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Experimental Beamlines of
GSI Materials Research
CARAT Workshop * GSI * 13. – 15.12.2009Daniel SeverinGSI Materials Research
GSI - Facility
Cave AHigh Energy
UNILAC3.6-11.4 MeV/uRange ~ 100µm
X0
SISup to
2 GeV/u
ERDAIon-Beam Analysis
Sample irradiation
Heavy ion irradiation
X0 Autosampler
single ionrandom
• Automatic load-lock system
• Defocused beam (5x5cm2)
• Random ion distribution
• Fluence regime: 1 – 1E13 ions/cm2
• Single ion irradiation
• 50 samples per hour(for 1E8 ions/cm2 per sample)
Ion track membranes
pores in mica
10 µm
etch pits in SiO2 perforated dead-end pores
pores in Kapton conical pores in Kapton
1 µm
cigar-shaped pores in PC funnel-shaped pores
Heavy-ion beam Microprobe
Heavy-ion beam Microprobe
3m
object aperture
lens
target
electronic
deflectorhit detector
beamswitch
Heavy-ion beam Microprobe
3m
object aperture
lens
target
electronic
hit detector
beamswitch
deflector
Biology Setup
Fast and perfect dose control
10 µm
ions
Unsurpassed targeting accuracy
Heavy-ion beam Microprobe
typ. 20µm
100µm
single-ion lithography
10 µm
• Single ion irradiation
• Accuracy:… in vacuum: below 1µm… into air: 1.5 µm
• Speed: ~ 100 Hz
10.000 ions in regular pattern etched PET
Sample characterization
Off-line techniques atMaterials Research
Spectroscopy
1400 1200 1000 8000
2
1117
cm
-1
abso
rptio
n / a
rb. u
nit
wavenumber / cm-1
virgin 1x1010
1x1011
4x1011
2x1012
725
cm-1
1169
cm
-1
1456
cm
-1
Phase TransitionPolymer Degradation
UV/Vis & Infrared RamanMicroscopy
Shape and Size of Nanopores and -wires
Surface Analysis
AFM / STM SEM
Swelling effects
LaserspectroscopyProfilometry Chemistry
Lab
Template etching
Photon relaxation
In-situ and On-linesample characterization
GSI - Facility
UNILAC3.6-11.4 MeV/u
X0
New M-Branch
Cave A
M - Branch
M1 – Electron Microscopy
Fixed beam spot size:diameter = 3mm
On-line beam diagnostic(aperture current)
M1 – In-situ SEM
2 µm2 µm
• Zeiss SUPRA 40 high-resolution scanning electron microscope (1.3 nm at 15 keV)
• 5-axes motorised eucentricsample stage
• In-situ imaging without exposing the irradiated sample to air
M2 – In-situ XRD
• Small beam spot
• Scanning ion beam system(extreme homogeneousirradiation with high flux)
• On-line beam diagnostic(aperture current)
• SEIFERT 4-circle x-ray diffractometer (Cu-Kα)
• Position sensitive detector
• Investigation under any angle of incidence enables the quantitative analysis of structural modifications
XRD - Application
10 20
inte
nsity
(a.u
.)
two theta (degrees)
unirradiated
1×1013 cm-2
5×1012 cm-2
• Amorphization
• Formation of new ion-beaminduced phases
• Special orientationtexturing
M3 – On-line Spectroscopy
• Variable beam spot size (Slit system with max. 4x4cm2)• On-line beam monitoring by SETRAM• Extreme sensitive beam view monitor (down to 1E3 ions/cm2)
Sample curvature detection
Irradiation-induced material stress measured by sample curvature detection
University of Jena(Wesch, Steinbach)
Residual Gas Analyser
0 10 20 30 40 50 60 70 80 90 10010-9
10-8
10-7
10-6
C2F4
C2F3
CF3
CF2pres
sure
/ m
bar
m/z
without beam with beam
CF
11.4 MeV/u Xe --> PTFE
Irradiation-induced outgassing of PTFE
University of Sao Paulo(Delgado)
On-line FT/IR Spectroscopy
-0,16
-0,14
-0,12
-0,10
-0,08
-0,06
-0,04
-0,02
-0,00
0,02
Abso
rban
ce
2330 2335 2340 2345 Wavenumbers (cm-1)
Transmission FT/IR spectroscopy
• Real on-line measurement possible
• Elimination of errors by sample preparation
M3 – All-in-one chamber
Cryostat UV/Vis and fluorescence
QMS Gas flow controller
FT-IRLong-distancemicroscopy
Ion beam
Sample curvaturemeasurement
Control of irradiation conditions:
• Cryostat
• Gas flow controller and QMS
High temperature irradiation
Sample temperature up to 950 °C (area 4x4cm2)
Outlook for the next 3 years…
Within a second BMBF project starting 2010– On-line Raman spectroscopy– In-situ AFM in an UHV Chamber– High energetic ERDA (UHV)– Photoluminescence
Summary
Sample irradiation …at X0 (random ion distribution)…at µ-Probe (controlled single-ion irradiation)
Off-line techniques: Electron microscopy, AFM, STM,optical spectroscopy (Raman, IR, UV/Vis) etc.
On-line and in-situ beamlines at the new M-branchSEM, XRD, IR etc.
Surface modificationM1 and M3
Structural bulk modificationM2 and M3
!
!
!
!
!
Thanks to…
… GSI Materials Research group
… collaborating Universities of the M-Branch(Darmstadt, Dresden, Göttingen, Heidelberg, Jena, Stuttgart)
… and thanks for your attention!
END
Dose distribution of swift heavy ions
photons ions
Ion track membranes
10 nm
10-1000 µm
Track morphology
5.0 keV/nm
0
2
4
6
8
10
12
0 2 4 6 8 10 12 14
ener
gy lo
ss (k
eV/n
m)
energy (MeV/u)
O
Xe
Ar
Krhomogeneous
inhomogeneous
no etching
4.5 keV/nm
NIM B 116 (1996) 429
Track etching
PETpolycarbonate
Kapton
UV treatment
chemicaletching
(NaOH, NaOCl. HF)
Irradiation
Polymers / Pore size
2 µmTrack etchable POLYMERS
PET polyethylene terephthalate (Mylar, Hostaphan)PC polycarbonate (Lexan, Makrofol, CR39)PI polyimide (Kapton, Upilex)PP polypropylenePVDF polyvinyidene fluoride 30 µm Makrofol N
6M NaOH @ 50 °C
2 µm
SAXS
α = 15°
Characteristics: pattern is very sensitive to alignment due to large aspect ratio of pores
α = 0° coaxialq [Å-1]
ln(in
tens
ity)
polyarylate foil5×108 pores/cm2
∅ = 240 nm
Θα SAXSx-rays
Replica method
10 µmion track membrane
filling of pores in galvanic cell
free-standing metal needlesdissolution ofpolymer