a geometric field enhancement of both the individual micro-tip and the narrow conducting channels in the tip body. Received: 3 May 2002 / Accepted: 1 July 2002 / Published online: 28 October 2002 RID="*" ID="*"Corresponding author. Fax: +7-095/135-82-34, E-mail: shafeev@kapella.gpi.ru     

Femtosecond regenerative amplification in Cr:forsterite at 5–10 kHz

We developed a high-power oscillator–regenerative amplifier femtosecond laser system. Based on chromium-doped forsterite. The system is operating near 1.25 μm at a 5–10 kHz repetition rate. Chirped-pulse amplification produced 0.86 W (0.75 W) of average power, or 465 mW (400 mW) after compression at 5 kHz (10 kHz). Nearly bandwidth-limited pulses of duration 135 fs (shortest) and 150 fs (typical) are available with an energy of 93 μJ and 40 μJ at 5 and 10 kHz, respectively. Received: 7 June 2002 / Published online: 15 November 2002 RID="*" ID="*"Corresponding author. Fax: +49-30/63921289, E-mail: petrov@mbi-berlin.de     

Inhomogeneity of calcium phosphate coatings deposited by laser ablation at high deposition rate

Calcium phosphate coatings were deposited with a KrF excimer laser onto titanium alloy to study their homogeneity. Deposition was performed at a high deposition rate under a water vapour atmosphere of 45 Pa and at a substrate temperature of 575 °C. Samples were also submitted to annealing under the same conditions of deposition for different times just after deposition. The effects of the annealing were also investigated. The morphology of the coatings was studied by scanning electron microscopy. Their structure and phase distribution was analysed by X-ray diffractometry and infrared and micro-Raman spectroscopies. Besides the non-uniform thickness, the results reveal an inhomogeneity in the spatial distribution of calcium phosphate phases in the coatings. The phase distribution can be almost completely correlated with the deposition rate. High deposition rates (0.5 nm/pulse) occurring in the centre of deposition results in the formation of amorphous calcium phosphate, while lower deposition rates favour the presence of hydroxyapatite and alpha tricalcium phosphate. At intermediate deposition rates, beta tricalcium phosphate is found, probably because the superimposed effect of energetic particles bombardment. The annealing process promotes the crystallisation of the amorphous material. The importance of the deposition rate in the phases obtained is stated after comparing these results with a previous work where homogeneous hydroxyapatite coatings were obtained under the same conditions of laser fluence, temperature and pressure, but at lower deposition rates. Received: 22 November 2001 / Accepted: 12 March 2002 / Published online: 5 July 2002 RID="*" ID="*"Corresponding author. Fax: +34-93/402-1138, E-mail: jmfernandez@fao.ub.es     

Investigation of the interaction of evaporated aluminum with vapor deposited Teflon AF films via X-ray photoelectron spectroscopy

The interfacial bonding and mixing between evaporated aluminum and a vapor deposited Teflon AF (abbreviated to AF) film have been investigated with X-ray photoelectron spectroscopy. Graphite carbon (C–C), and aluminum carbide (Al–C), oxide (Al–O–C) and fluoride (Al–F) are formed when aluminum atoms are deposited on to the AF film. With increasing deposition of aluminum, the concentrations of these newly formed components increase gradually. Moreover, in situ annealing results in remarkable increases in the C–C, Al–C, Al–O–C and Al–F configurations and a decrease in metallic aluminum. No significant diffusion of aluminum into the AF film was observed during the annealing. The Al compounds form a layer at the Al/AF interface that acts as an adhesion promoter and diffusion barrier. Received: 21 October 2002 / Accepted: 22 October 2002 / Published online: 15 January 2003 RID="*" ID="*"Corresponding author. Fax: +49-431/880-6229, E-mail: sjding@yahoo.com     

Ultra-sensitive mid-infrared cavity leak-out spectroscopy using a cw optical parametric oscillator

We report a portable, all-solid-state, mid-infrared spectrometer for trace-gas analysis. The light source is a continuous-wave optical parametric oscillator based on PPLN and pumped by a Nd:YAG laser at 1064 nm. The generated single-frequency idler output covers the wavelength region between 2.35 and 3.75 μm. With its narrow line width, this light source is suitable for precise trace-gas analysis with very high sensitivity. Using cavity leak-out spectroscopy we achieved a minimum detectable absorption coefficient of 1.2×10^-9 /cm (integration time: 16 s), corresponding, for example, to a detection limit of 300 parts per trillion ethane. This sensitivity and the compact design make this trace-gas analyzer a promising tool for various in situ environmental and medical applications. Received: 19 September 2002 / Published online: 15 November 2002 RID="*" ID="*"Corresponding author. Fax: +49-228/733-474, E-mail: frank.kuehnemann@iap.uni-bonn.de     

Property study of Si + -ion-implanted Nd:YVO 4 waveguides

Planar waveguides were formed in Nd:YVO₄ crystals by 3.0-MeV Si⁺-ion implantation at doses of 1×10¹³–1.5×10¹⁵ ions/cm² at room temperature. The effective refractive indices of the waveguide propagation modes were measured by using a prism-coupling method. It was found that the number of the propagation modes is dependent on the doses for the waveguides in Nd:YVO₄. The atom displacement in the near-surface region (about 2 μm beneath the surface) of the Nd:YVO₄ crystal induced by the implantation was simulated by using the TRIM 98 (transport and range of ions in matter) code. The possible reasons for the waveguide formation are discussed in a primary way. Received: 17 July 2002 / Revised version: 20 September 2002 / Published online: 11 December 2002 RID="*" ID="*"Corresponding author. Fax: +86-531-8565167, E-mail: drfchen@sdu.edu.cn     

Characteristics of SrBi2Ta2O9 ferroelectric films on GaAs with a TiO2 buffer layer

Mainly [115]-oriented SrBi₂Ta₂O₉ (SBT) films were prepared on GaAs(100) substrates with TiO₂ buffer layers. Both the SBT films and the TiO₂ buffer layers were deposited by pulsed laser deposition (PLD) using a KrF excimer laser. The depth profile of the constituent elements observed by Auger electron spectrometry (AES) shows no remarkable diffusion at both the interfaces between SBT and TiO₂ and between TiO₂ and the GaAs substrate. The electrical characteristics of the Pt/SBT/TiO₂/GaAs(100) structures show a ferroelectric hysteresis loop with a small remanent polarization (∼0.5 μC/cm²). Received: 1 March 2002 / Accepted: 3 March 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +86-25/3595535, E-mail: xhliu81@hotmail.com RID="**" ID="**"Present address: Data Storage Institute, DSI Building, 5, Engineering Drive 1 (off Kent Ridge Crescent, NUS) 117608 Singapore     

The synthesis of highly oriented GaN nanowire arrays

Highly oriented GaN nanowire arrays have been achieved by the catalytic reaction of gallium with ammonium. The resulting materials were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). SEM images show that the resulting materials are nanowire arrays with a uniform length of about 10 μm. XRD, EDS, TEM and SAED indicate that the nanowire arrays are single-crystal hexagonal GaN with a wurtzite structure. They have diameters of 10 to 20 nm. Received: 2 October 2002 / Accepted: 7 October 2002 / Published online: 17 December 2002 RID="*" ID="*"Corresponding author. E-mail: wwwangjc@sina.com     

The characteristics of surface acoustic waves on AlN/LiNbO3 substrates

The characteristics of surface-acoustic-wave (SAW) devices on various substrates were measured by a network analyzer in the temperature range from 0 to 80 °C. Based on the structure of IDT/AlN/LiNbO₃, it was revealed that the magnitude of the temperature coefficient of frequency (TCF) of a SAW on a LiNbO₃ substrate was significantly decreased due to the thickness increase of AlN thin film deposited on the LiNbO₃ substrate. The TCF of a SAW on an AlN/LiNbO₃ device was measured to be about -51 ppm/°C at h/λ=0.1, where h is the thickness of the AlN film and λ is the wavelength of the SAW. This indicates that the deposition of an AlN film on a LiNbO₃ substrate could improve the temperature stability, as compared with that of a SAW on a LiNbO₃ substrate (-73 ppm/°C). The SAW device on the ST-X quartz is shown to have a positive TCF as the AlN thin film is deposited on the surface of the ST-X quartz. In addition, the phase velocity (V_p) of the SAW on an AlN/LiNbO₃ substrate was significantly increased by the increase of AlN thickness (h/λ). Received: 14 October 2002 / Accepted: 15 October 2002 / Published online: 29 January 2003 RID="*" ID="*"Corresponding author. Fax: +886-7/525-4199, E-mail: ycc@ee.nsysu.edu.tw