Surface amorphization, sputter rate, and intrinsic stresses of silicon during low energy Ga focused-ion beam milling

Transmission electron microscopy (TEM) is a standard technique to characterize microelectronic device structures. As structures shrink to the nanoscale, surface damage produced by focused ion beam (FIB) sample preparation destroying the region of interest and degrading the resolution of TEM images becomes increasingly a problem. The thickness of the damaged layer at the sidewalls of a prepared cross section is around 20-30 nm for silicon at typical beam energies of 30 keV. In order to reduce these artifacts to a minimum low beam energies have been proposed for FIB polishing. We use a combination of molecular dynamics simulations and experiments to assess the influence of the focused ion beam on the surface structure of silicon for beam energies ranging from 1-5 keV and a grazing angle of 10° typically used in low voltage FIB polishing. Under these conditions, the thickness of the amorphous layer depends linearly on the beam energy. Intrinsic surface stresses introduced by FIB are always tensile and of a magnitude of around 1 GPa.     

Progress of in-air microbeam system at the Wakasa Wan Energy Research Center

Modifications of an in-air microbeam system at the Wakasa Wan Energy Research Center designed to improve its performance are described. In the previous setup, a silicon nitride membrane (area: 1 × 1 mm²; thickness: 100 nm) was used for the beam exit window and the distance between the window and the sample was restricted to ?1.7 mm. Due to this restriction, the beam spot size obtained using the previous setup was 13 × 13 μm². To reduce the beam spot size, the beam exit window was replaced by a silicon nitride membrane (area: 3 (horizontal) × 2 (vertical) mm²; thickness: 200 nm). In this setup, the sample can be moved as close as 0.7 mm to the window, enabling a beam spot size of 7 × 6 μm² to be achieved. An additional Si-PIN X-ray detector was installed to estimate the relative number of beam particles. It detects X-rays from the beam exit window. The number of the X-rays from the beam exit window (which is proportional to the number of beam particles) is used for quantitative analysis and for online monitoring of the beam current. This system has the potential to be used for simultaneous particle-induced X-ray emission (PIXE) and particle-induced gamma-ray emission (PIGE) measurements and for studying dental medicine.     

Proton beam induced luminescence of silicon dioxide implanted with silicon

Light emission from a silicon dioxide layer enriched with silicon has been studied. Samples used had structures made on thermally oxidized silicon substrate wafers. Excess silicon atoms were introduced into a 250-nm-thick silicon dioxide layer via implantation of 60 keV Si⁺ ions up to a fluence of 2 × 10¹⁷ cm⁻². A 15-nm-thick Au layer was used as a top semitransparent electrode. Continuous blue light emission was observed under DC polarization of the structure at 8-12 MV/cm. The blue light emission from the structures was also observed in an ionoluminescence experiment, in which the light emission was caused by irradiation with a H₂⁺ ion beam of energy between 22 and 100 keV. In the case of H₂⁺, on entering the material the ions dissociated into two protons, each carrying on average half of the incident ion energy. The spectra of the emitted light and the dependence of ionoluminescence on proton energy were analyzed and the results were correlated with the concentration profile of implanted silicon atoms.     

Fabrication of smooth silicon optical devices using proton beam writing

This work gives a brief review of proton beam writing and electrochemical etching process for the fabrication of smooth optical devices in bulk silicon. Various types of structures such as silicon-on-oxidized porous silicon waveguides, waveguide grating and disk resonators have been produced. Optical characterization has been carried out on the waveguides for both TE and TM polarization using free space coupling at 1.55 μm. Various fabrication and processing parameters have been optimized in order to reduce the propagation loss to approximately 1 dB/cm. A surface smoothening technique based on controlled oxidation has also been used to achieve an RMS roughness better than 3 nm.     

On the comparison of three methods of assessing beam quality for broad beam in vitro cell irradiation

The interaction of charged particles with living matter has recently attracted increasing interest in the field of biomedical applications such as hadron therapy, radioprotection and space radiation biology. Particle accelerators are particularly useful in this area.In vitro radiobiological studies with a broad beam configuration require beam homogeneity. The goal is to produce a dose distribution given to a cell population that is as close to uniform as possible.In this paper, we compare the results of three devices used to assess the beam quality for broad beam irradiation: a passivated implanted planar silicon (PIPS) particle detector, a position-sensitive solid state detector, which is camera-like, and a solid state nuclear track detector (CR39).The first device is a PIPS detector of 300 μm nominal depletion depth and an entrance window with a thickness of about 500 Å. It is collimated with a 0.5 mm aperture and mounted in air on an XY moving table as close as possible to the exit window of the beam line.The second device is a CMOS position-sensitive detector (technological process 0.6 μm AMS CUA), 112 × 112 pixels, with 153 × 153 μm² pixel size. It allows the user to rapidly obtain dose uniformity over a surface of 1 × 1 cm². During uniformity and dose rate assessment it is placed in air at the PIPS location.For both detectors, beam profile was obtained for various proton fluxes (from ∼5 × 10⁴ to 10⁶ particles cm⁻² s⁻¹). Preliminary tests were made with CR39 using 4 MeV He⁺⁺ ions.Results are analysed using Poisson distribution and cell hit probability.     

Microstructure evolution of Ge implanted silicon oxide thin films upon annealing treatments

The structural evolution of silicon oxide films with Ge⁺ implantation was traced with a positron beam equipped with positron annihilation Doppler broadening and lifetime spectrometers. Results indicate that the film structure change as a function of the annealing temperature could be divided into four stages: (I) T < 300 °C; (II) 300 °C ? T ? 500 °C; (III) 600 °C ? T ? 800 °C; (IV) T ? 900 °C. In comparison with stage I, the increased positron annihilation Doppler broadening S values during stage II is ascribed to the annealing out of point defects and coalescence of intrinsic open volumes in silicon oxides. The obtained long positron lifetime and high S values without much fluctuation in stage III suggest a rather stable film structure. Further annealing above 900 °C brings about dramatic change of the film structure with Ge precipitation. Positron annihilation spectroscopy is thereby a sensitive probe for the diagnosis of microstructure variation of silicon oxide thin films with nano-precipitation.     

Visible light emission from silicon dioxide with implanted excess silicon

Light emission from silicon dioxide doped with excess silicon by silicon ion implantation was investigated. Photoluminescence of silicon dioxide after silicon ion implantation and subsequent annealing at temperatures exceeding 1000 °C was observed. Excitation with monochromatic light with wavelength ranging from λ = 488 nm to λ = 266 nm leads to wide wavelength band emission ranging from about 650 nm up to about 850 nm with a maximum located at about 750 nm. This red/infrared photoemission is attributed to silicon nanocrystals created in silicon dioxide matrix. However, the same material used in electroluminescent experiments emitted blue and green light as well. In this paper the results of photo- and ionoluminescence experiments will be presented. The interest of the paper is focused on the problem of identification of different regions in the structure responsible for light emission of different wavelengths.     

Volume reflection observations in bent crystals with 13 GeV/c particles

The article presents the results on the investigation of the channeling and volume reflection effects in a bent silicon crystal with 13 GeV/c positive and negative hadrons (mainly π+, p and π−) at the CERN PS T9 line. In particular, this is the first study carried out on volume reflection at this energy providing a deflection angle of 69.4 ± 4.7 μrad and an efficiency of 92.7 ± 3.3%, with positive particles.The measurements have been carried out on a bent silicon strip crystal, using a high precision tracking system based on microstrip silicon detectors; this setup is allowed to trigger on the desired beam portion and to select the incoming particle angular range. The article presents a brief introduction on the bent crystal phenomena, the experimental setup and the results of the measurements.     

A systematic study on analysis-induced radiation damage in silicon during channeling Rutherford backscattering spectrometry analysis

Channeling Rutherford backscattering spectrometry (RBS) is an essential analysis technique in materials science. However, the accuracy of RBS can be significantly affected by disorders in materials induced by the analyzing ion beam even under channeling mode. We have studied RBS analysis-induced radiation damage in silicon. A 140-keV H⁺ ion beam was incident along 〈1 0 0〉 Si axis at room temperature to a fluence ranging from 1.6 × 10¹⁶ cm⁻² to 7.0 × 10¹⁶ cm⁻². The evolution of the aligned yields versus fluences has been examined and found to agree well with a model proposed by us.     

Structural studies of silicon oxynitride layers formed by low energy ion implantation

Silicon oxynitride (Si_xO_yN_z) layers were synthesized by implanting ¹⁶O₂⁺ and ¹⁴N₂⁺ 30 keV ions in 1:1 ratio with fluences ranging from 5 × 10¹⁶ to 1 × 10¹⁸ ions cm⁻² into single crystal silicon at room temperature. Rapid thermal annealing (RTA) of the samples was carried out at different temperatures in nitrogen ambient for 5 min. The FTIR studies show that the structures of ion-beam synthesized oxynitride layers are strongly dependent on total ion-fluence and annealing temperature. It is found that the structures formed at lower ion fluences (∼1 × 10¹⁷ ions cm⁻²) are homogenous oxygen-rich silicon oxynitride. However, at higher fluence levels (∼1 × 10¹⁸ ions cm⁻²) formation of homogenous nitrogen rich silicon oxynitride is observed due to ion-beam induced surface sputtering effects. The Micro-Raman studies on 1173 K annealed samples show formation of partially amorphous oxygen and nitrogen rich silicon oxynitride structures with crystalline silicon beneath it for lower and higher ion fluences, respectively. The Ellipsometry studies on 1173 K annealed samples show an increase in the thickness of silicon oxynitride layer with increasing ion fluence. The refractive index of the ion-beam synthesized layers is found to be in the range 1.54-1.96.     

Investigation of MeV-Cu implantation and channeling effects into porous silicon formation

P-type (1 1 1) silicon wafers were implanted by copper ions (2.5 MeV) in channeling and random directions using ion beam accelerator of the Atomic Energy Commission of Syria (AECS). The effect of implantation direction on formation process of porous silicon (PS) using electrochemical etching method has been investigated using scanning electron microscope (SEM) and photoluminescence (PL) techniques. SEM observations revealed that the size, shape and density of the formed pores are highly affected by the direction of beam implantation. This in turn is seen to influence the PL behavior of the PS.     

Gamma-ray shielding and structural properties of PbO-SiO2 glasses

Gamma-ray attenuation coefficients have been determined experimentally using a narrow beam transmission method for the xPbO(1−x)SiO₂ (x = 0.45-0.70) glass system at 662, 1173 and 1332 keV photon energies. These values have also been obtained theoretically using the ‘mixture rule’ and the ‘XCOM’ computer software. The results have been used to calculate half value layer parameters. Gamma-ray shielding properties of PbO-SiO₂ glass samples have been compared with standard radiation shielding concretes. The molar volume, FTIR and acoustic investigations have been used to study the structural properties of the prepared glass system.     

On the understanding of positive and negative ionization processes during ToF-SIMS depth profiling by co-sputtering with cesium and xenon

In this paper, ionization processes of secondary ions during ToF-SIMS dual beam depth profiling were studied by co-sputtering with 500 eV cesium and xenon ions and analyzing with 25 keV Ga⁺ ions. The Cs/Xe technique consists in diluting the cesium sputtering/etching beam with xenon ions to control the cesium surface concentration during ToF-SIMS dual beam depth profiling. Several depth profiles of a H-terminated silicon wafer were performed with varying Cs beam concentration and the steady state Si, Xe and Cs surface concentrations were measured in situ by Auger electron spectroscopy. It was found that the implanted Cs surface concentration increases with the Cs fraction in the beam from 0% for the pure Xe beam to a maximum Cs surface concentration for the pure Cs beam. Secondly, the variation of the silicon work function, due to the Cs implantation, was measured in situ and during depth profiling as the shift of the secondary ion kinetic energy distributions. Finally, the positive and negative elemental ion yields generated by the Ga analysis beam were recorded and modeled with respect to varying Cs/Xe mixture. We found that the Si⁻ and the Cs⁻ yields increase exponentially with the decrease of the silicon’s work function while that of Cs⁺ and Si⁺ decrease exponentially, as expected by the electron tunneling model.     

Design of the thermal neutron beam for neutron radiography at the Syrian MNSR

Neutron beam design was studied at the Syrian reactor (MNSR, 30 kW) with a view to generating thermal neutron beam in the vertical irradiation sites for neutron radiography. The design of the neutron collimator was performed using MCNP4C and the ENDF/B-V cross-section library. Thermal, epithermal and fast neutron energy ranges were selected as <0.4 eV, 0.4 eV–10 keV, >10 keV, respectively. To produce a good neutron beam quality, bismuth was used as photon filter. In this design, the L/D ratio of this facility had the value of 125. The thermal neutron flux at the beam exit was about 2.548 × 10⁵ n/cm² s. If such neutron beam were built into the Syrian MNSR many scientific applications would be available using the neutron radiography.     

A single line linearly polarized source for Mössbauer spectroscopy

A single line source of linearly polarized radiation in a conventional Mössbauer setup working at room temperature with ⁵⁷Co in Cr matrix was constructed. The ordered Fe₃Si was used as a filter. The estimated degree of polarization of the source depends on the preparation and thickness of the polarizer. The best polarization degree (92 ± 8)% was achieved. The measurements with polarized radiation lead to significant simplification of the complex spectra and allow to study components arising from various polarizations separately. In particular, it is possible to extract Δm = (1, −1) and Δm = 0 transitions by use of a linearly polarized beam. Moreover polarized beam can be used for determination of texture parameters related to spatial arrangements of spins in the plane perpendicular to the radiation beam. Such parameters are not easily measurable by other methods. The Mössbauer spectra of invar Fe₆₅Ni₃₅ measured by monochromatic linearly polarized radiation are shown as an example.     

Characterisation of a pre-cell hit detector to be used in single cell irradiation experiments at the Lund Nuclear Microprobe

This paper describes the characterisation of an ultra-thin silicon semiconductor ΔE detector to be used as a pre-cell ion hit detector in single ion experiments on individual, living cells. The characteristics of interest for this specific application are the hit detection efficiency, which has to be close to 100% to enable bombardment with either a single ion or a counted number of ions, the beam spreading, which should be as small as possible to maintain the targeting accuracy, and the vacuum tightness, since the detector is intended, if possible, to be used simultaneously as vacuum window. The hit detection efficiency was shown to be above 99% when detecting alpha particles or 2 MeV protons, the increase in beam size was about 1 μm and the vacuum tightness was comparable to that of the Si₃N₄ wafer which is normally used as vacuum window, thus the ΔE detector fulfils the main criteria to function properly as a single ion hit detector.     

Formation of dislocation loops in silicon by ion irradiation for silicon light emitting diodes

We have studied the influence of the ion species, ion energy, fluence, irradiation temperature and post-implantation annealing on the formation of shallow dislocation loops in silicon, for fabrication of silicon light emitting diodes. The substrates used were (1 0 0) Si, implanted with 20-80 keV boron at room temperature and 75-175 keV silicon at 100 and 200 °C. The implanted fluences were from 5 × 10¹⁴ to 1 × 10¹⁵ ions/cm². After irradiation the samples were processed for 15 s to 20 min at 950 °C by rapid thermal annealing. Structural analysis of the samples was done by transmission electron microscopy and Rutherford backscattering spectrometry. In all irradiations the silicon substrates were not amorphized, and that resulted in the formation of extrinsic perfect and faulted dislocation loops with Burgers vectors a/2〈1 1 0〉 and a/3〈1 1 1〉, respectively, sitting in {1 1 1} habit planes. It was demonstrated that by varying the ion implantation parameters and post-irradiation annealing, it is possible to form various shapes, concentration and distribution of dislocation loops in silicon.     

The formation and evolution of vacancy-type defects in Ar-implanted silicon studied by slow-positron annihilation spectroscopy

The Doppler broadening spectrum of a silicon wafer was measured using a variable-energy positron beam to investigate the effects of vacancy-type defects induced by 180 keV Ar ion implantation. The S-parameter in the damaged layer decreases with annealing temperature up to 673 K, and then increases with annealing temperature from 673 to 1373 K. At low annealing temperatures ranging from room temperature to 673 K, argon-decorated vacancies are formed by argon atoms combining with open-volume defects at inactive positron sites. With further increase of annealing temperature, argon-decorated vacancies dissociate and subsequently migrate and coalesce, leading to an increase of S-parameter. Furthermore, the buried vacancy-layer becomes narrow with increasing annealing temperature. At 1373 K, the buried vacancy-layer moved towards the sample surface.     

Laser induced plasma plume imaging and surface morphology of silicon

Shot-to-shot variation in the characteristics of laser produced plasma plume and surface profile of N-type silicon (1 1 1) are investigated. In order to produce plasma, a Q-switched Nd: YAG laser (1064 nm, 10 mJ, 9-14 ns) is tightly focused on silicon target in air at room temperature. Target was exposed in such a way that number of laser shots was increased from point to point in ascending order starting from single shot at first point. Target was moved 2 mm after each exposure. In order to investigate shot-to-shot variation in the time integrated emission intensity regions within the plasma plume, a computer controlled CCD based image capture system was employed. Various intensity regimes were found depending strongly on the number of incident laser pulses. Plasma plume length was also found to vary with the number of pulses. The topographic analysis of the irradiated Si was performed by Scanning Electron Microscope (SEM) which shows the primary mechanisms like thermal or non-thermal ablation depend on the number of shots. Surface morphological changes were also studied in terms of ripple formation, ejection, debris and re-deposition of material caused by laser beam at sample surface. The micrographs show ripples spacing versus wavelength dependence rule [Λ ≈ λ/(1 − sin θ)]. Intensity variations with number of shots are correlated with the surface morphology of the irradiated sample.     

Scintillation light produced by low-energy beams of highly-charged ions

Measurements have been performed of scintillation light intensities emitted from various inorganic scintillators irradiated with low-energy beams of highly-charged ions from an electron beam ion source (EBIS) and an electron cyclotron resonance ion source (ECRIS). Beams of xenon ions Xe^q+ with various charge states between q = 2 and q = 18 have been used at energies between 5 and 17.5 keV per charge generated by the ECRIS. The intensity of the beam was typically varied between 1 and 100 nA. Beams of highly charged residual gas ions have been produced by the EBIS at 4.5 keV per charge and with low intensities down to 100 pA. The scintillator materials used are flat screens of P46 YAG and P43 phosphor. In all cases, scintillation light emitted from the screen surface was detected by a CCD camera. The scintillation light intensity has been found to depend linearly on the kinetic ion energy per time deposited into the scintillator, while up to q = 18 no significant contribution from the ions’ potential energy was found. We discuss the results on the background of a possible use as beam diagnostics, e.g. for the new HITRAP facility at GSI, Germany.