ion-beam techniques rbs: rutherford backscatteringmesonpi.cat.cbpf.br/e2012/arquivos/pg07/chapter 8...
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M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 11
RBS: Rutherford backscatteringERD: Elastic recoil detectionPIXE: Particle induced x-ray emissionPIGE: Particle induced gamma emissionNRA: Nuclear
reaction
analysisSTIM: Scanning Transm. Ion Microscopy SE: Secondary emission CH: Channeling
RBS
Ion beam
Target nucleus
PIXE
STIM
PIGESE
Ion-beam
techniques
Electrostatic
Accelerators
Van de Graaff
acceleratorPelletronTandem Van de Graaff
TECHNIQUE ION BEAM ENERGY(MeV)
PIXE H+ 1 -
4
RBS 4He+, H+ ≤
2
ERD 35Cl+, 20Ne+3He+, 4He+ 2 -
40
NRA H+, D+ 0.4 -
3
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 2
PIXE: A Novel Technique for Elemental Analysis Sven A. E. Johansson and John L. Campbell
Publisher: John Wiley & Sons, 1988
Materials Analysis using a Nuclear Microprobe M B H Breese, D N Jamieson and P J C King
Publisher: John Wiley & Sons, 1996
Handbook of Modern Ion Beam Materials Analysis Edited by Joseph R. Tesmer
and Michael Nastasi
Publisher: Materials Research Society, Pittsburgh, Pa., 1995
Handbook of X-Ray Spectrometry Edited by Rene E. Van Grieken
and Andrzej
A. Markowicz
Publisher:
Marcel Dekker, Inc., 2nd Edition, 2002
Some
literature
on ion
beam
analysis
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 33
Faraday cup
VacuumChamber
Annular particledetector (for ERDA)
Target
Ge(Li) γ-ray detector(for PIGE)
Annular particleDetector (for RBS)
Collimators
Si
(Li) x-ray detector(for PIXE)
Ion beam
ElectrostaticAccelerator
Experimental Setup for Ion Beam Analysis
H, . . . ,U(eV
-
MeV)
Detectors: ΔESi (Li) 120 –
200 eVGe (high purity) 120 –
600 eVSi (drift chamber) 150 –
200 eVCrystal spectrometer
1 eV
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 44
Electrostatic
Accelerator
High VoltageGenerator
TargetIon beamVacuum
Vessel
Ion source
Ground
E field
Kinetic
particle
energy: Ekin
= q U = Ze
U
Van de Graaff: U ≤
10
MVTandem: U ≤
20
MV
Tandem Pelletron:
U ≤
30
MV
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 55
Van de Graaff
accelerator
≤
100 µA
≤
10
MV
ΔE/E ≥
10-3
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 66
Tandem van de Graaff
accelerator
Electron
stripping
in carbon
foil: -e → +N
e
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 77
Pelletron
charging
system
PelletronRubber belt is replaced by a chain of short conductive rods connected by insulating links. Can be operated at much higher velocity than a belt, so both the voltage and currents attainable are higher than a conventional Van de Graaff
machine.
Pelletron
Tandem DC voltage: ≤
30 MV
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 88
USP 8UD Pelletron
tandem
accelerator
Beam
energies
available
at Tsukuba
12UD Pelletron
tandem
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 9
TECHNIQUE ION BEAM ENERGY(MeV) REMARK
PIXE H+ 1 -
4Maximum sensitivity in atomic ranges 10<Z<35 and 75<Z<85
RBS 4He+, H+ ≤
2
Non-Rutherford scattering becomes significant for energy >2 MeV
ERDA35Cl+, 20Ne+3He+, 4He+ 2 -
40
Mass of incident ion must be greater than that of target nucleus. 3He+ and 4He+ are used only for the measurement of H.
NRA H+, D+ 0.4 -
3Reactions used include (p,g) (p,p'g), (p,ag), (d,p), (d,pg)
TYPICAL ION BEAMS AND INCIDENT ENERGIES USED IN VARIOUS ION BEAM TECHNIQUES
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 1010
Proton Induced X-ray Emission = PIXE
Lund Institute of Technology -
1970
MeV proton
Energy
hν
1s
2s
2p
3s
K
L1
L2,3
M1
Kα
Bohr:
Kα
-linehν
Z E(Kα) (keV)8 O 0.524920
Ca 3.6916840
Zr 15.775170
Yb 52.388992 U 98.439
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 11
PIXE System (Harvard) PIXE Spectra
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 1212
Raster generator
X-ray spectrometer
Quadrupole lens multiplet
forms image of aperture on sample
MeV
ion beam
Aperture
Sample
Scan coils
PIXE microscope
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 1313
SP Ca
Fe WTi
Nuclear microprobe PIXE elemental maps from 400 mm x 400 mm scanover a section of a lung tissue taken from a patient suffered from
hard metal lung disease:
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 1414
All elements with Z > 14 (Si)
(Kα= 1.73998 KeV) can be analyzed. For instance in biological samples the concentrations of about 15 elements are
normally determined
simultaneously.
The method is
fast.
A typical irradiation lasts about
10 min.
Highly sensitive:
Concentrations of elements down to
a few 100 ppb
(10-8)can be measured.
The spatial resolution of the beam is 1 mm.
The penetration depth in a solids: ~ 100 µm; allows determinations of
elemental distributions or profiles
High
accuracy: relative errors are between 1-10 %
Small-size samples
≥
few mg
Non-destructive technique: This enables analyses of precious objects, e.g. ancient coins or paintings.
PIXE features
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 15
Competition
to PIXE: Neutron Activation
Analysis (NAA)
109Ag+n ⇒110Ag* ⇒110Cd+ γ
(658 KeV)
Nuclear reactions3H(p,n)3He, 6Li(p,n)6Be, 7Li(p,n)7Be, 9Be(p,n)9B,
Neutron sourcesNuclear reactors
RadioisotopesSpontaneous fission Cf-252(α,n) reactionse.g. 241Am:Be
14N+n ⇒15N* ⇒15N+ γ
(10.8 MeV)
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 16
Neutron Activation
Analysis
Sensitivity
(picograms) Elements
1 Dy, Eu
1–10 In, Lu, Mn
10–100 Au, Ho, Ir, Re, Sm, W
100–1E3 Ag, Ar, As, Br, Cl, Co, Cs, Cu, Er, Ga, Hf, I, La, Sb, Sc, Se, Ta, Tb, Th, Tm, U, V, Yb
1E3–1E4 Al, Ba, Cd, Ce, Cr, Hg, Kr, Gd, Ge, Mo, Na, Nd, Ni, Os, Pd, Rb, Rh, Ru, Sr, Te, Zn, Zr
1E4–1E5 Bi, Ca, K, Mg, P, Pt, Si, Sn, Ti, Tl, Xe, Y
1E5–1E6 F, Fe, Nb, Ne
1E7 Pb, S
Gamma spectrum
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 17
( ) ⎥⎦
⎤⎢⎣
⎡
+=Λ=
⎩
φ22
21
21002 cos4
MMMMEEE
Coulomb
repulsion between high energy incident ions and target nuclei
RBS -
Rutherford Backscattering
Spectrometry
ERD –
Elastic
recoil
detection
M1
M2
φ
θ+= 210 EEE
p, α
E0
≤
2 MeV
( )( ) ⎪⎭
⎪⎬⎫
⎪⎩
⎪⎨⎧
+−+
==θθ
2
221
2221
001 /1sin/cos
MMMM
EKEE
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 1818
•
RBS –
Projectile is the detected particle M1
<<M2
–
Depth and mass information encoded on detected particle energy
Detector
Elastic RecoilDetection
(b)
M1
M2
Detector
BackscatteringSpectrometry
(a)
M1
M2
•
ERDA–
The target atom is the detected particle M1
>>M2–
Depth information encoded on energy
–
Isotopic identity carried directly by recoil
RBS vs. ERDA
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 1919
RBS (Rutherford Backscattering
Spectrometry)
Recoil
energy
substrate
metalimpurities
Intensity
E0
E1
0 20 40 60 80 100
0.0
0.2
0.4
0.6
0.8
1.0
E1/E0
E1/E
0
M2/M1
The
recoil
energy
depends
on the
target
mass
and the
path
length
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 20
RBS spectrum
of Ta implanted
in Si
Si (A=28)
Si
230 nm Ta
590 nm Ta (A=181)
0 20 40 60 80 100
0.0
0.2
0.4
0.6
0.8
1.0
E1/E0
E1/E
0M2/M1
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 2121
0 10 20 300.0
0.1
0.2
0.3
M2 (target) = 2
M2 (target) = 1
E 2/E0
M1 (projectile)
ERD –
Elastic
recoil
detection
Analysis of the
distribution
of light elements
(H, He, etc) in solids
M (projectile) > M (target)
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 22
Nuclear Resonant Reaction Analysis (NRRA)
NRRA with
the
15N(p,αγ)12C reaction
measures
the
hydrogen
concentration
Nuclear
reactions
with
sharp
resonances
are
usedto study
impurity
concentration
in solids
Example: The
reaction
1H(15N, αγ)12C
equiv.
15N(p,αγ)12C
6.2 6.3 6.4 6.5 6.6 6.7 6.8 6.9 710-1
100
101
102
103
104
105
Energy (MeV)
1H(15N,αγ)12C
cros
s se
ctio
n
6.400 MeV
4.44 MeV
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 23
Resonances
used
in NRRA
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 24
The
Channeling
Effect
Ion beam
p or
α
Single crystalle.g. Al2
O3
detector
Tilt
angle
coun
ts
M. Forker, Nuclear Methods in Solid State Research, CBPF 2012 2525
ß-
Determination of the
position
of implanted
ions
Emission channeling