presentation a...title presentation a author iaea created date 11/3/2008 4:24:15 pm
TRANSCRIPT
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ANSTO Accelerator Capabilities for Materials Characterisation
Mihail Ionescu, Rainer Siegele, David [email protected]
IAEA Vienna15-19 Sept 2008
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Outline:
• ANSTO’s Ion Beam Accelerators
• Examples from ANSTO’s research projects on the use of accelerators for characterization of materials
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ANSTO’s Ion Beam Accelerators
ANTARES (Australian National Tandem for Applied Research). • Opened in September 1991.• 10 MV heavy ion machine (HVEE) with 3 ion sources and 5 high energy beamlines (2 IBA and 3 AMS).
• Can accelerate most ions in the periodic table (H- U)
STAR (Small Tandem for Applied Research). • Opened in January 2005.• 2 MV heavy ion machine (HVEE) with 3 ion sources and 3 high energy beamlines (2 IBA and 1 AMS 14C).
• Can accelerate (H, He, C)
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Ion Beam Accelerators Usage
• To provide accelerator based expertise for: - internally and externally driven research with
Australian Universities, CSIRO, Local and State Governments, industry and international organisations including the International Atomic Energy Agency (IAEA)
- training for local and international researchers, workshops, fellowships etc for developing countries in our region• Main techniques include:
- Ion Beam Analysis (IBA): PIXE, PIGE, RBS, ERDA, RToF, NRA and Heavy ion µ-probe (X-ray mapping; lithography; IBIC)
- Accelerator Mass Spectrometry (AMS) – 14C, 10Be, 26Al, 129I, Actinides
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ANTARES
ANTARES10 MV Tandem
HVEE 846multi sample
860single
NECalphatross
Microprobe
IBA-ToF
AMS: C, Be, Al
AMS:Actinides
10m• Microprobe: µ-PIXE; µ-RBS• ToF: Heavy ion ERDA; RBS; ion implantation• AMS: 14C, 10Be, 26Al, 129I, Actinides
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5m
STAR
• SIBA1: Automated PIXE; PIGE; RBS; PESA• SIBA2: He-ERDA; Variable angle RBS; NRA• AMS (14C) dating
358Ion Source
846BIon Source
2MV HVEETandetron Accelerator
AMS 14C
IBABeam line 1
IBABeam line 2
Ionisationchamber
Recombinator
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IBA Materials Projects at ANSTO• Elemental analysis (PIXE, PIGE)• Characterization of thin films near-surface layers and interfaces:
- thickness (RBS, NRA, variable angle RBS) - depth profile of elements (RBS, NRA, ERDA)- defects (variable angle RBS-channelling)- 2D mapping (µ-PIXE; µ-RBS)
• Modification of thin films, near-surface layers and interfaces:- ion implantation (conductive polymers; ZnO/STO; other)
• Device testing (IBIC, single event upset)Can do:
• Materials testing for radiation damage• Micro-machining• Ion beam induced chemical reactions
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PIXE, PIGE: Aerosols in AsiaPIXE, PIGE: Aerosols in Asia
Cheju Is.
Sado Is.D
ust
S
Hong KongHanoi
Manila
• Large throughput of samples• PMF→Source identification• Events correlation (back trajectories)• Large database
Lead vs Bromine Mascot 1992-2000
0200400600800
10001200
0 100 200 300 400 500Br (ng/m3)
Pb (n
g/m3 )
Pb=(2.12±0.30)*Br +(27±29)R2=0.98
Mascot 1992-2000
01002003004005006007008009001000
D ec - 90
D ec - 91
D ec - 92
D ec - 93
D ec - 94
D ec - 95
D ec - 96
D ec - 97
D ec - 98
D ec - 99
D ec - 00
Lead
(ng/m
3 )
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PIXE, PIGE: Study of Archaeological Artefacts [1]
• Non destructive• Large throughput • PMF→Source identification• Ancient trade routs identified
[1] T. Doelman, R. Torrence, V. Popov, M. Ionescu, N. Kluyev, I. Sleptsov, I. Pantyukhina, P. White and M. Clements, Geoarchaeology 23, 234, (2008)
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PIXE Bremsstrahlung [1]
[1] D. D. Cohen, E. Stelcer, R. Siegele, M. Ionescu, M. Prior, NIM B 266, 1149-1153, (2008) [2] K. Murozono, K. Ishii, H. Yamazaki, S. Matsuyama, S. Iwasaki, NIM B 150, 76, (1999)
• Important for quantitative analysis• Theoretical background calculated for 3MeV protons on C[2]
Be 1843 µg/cm2
C 1767 µg/cm2
• Data corrected for self absorption; detector efficiency; γ-ray background component and normalised to unit charge
(µC), unit solid angle (Sr) and unit target thickness (µg/cm2)• Normalised yield (Yld) was fitted to a 9-th order polynomial ln(Yld)=a0+a1ln Ex+a2 (ln Ex)2+…+a9(lnEx)9
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Heavy Ion MicroprobeHeavy Ion Microprobe• Spot sizes of 1-10µm• 1-10 nA target current• Focussing of ions with Me/q2 = 100 (H to U)• 2D mapping• Applications: 2D mapping (µ-PIXE, µ-RBS) Nuclear reactions Resonances Heavy Ion Elastic Recoil Detection IBIC Ion Beam Lithography
Au50 x 50 µm Cr
1-2 µm spot size at 100 pA; 3MeV H
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Elemental Mapping using the Ion MicroprobeElemental Mapping using the Ion Microprobe
PIXE Spectrum of Aerosol Filter
Exposed Filter
Unexposed Filter
soil
cars
sea spray FeS ores
50µm
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KCa Ni
Characterization of Characterization of MicrodosimetersMicrodosimeters by IBIC by IBIC [1][1]
Charge collection maps of 20 MeV C4+ beams onSilicon on Insulator (SOI) micro-dosimeters
K
[1] I. M. Cornelius, R. Siegele, I. Orlic, A. B. Rosenfeld, D. D. Cohen, NIM B 210, 191, (2003)
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Single Ion irradiation [1]
• Damage in tracks depend on LET• Diameter of a damage track is
~10nm • Used in single ion implant and high
resolution IB lithography
Low Medium HighPMMASi
Ion E (MeV)
LET elect
(eV/nm)LET nucl (eV/nm)
H 2 15 <0.1 MARCHe 2 150 0.1 MARCC 30 44 0.3 ANSTOC 9 760 0.8 ANSTOF 8 1380 2.8 ANSTOCu 6 1460 77 ANSTO
AFM
100nm
F damagetracks
[1] A. Alves, P. Reichart, R. Siegele, P. N. Johnston, D. N. Jamieson, NIM B 249, 730, (2006)
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Ni Uptake in Plants [1]
Ca
100 µm
Leaf cross-section scan : - current 0.8 nA- spot size 3 µm - count rate 2 kHz
• Study of Hybantus Floribundus- a Ni hyperaccumulator• Thin sections (~10 µm) freeze substitution• Localization of Ni in various parts of the plant
Ni
100 µm
50 µm
K[1] R. Siegele, A. G. Kachenko, N. P. Bhatia, Y. D. Wang, M. Ionescu, B. Singh, A. J. M. Baker, D. D. Cohen, X-ray Spectrometry 37, 133, (2008)
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RBS: multi-layer MgB2/Mg2Si/Al2O3 [1]
50 100 150 200 250 300
0.0
5.0x103
1.0x104
1.5x104
2.0x104
75o
8x 15
nm M
g 2Si
9x 80
nm M
gB2
Yield
[cts/2µC
]
Channel No
experimental simulated B O Mg Al Si
2MeV He1+
15o
C-Al 2
O 3
• Role of Mg2Si layers in increasing the pinning• comparison with single MgB2 film• Increase in activation energy U0• Increase in anisotropy of U0
[1] Y. Zhao, M. Ionescu, P. Munroe, S. X. Dou, APL 88, 012502, (2006)
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RBS: channelling in Si
200 400 600 800 1000 1200 1400
0
1000
2000
3000
4000
5000
RBS y
ield [
cts/20
0µC]
Energy [keV]
(101)
(111)
C
Surface
Surface
(101)1MeV He+
Detector
1MeV He+
Detector
(111)
• Study of Al-Ti-C MAX phase [1]• Part of C diffused in Si (001) substrate• A buried layer of C by channelling of 2MeV He+ in Si• Substrate replaced by MgO
[1] J. Rosen, P. O. A. Persson, M. Ionescu, A. Kondyurin, D. R. McKenzie, M. M. M. Bilek, APL 92, 064102, (2008)
50 100 150 200 250 300 350
0
100
200
300
400
500
600
700
C
Mg
Nd
Exp Simul C O Mg Al Ti Nd
Yield
[cts/1
.2µC
Channel No
Ti
Al
O in
MgO
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HeERDA-SBD: Hydrogen in SiNx thin film [1]
recoiled (H)
)( 22 EEEE foild ∆−=dxdExEE x
x1
12cosβ−=
−=dxdExEkE x
x0
01 cosα)( 11 EEEE foild ∆−=
E0x
At depth x:2
21
221
01 )(cos4MM
MMEE+
= θ
θσ
cos4)]([
22
20
221
221
MEMMeZZ
dd +=Ω
ΩΩ
=
ddN
ctsYcmatNi
σ
αcos][]/[ 2
Ed
E2
E0E1x
M1 (He)M2 (H)
αβ
θ E1
x
scattered (He)
recoiled (He)
At the surface:
Filter
Energy Detector
N- number of ions incident on sample surfaceΩ - detector solid angleσ - scattering cross section
0 200 400 600 800 1000
0
10
20
30
40
50
60
H Yie
ld [co
unts]
Energy [keV]
Si Wafer thin SiN thick SiN
He
H
S iSiN x
:H
S urfa
ce H
• Passivating role of Hydrogen in thin SiNx films
• Depth of analysis: up to few 100nm• Depth resolution: few nm• Sensitivity: ~0.1 at%
0 200 400 600 800 100005
10152025
Depth [x1015 at/cm2]
Si
05
10152025
Hydro
gen [
x1015
H/cm
2 ]
SiN20
05
10152025
SiN70
[1] M. Ionescu, B. Richards, K. McIntosh, R. Siegele, E. Stelcer, O Hawas, D. D. Cohen, T. Chandra, Materials Science Forum Vols. 539-543, pp. 3551-3556, (2007)
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ANSTO Heavy Ion ERDA-ToF [1]
T2
Secondary Electron
MCP
W electrodes C foilsRecoils
0.5m
ElectrostaticMirrors
SBD
45o
4-way slitsIon Beam
67.5o
Secondaryelectron
Anode plateEnergyTime
T1
0 25 50 75 100 125 150 175 200 225 250 275 300 325
17
18
19
20
21
22
23
24
Depth
reso
lution
[nm]
C foil thickness [µg/cm2]
82.5 MeV Iodine
• Ion beams: C; O; F; Na; Si; Cl; Ca; Ti; Co; Ni; Cu; Br; Nb; Ag, I; W; Pt; Au
• Beam shape: rectangular• Incident angle: 67.5o• Exit angle: 45o• Scattering angle: 45o• C foils: 25µg/cm2• Sample manipulation: XYZ, rotation• Sample heating up to 1,000oC• Gas ports (O, N)• Further development:
- H absorption/desorption- In-line sample preparation: ion implanter + EB evaporatorTRIG (86)
QD (821)
CH3
CH1
CH0(94)
STOP START
(T)
(93)
(E)
QD (821)
Sample
CFD
Delay
CFD
PAFPAFPA
e-e-
T2
TOF-ERDA DiagramIon Beam
Recoils T1SBD
PC
(571)AMP
(474)TFA
(463)CFD
(89)NIM-TTL(567)
TAC
(419)MCA
[1] J. W. Martin, D. D. Cohen, N. Dytlewski, D. B. Garton, H. J. Whitlow,G. J. Russell, NIM B 94, 277, (1994)
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ERDA-ToF: analysis of MgB2 thin film with 82MeV I [1]
0 400 800 1200 1600 2000 2400 2800 3200 3600 40000
400
800
1200
1600
2000
2400
2800
3200
3600
4000
Time [
chan
nel n
o]
Energy [channel no]
10B11B O
Mg
Al
82MeV I
A l 2O 3
M gB 2 112.5o
0 50 100 150 200 250
0
500
1000
1500
2000
2500
3000
3500
4000
4500
5000 Substrate 10B 11B O Mg Al
Yield
[coun
ts]
Depth [nm]
Film
16 18 20 22 24 26 28 30 32 34 36 38
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
1.2
3786
542
On axis-Si On axis-Al2O3 Off axis; Mg cap layer Off axis; ion beam sputtered
Norm
alize
d Oxy
gen i
n MgB2 fi
lm
Tc [K]
1
• Isotope effect in MgB2 can be measured as a function of 10B/11B
• Magnesium is diffusing into the substrate• Oxygen amount critical for the quality of the film• Tc correlated with the amount of Oxygen, type of substrate, and deposition geometry[1] M. Ionescu, Y. Zhao, R. Siegele, D. D. Cohen, E. Stelcer, M. Prior, NIM B 266, 1701–1704, (2008)
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NRA: Oxygen in Ta2(16O1-x+18Ox)5 thin film [1]
25 50 75 100 125 150 175 200
0
100
200
300
400
500
600
700
800
900
1000
α yie
ld [co
unts]
Channel Number
0.2 0.6 1 1.6 1.8 2.1 2.5 4
18O concentrations [at%]
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
0.0
2.0x1034.0x1036.0x1038.0x1031.0x1041.2x1041.4x1041.6x1041.8x1042.0x1042.2x104 Standard samples
Liniar Fit
α yi
eld [c
ounts
]18O concentration [at%]
y=4577 x+148R=0.99964
α
Ta2(16O1-x
18Ox)5
p 845keV
18O(p,α)15N
200nm
Ta
500 600 700 800 900 10000
10
20
30
40
50
60
70
dσ/dΩ
[mb/s
r]
Energy [keV]
18O(p,α)15N
845 keV
641 keV
[1] M. Ionescu, D. Bradshaw, R. Siegele, D. D. Cohen, O. Hawas, E. Stelcer, D. Button, D. Garton, NTA 14 Conference, 20-22 November 2005, Wellington, New Zealand
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NRA: Hydrogen in thick DLC film
Γ=
σπ iNdxdEctsY
cmatN][2
]/[ 2
σΩ=
iNctsYcmatN ][]/[ 2E4
E3
E2x
γ
dxdExEE x0
00cosα−=
1H(15N,αγ)12C
dxdExEE x
x1
12 cosβ−=
E0x
At depth x:
E2
E0≥ 6.385 MeVE1x
15N
α
β
θ
E1
x
At the surface:
Energy Detectors
Ni - number of ions incident on sampleΩ − detector solid angleσ − 15N reaction cross section Γ − FWHM of resonance (1.8keV)
4He
1H12C
γ E1= 4.43 MeV
• Depth of analysis: few nm up to few microns
• Depth resolution: 5-20nm• Sensitivity: 1-100ppm
5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.51
10
100
1000
10000
Siγ Y
ield [
coun
ts/2.5
µC]
Energy 15N+ ions [MeV]
15N+
γ Detector
Si
DLC film ~700nm
• Thick DLC film grown by CVD for implants• Hydrogen content plays a role in the biologic
response [1]• Hydrogen content is higher at the surface and
decreases toward the interface• Questions remains on Hydrogen yield due to
the production of 15N- (15NH3-), the flux measurement, energy spread, etc
[1] W. J. Ma, A. J. Ruys, R. S. Mason, P. J. Martin, A. Bendavid,Z. Liu, M. Ionescu, H. Zreiqat, Biomaterials 28, 1620–1628, (2007)
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Ion beam implantation and mixing
nanostructures
depth
Ion implantation
burriedlayersupersaturation
nucleationgrowth
ripeningcoalescence
timeannealing
surface
nanostructures
interface
Ion irradiation timeannealing
surface
interface mixing phase separation
• Near surface layers and interfaces can be engineered for specific properties
10K
Zn0.99Co0.01O
Zn0.99Co0.005Eu0.005OZn0.99Eu0.01O
0
0 103 2x103-103-2x103
B [Oe]
Magn
etiza
tion [
amu]
2x10-4
10-4
-10-4
-2x10-4
• ZnO thin film implanted with Eu and Co• Annealed• Magnetization measured at 300K and
10K
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Conclusions• IBA nuclear techniques at ANSTO suitable for characterisation of thin films, near surface layers and interfaces
- film thickness- depth profile of light and heavy elements- defects in single crystals- 2D X-ray mapping of surfaces- radiation damage in materials- ion beam-induced chemical reactions- micro-machining
• Modification of properties by ion implant • Micro device testing (IBIC, single event upset)
Acknowledgment:D. Garton, G. Cooke; O. Evans; M. Mann; D. Lynch; E. Stelcer; P. Bond; P. Druer