Scanning transmission ion microscopy tomography at the Leipzig nanoprobe LIPSION

Scanning transmission ion microscopy (STIM) of joint cartilage could visualise single collagen fibrils. Thus, answers to the controversial questions of their alignment could be given. However, the fibrils form three-dimensional structures that are not yet fully disclosed. STIM tomography is needed to give more detailed information. The size of the structures requires a challenging resolution of about 100 nm. The first STIM tomographic experiment has been performed at the Leipzig nanoprobe LIPSION. 360 projections of a cartilage sample (30 μm×32 μm×10 μm) were taken. The pixel resolution was 250×250 pixels for each projection. The data set was reconstructed at MARC Melbourne using the backprojection of filtered projections technique. The data show the feasibility of STIM tomography in cartilage research. However, experimental inaccuracies (rotational displacement and magnetic stray fields) have limited the resolution thus far. Improvements in the experimental set-up will lead to higher resolution.     

Criticality in the fabrication of ion extraction system for SST-1 neutral beam injector

For the heating of plasma in steady-state superconducting tokamak (SST-1) (Y.C. Saxena, SST-1 Team, Present status of the SST-1 project, Nucl. Fusion 40 (2000) 1069–1082; D. Bora, SST-1 Team, Test results on systems developed for the SST-1 tokamak, Nucl. Fusion 43 (2003) 1748–1758), a neutral beam injector is provided to raise the ion temperature to 1 keV. This injector has a capability of injecting hydrogen beam with the power of 0.5 MW at 30 keV. For the upgrade of SST-1, power of 1.7 MW at 55 KeV is required. Further, beam power is to be provided for a pulse length of 1000S. We have designed a neutral beam injector (S.K. Mattoo, A.K. Chakraborty, U.K. Baruah, P.K. Jayakumar, M. Bandyopadhyay, N. Bisai, Ch. Chakrapani, M.R. Jana, R. Onali, V. Prahlad, P.J. Patel, G.B. Patel, B. Prajapati, N.V.M. Rao, S. Rambabu, C. Rotti, S.K. Sharma, S. Shah, V. Sharma, M.J. Singh, Engineering design of the steady-state neutral beam injector for SST-1, Fusion Eng. Des. 56 (2001) 685–691; A.K. Chakraborty, N. Bisai, M.R. Jana, P.K. Jayakumar, U.K. Baruah, P.J. Patel, K. Rajasekar, S.K. Mattoo, Neutral beam injector for steady-state superconducting tokamak, Fusion Technol. (1996) 657–660; P.K. Jayakumar, M.R. Jana, N. Bisai, M. Bajpai, N.P. Singh, U.K. Baruah, A.K. Chakraborty, M. Bandyopadhyay, C. Chrakrapani, D. Patel, G.B. Patel, P. Patel, V. Prahlad, N.V.M. Rao, C. Rotti, V. Sreedhar, S.K. Mattoo, Engineering issues of a 1000S neutral beam ion source, Fusion Technol. 1 (1998) 419–422) satisfying the requirements for both SST-1 and its upgrade. Since intense power is to be transported to SST-1 situated at a distance of several meters from the ion source, the optical quality of the beam becomes a primary concern. This in turn, is determined by the uniformity of the ion source plasma and the extractor geometry. To obtain the desired optical quality of the beam, stringent tolerances are to be met during the fabrication of ion extractor system.

SST-1 neutral beam injector is based on positive ion source. The extraction system consists of three grids, each having extraction area of (width) 230 mm × (height) 480 mm and 774-shaped apertures of 8-mm diameter. To obtain horizontal focal length of 5.4 m and vertical of 7 m, each grid consists of two halves with 387 apertures. Two halves are inclined at an angle of 1.07 ± 0.01°. For long pulse operation, active water cooling is provided by in-laid down of dense network of 22 wavy semicircular (r = 1.1 ± 0.05 mm) cooling channels in the space available between the apertures. The required flatness of the copper plate is 100 μm and positioning tolerance of aperture is ±60 μm. The measurement obtained after fabrication is compared with the specifications. It is pointed out that fabrication within set tolerance limit could be achieved only through process of fabrication and high-resolution measurements.     

Heavy ion and proton beams in high resolution imaging of a fungi spore specimen using STIM tomography

Scanning transmission ion microscopy (STIM) tomography as a 3-D imaging technique has been shown to have a range of applications. The energy of the transmitted ion is detected with nearly 100% efficiency as a function of position in the transverse plane. The parameters relating to transmitted ion energy loss in the sample are imaged with statistics given by the energy loss process rather than Poisson counting statistics. This enables very fast collection of a set of relatively noise-free 2-D images. Each image is collected after a small rotation of the sample, and a complete 3-D representation of the sample may be tomographically reconstructed. The small beam currents necessary mean that the technique is non-destructive. One of the fields where these non-destructive 3-D density structure maps are particularly useful is in the analysis of biological tissue. The variation of energy loss with projectile atomic number may be exploited to tune the energy loss contrast to the size and density of the sample (heavy ion STIM). This work develops this point, and applies it to the imaging of the microscopic structure of a 90 μm diameter mycorrhiza fungi spore. This specimen has been imaged non-destructively in 3-D using both a 36 MeV ¹²C beam and a 2.2 MeV proton beam, both with a spatial resolution of about 1 μm. The gain in contrast in the carbon median energy loss maps was dramatic as expected. The corresponding improvement in the tomogram was found to be visible but less dramatic. The tomographic sections as well as the median energy loss maps of the vesicular-arbuscular mycorrhiza fungi spore clearly show the internal structure. Wall morphology data has relevance to germination behaviour of the spores.     

The external beam microprobe facility in Florence: Set-up and performance

An external beam microprobe facility, based on a quadrupole doublet supplied by Oxford Microbeam Ltd, has been installed on a new beamline at the 3 MV single-ended Van de Graaff accelerator in Florence. The goal was to obtain a beam with a spot size on target of 10–20 μm and a current in the order of at least 1 nA, in order to allow PIXE, PIGE and RBS elemental analysis in air or in a helium atmosphere. The beam was extracted from the vacuum lines through a 0.1 μm thick Si₃N₄ window to minimise lateral straggling. The design goals have been successfully achieved; the measurements of the beam spot characteristics in vacuum as well as in air and in helium atmosphere, are here reported.     

On the accuracy of element concentrations and masses of micron sized samples determined with the Heidelberg proton microprobe

We have already tested the reliability of element-normalized PIXE (Proton Induced X-ray Emission) data on small (10–100 μm) particles that we routinely obtain with the Heidelberg proton microprobe. Thus, we here discuss the accuracy of quantitative results, i.e., absolute concentrations inferred from PIXE analyses of such particles. We investigated and reduced the effects of mechanical vibrations and of the instability of the electronic devices on the achievable minimum beam spot. We implemented into our computer code a mapping software for qualitative element distributions (PIXE) and quantitative mass images using STIM (Scanning Transmission Ion Microscopy). The STIM images determine the area density required to calculate from PIXE spectra the absolute element concentrations in thin samples. The accuracy of absolute PIXE concentrations is tested by measurements on 15 μm soda lime glass microspheres. Finally, the complete results of PIXE and STIM analyses of an interplanetary dust particle (IDP) are described.     

Electronic excitation effects in CeO2 under irradiations with high-energy ions of typical fission products

In order to understand the formation mechanism of a crystallographic re-structuring in the periphery region of high-burnup nuclear fuel pellets, named as “rim structure”, information on the accumulation process of radiation damage and fission products (FPs), as well as high-density electronic excitation effects by FPs, are needed. In order to separate each of these processes and understand the high-density electronic excitation effects, 70–210 MeV FP ion (Xe^10–14+, I⁷⁺ and Zr⁹⁺) irradiation studies on CeO₂, as a simulation of fluorite ceramics of UO₂, have been done at a tandem accelerator of JAEA-Tokai and the microstructure changes were determined by transmission electron microscope (TEM). Measurements of the diameter of ion tracks, which are caused by high-density electronic excitation, have clarified that the effective area of electronic excitation by high-energy fission products is around 5–7 nm  and the square of the track diameter tends to follow linear function of the electronic stopping power (S_e). Prominent changes are hardly observed in the microstructure up to 400 °C. After overlapping of ion tracks, the elliptical deformation of diffraction spots is observed, but the diffraction spots are maintained at higher fluence. These results indicate that the structure of CeO₂ is still crystalline and not amorphous. Under ion tracks overlapping heavily (>1 × 10¹⁵ ions/cm²), surface roughness, with characteristic size of the roughness around 1 μm, is observed and similar surface roughness has also been observed in light-water reactor (LWR) fuels.     

Porous track cores along wakes of swift Pb ions in LiF

Continuous density decreases of 50% within 98 μm long and 3.2 nm wide cylindrical ion damage trails, latent ion tracks, created in a {1 0 0} LiF platelet by 2.31 GeV Pb ions, have been measured by small-angle X-ray scattering. Structural alteration is attributed mainly to radiolytic decomposition of the crystal into Li atoms and fluorine molecules, and subsequent transport and release of the fluorine gas through the low-density tracks. Free volume and Li residues undoubtedly account for the observed enhanced etchability of the track-core region.     

Superconductivity in MgB2 films synthesized by ablation from high-power ion beam

MgB₂ thin films with T_c = 19 K were fabricated by the ion ablation technique utilizing a high-energy pulsed ion beam. A target remains pure MgB₂ after ablation, proving the excellent capability of ablation by the high-power ion beam. Chemical compositions of the deposited material, however, may vary with positions of the substrates from the beam axis. X-ray diffraction patterns exhibit only (0 0 1) and (0 0 2) peaks, which indicate a c-axis orientation of the films. Scanning electron microscopy images show a possible growth of single crystals with hexagonal shape and 1 μm size.     

Axial ion–electron emission microscopy of IC radiation hardness

A new system for performing radiation effects microscopy (REM) has been developed at Sandia National Laboratory in Albuquerque. This system combines two entirely new concepts in accelerator physics and nuclear microscopy. A radio frequency quadrupole (RFQ) linac is used to boost the energy of ions accelerated by a conventional Tandem Van de Graaff–Pelletron to velocities of 1.9 MeV/amu. The electronic stopping power for heavy ions is near a maximum at this velocity, and their range is 20 μm in Si. These ions therefore represent the most ionizing form of radiation in nature, and are nearly ideal for performing single event effects testing of integrated circuits. Unfortunately, the energy definition of the RFQ-boosted ions is rather poor ( a few %), which makes problematic the focussing of such ions to the submicron spots required for REM. To circumvent this problem, we have invented ion electron emission microscopy (IEEM). One can perform REM with the IEEM system without focussing or scanning the ion beam. This is because the position on the sample where each ion strikes is determined by projecting ion-induced secondary electrons at high magnification onto a single electron position sensitive detector. This position signal is then correlated with each REM event. The IEEM system is now mounted along the beam line in an axial geometry so that the ions pass right through the electron detector (which is annular), and all of the electrostatic lenses used for projection. The beam then strikes the sample at normal incidence which results in maximum ion penetration and removes a parallax problem experienced in an earlier system. Details of both the RFQ-booster and the new axial IEEM system are given together with some of the initial results of performing REM on Sandia-manufactured radiation hardened integrated circuits.     

Scanning transmission ion microscopy of polycarbonate nanocapillaries

Polycarbonate membranes containing statistically scattered heavy ion track nanocapillaries have been studied by scanning transmission ion microscopy (STIM) method. The geometry of the samples was characterized by pore diameters of about 172 nm and by 30 μm membrane thickness. The porosity has to be relatively low in order to avoid too many overlapping capillaries. The transparency of the sample is reduced by changing its tilt angle to the beam. While the acceptance angle for transmission of a single capillary is below 0.3°, the STIM results have showed that the angular spread was about 1° full width at half maximum (FWHM). This indicates that the capillaries are not perfectly parallel, i.e. the capillary directions have a finite angular spread.Our results are important for the recent use of these types of insulator membranes in ion guiding studies, and the related potential applications.     

Heavy-ion-induced luminescence of amorphous SiO2 during nanoparticle formation

Silica glass was implanted with negative 60 keV Cu ions at an ion flux from 5 to 75 μA/cm² up to a fluence of 1 × 10¹⁷ ions/cm² at initial sample temperatures of 300, 573 and 773 K. Spectra of ion-induced photon emission (IIPE) were collected in situ in the range from 250 to 850 nm. Optical absorption spectra of implanted specimens were ex situ measured in the range from 190 to 2500 nm.

IIPE spectra showed a broad band centered around 560 nm (2.2 eV) that was assigned to Cu⁺ solutes. The band appeared at the onset of irradiation, increased in intensity up to a fluence of about 5 × 10¹⁵ ions/cm² and then gradually decreased indicating three stage of the ion beam synthesis of nanoclusters: accumulation of implants, nucleation and growth nanoclusters. The IIPE intensity normalized on the ion flux is independent on the ion flux below 20 μA/cm²at higher fluences. The intensity of the band increased with increasing samples temperature, when optical absorption spectra reveal the increase of Cu nanoparticles size.     

Ion beam induced charge characterisation of a silicon microdosimeter using a heavy ion microprobe

An ion beam induced charge (IBIC) facility has been added to the existing capabilities of the ANSTO heavy ion microprobe and the results of the first measurements are presented. Silicon on insulator (SOI) diode arrays with microscopic junction sizes have recently been proposed as microdosimeters for hadron therapy. A 20 MeV carbon beam was used to perform IBIC imaging of a 10 μm thick SOI device.     

Magnetic force microscopy studies on the magnetic ordering in organic materials induced by high-energy proton irradiation

In this study, ferromagnetic microstructures in highly oriented pyrolytic graphite and superparamagnetic spots in polyimide foils were created by 2.25 MeV proton microbeam irradiation and characterized using atomic and magnetic force microscopy. For this purpose, graphite samples were irradiated with cross-like patterns of 15 μm × 15 μm size using ion fluences in the range of (0.003–2.5) × 10¹⁸ cm⁻². The irradiated crosses showed strong magnetic signals and a complex domain structure in the magnetic images depending on the geometrical dimensions of the crosses. Furthermore, polyimide foils were irradiated with microspots and fluences in the range of (0.016–3.1) × 10¹⁹ cm⁻². Magnetic force microscopy shows very strong phase shifts in these irradiated areas.     

The Singapore high resolution single cell imaging facility

The Centre for Ion Beam Applications, National University of Singapore has recently expanded from three state-of-the-art beam lines to five. Two new beam lines have been constructed: A second generation proton beam writing line, and a high resolution single cell imaging facility. Both systems feature high demagnification lens systems based on compact Oxford Microbeams OM52 lenses, coupled with reduced lens/image distances.The single cell imaging facility is designed around OM52 compact lenses capable of operating in a variety of high demagnification configurations including the spaced Oxford triplet and the double crossover Russian quadruplet. The new facility has design specifications aimed at spatial resolutions below 50 nm, with a variety of techniques including STIM, secondary electron and fluorescence imaging, and an in-built optical and fluorescence microscope for sample imaging, identification and positioning.Preliminary tests using the single space Oxford triplet configuration have indicated a beam spot size of 31 × 39 nm in the horizontal and vertical directions respectively, at beam currents of ∼10,000 protons per second. However, a weakness in the specifications of the electrostatic scanning system has been identified, and a more stable scanning system needs to be implemented before we can fully realize the optimum performance. A single whole fibroblast cell has been scanned using 1.5 MeV protons, and a median fit to the proton transmission energy loss data has shown that proton STIM gives excellent details of the cell structure despite the relatively poor contrast of proton STIM compared with alpha STIM.     

Effect of annealing on the optical absorption of Ni nanoparticles in MgO single crystals

Ni⁺ ion implantation with an energy of 64 keV in MgO single crystals was conducted at room temperature up to a fluence of 1 × 10¹⁷ ion/cm². The as-implanted crystals were annealed isochronally at temperatures up to 900 °C. Optical absorption spectroscopy, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) have been utilized to characterize the changes of optical properties and the microstructure of the annealed samples. XPS results showed that the charge state of implanted Ni was still mainly in metallic Ni⁰ after annealing at 900 °C. TEM analysis revealed metallic Ni nanoparticles with depth-dependant dimensions of 1–10 nm in the annealed sample. Optical absorption spectroscopy indicated that the Ni nanoparticles exhibited a broad surface plasmon resonance absorption band in annealed samples and the band shifted to a longer wavelength with the increasing annealing temperature.     

Medium energy ion-nanoprobe with TOF-RBS for semiconductor process analysis

100–200 keV Be and Si ion beams from an ion-nanoprobe have been used to provide good lateral resolution and enhanced scattering cross section in Rutherford backscattering spectroscopy. A time-of-flight detecting system combining 1–2 ns beam pulses with a large area micro-channel-plate detector was installed to obtain high counting rates at moderate sample damage. A small (6 pC) measuring fluence, corresponding to a dose of 9×10¹² cm⁻², already results in useful spectra. Time resolution of 6 ns provides adequate mass and depth resolution, the latter around 0.06 μm for 100 keV Be in Si, while a chopping frequency of 100 kHz enables short measuring times.     

电子束辐照制备纳米镍

在水溶液中,常温常压下不加入任何催化剂,用电子束加速器辐照作为一种新的方法可成功制备纳米镍。利用X射线衍射(XRD)、透射电子显微镜(TEM)、激光衍射粒度分布仪(LSPSDA)、紫外可见光分光光度计(UV)、样品振荡磁力计(VSM)和差热分析仪(DSC)来分别表征材料的结构、形貌、大小、粒径分布、光学特征、磁学性能以及材料的熔点。TEM图像和LSPSDA分布图证明颗粒大小为39nm,这与XRD实验通过Scherer理论公式计算的结果相一致。     

Microbeam RBS on flat panel displays

We have demonstrated the utility of microbeam-Rutherford BackScattering (μ-RBS) in spatially resolved studies of operational plasma effects on the interior surfaces of plasma flat panel displays manufactured by Photonics Imaging. The experiments were performed at the Sandia Nuclear microprobe using a 2.8 MeV He beam with an average beam spot size of less than 8 μm. The interior surface of the top panes of the flat panels is composed of approximately 800 nm of MgO on top of a 2000 nm thick PbO layer. μ-RBS of sample panels operated under varying conditions measured changes in the surface MgO film thickness due to plasma erosion and redeposition as accurately as ± 1.5 nm. The high accuracy in the MgO thickness measurement was achieved by inferring the MgO thickness from the shift of the Pb front edge in the RBS spectrum. An estimate for the thickness accuracy as a function of the acquired statistics is presented. The surface of the flat panels' bottom panes is also comprised of MgO on top of PbO. However, troughs 100 μm wide by 10 μm deep were partially filled with phosphor and cover the entire width of the surface. This leaves only 100 μm long sections of MgO within the trough exposed. Using μ-RBS, we were able to analyze the surface composition of these regions.     

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.     

Corrosion of steels with surface treatment and Al-alloying by GESA exposed in lead–bismuth

Corrosion tests were performed for T91, E911 and ODS (oxide dispersion strengthened) with surface treatment and Al-alloying by pulsed electron beam (GESA—GepulsteElektronenStrahlAnlage) in flowing lead bismuth eutectic (LBE) with an oxygen content of 10⁻⁶ wt% at 550 °C for 2000 h. The result was that the surface treatment by GESA led to a faster growing multiphase oxide layer which was very homogenous in thickness. After exposure of specimens to LBE, the average oxide layer at the surface was 14–15 μm thick for ODS, 19–20 μm for E911 and 8–22 μm for T91. No dissolution attack occurred. On the surface of the Al-alloyed specimens, thin protective alumina layers were observed at the places where FeAl was formed by the GESA process, otherwise multiphase oxide layers or corrosion attack were observed.