Elastic modulus-density relationship for amorphous boron suboxide thin films

Boron suboxide thin films have been deposited on Si(100) substrates by reactive RF magnetron sputtering of a sintered B target in an Ar/O₂ atmosphere. Elastic recoil detection analysis was applied to determine the film composition and density. Film structure was studied by X-ray diffraction and transmission electron microscopy. The elastic modulus, measured by nanoindentation, was found to decrease as the film density decreased. The relationship was affected by tuning the negative substrate bias potential and the substrate temperature during film growth. A decrease in film density, by a factor of 1.55, caused an elastic modulus reduction by a factor of 4.5, most likely due to formation of nano-pores containing Ar. It appears evident that the large scattering in the published data on elastic properties of films with identical chemical composition can readily be understood by density variations. These results are important for understanding the elastic properties of boron suboxide, but may also be qualitatively relevant for other B-based material systems. Received: 22 February 2002 / Accepted: 11 April 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +46-13/288-918, E-mail: denmu@ifm.liu.se     

Transmission electron microscopy studies of femtosecond laser induced modifications in quartz

Cross-sectional transmission electron microscopy investigations of femtosecond laser induced sub-micrometer structural modifications inside crystalline quartz were carried out. Modifications from single laser shots and from lines built of overlapping shots were imaged. Both single laser shot modifications and line structures show an amorphous core surrounded by a disturbed crystalline structure. A strong strain field surrounding the central, irradiated, core is responsible for an increase of the refractive index. Finite element method calculations of the strain field show maxima on both sides of the irradiated core, which are in good agreement with optical measurements of the refractive-index change. Received: 29 September 2001 / Accepted: 9 July 2002 / Published online: 25 October 2002 RID="*" ID="*"Corresponding author. Fax: +49-3641/947792, E-mail: tatiana.gorelik@rz.uni-jena.de     

Sensors for scanning probe microscopy

Scanning probe microscopy is still suffering from reproducible fabrication of the corresponding sensors for mechanical, electrical, optical, thermal and chemical material characterisation with highest lateral and/or time resolution. For batch-fabrication techniques lithographic, dry etching and material problems have to be solved. Using such techniques, several types of cantilevers and tips including piezoresistive detection systems have been demonstrated world-wide for the first time. Only an overview is given here. Received: 2 September 2002 / Accepted: 6 November 2002 / Published online: 5 March 2003 RID="*" ID="*"Corresponding author. Fax: +49-561/804-4136, E-mail: kassing@physik.uni-kassel.de     

Rate dependence of short-pulse laser ablation of metals in air and vacuum

Ablation rates of aluminum and stainless steel are studied as a function of fluence, hole depth, pulse duration and ambient pressure (air vs vacuum). We find a weak rate dependence on pulse duration from 150 fs to 500 ps, and a strong rate dependence on hole depth due to surface roughness. Machining in air plays an important role in deep holes, but has a weaker influence on initial surface ablation rates. Oxidation greatly reduces drilling rates for deep holes in aluminum. Received: 26 December 2001 / Accepted: 9 July 2002 / Published online: 4 November 2002 RID="*" ID="*"Corresponding author. Fax: +1-925/422-5537, E-mail: stuart3@llnl.gov     

Photoacoustic characteristics of dynamical adhesion of films on a metallic substrate

In this communication, we report a numerical model that predicts the mechanical deformations associated with the pulsed laser irradiation of a film surface, based on thermal diffusion theory. The model is consequently advanced to produce a method for evaluating film adhesion strength. The epicenter surface displacements within the irradiated fields have been measured using a heterodyne interferometer. The comparison of the experimental data and the displacements calculated by the model shows good agreement. By investigating the propagating acoustic modes under non-destructive and destructive modes, we reveal that, with or without interface delamination, the phase structure of the longitudinal waves will be altered due to the change of reflection mode at the interface. Applying shock dynamics theory, we evaluate the adhesion strength of the TiN/stainless interface. We also indicate the strain rate can be up to 10⁵∼10⁶ s^-1 during film interface delamination. Received: 5 April 2002 / Accepted: 24 June 2002 / Published online: 26 February 2003 RID="*" ID="*"Corresponding author. Fax: +86-511/879-1919, E-mail: mzhou@ujs.edu.cn     

Giant field amplification in tungsten nanowires

The original RF-sputtering-assisted technique to produce metal wires with tip-curvature radii at the nanometer scale was developed and applied to tungsten. The wire tips were characterized by scanning electron microscopy. Field-emission tests of those wires exhibit excellent performance and reliable processability. Very high field-amplification factors of 18000 were demonstrated. Received: 1 November 2002 / Accepted: 30 November 2002 / Published online: 11 April 2003 RID="*" ID="*"Corresponding author. Fax: +1-972/479-4482, E-mail: alexander.umnov@fla.fujitsu.com     

Electron structure and electron dynamics at InSb(111)2×2 semiconductor surface

The conduction band electronic structure and the electron dynamics of the clean InSb(111)2×2 surface have been studied by laser based pump-and-probe photoemission. The results are compared to earlier studies of the InSb(110) surface. It is found that both the energy location and the time dependence of the photoexcited structures are very similar for the two surfaces. This indicates that the dominant part of the photoemission signal in the conduction band region is due to excitations of electrons in the bulk region and that the surface electronic states play a minor role. The fast decay of the excited state, τ∼12 ps, indicates that diffusion of hot electrons into the bulk is an important mechanism. Received: 9 May 2001 / Accepted: 9 July 2002 / Published online: 25 October 2002 RID="*" ID="*"Corresponding author. Fax: +46-0824/913-1, E-mail: gm@matphys.kth.se     

VUV F<Subscript>2</Subscript> laser ablation of sodium chloride

We report an investigation of the ablation of NaCl crystals at the 157-nm wavelength of the F₂ laser where there is very strong excitonic absorption. Probe-beam deflection and etch-rate measurements show that the interaction is characterised by a low ablation threshold (∼80 mJ cm^-2) and a capability for controllable material removal at the nanometer level. Scanning electron microscopy of the exposed surfaces show this to be microscopically smooth but with fine cracks present. It is demonstrated that micron-scale features can be formed in NaCl using 157-nm laser ablation, a result attributed to the strongly localised optical and thermal nature of the interaction. The results are discussed within the framework of a thermal vaporisation model. Received: 29 May 2002 / Accepted: 17 July 2002 / Published online: 4 November 2002 RID="*" ID="*"Corresponding author. Fax: +44-1482/465606, E-mail: p.e.dyer@hull.ac.uk     

Influence of the oxidation temperature on the fabrication process of silicon dioxide aperture tips

The thermal oxidation of structured silicon surfaces was successfully used to reproducibly define apertures of approximately 100 nm in silicon dioxide tips at reduced oxidation temperatures. In this paper we theoretically investigate the oxidation process in more detail, describing the rheological behavior of silicon dioxide as a Maxwell fluid with non-linear viscosity. For this purpose numerical calculations of the oxidation process of trench-like silicon structures were performed. Contrary to former assumptions, our theoretical results indicate that oxide-growth retardation is more effective at raised oxidation temperatures. This is experimentally confirmed in the case of trench structures. The more pronounced oxide retardation at elevated temperatures is exploited to obtain apertures in silicon dioxide tips of 60 nm for oxidation temperatures of 1100 °C. Received: 8 April 2002 / Accepted: 11 April 2002 / Published online: 4 November 2002 RID="*" ID="*"Corresponding author. Fax: +49-561/804-4136, E-mail: oester@physik.uni-kassel.de     

Microexplosions in tellurite glasses

Femtosecond laser pulses were used to produce localized damage in the bulk and near the surface of baseline, Al₂O₃-doped and La₂O₃-doped sodium tellurite glasses. Single or multiple laser pulses were non-linearly absorbed in the focal volume by the glass, leading to permanent changes in the material in the focal volume. These changes were caused by an explosive expansion of the ionized material in the focal volume into the surrounding material, i.e. a microexplosion. The writing of simple structures (periodic array of voxels, as well as lines) was demonstrated. The regions of microexplosion and writing were subsequently characterized using scanning electron microscopy (SEM), energy-dispersive spectrometry (EDS) and atomic force microscopy (AFM). Fingerprints of microexplosions (concentric lines within the region and a concentric ring outside the region), due to the shock wave generated during microexplosions, were evident. In the case of the baseline glass, no chemistry change was observed within the region of the microexplosion. However, Al₂O₃-doped and La₂O₃-doped glasses showed depletion of the dopant from the edge to the center of the region of the microexplosions, indicating a chemistry gradient within the regions. Interrogation of the bulk- and laser-treated regions using micro-Raman spectroscopy revealed no structural change due to the microexplosions and writing within these glasses. Received: 27 December 2001 / Accepted: 9 July 2002 / Published online: 25 October 2002 RID="*" ID="*"Corresponding author. +1-509/376-3108, E-mail: sk.sundaram@pnl.gov     

Efficient submicron processing of metals with femtosecond UV pulses

The generation of submicron-sized holes on metal surfaces by applying femtosecond UV laser pulses was investigated. Different optical schemes based on a Schwarzschild-type reflective objective were used to reach optimized ablation quality and efficiency in different applications (hole ablation, through-hole drilling, generation of surface patterns consisting of holes, etc.). Submicron-sized holes and hole patterns were ablated onto metal surfaces and drilled through ∼5-μm-thick steel foils with 600-nm diameter on the output side. Using a special optical interferometric method, large-area surface processing of high-conductivity materials in the submicron regime was performed. Combining these techniques with the application of high-repetition-rate ultra-short UV laser sources, large-area sub-μm processing of all kinds of materials in industrial environments is possible. Received: 28 February 2002 / Accepted: 12 March 2002 / Published online: 25 October 2002 RID="*" ID="*"Corresponding author. Fax: +49-551/503599, E-mail: psimon@llg.gwdg.de     

Self-assembly of length-tunable gold nanoparticle chains in organic solvents

The one-dimensional coagulation of gold colloidal particles dispersed in organic solvent was investigated with transmission electron microscopy. The results indicate that the length of the nanoparticle chains can be modulated by changing the concentration of the solutions. It was also demonstrated that the wetting of the substrate surface hardly influenced the morphology of the nanoparticle chains, which revealed that the particle chains had been formed in the solution before deposition on the substrates. A general theoretical interpretation is provided to explain the linear coagulation of gold colloidal particles, on the basis of the asymmetrical distribution of the charges absorbed on the surface of the gold colloidal particles, as well as the action of the solvent molecules. Received: 8 April 2002 / Accepted: 1 July 2002 / Published online: 4 December 2002 RID="*" ID="*"Corresponding author. Fax: +86-025/361-9983, E-mail: jhliao@seu.edu.cn     

A simple wet-chemical synthesis and characterization of CuO nanorods

Using a simple wet-chemical route, we synthesized CuO nanorods with diameters of ca. 5–15 nm and lengths of up to 400 nm. The purity, crystallinity, morphology, structure features, and chemical composition of the as-prepared CuO nanorods were investigated by powder X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, and Raman spectroscopy. Received: 22 March 2002 / Accepted: 12 June 2002 / Published online: 28 October 2002 RID="*" ID="*"Corresponding author. Fax: +86-25/359-5535, E-mail: wangqun@nju.edu.cn     

Orientation studies of Si-phthalocyanine sulfonic acids cast on SiOx substrates

Layers of dihydroxy silicon phthalocyanine tetrasulfonic acid and oligo-μ-oxo silicon phthalocyanine tetrasulfonic acid were prepared by solution-casting methods. The purity of the material was checked by X-ray photoemission spectroscopy. The orientation of the molecules in respect to the substrate plane was investigated by angle-dependent near-edge X-ray absorption fine-structure spectroscopy. The morphology was characterized by atomic force microscopy. Most samples exhibited a significant orientation that was accompanied by crystalline structures; others had no orientation at all with a dominant amorphous morphology. This behavior indicates that several preparation parameters affect the crystallinity and the orientation of the phthalocyanines. Received: 16 January 2002 / Accepted: 11 February 2002 / Published online: 3 May 2002 RID="*" ID="*"Corresponding author. Fax: +1-919/515-7331, E-mail: harald_ade@ncsu.edu RID="**" ID="**"Present address: Southern Illinois University, Physics, Mailcode 4401, Carbondale, IL 62901, USA     

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     

Femtosecond study of surface structure and composition and time-resolved spectroscopy in metals

Surface structuring and compositioning in aluminum alloy 2024-T3 were demonstrated using a femtosecond pulse laser. Surface nanostructuring was developed as a function of laser parameters and the surface micrographs of the scanning electron microscopy were characterized as a function of incident laser fluence. Surface compositioning was performed by selectively removing the elements on the surface of the sample. Femtosecond studies of highly excited electrons were performed by a pump–probe technique, and the thermalization time was found to be in a range of 1.5–3 ps, increasing with incident fluence. The time-resolved measurement is well matched to the numerical calculation. Received: 6 September 2001 / Accepted: 18 July 2002 / Published online: 25 October 2002 RID="*" ID="*"Corresponding author. Fax: +1-405/744-6811, E-mail: dou@okstate.edu     

Buried interfaces studied by photoelectron diffraction

Angle- and energy-scanned photoelectron diffraction data can be used to investigate structures below surfaces. The modulations in photoelectron intensity result from diffraction of the emitted electron wave at neighbor atoms. In the past, scanned-energy photoelectron diffraction had been mainly used to determine the adsorption site of molecules at surfaces. Recent data show, however, that the technique can also be employed to obtain information about the upper substrate layer(s). At low kinetic energies, backward scattering is strong and in scanned-angle photoelectron diffraction the recorded patterns result from backward- and multiple-scattering effects. For a structural analysis, the intensity modulations have to be compared with the results for simulations performed for model clusters. As an example, recent angle-scanned photoelectron diffraction patterns recorded for the technologically important silicon oxide/silicon interface were compared with simulations. At the Si(001) surface orientation, the interface is extended over a few layers, whereas at the Si(111) surface orientation the transition is rather abrupt and occurs within one or two layers. Received: 9 September 2002 / Accepted: 2 October 2002 / Published online: 5 February 2003 RID="*" ID="*"Corresponding author. Fax: +49-231/755-3657, E-mail: carsten.westphal@physik.uni-dortmund.de     

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     

Femtosecond laser processing of nitride-based thin films to improve their tribological performance

The ability of femtosecond laser pulses to pattern coated tribological surfaces in order to improve their wear behavior was investigated. Experiments were performed with a Ti:sapphire laser (wavelength: 800 nm, energy density: 2 J/cm², pulse duration: 100 fs) on TiN- and on TiCN-coated surfaces. Morphological analyses of the laser-treated surfaces were carried out and did not reveal any film delamination or other coating damage after laser processing. Tribological tests simulating rapidly increasing contact pressures under boundary friction were performed on both unpatterned and laser-patterned coated surfaces using a steel counter body. The patterned surfaces showed significantly better tribological performance with respect to stability and the value of the friction coefficient during testing. EDX analyses of the tested unpatterned samples revealed complete coating removal and material transfer from the counter body to the sample surface. In the case of the laser-patterned surfaces, only slight coating damage and an accumulation of debris from the steel counter body in the laser-induced pores were observed. PACS 42.62.Cf; 81.40.Wx