Depth resolved Doppler broadening measurement of layered Al-Sn samples

The accumulation of positrons in a two-dimensional layer of tin embedded in aluminum is examined by Doppler broadening spectroscopy (DBS). For this purpose samples are grown out of high purity materials consisting of a step-shaped layer (0.1-200 nm) of tin on a substrate of aluminum and covered by an aluminum layer of constant thickness (200 nm).The positron implantation profile is varied by different positron acceleration energies of up to 15 keV. The pre-thermal implantation profile of the monoenergetic positron beam is examined since the effect of thermal positron diffusion is less significant at tin layers thicker than 50 nm. At thin layers (<50 nm), the positrons greatly accumulate either at the aluminum-tin interface or in the tin layer due to its higher positron affinity compared to aluminum. Thus a very high sensitivity of the measurement for low densities of tin is observed. Consequently from the experimental results, a sensitivity threshold for the detection of a low amount of tin in an aluminum matrix with DBS is determined. The DB results are compared to theory by an approximation for pre-thermal implantation in layered materials.     

Surface structure and phase transition of Ge(1 1 1)-3 × 3-Pb studied by reflection high-energy positron diffraction

We studied the structures and the phase transition of Pb/Ge(1 1 1) surface by using the reflection high-energy positron diffraction. The surface structures at 60 K and 293 K have the 3 × 3 and √3 × √3 periodicities, respectively. The rocking curves measured at both temperatures are nearly the same. This indicates that the equilibrium positions of the surface atoms do not change according to the phase transition. From the analysis of the rocking curve based on the dynamical diffraction theory, we found that at both temperatures the surface structures are composed of the so-called one-up and two-down model. The 3 × 3-√3 × √3 phase transition for the Pb/Ge(1 1 1) surface is interpreted in terms of order-disorder transition.     

Microstructure characterization of porous silicon as studied by positron annihilation measurements at low temperatures and high vacuum

Atomic scale properties of thin porous silicon (PSi) layers, characterized by the formation of positronium, are investigated using positron annihilation lifetime spectroscopy in the temperature range 20-300 K under 10⁻⁷ Torr vacuum. The longest orthopositronium as well as the shortest parapositronium components are found to have quite low intensities in the thin layer at room temperature. It is also found that at temperatures ≤240 K, these two components do not show up in the spectrum. The reason for this absence of the longest lifetime component is suggested.     

Vacancy profiles and clustering in light-ion-implanted GaN and ZnO

We present experimental results obtained in H-implanted GaN and He- and Li-implanted ZnO. The ion energies were varied in the range 100-850 keV, and the implantation fluences in the range 5 × 10¹³ to 1 × 10¹⁸ cm⁻². In addition, conventional and flash anneals at temperatures 500-1400 °C were performed on the ZnO samples. The data obtained with a slow positron beam show that vacancy clusters are formed in as-implanted samples with fluences above 1 × 10¹⁷ cm⁻². Below this value only single vacancies are detected after implantation, but vacancy clusters can be formed and subsequently dissociated by thermal annealings.     

Slow positron beam study of nitrogen implanted CZ-Si subjected to rapid thermal processing

In this experiment, nitrogen ions were implanted into CZ-silicon wafer at 100 keV at room temperature with the fluence of 5 × 10¹⁵ N₂⁺/cm², followed by rapid thermal processing (RTP) at different temperatures. The single detector Doppler broadening and coincidence Doppler broadening measurements on slow positron beam were carried out to characterize the defects in the as-implanted silicon and RTP-treated samples. It is found that both nitrogen-vacancy complexes (N-Vsi) and oxygen-vacancy complexes (O-Vsi) produced by nitrogen implantation diffuse back to the sample surface upon annealing. But the N-Vsi and the O-Vsi complete with each other and give a summed effect on positron annihilation characteristics. It is shown that the N-Vsi win out the O-Vsi in as-implanted sample and by RTP at 650 °C, 750 °C, which make the S-parameter increase; O-Vsi plays a dominant role after annealing above 850 °C, which makes the S parameter decrease.     

Characterization of n-GaN dilute magnetic semiconductors by cobalt ions implantation at high-fluence

In this study, we present the structural and magnetic characteristics of cobalt ions implantation at a high-fluence (5×10¹⁶ cm⁻²) into n-GaN epilayer of thickness about 1.6 μm. The n-GaN was grown on sapphire by metal organic chemical vapor deposition (MOCVD). Rutherford backscattering channeling was used for the structural study. After implantation, samples were annealed at 700, 800 and 900 °C by rapid thermal annealing in ambient N₂. XRD measurements did not show any secondary phase or metal related-peaks. High resolution X-ray diffraction (HRXRD) was performed as well to characterize structures. Well-defined hysteresis loops were observed at 5 K and room temperature using alternating gradient magnetometer AGM and Superconducting Quantum Interference Device (SQUID) magnetometer. Temperature-dependent magnetization indicated magnetic moment at the lowest temperatures and retained magnetization up to 380 K for cobalt-ion-implanted samples.     

Sticking coefficient of nitrogen on solid N2 at low temperatures

The sticking coefficient of nitrogen gas on a thick solid nitrogen film on a copper cold finger was studied at low temperature. For surface temperatures of about 12 K the sticking coefficient is measured to be 99.0 ± 0.6%. Our result implies that it will be possible to make a intense and high brightness slow positron source starting from a small diameter deposit of the gaseous positron emitter ¹³N₂ produced in the reaction ¹²C(d,n)¹³N.     

The resistive-heating characterization of laser heating system and LaB6 characterization of X-ray diffraction of beamline 12.2.2 at advanced light source

X-ray diffraction from LaB₆ standards document a precision of 478 ppm in lattice-parameter determinations for beamline 12.2.2 at Lawrence Berkeley National Laboratory′s Advanced Light Source, a facility for characterizing materials at high pressures and temperatures using laser- and resistance-heated diamond cells. Melting of Ni, Mo, Pt and W, resistively heated at 1 atm pressure in Ar, provides a validation of the beamline spectroradiometric system that is used to determine sample temperatures. The known melting temperatures, which range from 1665 to 3860 K for these metals, are all reproduced to within ±80 K.     

Self-implantation of Cz-Si: Clustering and annealing of defects

Observations of vacancy clusters formed in Czochralski (Cz) Si after high energy ion implantation are reported. Vacancy clusters were created by 2 MeV Si ion implantation of 1 × 10¹⁵ ions/cm² and after annealing between 600 and 650 °C. Doppler broadening measurements using a slow positron beam have been performed on the self-implanted Si samples, both as-implanted and after annealing between 200 and 700 °C for time intervals ranging from 15 to 120 min. No change in the S parameter was noted after the thermal treatment up to 500 °C. However, the divacancies (V₂) created as a consequence of the implantation were found to start agglomerating at 600 °C, forming vacancy clusters in two distinct layers below the surface; the first layer is up to 0.5 μm and the second layer is up to 2 μm. The S-W plots of the data suggest that clusters of the size of hexavacancies (V₆) could be formed in both layers after annealing for up to an hour at 600 °C or half an hour at 650 °C. After annealing for longer times, it is expected that vacancies are a mixture of V₆ and V₂, with V₆ most probably dominating in the first layer. Further annealing for longer times or higher temperatures breaks up the vacancy clusters or anneals them away.     

Structural and electrical transport properties of Nb-doped TiO2 films deposited on LaAlO3 by rf sputtering

We have investigated the structural and electrical transport properties of Nb-doped TiO₂ films deposited on (1 0 0) LaAlO₃ substrates by rf magnetron sputtering at temperatures ranging from 873 K to 1073 K. Films deposited below 998 K are anatase, and mixed phases between anatase and rutile exist in the film grown at higher temperatures. We find that films deposited at low temperatures exhibit semiconductor behavior, while metallic conductivity is observed in the most conducting film deposited at 998 K. For this sample, compared to electron-phonon scattering mechanism, electron-phonon-impurity interference effect plays an important role in its electron transport process. Moreover, the temperature coefficient of the resistivity for the film deposited at 1073 K is negative from 2 K to 300 K. The temperature dependence of resistivity for the film is described by ∼exp(b/T)^1/2 at temperatures from 80 K down to 30 K, and by the fluctuation induced tunneling model from 80 K to 300 K.     

Application of spectroscopic ellipsometry to the investigation of the optical properties of cobalt-nanostructured silica thin layers

Spectroscopic ellipsometry is used to investigate optical properties of cobalt-implanted silica thin films. The films under investigation are 250 nm thick thermal SiO₂ layers on Si substrates implanted with Co⁺ ions at energy of 160 keV and at fluences of 10¹⁷ ions/cm² for different temperatures of substrate during implantation (77 and 295 K). Changes due to Co⁺ implantation are clearly observed in the optical response of the films. Optical behaviours are furthermore different for the three implantation temperatures. To understand the optical responses of these layers, the ellipsometric experimental data are compared to different models including interference effects and metal inclusions effects into the dielectric layer. The simulated ellipsometric data are obtained by calculating the interferences of an inhomogeneous layer on a Si substrate. The material within this layer is considered as an effective medium which dielectric function is calculated using the Maxwell-Garnett effective medium approximation. We show that although the structures of these layers are very complicated because of ion-implantation mechanisms, quite simple models can provide relatively good agreement. The possibilities of ellipsometry for the study of the optical properties of such clusters-embedded films are discussed. We especially provide the evidence that ellipsometry can give interesting information about the optical properties of nanostructured layers. This is of special interest in the field of nanostructured layered systems where ellipsometry appears to be a suitable optical characterization technique.     

Positron and deuteron depth profiling in helium-3-implanted electrum-like alloy

In spite of previous extensive studies, the helium behavior in metals still remains an issue in microelectronics as well as in nuclear technology. A gold-silver solid solution (Au₆₀Ag₄₀: synthetic gold-rich electrum) was chosen as a relevant model to study helium irradiation of heavy metals. After helium-3 ion implantation at an energy ranging from 4.2 to 5.6 MeV, nuclear reaction analysis (NRA) based on the ³He(d,p)⁴He reaction, was performed in order to study the thermal diffusion of helium atoms. At room temperature, NRA data reveal that a single Gaussian can fit the He-distribution, which remains unchanged after annealing at temperatures below 0.45 of the melting point. Slow positron implantation spectroscopy, used to monitor the fluence dependence of induced defects unveils a positron saturation trapping, which occurs for He contents of the order of 50-100 appm, whereas concentrations larger than 500 appm seem to favor an increase in the S-parameter of Doppler broadening. Moreover, at high temperature, NRA results clearly show that helium long range diffusion occurs, though, without following a simple Fick law.     

Defects in nanocrystalline Nb films: Effect of sputtering temperature

Thin niobium (Nb) films (thickness 350-400 nm) were prepared on (1 0 0)Si substrate in a UHV chamber using the cathode beam sputtering. The sputtering temperature T_s was varied from 40 up to 500 °C and the influence of the sputtering temperature on the microstructure of thin Nb films was investigated. Defect studies of the thin Nb films sputtered at various temperatures were performed by slow positron implantation spectroscopy (SPIS) with measurement of the Doppler broadening of the annihilation line. SPIS was combined with transmission electron microscopy (TEM) and X-ray diffraction (XRD). We have found that the films sputtered at T_s = 40 °C exhibit elongated, column-like nanocrystalline grains. No significant increase of grain size with T_s (up to 500 °C) was observed by TEM. The thin Nb films sputtered at T_s = 40 °C contain a high density of defects. It is demonstrated by shortened positron diffusion length and a high value of the S parameter for Nb layer compared to the well-annealed (defect-free) bulk Nb reference sample. A drastic decrease of defect density was found in the films sputtered at T_s ≥ 300 °C. It is reflected by a significant increase of the positron diffusion length and a decrease of the S parameter for the Nb layer. The defect density in the Nb layer is, however, still substantially higher than in the well-annealed reference bulk Nb sample. Moreover, there is a layer at the interface between the Nb film and the substrate with very high density of defects comparable to that in the films sputtered at T_s < 300 °C. All the Nb films studied exhibit a strong (1 1 0) texture. The films sputtered at T_s < 300 °C are characterized by a compressive macroscopic in-plane stress due to lattice mismatch between the film and the substrate. Relaxation of the in-plane stress was observed in the films sputtered at T_s ≥ 300 °C. The width of the XRD profiles of the films sputtered at T_s ≥ 300 °C is significantly smaller compared to the films sputtered at lower temperatures. This is most probably due to a lower defect density which results in reduced microstrains in the films sputtered at higher temperatures.     

Application of positron annihilation spectroscopy on the ion implantation damaged Fe-Cr alloys

Four different Fe-Cr binary alloys with Cr content 2.5-11 wt% were studied in details using various methods. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were applied to obtain basic information, required for standard positron annihilation lifetime spectroscopy (PALS) spectra analysis. Additionally, PALS measurements were performed on as-received state as well as on helium implanted specimens. The He implantation was proposed for simulation of radiation damage and obtain high doses even in near surface areas (up to 1 μm). The implantation was based on the SRIM code simulation and next DPA calculations. Final concentration of vacancy type defects were calculated for 250 keV He²⁺ beam and the maximum was determined in 600 μm depth. Such specimens are very suitable for positron beam study of vacancy type defect mobility as a result of thermal treatment, which will be performed simultaneously in the future.     

Determination of the positron diffusion length in Kapton by analysing the positronium emission

Doppler profile spectroscopy and Compton-to-peak ratio analysis have been used to study the positronium (Ps) emission from the Kapton surface as a function of the positron implantation energy E.Two different positions for the sample have been performed in the experiment.In the first case the sample and the Ge-detector are perpendicular to the positron beam. With this geometry the emission of para-positronium (p-Ps) is detected as a narrow central peak.In the second case, by rotating the sample 45° with respect to the beam axis, the emission of p-Ps is detected as a blue-shifted fly away peak. The implantation of the positrons is described by the Makhov profile, where we used the modified median implantation for polymers as given by Algers et al. [J. Algers, P. Sperr, W. Egger, G. Kögel, F.H.J. Maurer, Phys. Rev. B 67 (2003) 125404].Thermalised positrons can diffuse to the surface and may pick up an electron to be emitted as Ps. We found a thermal and or epithermal positron diffusion length L₊ = 5.43 ± 0.71 nm and L₊ = 5.51 ± 0.28 nm correspondingly for both cases, which is much more than the one found by Brusa et al. [R.S. Brusa, A. Dupasquier, E. Galvanetto, A. Zecca, Appl. Phys. A 54 (1992) 233]. The respective efficiency for the emission of Ps by picking up an electron from the surface is found to be f_pu = 0.247 ± 0.012 and f_pu = 0.156 ± 0.003.     

Hydrogen indium vacancy complex VInH4 in n-type InP studied by positron-lifetime

Positron-lifetime experiments have been carried out on two undoped n-type liquid encapsulated Czochralski (LEC)-grown InP samples with different stoichiometric compositions in the temperature range 10-300 K. For temperatures below 120 K for P-rich InP and 100 K for In-rich InP, the positron average lifetime began to increase rapidly and then leveled off, which was associated with the charge state change of hydrogen indium vacancy complexes from (V_InH₄)⁺ to (V_InH₄)⁰. This phenomenon was more obvious in P-rich samples that have a higher concentration of V_InH₄. The transformation temperature of approximately 120 K suggests that the complex V_InH₄ is a donor defect and that the ionization energy is about 0.01 eV. The ionization of neutral V_InH₄ accounted for the decrease of the positron average lifetime when the sample was illuminated with a photon energy of 1.32 eV at 70 K. These results provide evidence for hydrogen complex defects in undoped LEC InP.     

Core level photoemission and STM characterization of Ta/Si(1 1 1)-7 × 7 interfaces

We present the results of scanning tunneling microscopy (STM) and photoemission spectroscopy (PES) of the Ta/Si(1 1 1)-7 × 7 system after deposition of Ta at substrate temperatures from 300 to 1250 K. The coverage of Ta varied from 0.05 up to 2.5 of a monolayer (ML). STM shows that at 300 K and coverage less than 1 ML, a disordered chemisorbed phase is formed. Deposition on a hot surface (above 500 K) produces round 3D clusters randomly distributed on the surface. Cluster height and their diameter are found to change drastically with annealing temperature and the Ta coverage. Analysis of photoemission data of the Si 2p core levels shows that at room temperature and at coverage ?1 ML core level binding energy shifts and intensity variations of Si surface related components are observed, which clearly indicate that the reaction starts already at 300 K. Shifts in the binding energy, changes of the peak shapes and intensity of the Ta 4f doublet at higher temperatures can be explained by the formation of stable silicide on the surface.     

Surface structure of In/Si(1 1 1) studied by reflection high-energy positron diffraction

We have investigated a quasi-one-dimensional structure of In/Si(1 1 1) surface using reflection high-energy positron diffraction (RHEPD), which is sensitive to the topmost surface structure under the total reflection condition. From the rocking curves, we found that In atoms are located at two different vertical positions, i.e., 0.99 Å and 0.55 Å from the Si zigzag chain in both 4 × 1 (210 K) and 8 × 2 (60 K) phases.     

The influence of the oxygen exposure on the thermal faceting of W[1 1 1] tip

The oxygen induced faceting of the macroscopic W[1 1 1] tip has been studied for oxygen exposures in the range 0.5-31 L and annealing temperatures 800-1800 K using the field ion microscopy (FIM) technique. After annealing at temperatures lower than 800 K, higher than 1850 K or for exposures lower than 0.5 L faceting was not observed. For exposures 0.5-1.9 L and annealing temperatures 800-1600 K well developed {1 1 2} facets with sharp edges formed. For exposures higher than 2.0 L edges of the {1 1 2} facets were broadening and disappearing, what has been attributed to the formation of three-dimensional tungsten oxides. The oxides could be easily removed by annealing the tip at 1700 K, what leads to formation of sharp facet edges. On the basis of these results a modified procedure of the ultrasharp tip fabrication has been proposed.     

Microstructural, optical and spectroscopic studies of laser ablated nanostructured tantalum oxide thin films

Thin films of tantalum oxide (Ta₂O₅) have been prepared by pulsed laser deposition technique at different substrate temperatures (300-973 K) under vacuum and under oxygen background (pO₂ = 2 × 10⁻³ mbar) conditions. The films are annealed at a temperature of 1173 K. The as-deposited films are amorphous irrespective of the substrate temperature. XRD patterns show that on annealing, the films get crystallized in orthorhombic phase of tantalum pentoxide (β-Ta₂O₅). The annealed films deposited at substrate temperatures 300 K and 673 K have a preferred orientation along (0 0 1) plane, whereas the films deposited at substrate temperatures above 673 K show a preferred orientation along (2 0 0) crystal plane. The deposited films are characterized using techniques such as grazing incidence X-ray diffraction (GIXRD), atomic force microscopy (AFM), micro-Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy and UV-visible spectroscopy. FTIR and micro-Raman measurements confirm the presence of Ta-O, Ta-O-Ta and O-Ta-O bands in the films. Grain size calculations from X-ray diffraction and AFM show a decrease with increase in substrate temperature. The variation of transmittance and band gap with film growth parameters are also discussed.