Self-organization of ripples on Ti irradiated with focused ion beam

30 keV focused Ga⁺ ions were used to raster the metallographically polished surface of commercially pure Ti (CP Ti) at various FIB incidence angles over a wide range of doses (10¹⁶-10¹⁸ ions/cm²) at room temperature. The sputtered surfaces were observed in situ using FIB imaging and later carefully characterized ex situ under scanning electron microscope (SEM) and atomic force microscope (AFM). Ripples were observed on the irradiated surfaces even at the normal FIB incidence angle. The ripple evolution is analyzed as functions of surface diffusion, surface crystallographic orientation, ion dose and incidence angle. It is found that the ripple orientation was progressively influenced by the ion beam direction with incidence angle increasing and in some cases curved ripples or fragmented rods viewed from different angles occurred at high ion doses. The morphological evolution from the well-developed straight ripples to the curved ones is never observed. The formation of ripples is attributed to the competition between the formation of ripples due to anisotropic surface diffusion and the formation of incidence-angle dependent ripples determined by Bradley-Harper (BH) model.     

Pulse laser acoustics for the characterization of inhomogeneities at interfaces of microstructures

Interfaces between neighbouring materials are often subjected to diffusion processes which cause layers having gradually varying mechanical properties--like densities, Young's moduli or shear moduli--perpendicular to the surface or interface. In this investigation particular interest is drawn on the question how the propagation characteristics of bulk acoustic waves are affected by diffusion layers. The reflection and transmission behavior of bulk acoustic waves encountering a continuum having a spatially dependent sound velocity is discussed based on numerical simulations as well as on experimental verifications. The simulated results are part of an on-going project in which material properties of MEMS devices are investigated by short pulse laser acoustic methods. Mechanical waves are excited and detected thermoelastically using laser pulses of 70 fs duration. For metals this leads to wavelengths of 10-20 nm and the corresponding frequencies amount to 0.3-0.6 THz. In contrast to previous work done in this field in which diffusion effects are generally considered as undesirable phenomena, the deliberate realization of microstructures having well defined gradually varying material properties in one or more dimensions represents a goal of this investigation. For metallic thin film multilayers thermally induced diffusion processes have shown to be an easy and reliable technique for the realization of layered structures having continuously varying mechanical properties within several 10 nm. Among the experimental methods suitable for the in-depth profiling of submicron metallic thin films providing resolutions of several nanometers, are short pulse laser acoustic methods, Rutherford backscattering spectroscopy (RBS), and glow discharge optical emission spectroscopy (GDOES). Short pulse laser acoustic methods and RBS have the advantage to be nondestructive. The short pulse laser acoustic method is described in detail and RBS measurements are presented for verification purposes. Finally potential engineering applications like micro-machined spectrum analyzers, acoustic isolation layers, and band pass filters, operating at very high frequencies are presented.     

Investigation of the structural and electrical properties of air-annealed ruthenium thin films on 6H–SiC at different temperatures

Ruthenium (Ru) Schottky contacts and thin films on n-type 6H–SiC were fabricated and characterised by physical and electrical methods. The characterisation was done after annealing the samples in air at various temperatures. Rutherford backscattering spectroscopy (RBS) analysis of the thin films indicated the oxidation of Ru after annealing at a temperature of 400 °C, and interdiffusion of Ru and Si at the Ru–6H–SiC interface at 500 °C. XRD analysis of the thin films indicated the formation of RuO₂ and RuSi in Ru–6H–SiC after annealing at a temperature of 600 °C. The formation of the oxide was also corroborated by Raman spectroscopy. The ideality factor of the Schottky barrier diodes (SBD) was seen to generally decrease with annealing temperature. The series resistance increased astronomically after annealing at 700 °C, which was an indication that the SBD had broken down. The failure mechanism of the SBD is attributed to deep inter-diffusions of Ru and Si at the Ru–6H–SiC interface as evidenced by the RBS of the thin films.     

(Co, Zn)O compound obtained from ZnTe vapor deposition on Co/Si substrates

(Co, Zn)O compound has been obtained by a non-expensive synthesis route. ZnTe thin films were obtained by isothermal close space sublimation on the Co thin layer previously sputtered on silicon substrates. After the annealing process in humid ambient cobalt atoms diffusion and Zn oxidation were obtained besides partial Te evaporation. The detailed characterization of the samples by using XRD, RBS, AFM, XPS, VSM and MFM techniques point to the formation of room temperature ferromagnetic Co _x Zn_(1−x)O phase (x<0.15). This ferromagnetic behavior is mainly attributed to Co atoms substituting Zn atoms in the ZnO network.     

Focused ion beam based sputtering yield measurements on ZnO and Mo thin films

In order to facilitate the lateral structuring of solar cell multilayer structures, the ion beam sputtering behaviour of Mo and ZnO thin films deposited onto soda-lime glass and single crystalline Si substrates was studied. Prior to ion beam processing the layers were analyzed by Energy Dispersive X-Ray Spectrometry (EDS), X-Ray Diffractometry (XRD) and Rutherford Backscattering (RBS). In order to characterize the ion beam sputtering of the investigated layers, 2×2 μm² fractions of the thin films were removed by a scanned 30 keV focused Ga⁺ ion beam (FIB) in a dual beam system. SEM images taken during the milling process allowed continuous monitoring of the process without breaking the vacuum. The depth of the groove after removal of the layers was measured by Atomic Force Microscopy (AFM) and was plotted as a function of the ion dose. The sputtering depth has a dependence on the ion dose that is close to linear. The deviation from linearity is produced by heating effects at high beam currents. Sputtering yield values calculated from the experiments and simulations showed good agreement in the case of Mo but deviation was found in the case of ZnO.     

Model of silicon carbide formation on porous substrates

The formation of thin silicon carbide layers as a result of solid-phase processes is related to the evolution of nanoscale porosity and chemical reactions on pore surfaces. Numerical experiments, which simulate blistering under the action of Xe+ ions in the metal-insulator (Mo/Si) bilayer make it possible to establish the relationship between the porosity parameters and layer stresses and the irradiation conditions. Similar patterns in the formation of defects (pores and cracks) in crystalline silicon characterize its interaction with carbon dioxide when silicon carbide is formed. The calculated characteristics of the nucleation in the Mo/Si bilayers are analyzed to optimize the solid-phase epitaxy of silicon carbide.     

Short- and long-range ion-beam mixing in Cu:Al

Ion-beam mixing by 500-keV xenon ions has been studied in targets consisting of 2000-Å films of aluminium on a polycrystalline aluminium substrate, onto which has been evaporated a 500-Å overlayer of copper. Both long- and short-range-mixing processes have been identified, by RBS analysis of the irradiated targets, as a deep copper tail in the aluminium and interfacial broadening, respectively. The long-range component varies linearly with xenon fluence, is temperature-independent in the interval 40–500 K, and is not influenced by the presence of an interfacial oxide layer between the copper and aluminium layers. The number of long-range-mixed atoms is in agreement with theoretical estimates of the recoil mixing. The short-range mixing, which is the dominating process, has a squareroot dependence on xenon fluence and is independent of temperature between 40 and 300 K, increasing rapidly at higher temperatures. The broadening attributed to the short-range mixing is explained by interstitial diffusion within the cascade. For small xenon fluences, interfacial oxide layers inhibited both short-range mixing and thermal diffusion. Higher xenon fiuences subdued the inhibition.     

Stoichiometry dependent changes in the optical properties and nanoscale track formation of PECVD grown a-SiNx:H thin films upon 100 MeV Au8+ ion irradiation

a-SiN_x:H thin films of different stoichiometry grown by PECVD were subjected to irradiation by 100 MeV Au⁸⁺ ions with various fluences to understand the effect of stoichiometry on properties of thin films upon irradiation. Ellipsometry and UV–Vis study suggest the variation in the refractive index of thin films with fluence. The evolution of Hydrogen due to irradiation is quantified with the help of ERDA. RBS was probed to study the change in thin films' composition upon irradiation, which further helps understand the change in thin films' optical properties. Quenching of photoluminescence in the films with all stoichiometries was also observed due to ion irradiation. X-TEM images show the formation of discontinuous ion tracks of radius 2.5 nm in the film closer to silicon nitride stoichiometry. However, Si rich film does not show the clear formation of tracks. Results are explained in the framework of the Thermal spike mechanism of ion-solid interaction.     

Diffusion of Au atoms and (5×2) phase formation on the Si(111) (7×7) surface

In this article we investigate the complex 1D mesoscopic model of adatom diffusion and the evolution of an ordered phase on the substrate surface. The analysis of the theoretical model is compared with the experimental results of the spreading of Au adatoms on Si(111)-(7×7) surface. The steady state solutions and their stability conditions are determined within the concept of the traveling-wave solution. It is shown that the formation of the ordered phase (5×2) and the difference in the diffusion of Au on (7×7) and on (5×2) structure results in a sharp edge of diffusion front which corresponds to the coverage of a saturated (5×2) phase. This edge moves linearly in time and α can be determined by experiment. The system of model equations enables the damped waves solution or temporary evolution of two steps.     

Diffusion of Ta in α-Ti

The diffusion of Ta in the hcp (α) phase of high-purity Ti (99.99%) was studied at different temperatures from 911 K up to 1123 K. The Rutherford Backscattering Spectrometry (RBS) and Heavy Ion RBS (HIRBS) techniques were used to obtain the penetration profiles. The evolution of the diffusion coefficient, D, as a function of temperature follows prediction of the Arrhenius law. The activation energy of the diffusion process is (318±7)kJ/mol, similar to that corresponding to self-diffusion in α-Ti. On the other hand, the measured values of D are systematically lower than those corresponding to self-diffusion by a factor of approximately 5. This reduction could be explained by taking into account the mass difference between Ta and Ti. An increase of the diffusion coefficient was measured when the diffusion proceeds on a less pure Ti (99.9%) matrix. This increment is higher at lower temperatures. Received: 12 November 2001 / Accepted: 12 March 2002 / Published online: 5 July 2002 RID="*" ID="*" RID="*" ID="*" RID="**" ID="**"Corresponding author. Fax: +54-11/6772-7362, E-mail: dyment@cnea.gov.ar RID="*" ID="*"Members of the Carrera del Investigador Científico del Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Argentina     

Electric dipolar interaction assisted growth of single crystalline organic thin films

We report on a forest-like-to-desert-like pattern evolution in the growth of an organic thin film observed by using an atomic force microscope. We use a modified diffusion limited aggregation model to simulate the growth process and are able to reproduce the experimental patterns. The energy of electric dipole interaction is calculated and determined to be the driving force for the pattern formation and evolution. Based on these results, single crystalline films are obtained by enhancing the electric dipole interaction while limiting effects of other growth parameters.     

Growth of Bi-Sb alloy thin films and their characterization by TEM, PIXE and RBS

Polycrystalline bulk materials of Bi₉₃Sb₇ Bi₈₈Sb₁₂, Bi₈₅Sb₁₅ and Bi₈₀Sb₂₀ were synthesized by melt-quench technique starting from the stoichiometric mixture of constituent elements. The phase purity and compositional uniformity of bulk materials were investigated using powder X-ray diffraction (XRD) and proton induced X-ray emission (PIXE) experiments. The single phase formation and the compositional analysis of thin films were confirmed by transmission electron microscopy (TEM) and Rutherford backscattering spectroscopy (RBS). X-ray diffraction studies confirmed the phase homogeneity of the materials. Atomic concentration ratio of constituent elements (Bi and Sb) determined by PIXE and RBS revealed that near-stoichiometric composition is nearly the same in the bulk as well as in thin film forms.     

Magnetic nanowire arrays in anodic alumina membranes: Rutherford backscattering characterization

Systematic study of magnetic nanowire arrays grown in anodic alumina membranes (AAM) has been done by means of Rutherford backscattering spectroscopy (RBS). The AAM used as templates were morphologically characterized by using high resolution scanning electron microscopy (HRSEM), fast Fourier transform (FFT) and atomic force microscopy (AFM). The highly ordered templates with a mean pore diameter size of 30 nanometers, a mean inter-pore spacing of 100 nm and lengths ranging from 4 to 180 microns were obtained through two-steps anodization process, and the Ni and Co nanowire arrays were grown by electrodeposition techniques. The main attention is addressed to Ni nanowire arrays. RBS results allowed us to determine the real depth profile of atomic composition of the obtained nanowire arrays. In addition, the RBS spectra fitting showed that the porosity increased from the top to the bottom of the samples. Two phenomenological models are proposed to understand the apparition of that secondary porosity and a linear relation between the total amount of electrodeposited Ni and the electrodeposition time was obtained. As an example, it is also reported the relation between RBS results and magnetic properties, such as coercive field and remanence/saturation magnetization ratio of the samples. Particularly, for Ni nanowires arrays obtained by using voltage pulses, it is demonstrated that the larger the nanowires, the higher the definition for easy axis parallel to the nanowire length is possible. PACS 82.80.Yc; 81.16-c; 75.75.+a     

Enhancements in specimen preparation of Cu(In,Ga)(S,Se)2 thin films

When producing slices from Cu(In,Ga)(S,Se)(2) thin films for solar cells by use of a focused ion beam (FIB), agglomerates form on the Cu(In,Ga)(S,Se)(2) surfaces, which deteriorate substantially the imaging and analysis in scanning electron microscopy. Similar problems are also experienced when depth-profiling Cu(In,Ga)(S,Se)(2) thin films by means of glow-discharge or secondary ion mass spectrometry. The present work shows that the agglomerates are composed of (mainly) Cu, and that their formation may be impeded considerably by either cooling of the sample or by use of reactive gases during the ion-beam sputtering. The introduction of XeF(2) during FIB slicing resulted in excellent images, in which the microstructures of most layers in the Cu(In,Ga)(S,Se)(2) thin film stack are visible, including the microstructure of the 20 nm thin MoSe(2) layer. Acquisition of high-quality two-dimensional and also three-dimensional electron backscatter diffraction data was possible. The present work gives a basis for enhanced SEM imaging and analysis not only in the case of Cu(In,Ga)(S,Se)(2) thin films but also when dealing with further material systems exhibiting similar formations of agglomerates.     

Autoignition-controlled flame initiation and flame stabilization in a reacting jet in crossflow

This paper describes an analysis of the mechanisms of autoignition-controlled flame initiation and flame stabilization in a nonpremixed jet in crossflows, using simultaneous high-speed (10 kHz) tomographic particle image velocimetry, OH-PLIF and line-of-sight flame emissions. Measurements are conducted on a turbulent, transverse, reacting propane jet issued into a crossflow generated by combustion of natural gas at an equivalence ratio of 0.4 with the crossflow velocity of 10 m/s, the crossflow temperature of 1350 K and the jet momentum flux ratio of 41. While several prior studies have analyzed the lifted character of the flame in similar configurations, we show that several dynamic processes precede the leading edge of the lifted diffusion flame, including formation and evolution of “autoignition kernels”, “flame kernels” and “flame fragments”. “Autoignition kernels”, i.e., discrete compact reaction zones with the peak hydroxyl (OH) fluorescence intensity below that of the diffusion flame, initiate preferably at bulges along the jet periphery where the strain rates and the scalar dissipation rates are lower. The autoignition kernel grows in both size and the OH-fluorescence intensity as it convects downstream. An autoignition kernel transitions into a propagating flame kernel, which quickly gets distorted and elongated in the direction of the principal expansion strain rate to form a flame fragment. Neighboring flame fragments merge with each other and with the downstream diffusion flame via edge-flame propagation. Merging of upstream flame fragments with the downstream diffusion flame results in an upstream advancement of the diffusion-flame front. The diffusion flame front is intrinsically unsteady because of the rather random formation and evolution of autoignition kernels, flame kernels and flame fragments, presumably due to the stochastic velocity, the strain rate and mixture-fraction oscillations.     

Evaporation of an emulsion trapped in a yield stress fluid

The present work deals with emulsions of volatile alkanes in an aqueous clay suspension, Laponite, which forms a yield stress fluid. For a large enough yield stress (i.e. Laponite concentration), the oil droplets are prevented from creaming and the emulsions are thus mechanically stabilized. We have studied the evaporation kinetics of the oil phase of those emulsions in contact with the atmosphere. We show that the evaporation process is characterized by the formation of a sharp front separating the emulsion from a droplet-free Laponite phase, and that the displacement of the front vs. time follows a diffusion law. Experimental data are confronted to a diffusion-controlled model, in the case where the limiting step is the diffusion of the dissolved oil through the aqueous phase. The nature of the alkane, as well as its volume fraction in the emulsion, has been varied. Quantitative agreement with the model is achieved without any adjustable parameter and we describe the mechanism leading to the formation of a front.     

Surface morphology and reaction at Cu/Si interface—Effect of native silicon suboxide

Copper thin films are deposited by thermal evaporation on unetched and etched monocrystalline silicon. The study by alpha particles backscattering (RBS) raises a strong diffusion of copper in silicon substrates with and without native suboxide layer. On the other hand, the X-rays diffraction shows the formation and the growth of Cu₃Si and Cu₄Si silicides. Whereas the scanning microscopy underlines large crystallites growth surrounded by black zones of silicon coming from the uncovered substrate, independently to the surface state of the substrate, after annealing at high temperature. The presence of native silicon suboxide at Cu/Si interface, influences in a drastic way the minimal temperature to which the interfacial reaction occurs. The oxygen impurities detected by microanalysis, after heat treatment under vacuum, are closely related to the growth of silicides crystallites.     

Investigation of a stainless-steel surface irradiated with protons in an iodine medium

The surface of 1Cr18Ni10Ti stainless steel irradiated by protons with an energy of 5.7 MeV in an iodine medium is studied by Rutherford backscattering (RBS) and X-ray photoelectron spectroscopy (XPS). Iodine bonded with oxygen and molecular I₂ is observed in a thin 10-nm-thick steel surface layer. Iodine depth profiles are obtained using the RBS and XPS spectra. The possibility of the formation of chemical compounds containing iodine on the steel surface with allowance for the proton-irradiation effect on iodine adsorption is discussed.