Oxford Microbeams Research Articles

The radiobiology beam line facility at the Centre for Ion Beam Applications, National University of Singapore

A new beam line facility dedicated to investigations into the radiobiology of biological single cells has been constructed at the Centre for Ion Beam Applications, National University of Singapore. This facility, which has a horizontal layout, has some novel features including post lens magnetic ion deflection and scanning and provision for a diamond exit window and confocal fluorescence microscope for high performance online investigations.The radiobiology facility uses a system of Oxford Microbeam compact magnetic quadrupole lenses enabling high demagnifications (up to 123 × 51) at the cell plane, and a relatively short lens to cell distances (22.5 cm). Beam optics and SRIM calculations have indicated a theoretical design performance of up to 450 nm for the proton spot size at the cell surface.To measure the spatial resolution of the proton beam at the cell position, we positioned a gold calibration grid inside the external cell chamber at a position normally occupied by cells. Preliminary results were obtained by scanning a 2 MeV focused beam over a grid and using a surface barrier detector to construct a STIM image of the grid we have measured an in-air spot size of sub-500 nm at the cell position.In this paper, the design of the new radiobiology beam line, preliminary results of resolution tests, as well as presenting first investigations into the damage caused by focused proton beam irradiation of human liver cancer cells by detecting DNA damage markers gamma-H2AX and 53BP1.

A simple edge-following scanning algorithm for proton beam writing and other direct-write lithographies

The quality of the structures fabricated using proton beam writing (PBW) and other direct-write microfabrication methods is strongly influenced by the path followed by the writing beam during the exposure. In particular, it is necessary to avoid paths in which the beam makes large jumps or changes in direction close to the edges of the structure, and ideally the scan path should follow the outline of the pattern to be exposed (sometimes referred to as turtle scanning). While this is relatively easy to implement when the patterns to be created can be built up from simple geometric shapes (circles, rectangles, etc), it has not been possible to do this in the case of arbitrarily complex images, at least using software available to the PBW community.This paper describes a simple edge-following algorithm (EFA) which uses a method of spiral searching around each pixel to determine a scan path which not only optimizes the conformity of the scan path to the edges of the required pattern, but also minimizes jumps (and hence blanking time) and scan reversals which can cause artefacts due to scanning system transients. The EFA operates on a 1-bit BMP format input image file and has been implemented in the OMDAQ-3 software package (Oxford Microbeams Ltd).The paper is illustrated with examples of complex structures written using the EFA at the University of Surrey Ion Beam Centre which demonstrate enhanced edge smoothness compared with simple blanked raster scanning.

Development of a microbeam PIXE system for additive light elements in structural materials

A new submicron scanning nuclear microprobe beam line was constructed in early 2016 at the accelerator facility of the University of Tsukuba, Japan. A microbeam scanning endstage (OM-2000, Oxford Microbeams, Oxford, UK) was installed at the end of this system. The distance from the object slit to the target position is 8730mm and the working distance is 180mm. This ion microbeam system will be used mainly for X-ray imaging of two-dimensional distributions of light elements in structural materials using particle-induced X-ray emission (PIXE). A silicon drift detector (SDD) with a thin window of Si3N4 was installed to detect characteristic X-rays emitted from light elements such as B, C, and N, which are common additive elements in structural materials. In addition, a superconducting tunnel junction (STJ) array detector is going to be installed to perform PIXE measurements more efficiently. By combining a microbeam scanning technology with the X-ray detectors, we plan to obtain two-dimensional maps of additive light elements in structural materials. Experiments for obtaining proton microbeams are ongoing, and a 6MeV proton beam with a diameter of between 12 and 20μm has been obtained to date.

Development of a new in-air micro-PIXE set-up with in-vacuum charge measurements in Atomki

A new external microbeam set-up has recently been installed as the extension of the existing microprobe system at the Laboratory of Ion Beam Applications of Atomki, Debrecen, Hungary. The external beam set-up, based on the system of Oxford Microbeams (OM), is equipped with two X-ray detectors for PIXE analysis, a digital microscope, two alignment lasers and a precision XYZ stage for easy and reproducible positioning of the sample. Exit windows with different thicknesses and of different materials can be used according to the actual demands, currently silicon-nitride (Si3N4) film with 200nm thickness is employed in our laboratory. The first application was demonstrated in the field of archaeometry, on Bronze Age hoards from Hungary.

A gas ionisation Direct-STIM detector for MeV ion microscopy

Direct-Scanning Transmission Ion Microscopy (Direct-STIM) is a powerful technique that yields structural information in sub-cellular whole cell imaging. Usually, a Si p-i-n diode is used in Direct-STIM measurements as a detector. In order to overcome the detrimental effects of radiation damage which appears as a broadening in the energy resolution, we have developed a gas ionisation detector for use with a focused ion beam. The design is based on the ETH Frisch grid-less off-axis Geiger–Müller geometry. It is developed for use in a MeV ion microscope with a standard Oxford Microbeams triplet lens and scanning system. The design has a large available solid angle for other detectors (e.g. proton induced fluorescence). Here we report the performance for imaging ReNcells VM with μm resolution where energy resolutions of <24keV fwhm could be achieved for 1MeV protons using isobutane gas.

Micro-PIXE analysis system at NIRS-electrostatic accelerator facility for various applications

A micro-PIXE analysis system based on the ion beam analysis system by Oxford Microbeams Ltd. has been developed at the NIRS-electrostatic accelerator facility. The introduction of the CdTe X-ray detector dramatically improved the detection efficiencies for heavy elements that are important in the life sciences and environmental science. This system has been used for various projects and has provided several meaningful results, thus establishing the micro-PIXE system as an effective tool for the determination of elemental distribution with a high spatial resolution. In this paper, outline of the features of the micro-PIXE system at NIRS along with its recent application in research are introduced.

A new external microbeam system in Fudan University

A cost-effective and removable external beam system is set up based on the Oxford Microbeam system in Fudan University. In our external beam system, 7.5-μm-thick Kapton film is used as exit window with a diameter of 3.5mm. The spatial resolution is about 18μm full width at half maximum (FWHM) on a copper grid. As an example, calcium distribution in otolith is present by the external micro-PIXE. In addition, little change can be done to the external system mentioned above for radiobiology experiments. The exit window can be changed from the focal plane to the observation window of vacuum chamber. By calculation, the beam spot size can reach less than 30μm. Since the Oxford type octagonal target chamber is popular among the nuclear microprobe facilities, this method can be provided to easily replace the in-vacuum system with the external system, extending the in-vacuum analysis to external beam analysis.

A new external microbeam system in Fudan University

A cost-effective and removable external beam system is set up based on the Oxford Microbeam system in Fudan University. In our external beam system, 7.5-μm-thick Kapton film is used as exit window with a diameter of 3.5mm. The spatial resolution is about 18μm full width at half maximum (FWHM) on a copper grid. As an example, calcium distribution in otolith is present by the external micro-PIXE. In addition, little change can be done to the external system mentioned above for radiobiology experiments. The exit window can be changed from the focal plane to the observation window of vacuum chamber. By calculation, the beam spot size can reach less than 30μm. Since the Oxford type octagonal target chamber is popular among the nuclear microprobe facilities, this method can be provided to easily replace the in-vacuum system with the external system, extending the in-vacuum analysis to external beam analysis.

Editorial

Editorial

First results obtained using the CENBG nanobeam line: Performances and applications

A high resolution focused beam line has been recently installed on the AIFIRA (“Applications Interdisciplinaires des Faisceaux d’Ions en Région Aquitaine”) facility at CENBG. This nanobeam line, based on a doublet–triplet configuration of Oxford Microbeam Ltd. OM-50™ quadrupoles, offers the opportunity to focus protons, deuterons and alpha particles in the MeV energy range to a sub-micrometer beam spot. The beam optics design has been studied in detail and optimized using detailed ray-tracing simulations and the full mechanical design of the beam line was reported in the Debrecen ICNMTA conference in 2008. During the last two years, the lenses have been carefully aligned and the target chamber has been fully equipped with particle and X-ray detectors, microscopes and precise positioning stages. The beam line is now operational and has been used for its first applications to ion beam analysis. Interestingly, this set-up turned out to be a very versatile tool for a wide range of applications. Indeed, even if it was not intended during the design phase, the ion optics configuration offers the opportunity to work either with a high current microbeam (using the triplet only) or with a lower current beam presenting a sub-micrometer resolution (using the doublet–triplet configuration).The performances of the CENBG nanobeam line are presented for both configurations. Quantitative data concerning the beam lateral resolutions at different beam currents are provided. Finally, the first results obtained for different types of application are shown, including nuclear reaction analysis at the micrometer scale and the first results on biological samples.

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 50nm, 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 31×39nm 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 1.5MeV 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.

Technical description of the CENBG nanobeam line

Two years ago, the CENBG has commissioned the AIFIRA (Application Interdisciplinaire des Faisceaux d’Ions en Aquitaine) facility for the development of an interdisciplinary research program based on a 3.5 MV Singletron ™ accelerator (HVEE, The Netherlands). In addition to the existing beam lines, this facility is being equipped with a high demagnification focused beam line allowing the focusing of protons, deuterons and alpha particles down to a sub-micrometer resolution. This so-called “nanobeam line”, based on a long working distance doublet–triplet of Oxford Microbeams Ltd., OM-50 ™ quadrupoles, is at its final stage of development. The chosen layout of the beam line has been computed in details using the GEANT4 simulation toolkit. In the simulations, experimental measurements of the beam emittance at the entrance slits have been used to obtain more realistic beam distributions and intensities along the full beam line. According to these simulations, a beam resolution of about 300 nm in high current mode and below 100 nm in STIM mode is expected. The components of the beam line have been mounted at the 0° output of the Singletron ™ switching magnet and the fine alignment will be performed using the ion beam in the coming weeks. In the present paper, all the major components of the CENBG nanobeam line are described in details.

Applications to cultural heritage diagnostics at the new nuclear microprobe beam line at CEDAD

A nuclear microprobe beam line has been installed at CEDAD (Centre for Dating and Diagnostics), University of Salento, Lecce, Italy. The beam line is connected to the −30° port of the high energy switching magnet of a 3 MV HVEE 4130HC Tandetron accelerator. It is based on an Oxford Microbeam magnetic quadrupole triplet and its general features are presented. The results of functional tests are presented showing how a lateral spatial resolution as low as ∼2 μm has been achieved in vacuum by analysing standard reference material. The results obtained in the analysis of ancient radiocarbon dated biological tissues are presented for the identification and distribution of toxic elements such as Pb.

A detailed ray-tracing simulation of the high resolution microbeam at the AIFIRA facility

The AIFIRA (Applications Interdisciplinaires des Faisceaux d’Ions en Région Aquitaine) ion beam facility at the CENBG (Centre d’Etudes Nucléaires de Bordeaux-Gradignan) is being equipped with a high demagnification focused microbeam line. This beam line, which is under its final stage of development, should allow focusing of protons and alpha particles down to a sub-micrometer resolution, and is therefore referred to as a “nanobeam line” in the following paper.We present the complete beam transport simulation along the chosen configuration for the nanobeam line, which consists of a long working distance doublet–triplet of Oxford Microbeam Ltd. OM-50® quadrupoles. These simulations have been performed using the Geant4 Monte Carlo simulation toolkit, which has been previously validated for ray-tracing studies in the design of quadrupole microbeam systems. They include a fine modelling of the quadupole magnetic field, based on the analytical Enge’s model, which is compared to a classical square field model and to a high granularity tri-dimensional field map computed with the OPERA3D® software. The beam emittance model is parameterized from experimental measurements performed directly on the HVEE Singletron® at the AIFIRA facility, allowing the computation of the beam transmitted current along the nanobeam line. Grid shadow images, acquired from simulations, for system alignment purposes and beam deflection studies on target are presented as well.

The Fudan nuclear microprobe set-up and performance

A new scanning nuclear microprobe has been constructed at the Institute of Modern Physics in Fudan University, to replace the old microbeam system which had been running for more than ten years. The key parts were purchased from Oxford Microbeams Ltd., including triplet quadrupole lens (model OM-150), collimator slits, scanning system, target chamber, and data acquisition system. Ion beams are provided from a NEC 9SDH-2 Tandem accelerator. Three CCD cameras and multiple monitors were installed to assist beam adjust. The design of beam line and beam monitors is described. Beam optics calculations were carried out based on the specific Fudan microprobe system geometry, and the results regarding beam line performance and limitations of the spacial resolution are presented and discussed here. A comparison with experimental results is given as well. About 1.5 μm beam spot size could be achieved with a 3 MeV proton beam at a current of around 10 pA. Recently, the new microprobe is applied to obtain information of fly ash particle, algae cell and otoliths.

The new external microbeam facility at the 5 MV Tandetron accelerator laboratory in Madrid: beam characterisation and first results

This paper describes the new external microbeam on the 15° beamline of the 5 MV Tandetron accelerator recently installed at the CMAM in Madrid. The focusing and beam extraction system was supplied by Oxford Microbeams Ltd. and consists of a high precision quadrupole doublet with an interchangeable Kapton window exit nozzle and front-viewing video microscope. The sample is positioned in the beam using a stepper motor stage. The beam current and beam profile have been determined under different experimental conditions. A simple method based on the signal processing of ion-induced luminescence from quartz targets has been used to determine the beam profile in two dimensions simultaneously, without scanning. This is the first step in the development of a real time beam profile monitoring system, which could be used as part of an automated beam focusing procedure. The beam line will be primarily devoted to archaeometry and cultural heritage studies. As an example we report the characterisation of two Tang appearance antique porcelains.

The scanning microbeam PIXE analysis facility at NIRS

In March 1999, a HVEE Tandetron was installed in the Electrostatic Accelerator Building of National Institute of Radiological Sciences (NIRS) for particle induced X-ray emission (PIXE) analysis. The specifications of the Tandetron accelerator system operating at NIRS are as follows: the accelerating voltage is 0.4–1.7 MV, and the maximum beam current is 500 nA at 3.4 MeV. The accelerator facility incorporates three beam lines for conventional, in-air and microbeam PIXE analysis. The scanning microbeam PIXE analysis line is based around an Oxford Microbeams OM2000 nuclear microscope end stage. This system provides the ability of multi-elemental mapping over sample areas up to 2 × 2 mm area with spatial resolutions routinely at 1 × 1 μm. The scheduled operation of this facility started in April 2000 and is controlled by the Division of Technical Service and Development. The result of beam resolution tests carried out in 2001 are as follows: for scanning transmission ion microscopy, the estimated beam size is 100 × 200 nm, measured using a 2.6 MeV proton beam scanned over a 12.7 μm repeat distance copper grid. For PIXE operation at 50 pA beam current the estimated best spot size is 0.4 × 0.6 μm. The microbeam facility is being used for research into the elemental distribution of small biological samples such as biological cells and tissue.

The National University of Singapore high energy ion nano-probe facility: Performance tests

The Research Centre for Nuclear Microscopy, National University of Singapore incorporates three state-of-the-art beam lines, connected to a high brightness High Voltage Engineering Europa 3.5 MV Singletron accelerator. One of these lines is a NEC (National Electrostatics Corporation, USA) ion channeling facility, utilising broad beam ion beam analysis techniques for advanced materials research. The other two lines are microbeam facilities; one is designed for nuclear microscopy of biomedical samples and advanced materials, where relatively high currents (>50 pA) are required, and the other for proton beam micromachining (PBM) and materials modification, where lower currents can be utilised. The resolution performances of the two microbeam lines have been measured, and the results are as follows: (1) The nuclear microscope line incorporates the Oxford Microbeams OM2000 endstation with the OM50 quadrupole lenses configured in the high excitation triplet mode. This line has achieved the world’s best performances for analytical applications of 290 × 400 nm for a 50 pA current of 2 MeV protons. (2) The PBM line, which is the first of its kind worldwide, utilizes the new generation of compact (OM52) quadrupole lenses (Oxford Microbeams Ltd.) also configured in a high excitation, triplet configuration. This facility, which has superior demagnification properties, has achieved the world’s best performances for low current applications. Spot sizes of 35 × 75 nm have been measured using direct scanning transmission ion microscopy for beam currents of 10,000 protons per second.

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 Si 3N 4 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.

External microbeam set-up at the CNA (Sevilla) and its application to the study of Tartesic jewellery

A new external microbeam system has been installed recently at the +45° beam line of the 3 MV Pelletron accelerator at the Centro Nacional de Aceleradores (Sevilla, Spain). The facility, based on the system from Oxford Microbeams (OM), includes two sets of slits, a doublet of magnetic quadrupole focusing lenses, a Faraday cup and an accurate positioning device. In addition, a beam profile monitor (BPM) and a quartz viewer have been installed in the line to facilitate the microbeam production. The first PIXE application of the new facility was made in the field of Archaeometry, on the study of Tartesic gold artefacts (700–500 BC, SW of Spain) from Ébora and other archaeological sites. The aim of the analysis was to perform an exhaustive and systematic study about the soldering procedures that were employed by the goldsmiths along the Valley of Guadalquivir River after the Phoenician colonisation.