Description

The Abdus Salam International Centre for Theoretical Physics (ICTP), Trieste, Italy, in cooperation with the International Atomic Energy Agency (IAEA), Vienna, Austria, has organized an Advanced Worskhop on High Sensitivity 2D & 3D Characterisation and Imaging with Ion Beams, held in Trieste from 26 to 30 September 2016. 

Accelerator-based analytical techniques using focussed ion beams are very powerful and versatile tools for elemental characterisation and mapping of broad range of materials. Beside their multi-elemental and fairly non-destructive feature, recent developments with regard of the imaging and detection systems make their performance exclusive both from the respect of sensitivity, accuracy, high lateral and depth resolution as well as 2D and 3D mapping. New applications have recently opened up by using swift heavy ions to create secondary ions and perform mass spectrometry on these, and to provide molecular information beyond the elemental analysis. These developments are extremely powerful spectroscopic tools, often providing complementary information on the structure and composition of materials, being applied to a wide range of scientific problems in material science, microelectronics, biology, biomedicine, geology, environmental science and archaeometry.

In the past few years, the advances in ion optics have allowed the use focused ion beams down to spot sizes in the micro- and nanometer range. This technical advancement has remarkably increased the analytical capability of conventional spectroscopic techniques for materials analysis, both in terms of spatial resolution and sensitivity to composition and physical-chemical properties. However, it is important to note that it also enhances effects which are more or less negligible with standard ion beam analysis (millimeter beamsize). Other challenges are the analysis of nanostructures with standard Ion Beam Analysis (IBA) or multiple measurements using multiple detectors which become more and more widespread. Recent data evaluation code developments make it possible to improve the analytical results also at the sub-micrometer level, but it requires a coordinated effort to transfer the new knowledge into good practice in the laboratories. 

IBA is considered to be a non-destructive technique. With increased beam brightness at small spot sizes however, radiation damage can take place. This Workshop aimed to increase the awareness of the analysts and provide guidelines on how to minimize the effect of radiation damage during the analysis.

The Workshop seeked to review the state-of-the-art in the area of analysis. Theoretical basic principles, recent developments and applications and software developments have been covered. Beside lectures, practical sessions on data evaluation are planned. The Workshop has provided an advanced training and information exchange platform for early stage researchers interested in this important subject.

As a complementary technique, visit of the beamline Elettra-Sincrotrone Trieste has been part of the programme. 

Participants had an opportunity to present and discuss their results in a poster session. Scientific discussions have stimulated further development and co-operation among the participants.


LECTURERS:

Nuno P. BARRADAS
Instituto Superior Técnico, 
Lisbon, Portugal

Thomas CALLIGARO
C2RMF-AGLAE Laboratory, Paris, France

Pedro Luis GRANDE
Federal University of Rio Grande do Sul, Porto Alegre, Brazil

Luca GREGORATTI
ELETTRA, Trieste, Italy


TOPICS:

•	Total IBA: synergistic treatment of data from multiple IBA techniques
•	Learning and using state of the art codes to affect the IBA analyses
•	Pitfalls in IBA data analysis
•	Beyond elemental analysis; MeV-SIMS High resolution PIXE
•	Multi-elemental characterisation and 2D mapping 
•	Depth profiling and 3D tomography
•	Radiation effects/Radiation damage
•	Applications and case studies to material science, biology-biomedicine, geology, environmental science, art and archaeometry
•	How to choose the best tools for analysis

POSTER SESSION
Participants have presented the results of their research in the form of a poster.

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Participation upon selection/invitation only.

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Contact for any queries: ICTP secretariat, Nicoletta Ivanissevich
Go to day
  • Monday, 26 September 2016
    • 08:00 - 20:30 DAY 1
      • 08:00 REGISTRATION 30'
        Registration of paid participants: 
        from 8:00 to 8:30 a.m. ONLY visitors receiving financial support by the ICTP are requested to register their stay at the Leonardo da Vinci Building (lobby, main entrance).
      • 08:30 Opening of the Workshop and Introduction of the participants 1h0'
      • 09:30 Overview of the ICTP and IAEA relevant activities 30'
        Speakers: Sandro Scandolo (ICTP), Aliz Simon (IAEA)
      • 10:00 External nuclear microprobe specificities and challenges 1h0'
        Heritage samples specificities (e.g. uniqueness, fragility, complexity, sensitivity to beam-induced modification)
        Large artefacts, complex shape (positioning)
        Often cannot stand vacuum
        Artefact safety (handling and damage risk reduction, AIEA TM)
        Main addressed questions (e.g. provenancing, manufacture, preservation)
        Which IBA techniques is suitable for each question
        Photon-based: PIXE/PIGE/IBIL
        Particle-based: RBS/NRA/ERDA/SIMS
        Ion imaging added value compared to classical imaging techniques 
        Limiting factors in external IBA imaging (SRIM simulations)
        Protons and helium ions: probe size
        Energy straggling
        Review of exit window material and size, and practically achieved resolution
        Gas atmosphere (impact zone cooling)
        Charge monitoring
        Mechanical scan
        Lowering beam intensity
        Current challenges
        IBA imaging of non-flat (3D) surfaces
        Stereoscopic view using multiple detectors
        Gamma-ray and particle detectors acceptance improvement
        Use of heavy ion beams (e.g. 19F and 15N beams for NRA)
        Speaker: Thomas Calligaro (C2RMF - AGLAE Laboratory, Paris, France)
      • 11:00 FINANCIAL/ADMINISTRATIVE FORMALITIES - LUNCH BREAK 3h0' ( Enrico Fermi Building ground floor / lunch at LB cafeteria )
        Registered paid participants please go first to Operations Office (E. Fermi Building) open until 12:00 (also from 13:30 to 15:00), and as second step, if advised so by the Operations Office, to the nearby Bank open until 13:20 (and from 14:30 to 15:30).
        
        Participants not receiving ICTP financial support should register their visit with the Secretariat in office 232, second floor, Leonardo da Vinci Building, from 11:00 to 12:00.
      • 14:00 Implementation of External Ion Beam Imaging 1h0'
        Beam scanning implementation (magnetic deflection + mechanical displacement)
        Optimization of counting statistics and dwell time/pixel
        Motorized X/Y/Z sample holder
        Safety: large view/ microscope camera with recording
        He gas flow
        Magnetic deflector (PIXE for light elements)
        Optimal Filters
        Simultaneous techniques
        Beam charge monitoring techniques
        Radiation safety with external beams: rules and procedures
        Speaker: Thomas Calligaro (C2RMF - AGLAE Laboratory, Paris, France)
      • 15:00 Beyong Elemental Analysis: Elemental, Chemical and Molecular Imaging 1h0'
        Ion Beam Analysis techniques have traditionally been largely focussed at obtaining detailed information on the elemental constituents of a sample. For this they have a proven and highly successful track record. Many new materials problems are associated with molecular materials and elemental information alone often can not provide such useful information in these situations. The case for looking beyond just elemental analysis is given. A technique first noticed utilized in the 1970s called Plasma Desorption Mass Spectrometry (PDMS) is described. Both the successes of this technique and what it accomplished, and also how it failed to take-off commercially will be detailed. How it led to a new set of ambient pressure techniques such as Matrix Assisted Laser Desorption Ionisation (MALDI) and then very recently to a new molecular concentration imaging technique MeV-SIMS will be described.
        Speaker: Roger Webb (University of Surrey, Guildford, UK)
      • 16:00 Coffee break 30'
      • 16:30 Total IBA: Synergistic treatment of data from multiple IBA techniques (I) 1h0'
        The suite of techniques which are available with the small accelerators used for MeV ion beam analysis (IBA) range from broad beams, microbeams or external beams using the various particle and photon spectrometries (including RBS, EBS, ERD, STIM, PIXE, PIGE, NRA and their variants), to tomography and secondary particle spectrometries like MeV-SIMS. However, these techniques separately give only partial information – the secret of “Total IBA” is to find synergies between techniques used simultaneously which efficiently give extra information. The essential point is to be able to analyse all data self-consistently and automatically, including any number of spectra from any combination of the techniques supported, taken from the same sample, with the same depth profile. The main concepts will be expanded with practical examples. 
        Speaker: Nuno P. Barradas (Instituto Superior Técnico, Lisbon, Portugal)
      • 19:00 Informal reception 1h30' ( Adriatico Guest House - Terrace )
        All participants are cordially invited to an informal reception at the Adriatico Guest House cafeteria
  • Tuesday, 27 September 2016
    • 08:30 - 18:30 DAY 2
      • 08:30 Fundamentals of Energy Loss 1h0'
        Pedro L. Grande
        In this talk, a review of of the energy-loss physics of ions interacting with matter will be presented. Special attention will be given to the electronic stopping power and energy loss straggling processes, which are of fundamental importance for depth profilling and for 3D characterization of nano-structures using the energy loss spectrum taken with high energy resolution. 
        Speaker: Pedro L. Grande (Federal University of Rio Grande do Sul, Porto Alegre, Brazil)
      • 09:30 Total IBA: Synergistic treatment of data from multiple IBA techniques (II) 1h0'
        This lecture will provide  additional practical examples on total IBA.
        Speaker: Nuno P. Barradas (Instituto Superior Técnico, Lisbon, Portugal)
      • 10:30 Coffee break 30'
      • 11:00 Principles and application of MEIS 1h0'
        MEIS is an ion beam characterization technique capable to determine with subnanometric depth resolution elemental composition and concentration-depth profiles in thin films. This technique is widely used for analysis of microelectronic materials as well as for the determination of structural and vibrational parameters of crystalline surfaces. In this talk the principles of MEIS will be given and a comparison with other high resolution techniques will be shown. Applications for depth profilling of  thin and ultra thin films using ions and cluster ions will be provided and typical pitfalls will be discussed.
        Speaker: Pedro L. Grande (Federal University of Rio Grande do Sul, Porto Alegre, Brazil)
      • 12:00 3D Characterization with MEIS 1h0'
        Examples of the use of MEIS for the characterization of nanostructured materials through the software PowerMeis wil be given.  Some illustrative examples will be shown in this talk namely, characterization of Au and core-shell NPs exposed on the surface, system of buried NPs synthesized by ion implantation, swift-heavy ion-sputtered CaF2 nanoparticles, and finally trench arrays used to build 3D transistors. 
        Speaker: Pedro L. Grande (Federal University of Rio Grande do Sul, Porto Alegre, Brazil)
      • 13:00 Lunch break 1h0'
      • 14:00 Poster presentations: short oral presentation by each participant 2h0'
        Speaker: All participants and faculty
      • 16:00 Coffee break 30'
      • 16:30 POSTER SESSION 2h0' ( LB Terrace )
  • Wednesday, 28 September 2016
    • 08:30 - 13:00 DAY 3
      • 08:30 Pitfalls in IBA data analysis (I) 1h0'
        Ion beam analysis is a quantitative analytical group of techniques, and the purpose of this lecture is to show how to avoid many pitfalls that often prevent IBA techniques from determining elemental depth profiles accurately. In fact, IBA is fraught with pitfalls. There are very many things that can be done wrong or simply go wrong unless great care is taken. We will first address pitfalls coming from experimental issues, namely: lost beam and events, calibration of fixed parameters, unwanted target-beam interactions, and other effects. These are not only relevant, but in fact essential to data analysis, because problematic data that are not what the analyst thinks it is, will lead to wrong conclusions,  and it is often possible to  identify issues in the data during data analysis. Then we will address pitfalls related to data analysis itself. With codes such as NDF (DataFurnace), that include a great deal of advanced physics and effects, and allow the user to fit parameters such as beam energy, angles of scattering and of incidence, or even the stopping powers and cross sections, the scope for error increased enormously. At the same time, many new IBA users no longer have a heavy background in nuclear or ion beam physics, and reliance on computer programs is a given. We will use real life examples to illustrate some of the most common pitfalls in IBA data analysis, along with steps that can be taken to prevent or remedy such problems.
        Speaker: Nuno P. Barradas (Instituto Superior Técnico, Lisbon, Portugal)
      • 09:30 Pitfalls in IBA data analysis (II) - Calculation of uncertainty budget 1h0'
        One of the advantages of IBA techniques over many other competitive techniques is that quantification can often be made from first principles, leading to claims of high traceable accuracy. However, many published works do not quote uncertainties on the values reported, and when they do, it is very common that the uncertainties quoted reflect only the statistics of the experiment. In fact, statistics is just one source of uncertainty in IBA experiments, and almost always not the most important. The uncertainty budget is specified as a formal approach to the systematic evaluation of the uncertainty of a measurement. It is the statement of a measurement uncertainty, of the components of that measurement uncertainty and of their calculation and combination. The concepts involved will be described with special reference to IBA, and practical examples will be developed, explaining the practical steps of how to calculate realistic uncertainties in IBA.
        Speaker: Nuno P. Barradas (Instituto Superior Técnico, Lisbon, Portugal)
      • 10:30 Coffee break 30'
      • 11:00 Secondary Ion Mass Spectroscopy - SIMS, Cluster-SIMS and MeV-SIMS 1h0'
        The basic concepts behind SIMS will be provided. The underlying models of the molecular and ion ejection process will be given. The similarities and differences between MeV-SIMS and the more conventional cluster keV-SIMS will be given. Simulations of molecular ejection from molecular material due to deposited energy spikes will be used to demonstrate the underlying physical mechanisms behind the MeV and cluster keV-SIMS process. A description of what can be expected to be achieved from MeV-SIMS and cluster SIMS and their position in the great collection of materials analysis techniques in existence today. Comparison is made with other molecular concentration mapping techniques.
        Speaker: Roger Webb (University of Surrey, Guildford, UK)
      • 12:00 Lunch break 1h0'
    • 13:00 - 18:00 DAY 3: VISIT TO SYNCHROTRON ELETTRA
      Location: Elettra Sincrotrone Trieste
      • 13:00 Bus transfer to Synchrotron Elettra 1h0'
        Pick up from LB parking lot at 13:15
      • 14:00 Welcome and overview of Synchrotron-based analytical techniques and Elettra 1h0'
        Speaker: Luca Gregoratti (Elettra Sincrotrone Trieste)
      • 15:00 Laboratory visit 1h0'
        Speaker: Luca Gregoratti (Elettra Sincrotrone Trieste)
      • 16:00 The SYRMEP X-ray imaging beamline at Elettra: recent achievements and future perspectives 30'
        Speaker: Giuliana Tromba (Elettra Sincrotrone Trieste)
      • 16:30 Presentation of the TwinMic beamline 1h0'
        Speaker: Alessandra Gianoncelli (Elettra Sincrotrone Trieste)
      • 17:30 Departure from Elettra Sincrotrone and return to the ICTP 30'
  • Thursday, 29 September 2016
    • 08:30 - 17:30 DAY 4
      • 08:30 Depth profiling and 3D tomography for 3D RBS such as Corteo, Maria, and for calculation of depth resolution 1h0'
        The main concepts in RBS are the kinematic factor, the scattering cross sections, and the energy loss, which allow us to answer three fundamental questions about a sample: what elements are present in the sample?; how much of each element is present?; and where are the elements located? When combined with spatially resolved measurements (e.g. using a microbeam), in  principle it should be possible to derive 3D information about inhomogeneous samples  - this is RBS tomography, a concept proposed many years ago, but not fully realized. However, new methods of data evaluation now exist, that are opening up possibilities to the analyst. This lecture will first focus on the possibilities and methods behind RBS tomography, and then will go on to show how to calculate depth resolution as function  of depth, which is one of the essential limitations and factors to be considered in analysis.
        Speaker: Nuno P. Barradas (Instituto Superior Técnico, Lisbon, Portugal)
      • 09:30 State of the art codes to affect the IBA analysis 1h0'
        Data acquisition and software processing tools
        GeoPIXE
        DAN32
        PYMCA fast fitting, PCA, NNMA
        AGLAEMaps (automated processing of datacube series)
        Future: RBS and NRA image processing
        Speaker: Thomas Calligaro (C2RMF - AGLAE Laboratory, Paris, France)
      • 10:30 Coffee break 30'
      • 11:00 Radiation damage during analysis 1h0'
        Ion beam analysis is a characterisation technique that is not deliberately destructive.  However, an energetic beam of particles is used to probe the sample, and  energy is deposited in the sample with a possibility to cause radiation damage during analysis.   The question is, does it change the sample for analytical purposes? What is the damage mechanism and how it can be minimized.
        Speaker: Roger Webb (University of Surrey, Guildford, UK)
      • 12:00 Case study (I) - Materials science 1h0'
        This lecture will show case examples of IBA applied to materials science, demonstrating the capabilities of the techniques in demanding situations.
        Speaker: Nuno P. Barradas (Instituto Superior Técnico, Lisbon, Portunga)
      • 13:00 Lunch break 1h30'
      • 14:30 PowerMeis software 1h0'
        The use of cloud computing for the simulation of MEIS/RBS
        spectra is showed. The integration of PowerMEIS with a
        web server provides to users worldwide a platform to make and
        analyze simulations through any modern web browser. An
        asynchronos server algorithm handles simultaneous simulations,
        allowing for multiple users at the same time. This platform was
        extensively used for all MEIS spectra fittings during a recent
        MEIS Round Robin Table.
        Speaker: Pedro L. Grande (Federal University of Rio Grande do Sul, Porto Alegre, Brazil)
      • 15:30 Comparison of External Ion Imaging Techniques with Alternative Techniques 1h0'
        With laboratory-based chemical imaging techniques (e.g. X-ray radiography, SEM-EDX, Raman, MA-XRF)
        With large scale facility (e.g. Synchrotron, Neutron sources)
         Synchrotron Neutron source external IBA
        XRF  NAA  PIXE, PIGE
        XAS  n-Radiography RBS, NRA
        XRD  n-Diffraction IBIL
        Emerging techniques 
        Full field XRF MeV-TOF SIMS
        Speaker: Thomas Calligaro (C2RMF - AGLAE Laboratory, Paris, France)
      • 16:30 Coffee break 1h0' ( LB Terrace )
      • 16:30 IBA-clinic 1h0' ( LB Terrace )
        In this session the participants can freely ask for advice about technical problems,  how to chose the best technique(s) for analysis, data evaluation etc. 
        
        Please bring your problematic spectra and feel free to ask! 
        Speakers: Roger Webb, and all lecturers
  • Friday, 30 September 2016
    • 08:30 - 13:00 DAY 5
      • 08:30 Case study (II) - Nanomaterials 1h0'
        This lecture will show case examples of MEIS and IBA applied to materials science, demonstrating the capabilities of the techniques in demanding situations.
        Speaker: Pedro L. Grande
      • 09:30 Case study (III) - Cultural Heritage materials and objects 1h0'
        Inventory of Lapis lazuli mineral phases and associated trace elements: determination of Lapis provenance and authentication of artefacts of unknown provenance
        Coupled IBIL/PIXE study of pre-Columbian jadeite
        Speaker: Thomas Calligaro (C2RMF - AGLAE Laboratory, Paris, France)
      • 10:30 Coffee break 30' ( LB Terrace )
        Group photograph 
      • 11:00 Hands-on processing of data recorded on real samples using PYMCA 1h0'
        Comparison of PIXE and XRF imaging of paintings: analysis of a 19th copy of ‘La Bohémienne’ by Frans Hals.
        Insights on damage induced in the most sensitive constituents.
        Exploring safe limits for IBA imaging of paintworks.
        Processing state-of-the-art MA-XRF datacubes recorded on da Vinci masterpieces.
        Speaker: Thomas Calligaro (C2RMF - AGLAE Laboratory, Paris, France)
      • 12:00 Evaluation of the Workshop: Best poster award, and Closing of the Workshop 1h0'
        Speakers: Aliz Simon (IAEA), Sandro Scandolo (ICTP)