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Introduction to IBA The RBS and ERD techniques Anastasios Lagoyannis Tandem Accelerator Laboratory Institute of Nuclear and Particle Physics N.C.S.R. Demokritos Outline Ion Beam Analysis Theoretical background Rutherford

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SLIDE 1

Anastasios Lagoyannis

Tandem Accelerator Laboratory Institute of Nuclear and Particle Physics N.C.S.R. “Demokritos”

Introduction to IBA – The RBS and ERD techniques

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SLIDE 2
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

Outline

  • Ion Beam Analysis
  • Theoretical background
  • Rutherford Back Scattering
  • Elastic Recoil Detection Analysis
  • Conclusions
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SLIDE 3

Pros / Cons

  • They are generally least destructive and are suitable for use with delicate materials.
  • They are to a certain extent multielementary and produce high‐accuracy quantitative

results.

  • They require little or no preparation of the sample with the result that a specimen (like

an artifact) could be directly analyzed.

  • Only very small quantities (mg) of sample are needed.
  • They permit the analysis of a very small portion of the sample by reducing the

diameter of the ion beam to less than 0.5 mm.

  • Some damage cannot be avoided (thermal, carbon buildup etc.)!
  • A VdG type of accelerator is required.
  • In most of the cases the experiments are carried out in vacuum chambers.
  • Several experimental issues need to be addressed, thus a minimum knowledge of

nuclear physics (experimental and theoretical) is mandatory.

  • No direct information about the chemical environment can be produced.
  • The analysis concerns only a few microns below the surface of the samples.
  • In most of the cases, a combination of techniques is required to solve a problem, and

this implies time consuming experiments!

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 4

Ion Beam Analysis

Ion Beam Analysis (IBA) is based on the interaction, at both the atomic and the nuclear level, between accelerated charged particles and the bombarded material. When a charged particle moving at high speed strikes a material, it interacts with the electrons and nuclei of the material atoms, slows down and possibly deviates from its initial trajectory. This can lead to the emission of particles or radiation whose energy is characteristic of the elements which constitute the sample material

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 5

Theoretical Background I

Nuclear Reaction:

The interaction between two nuclei which results in the emission of nuclei and/or gamma rays.

Cross Section:

σ =

tar

N

inc

Ω ꞏ ꞏ N N

det

The probability of a nuclear reaction to occur

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 6

Theoretical Background II

Loss of kinetic energy per length unit Inelastic collisions with the electrons and the nuclei

Energy Straggling: Scattering:

When a charged particle impinges on a material, it interacts with the electrons and the nuclei of the material. The result of the interaction is the loss of energy and the change of trajectory of the initial ion.

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 7

Theoretical Background II

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 8

Depth Profiling

YES

  • Rutherford Backscattering Spectroscopy (RBS)
  • Nuclear Backscattering Spectroscopy (NBS)
  • Elastic Recoil Detection Analysis (ERDA)
  • Nuclear Reaction Analysis (ΝRA)

NO

  • Charged Particle Activation Analysis (CPAA)
  • Particle Induced X‐Ray Emission (PIXE)
  • Neutron Activation Analysis (NAA)
  • Secondary Ion Mass Spectroscopy (SIMS)
  • Particle Induced γ –Ray Emission (PIGE)
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 9

The 5.5 MV VdG Tandem accelerator @ I.N.P.

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 10

Tandem Layout

γ ‐ calorimetry external beam μ‐PIXE RBS , NRA, ERDA … Charged‐particle induced X rays Auger Spectrom. Atomic physics multipurpose scattering chamber 4 HPGe detect. array γ ‐ spectrometry charged‐part. irradiations d‐filled gas‐cell Tritiated Ti‐target (rotating) neutron irradiations

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 11

AGLAE

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

Accelerateur Grand Louvre d’ Analyse Elementaire

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SLIDE 12

Sample Size Selection

There are three possibilities

Under Vacuum Small samples (1 to 10 cm) Can withstand vacuum (no wood) Preferably good electrical conductivity Greater accuracy External Beam No size limitation No vacuum conditions Flow of He Limited accuracy Microbem Small samples (less than 1 cm) Elemental mapping possibilities

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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External Beam Setup

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 14

Rutherford Backscattering Spectroscopy

Rutherford backscattering (RBS) is ideal for depth‐profiling heavy elements on lighter substrates. The beam ions impinge on the sample and they are Elastically Back Scattered Identification of material The identification of the sample Is done with the use of basic ideas: Conservation of Energy and Momentum High sample Ζ Higher Energy at the scattered beam

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 15

Rutherford Back Scattering

Quantification

N =

tar

N

inc

Ω ꞏ ꞏ σ N

det

Unknown The detected ions (known) Detector’s solid angle (known) Number of beam’s particles (known) Cross section (Analytical form unknown)

EXCEPT for

RUTHERFORD Cross Section

dσ z Z e ꞏ ꞏ 4πε dΩ

2( 1

4E )

2

1 sin

4 θ

2 =

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 16

Detection Apparatus

Most commonly used detectors are Surface Barrier Detectors (SSB)

  • Various thicknesses (μm) and apertures (mm2)
  • They work only under high vacuum
  • Can detect the energy of the particle (resolution ~ 15 keV)
  • Can’t detect the mass of the particle

Beams used

  • Protons from 0.5 to 3 MeV Probe larger depths
  • Heavier ions (12C, 160) 10 to 20 MeV Probe only surface layers

Higher mass resolution Higher depth resolution Sample considerations

  • Small size ( few cm)
  • Capable of being under vacuum (no wood e.t.c.)
  • Preferable good electrical conductivity
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 17

Experimental Setup

Motor driven goniometer Great angular accuracy (0.01 deg.) Up to 4 targets Water cooling available Motor driven goniometer Suitable for channeling studies 4 – axis target movement Place for PIGE detector

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 18
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

M1 < M2

  • r

Conceptual Examples

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  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

1200 1300 1400 1500 1600 1700 1800 1000 2000 3000 4000 5000 6000 7000 8000 9000

Counts Channel

200 400 600 800 1000 1200 1400 1600 20000 40000 60000 80000

Counts Channel

Conceptual Examples

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  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

800 1000 1200 1400 1600 1800 1000 2000 3000 4000

Counts Energy

800 1000 1200 1400 1600 1800 1000 2000 3000 4000

Counts Energy

Conceptual Examples

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  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

400 600 800 1000 1200 1400 1600 1800 5000 10000 15000

Counts Channels Cu Si Total

400 600 800 1000 1200 1400 1600 1800 2000 4000 6000

Counts Channels Cu Si Total

Conceptual Examples

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SLIDE 22

Conceptual Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

400 600 800 1000 1200 1400 1600 1800 5000 10000 15000 20000 25000

Counts Channel Cu Si Total

600 800 1000 1200 1400 1600 1800 2000 4000 6000 8000 10000 12000 14000

Counts Energy Si Cu

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SLIDE 23

Conceptional Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

2 MeV 4He, θ=165o

C h a n n e l

5 20 500 48 0 4 60 44 0 4 20 400 3 80 360 34 0 3 20 30 0 2 80 260 24 0 2 20 20 0 1 80 160 1 40 120 10 0 8 0 60

Counts

2,0 00 1,9 00 1,8 00 1,7 00 1,6 00 1,5 00 1,4 00 1,3 00 1,2 00 1,1 00 1,0 00 900 800 700 600 500 400 300 200 100 4 00 600 800 10 00 12 00 1 400 1 600 180 0 200 0 22 00 24 00 2 600

E n e rg y [k e V]

Au on SiO2

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SLIDE 24

Conceptional Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

2 MeV 4He, θ=165o

Channel

520 500 480 460 440 420 400 380 360 340 320 300 280 260 240 220 200 180 160 140 120 100 80 60

Counts

2,000 1,900 1,800 1,700 1,600 1,500 1,400 1,300 1,200 1,100 1,000 900 800 700 600 500 400 300 200 100 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600

Energy [keV]

Au/SiO2 multilayers

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SLIDE 25

Conceptional Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

Experimental Simulated O Na Mg Al Si Ca

Channel

300 290 280 270 260 250 240 230 220 210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10

Counts

300 290 280 270 260 250 240 230 220 210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 100 200 300 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500

Energy [keV]

Soda-lime glass 2 MeV 4He, θ=165o

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Examples

Sulphate mineral surfaces (e.g. gypsum) and dissolved heavy metal ions (e.g. Pb2+)

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 27

Proton beam examination of glass – an analytical contribution for preventive conservation

Examples

Proton beam examination of glass – an analytical contribution for preventive conservation

  • M. Mader et al. NIMB 226 (2004) 110
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 28

External Beam Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 29

External Beam Examples

Review of accelerator gadgets for art and archaeology

  • T. Calligaro et al. NIMB 226 (2004) 29
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 30

External Beam Examples

Review of accelerator gadgets for art and archaeology

  • T. Calligaro et al. NIMB 226 (2004) 29
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 31

The resolution is enhanced with the aid of a magnetic field

High Resolution RBS

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

Developments in RBS

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SLIDE 32

Mass resolution is enhanced due to the TOF technique

Time of Flight HI ‐ RBS

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

Developments in RBS

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SLIDE 33

Developments in RBS

300 ‐ 500 keV proton beam

“Benchtop” RBS

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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Elastic Back Scattering

500 1000 1500 2000 2500 3000 20 40 60 80 100

 / RUTH

Energy (keV)

Same as RBS with the difference That the cross section is not obeying Rutherford’s law Applicable only for specific combinations of beam and target nuclei and at very specific energies

12C (p,p) 12C

1000 1200 1400 1600 1800 2000 2200 8000 10000 12000 14000 16000 18000 20000

Counts Channels Rutherford Non - Rutherford

1200 1300 1400 1500 1600 14000 16000 18000 20000

Counts Channels Rutherford Non - Rutherford

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 35

Elastic Back Scattering

Applicable only for specific combinations of beam and target nuclei and at very specific energies

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 36

Examples

Metal oxide thin film technology

600 700 800 900 1000 1100 1200 200 400 600 800 1000 1200 1400 1600 1800

Ni O Counts Ed (MeV) Experimental Simulated

SIMNRA simulation of a NRA spectrum of a NiO thin film Deuteron beam of 1.35 MeV Detection angle of 170o

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 37

Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

External-RBS, PIXE and NRA analysis for ancient swords

  • H. C. Santos et al. NIMB B 345 (2015) 42

Differences in manufacturing between a Damascus and a Japanese blade

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SLIDE 38

Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

External-RBS, PIXE and NRA analysis for ancient swords

  • H. C. Santos et al. NIMB B 345 (2015) 42

Typical RBS spectrum Spectrum after subtraction

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Nuclear Reaction Analysis

Use of nuclear reactions, (d,p), (d,α), (p,α), (α,p) etc. Usually with high enough Q‐values e.g. The ‘carbon problem’: RBS is weak, EBS can be applied only in certain cases (no

  • ther light elements present, no high‐Z matrix, very case‐specific measurements):

Channel

360 340 320 300 280 260 240 220 200 180 160 140 120 100 80 60 40 20

Counts

7,000 6,500 6,000 5,500 5,000 4,500 4,000 3,500 3,000 2,500 2,000 1,500 1,000 500 200 400 600 800 1000 1200 1400 1600 1800

Energy [keV]

12C

Thin layer 70% Au + 30% C on Au backing Ep=1.8 MeV (~resonance)

Channel

700 650 600 550 500 450 400 350 300 250 200 150 100 50

Counts

150 145 140 135 130 125 120 115 110 105 100 95 90 85 80 75 70 65 60 55 50 45 40 35 30 25 20 15 10 5 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 3000 3200 3400

Energy [keV]

Ed=1.2 MeV

12C(d,p0)

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 40

Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

Analysis of Mexican obsidians by IBA techniques

  • G. Murillo et al. NIMB B 136-I 38 ( 1998) 888
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SLIDE 41

Examples

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

RBS and NRA with external beams for archaeometric applications

  • E. Ioannidou al. NIMB B 161±163 (2000) 730±736

Examination of patina layers on ancient steel

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SLIDE 42

Elastic Recoil Detection

Heavy ions are used as the ion beam Suitable for the detection of light elements on heavy substrates Detection of the light nuclei at forward angles In simple ERDA experiments necessary to use filters in front of the detector in order to stop the heavy beam ions

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 43

Elastic Recoil Detection

IBA and SIMS coupling to study glass alteration mechanisms

  • S. Djanarthany et al. Journal of Non-Crystalline Solids 353 (2007) 4830
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 44

Elastic Recoil Detection

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 45

Synopsis

  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”

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SLIDE 46

Conclusions

Summary

  • 1. Rutherford backscattering (RBS) is ideal for depth‐profiling heavy elements on

lighter substrates.

  • 2. Elastic recoil detection analysis (ERDA) is excellent for depth‐profiling very light

elements in thin films.

  • 3. Nuclear reaction analysis (NRA), is excellent for high resolution depth‐profiling of

specific isotopes.

Present Situation

  • 1. A lot of work is being done in PIGE and NRA.
  • 2. Micro‐beams and measurements in air (Louvre) have enhanced IBA capabilities.

Future Perspectives

  • 1. New techniques are always evolving (e.g. HR‐RBS).
  • 2. PIGE analytical algorithms?
  • 3. CAN WE SOLVE ALL THE PROBLEMS??? NO (BUT MANY YES…)
  • A. Lagoyannis

Institute of Nuclear and Particle Physics NCSR “Demokritos”