Thin Carbon Foils Research Articles

Probing the interaction range of electron beam-induced etching in STEM by a non-contact electron beam

Beside its main purpose as a high-end tool in material analysis reaching the atomic scale for structure, chemical and electronic properties, aberration-corrected scanning transmission electron microscopy (STEM) is increasingly used as a tool to manipulate materials down to that very same scale. In order to obtain exact and reproducible results, it is essential to consider the interaction processes and interaction ranges between the electron beam and the involved materials. Here, we show in situ that electron beam-induced etching in a low-pressure oxygen atmosphere can extend up to a distance of several nm away from the Ångström-size electron beam, usually used for probing the sample. This relatively long-range interaction is related to beam tails and inelastic scattering involved in the etching process. To suppress the influence of surface diffusion, we measure the etching effect indirectly on isolated nm-sized holes in a 2 nm thin amorphous carbon foil that is commonly used as sample support in STEM. During our experiments, the electron beam is placed inside the nanoholes so that most electrons cannot directly participate in the etching process. We characterize the etching process from measuring etching rates at multiple nanoholes with different distances between the hole edge and the electron beam.

Novel device to study double-alpha decay at the FRS Ion Catcher

A novel system has been developed to detect simultaneous double-alpha emission from purified and weightless sources. The system includes the collection of 224Ra low-energy recoils in purified helium buffer gas from the decay of 228Th. The recoil products are thermalized and collected in a cryogenic buffer gas cell and extracted into an RF-ion guide for mass selection. The mass-separated ions are implanted at low kinetic energy into a thin carbon foil placed between two large-area double-sided silicon strip detectors to observe correlated alpha-particle emission. The apparatus is described in detail, including insights into its experimental performance.

VADER: A novel decay station for actinide spectroscopy

A research programme focused on the study of the nuclear structure of actinide isotopes has recently been implemented at the IGISOL facility, University of Jyväskylä. Within this scope, a new decay station named VADER (Versatile Actinides DEcay spectRoscopy setup) has been developed and commissioned. The system consists of a compact array of silicon detectors, a liquid-nitrogen-cooled silicon lithium (Si(Li)) detector and three broad energy germanium detectors (BEGe), placed around a thin implantation carbon foil. The combined use of different detectors allows the measurement of α particles, conversion electrons and de-excitation γ rays in coincidence, enabling a full reconstruction of nuclear decay schemes. The measurement of basic nuclear decay observables provides a picture of the nuclear shell evolution in neutron-deficient actinides, and highlights the possible emergence of reflection-asymmetric shapes in the region.

Experimental benchmark data for Monte Carlo simulated radiation effects of gold nanoparticles. Part I: Experiment and raw data analysis

Electron emission spectra of gold nanoparticles (AuNPs) after photon interaction were measured over the energy range between 50 eV and 9500 eV to provide reference data for Monte Carlo radiation-transport simulations. Experiments were performed with the HAXPES spectrometer at the PETRA III high-brilliance beamline P22 at DESY (Hamburg, Germany) for photon energies below and above each of the gold L-edges, that is, at 11.9 keV, 12.0 keV, 13.7 keV, 13.8 keV, 14.3 keV, and 14.4 keV. The study focused on a sample with gold nanoparticles with an average diameter of 11.0 nm on a thin carbon foil. Additional measurements were performed on a sample with 5.3 nm gold nanoparticles and on reference samples of gold and carbon foils. Further measurements were made to calibrate the photon flux monitor, to characterize the transmission function of the electron spectrometer, and to determine the size of the photon beam. This allowed the determination of the absolute values of the spectral particle radiance of secondary electrons per incident photon flux. The paper presents the experimental and raw data analysis procedures, reviews the data obtained for the nanoparticle samples, and discusses their limitations.

Chemical Imaging of Organic Materials by MeV SIMS Using a Continuous Collimated Ion Beam

MeV SIMS is a type of secondary ion mass spectrometry (SIMS) technique where molecules are desorbed from the sample surface with ions of MeV energies. In this work, we present a novel system for molecular imaging of organic materials using a continuous analytical beam and a start trigger for timing based on the detection of secondary electrons. The sample is imaged by a collimated primary ion beam and scanning of the target with a lateral resolution of ∼20 μm. The mass of the analyzed molecules is determined with a reflectron-type time-of-flight (TOF) analyzer, where the START signal for the TOF measurement is generated by the secondary electrons emitted from a thin carbon foil (∼5 nm) placed over the beam collimator. With this new configuration of the MeV SIMS setup, a primary ion beam with the highest possible electronic stopping can be used (i.e., highest secondary molecular yield), and samples of any thickness can be analyzed. Since the electrons are collected from the thin foil rather than from the sample surface, the detection efficiency of secondary electrons is always the same for any type of analyzed material. Due to the ability to scan the samples by a piezo stage, samples of a few cm in surface size can be imaged. The imaging capabilities of MeV SIMS are demonstrated on crossing ink lines deposited on paper, a thin section of a mouse brain, and a fingerprint deposited on a thick Si wafer to show the potential application of the presented technique for analytical purposes in biology and forensic science.

Effect of molecular axis orientation of 3.6 MeV Si2+ projectiles on the ion-induced secondary electron emission from a carbon foil

We study ion-induced secondary electron emission from solid surfaces. This work focuses on the dependence of the energy distribution of secondary electrons on the orientation of Si-dimers impinging on thin carbon foils. The orientation was determined by the foil-induced Coulomb explosion method. Furthermore, the electron energy was measured with a retarding field analyzer. The correlation between the electron energy distribution and the cluster orientation was obtained through simultaneous measurements. A comparison of the electron energy distribution for parallel and perpendicular orientations indicated that the electron yields at an energy below 20 eV are lower for parallel orientation. This reduction can be explained by the orientation dependence of the energy loss of Si2+ in carbon. It was suggested that the orientation effect is due to the distant collision between the cluster and the target atom, in which low-energy electrons are produced.

Effects of background noise on fit parameters of plasma scattering angle distributions.

The presence of noise in plasma particle measurements by scientific instruments causes inaccuracies in the determined plasma bulk parameters. This study demonstrates and evaluates the effects of noise in the determination of typical distribution functions describing the scattering angles of plasma particles passing through thin foils. First, we simulate measurements of plasma particles passing through a thin carbon foil, considering that their scattering angles follow kappa-like distribution functions, as being addressed in previous studies. We work with these specific distributions because we can produce them in the laboratory. We add Poisson-distributed background noise to the simulated data. We fit the simulated measurements and compare the fit parameters with the input parameters. As expected, we find that the discrepancy between the initial parameters and those derived from the fits increases with the relative increase of the noise. The misestimations exhibit characteristic trends as functions of the signal-to-noise ratio and the input parameters. Second, we examine the scattering angle distributions measured with a laboratory experiment of protons passing through a thin carbon foil for different signal-to-noise ratios. These measurements support the simulation results, although they exhibit a larger discrepancy than found in the simulations. Finally, we discuss how we can improve the accuracy of estimated distribution parameters in space and ground-based applications by excluding data-points from the tails of the distribution functions. Although our results exhibit the effects of noise in a specific type of distribution functions, we explain that this technique can be applied to and optimized for other specific data-sets.

Development of an Energy-Sensitive Detector for the Atom Probe Tomography.

A position and energy-sensitive detector has been developed for atom probe tomography (APT) instruments in order to deal with some mass peak overlap issues encountered in APT experiments. Through this new type of detector, quantitative and qualitative improvements could be considered for critical materials with mass peak overlaps, such as nitrogen and silicon in TiSiN systems, or titanium and carbon in cemented carbide materials. This new detector is based on a thin carbon foil positioned on the front panel of a conventional MCP-DLD detector. According to several studies, it has been demonstrated that the impact of ions on thin carbon foils has the effect of generating a number of transmitted and reflected secondary electrons. The number generated mainly depends on both the kinetic energy and the mass of incident particles. Despite the fact that this phenomenon is well known and has been widely discussed for decades, no studies have been performed to date for using it as a means to discriminate particles energy. Therefore, this study introduces the first experiments on a potential new generation of APT detectors that would be able to resolve mass peak overlaps through the energy-sensitivity of thin carbon foils.

Sensitive multi-element profiling with high depth resolution enabled by time-of-flight recoil detection in transmission using pulsed keV ion beams

The potential of time-of-flight recoil detection for sensitive multi-element profiling of thin membranes and quasi-2D systems in transmission geometry using pulsed keV ion beams is assessed. While the time-of-flight approach allows for simultaneous detection of multiple elements, to the largest extent irrespective of recoil charge states, the keV projectile energies guarantee high recoil-cross sections yielding high sensitivity at low dose. We demonstrate the capabilities of the approach using 22Ne and 40Ar as projectiles transmitted through thin carbon foils featuring optional LiF-coatings and single-crystalline silicon membranes for different sample preparation routines and crystal orientations.Using a large position-sensitive detector (0.13 sr), a depth resolution below 6 nm and sensitivity below 1014 atoms/cm2 was achieved for H in a 50 nm thick silicon membrane. For crystalline targets, we show how the probability of creation and detection of recoils and their observed angular distribution depend on sample orientation.

Determination of phases of complex scattering amplitudes and two-particle structure factors by investigating diffractograms of thin amorphous foils

Abstract In this study we analyse diffractograms of elastically filtered images of thin amorphous foils of carbon, silicon and germanium using the weak object approximation. The use of this approximation leads to a contrast transfer function containing a phase η(u) depending on the spatial frequency u. Furthermore, the derivative of this phase is included in the envelope function of the contrast transfer function. The phase can be attributed to the breakdown of the first-order Born approximation leading to complex scattering amplitudes characterized by this phase η(u). We analyse contrast transfer characteristics to determine the phase of complex scattering amplitudes of carbon, silicon and germanium as a function of spatial frequency and to measure the two-particle structure factor of the corresponding amorphous specimens. The contrast transfer characteristics were calculated from diffractograms of focal series of elastically filtered images. The phases measured show a decay with increasing spatial frequency and additional oscillations. The results for the two-particle structure factor also decay with increasing spatial frequency and contain low local maxima. Both can be attributed to voids or inhomogeneities within the amorphous structure.

New approach to precisely measure [formula omitted]-ray intensities for long-lived fission products, with results for the decay of 95Zr

For many fission products, the γ rays emitted following β decay provide an easily-detectable signature that can be used to identify their quantities and distributions in a sample. As a result, γ-ray spectroscopy is often exploited to study fission-product yields, provided sufficiently accurate information on the γ-ray intensity is available. However, in many cases, the uncertainties in the existing nuclear data are large enough that they compromise the precision achievable for modern experiments and applications. To address this need, we have developed a new experimental method that is well suited to precisely measure absolute γ-ray intensities in the β decay of long-lived fission products. The approach involves the production of a radiopure sample by implantation of a mass-separated ion beam from the CAlifornium Rare Isotope Breeder Upgrade (CARIBU) facility on a thin carbon foil. The emitted β-decay radiation is detected with a 4π gas proportional counter and a meticulously efficiency-calibrated high-purity germanium (HPGe) detector. As a first measurement to demonstrate the approach, we studied the absolute γ-ray intensities of the strongest transitions following the β decay of 95Zr and its decay-daughter 95Nb, and determined them to fractional precisions of better than 1–2%. In addition, with a larger sample of activity produced through neutron irradiation of an isotopically-enriched Zr foil, we performed a high-precision measurement of the relative γ-ray intensities following the decay of 95Zr with just the HPGe detector. The sample-production method at CARIBU and the coincidence detection approach demonstrated here can be applied to study fission products with half-lives longer than a day, which includes isotopes important not only for nuclear-energy and national-security applications, but also for medical-isotope research and environmental monitoring.

Simultaneous assessment of energy, charge state and angular distribution for medium energy ions interacting with ultra-thin self-supporting targets: A time-of-flight approach

We demonstrate simultaneous measurements of the charge state, energy and angular distribution of keV ions in transmission experiments through self-supporting foils. Using a time-of-flight approach we have introduced an electrostatic deflection apparatus as an extension to existing medium energy ion scattering (MEIS) instrumentation. Different positive, neutral and negative charge states have been discriminated and quantified for initially singly charged beams of He, N, O and Ne in the energy range from 25 to 250 keV. In parallel, the ion energy after interaction with the target has been assessed for all detected particles, while particles can be discriminated by deflection angle. Self-supporting thin carbon foils were used as samples to benchmark our experiments with literature data where available.

Development and operation of an electrostatic time-of-flight detector for the Rare RI storage Ring

An electrostatic time-of-flight detector named E-MCP has been developed for quick diagnostics of circulating beam and timing measurement in mass spectrometry at the Rare-RI Ring in RIKEN. The E-MCP detector consists of a conversion foil, potential grids, and a microchannel plate. Secondary electrons are released from the surface of the foil when a heavy ion hits it. The electrons are accelerated and deflected by 90∘ toward the microchannel plate by electrostatic potentials. A thin carbon foil and a thin aluminum-coated mylar foil were used as conversion foils. We obtained time resolutions of 69(1) ps and 43(1) ps (standard deviation) for a 84Kr beam at an energy of 170 MeV/u when using the carbon and the aluminum-coated mylar foils, respectively. A detection efficiency of approximately 90% was obtained for both foils. The E-MCP detector equipped with the carbon foil was installed inside the Rare-RI Ring to confirm particle circulation within a demonstration experiment on mass measurements of nuclei around 78Ge produced by in-flight fission of uranium beam at the RI Beam Factory in RIKEN. Periodic time signals from circulating ions were clearly observed. Revolution times for 78Ge, 77Ga, and 76Zn were obtained. The results confirmed successful circulation of the short-lived nuclei inside the Rare-RI Ring.

Measurement of the 2+→0+ ground-state transition in the β decay of F20

We report the first detection of the second-forbidden, non-unique, $2^+\rightarrow 0^+$, ground-state transition in the $\beta$ decay of $^{20}$F. A low-energy, mass-separated $^{20}\rm{F}^+$ beam produced at the IGISOL facility in Jyv\"askyl\"a, Finland, was implanted in a thin carbon foil and the $\beta$ spectrum measured using a magnetic transporter and a plastic-scintillator detector. The $\beta$-decay branching ratio inferred from the measurement is $b_{\beta} = [ 0.41\pm 0.08\textrm{(stat)}\pm 0.07\textrm{(sys)}] \times 10^{-5}$ corresponding to $\log ft = 10.89(11)$, making this one of the strongest second-forbidden, non-unique $\beta$ transitions ever measured. The experimental result is supported by shell-model calculations and has significant implications for the final evolution of stars that develop degenerate oxygen-neon cores. Using the new experimental data, we argue that the astrophysical electron-capture rate on $^{20}$Ne is now known to within better than 25% at the relevant temperatures and densities.

Measurement of differential cross sections of deuteron elastic scattering on 31P for EBS purposes

The differential cross sections of deuteron elastic scattering on 31P were determined in the present work for the first time, in the projectile energy range Ed,lab = 900–2400 keV (in energy steps of ~10–30 keV), suitable for analytical purposes. The measurements were performed at the 5.5 MV TN11 HV Tandem Accelerator of N.C.S.R. “Demokritos”, Athens, Greece. The experimental setup consisted of five silicon surface barrier (SSB) detectors, placed at the angles between 130° and 170° (in steps of 10°) in a high-precision goniometer. The implemented target was a thin GaP layer evaporated on top of a thin carbon foil. The obtained differential cross-section datasets were benchmarked against a polished GaP crystal and the deviations from the corresponding ones using Rutherford’s formula will be discussed and analyzed.

Assessing the potentiality of the 250kV-SSAMS for stopping power measurements at low energies

Abstract Since 2012, a compact 250 kV Single Stage accelerator (250 kV-SSAMS) has been installed at Instituto de Fisica, Universidade Federal Fluminense, for radiocarbon analysis of natural samples. The system presents two magnets, for mass selection prior and post the gas stripper, and an electrostatic spherical analyzer (ESA). The overall performance of the machine makes it suitable for experimental researches in atomic collisions, in particular for studies of the stopping power of atomic projectiles at energies below 25 keV/u. Here we report on the energy loss measurements of 12C + and 16O + ions in a thin carbon foil at energies in the range of 10 to 25 keV/u. Energies of the ions after the foil are determined from the high-voltage applied to the ESA in order to recover the maximum intensity reading in a Faraday Cup (FC) after the ESA. Energies of the ions after the foil are determined from the high-voltage applied to the ESA. With this technique, experimental data for the stopping power within a precision of about 0.5%.

Measurements of 252Cf fission product energy loss through thin silicon nitride and carbon foils, and comparison with SRIM-2013 and MCNP6.2 simulations

Gas ionization detectors are very widely used for radiation detection and measurement, but for external sources an entrance window is used which can reduce particle energy. For heavy ions this energy loss can be significant enough to affect measurements and very thin windows, such as those composed of silicon nitride (SiN), may be utilized to minimize this effect. For fission spectroscopy, carbon conversion foils are also common in measurements. In the current work, energy losses were measured for 252Cf spontaneous fission products passing through thin foils of carbon and of silicon nitride. The foils ranged in from 22.5 to 131.0 µg/cm2 for C and from 56.4 to 402.2 μg/cm2 for SiN. For comparison, simulations were performed with the TRIM program in SRIM-2013 and with MCNP6.2. To understand calculation differences, effective charge from partial ionization was predicted by several methods and compared with results directly using the Bethe stopping power formula.

Enhanced Laser-Driven Ion Acceleration by Superponderomotive Electrons Generated from Near-Critical-Density Plasma.

We report on the experimental studies of laser driven ion acceleration from a double-layer target where a near-critical density target with a few-micron thickness is coated in front of a nanometer-thin diamondlike carbon foil. A significant enhancement of proton maximum energies from 12 to ∼30 MeV is observed when a relativistic laser pulse impinges on the double-layer target under linear polarization. We attributed the enhanced acceleration to superponderomotive electrons that were simultaneously measured in the experiments with energies far beyond the free-electron ponderomotive limit. Our interpretation is supported by two-dimensional simulation results.

Experimental technique for antiproton-nucleus annihilation cross section measurements at low energy

The interaction of very low energy antiprotons (ps) and antineutrons (ns) with nuclei is interesting for its influence on both fundamental cosmology and nuclear physics. Measuring the annihilation cross section of antimatter on matter can help in solving the universe matter-antimatter puzzle and could give relevant hints in the definition of strong interaction model parameters as well. The ASACUSA collaboration recently measured the antiproton-carbon annihilation cross section at 5.3 MeV of kinetic energy of the incoming antiproton. The experimental apparatus consisted in a vacuum chamber containing thin foils (~0.7-1 μm) of carbon crossed by a bunched beam of antiprotons from the CERN Antiproton Decelerator (AD). The fraction of antiprotons annihilating on the target nucleons gives origin to charged pions which can be detected and counted by segmented scintillators placed outside the chamber. This work describes the experimental details of the apparatus and the technique to perform the cross section measurements.

First observation of RDEC for gas (N2) targets with F9+

Radiative double electron capture (RDEC) is a fundamental atomic process predicted to occur in ion-atom collisions. Several attempts were made to show experimental evidence for RDEC after it was introduced theoretically in 1987. The first successful measurements were done for O8+ ions colliding with a thin carbon foil in 2010, followed by measurements for F9+ projectiles incident on carbon. The works reported here are the first observations giving preliminary results for RDEC in collisions of F9+ projectiles with gas (N2) targets. X-rays were observed in the region of interest and an estimation of RDEC cross section was calculated. These cross sections are compared with recent theoretical calculations.