Combined Secondary Ion Mass Spectrometry Depth Profiling and Focused Ion Beam Analysis of Cu Films Electrodeposited under Oscillatory Conditions

The recrystallization behavior of Cu films electrodeposited under oscillatory conditions in the presence of plating additives was studied by means of secondary ion mass spectrometry (SIMS) and focused ion beam analysis. When combined with bis-(sodium-sulfopropyl)-disulfide (SPS), Imep levelers (polymerizates of imidazole and epichlorohydrin) show characteristic oscillations in the galvanostatic potential/time transient measurements. These are related to the periodic degradation and restoration of the active leveler ensemble at the interface. The leveler action relies on adduct formation between the Imep and MPS (mercaptopropane sulfonic acid)-stabilized CuI complexes that appear as intermediates of the copper deposition when SPS is present in the electrolyte. SIMS depth profiling proves that additives are incorporated into the growing film preferentially under transient conditions during the structural breakdown of the leveler ensemble and its subsequent restoration. In contrast, Cu films electrodeposited in the presence of a structurally intact Imep–CuI–MPS ensemble remain largely contamination free.

An adjustable focusing system for a 2 MeV H- ion beam line based on permanent magnet quadrupoles

A compact adjustable focusing system for a 2 MeV H- RFQ Linac is designed, constructed and tested based on four permanent magnet quadrupoles (PMQ). A PMQ model is realised using finite element simulations, providing an integrated field gradient of 2.35 T with a maximal field gradient of 57 T/m. A prototype is constructed and the magnetic field is measured, demonstrating good agreement with the simulation. Particle track simulations provide initial values for the quadrupole positions. Accordingly, four PMQs are constructed and assembled on the beam line, their positions are then tuned to obtain a minimal beam spot size of (1.2 x 2.2) mm^2 on target. This paper describes an adjustable PMQ beam line for an external ion beam. The novel compact design based on commercially available NdFeB magnets allows high flexibility for ion beam applications.

MeV ion beam lithography of biocompatible halogenated Parylenes using aperture masks

Parylenes are poly(p-xylylene) polymers that are widely used as moisture barriers and in biomedicine because of their good biocompatibility. We have investigated MeV ion beam lithography using 16O+ ions for writing defined patterns in Parylene-C, which is evaluated as a coating material for the Cochlear Implant (CI) electrode array, a neuroprosthesis to treat some forms of deafness. Parylene-C and -F on silicon and glass substrates as well as 50 μm thick PTFE were irradiated to different fluences (1×1013-1×10161×1013-1×1016 1 MeV 16O+ ions cm−2) through aperture masks under high vacuum and a low pressure (<10−3 mbar) oxygen atmosphere. Biocompatibility of the irradiated and unirradiated surfaces was tested by cell-counting to determine the proliferation of murine spiral ganglion cells. The results reveal that an oxygen ion beam can be used to pattern Parylene-C and -F without using a liquid solvent developer in a similar manner to PTFE but with a ∼25× smaller removal rate. Biocompatibility tests showed no difference in cell adhesion between irradiated and unirradiated areas or ion fluence dependence. Coating the Parylene surface with an adhesion-promoting protein mixture had a much greater effect on cell proliferation.

A detector based on silica fibers for ion beam monitoring in a wide current range

A detector based on doped silica and optical fibers was developed to monitor the profile of particle accelerator beams of intensity ranging from 1 pA to tens of µA. Scintillation light produced in a fiber moving across the beam is measured, giving information on its position, shape and intensity. The detector was tested with a continuous proton beam at the 18 MeV Bern medical cyclotron used for radioisotope production and multi-disciplinary research. For currents from 1 pA to 20 µA, Ce3+ and Sb3+ doped silica fibers were used as sensors. Read out systems based on photodiodes, photomultipliers and solid state photomultipliers were employed. Profiles down to the pA range were measured with this method for the first time. For currents ranging from 1 pA to 3 µA, the integral of the profile was found to be linear with respect to the beam current, which can be measured by this detector with an accuracy of ∼1%. The profile was determined with a spatial resolution of 0.25 mm. For currents ranging from 5 µA to 20 µA, thermal effects affect light yield and transmission, causing distortions of the profile and limitations in monitoring capabilities. For currents higher than ∼1 µA, non doped optical fibers for both producing and transporting scintillation light were also successfully employed.

Development of a low energy ion source for ROSINA ion mode calibration

The European Rosetta mission on its way to comet 67P/Churyumov-Gerasimenko will remain for more than a year in the close vicinity (1 km) of the comet. The two ROSINA mass spectrometers on board Rosetta are designed to analyze the neutral and ionized volatile components of the cometary coma. However, the relative velocity between the comet and the spacecraft will be minimal and also the velocity of the outgassing particles is below 1km∕s. This combination leads to very low ion energies in the surrounding plasma of the comet, typically below 20eV. Additionally, the spacecraft may charge up to a few volts in this environment. In order to simulate such plasma and to calibrate the mass spectrometers, a source for ions with very low energies had to be developed for the use in the laboratory together with the different gases expected at the comet. In this paper we present the design of this ion source and we discuss the physical parameters of the ion beam like sensitivity, energy distribution, and beam shape. Finally, we show the first ion measurements that have been performed together with one of the two mass spectrometers.

Fabrication of cone-shaped boron doped diamond and gold nanoelectrodes for AFM-SECM

We demonstrate a reliable microfabrication process for a combined atomic force microscopy (AFM) and scanning electrochemical microscopy (SECM) measurement tool. Integrated cone-shaped sensors with boron doped diamond (BDD) or gold (Au) electrodes were fabricated from commercially available AFM probes. The sensor formation process is based on mature semiconductor processing techniques, including focused ion beam (FIB) machining, and highly selective reactive ion etching (RIE). The fabrication approach preserves the geometry of the original AFM tips resulting in well reproducible nanoscaled sensors. The feasibility and functionality of the fully featured tips are demonstrated by cyclic voltammetry, showing good agreement between the measured and calculated currents of the cone-shaped AFM-SECM electrodes.

AMS-C14 analysis of graphite obtained with an Automated Graphitization Equipment (AGE III) from aerosol collected on quartz filters

AMS-14C applications often require the analysis of small samples. Such is the case of atmospheric aerosols where frequently only a small amount of sample is available. The ion beam physics group at the ETH, Zurich, has designed an Automated Graphitization Equipment (AGE III) for routine graphite production for AMS analysis from organic samples of approximately 1 mg. In this study, we explore the potential use of the AGE III for graphitization of particulate carbon collected in quartz filters. In order to test the methodology, samples of reference materials and blanks with different sizes were prepared in the AGE III and the graphite was analyzed in a MICADAS AMS (ETH) system. The graphite samples prepared in the AGE III showed recovery yields higher than 80% and reproducible 14C values for masses ranging from 50 to 300 lg. Also, reproducible radiocarbon values were obtained for aerosol filters of small sizes that had been graphitized in the AGE III. As a study case, the tested methodology was applied to PM10 samples collected in two urban cities in Mexico in order to compare the source apportionment of biomass and fossil fuel combustion. The obtained 14C data showed that carbonaceous aerosols from Mexico City have much lower biogenic signature than the smaller city of Cuernavaca.

Radiochemical determination of 129I and 36Cl in MEGAPIE, a proton irradiated lead-bismuth eutectic spallation target

The concentrations of the long-lived nuclear reaction products 129I and 36Cl have been measured in samples from the MEGAPIE liquid metal spallation target. Samples from the bulk target material (lead-bismuth eutectic, LBE), from the interface of the metal free surface with the cover gas, from LBE/steel interfaces and from noble metal absorber foils installed in the cover gas system were analysed using Accelerator Mass Spectrometry at the Laboratory of Ion beam Physics at ETH Zürich. The major part of 129I and 36Cl was found accumulated on the interfaces, particularly at the interface of LBE and the steel walls of the target container, while bulk LBE samples contain only a minor fraction of these nuclides. Both nuclides were also detected on the absorber foils to a certain extent (≪ 1% of the total amount). The latter number is negligible concerning the radio-hazard of the irradiated target material; however it indicates a certain affinity of the absorber foils for halogens, thus proving the principle of using noble metal foils for catching these volatile radionuclides. The total amounts of 129I and 36Cl in the target were estimated from the analytical data by averaging within the different groups of samples and summing up these averages over the total target. This estimation could account for about half of the amount of 129I and 36Cl predicted to be produced using nuclear physics modelling codes for both nuclides. The significance of the results and the associated uncertainties are discussed.