High-Speed PIXE - Minerals at the chemical photo studio
R. Ziegenrücker1, J. Buchriegler2, J. v. Borany2, D. Hanf2, S. Ihle3, S. Nowak4, S. Merchel1,
F. Munnik2, A.D. Renno1, G. Rugel1, O. Scharf4
1
HZDR, Helmholtz Institute Freiberg for Resource Technology, Bautzner Landstraße 400, 01328 Dresden
2 HZDR, Institute of Ion Beam Physics and Materials Research, Bautzner Landstraße 400, 01328 Dresden
3 PNSensor GmbH, Römerstr. 28, 80803 München
4 IFG Institute for Scientific Instruments GmbH, Rudower Chaussee 29/31, 12489 Berlin
Motivation
Sample requirements

New technologies for exploration, mining, sustainable use and recycling of

Wide range of samples, from drill core to thin section
mineral and metallic resources have to be evaluated

Max. sample size: 250 x 250 x 15 mm³
Developing of a fast, lateral resolved analysis method for trace

Max. weight: 10 kg
element distribution by full field imaging

Surface roughness: <10 µm (sawed or polished)

Stability in vacuum: 10-6-10-7 mbar (dry, no hydrocarbon
Proton
+

PIXE = Particle-Induced X-ray Emission

Complete periodic table from magnesium, later upgrade from boron
Determination of lateral resolution (1:1 optics)
Mg

Lateral resolution: 10 µm

Analysis depth: 50 µm depending on matrix and analyte

contamination)

Mg Ka =
1253.6 eV
Gaussian fits: ≈70 µm

Detection limits: several µg/g depending on matrix, analyte and time
Visual test and verification using the Rayleigh criterion of the
Calculated by sigmoid-fits: ≈139 µm

100
150
200
74
74
Measuring time: few minutes to hours
Origin of X-ray
fluorescence.
Fast visualization for trace elements with predefined thresholds
200
200
D
C
200
E
Pixel
Experimental set-up
Super-SIMS source

High-Speed PIXE source
30
20
10
150
150
AMS sources
50
40
50

60
Counts
What is possible with High-Speed PIXE?
80
150
90
110
120
130
140
Pixel
100
100
A
B
Gaussian fit of an arbitrary line trough structure D.
For the left hand side the Rayleigh criterion is
fulfilled.
100
Unique set-up
5050
50
Ion source to detector:  77 m

100
150
00
Caesium sputter ion source with
H--ions)
titanium hydride (

6 MV tandem accelerator[1] with
H+-ions)
argon stripper gas (

HighSpeed
PIXE
detector
150
150

Pixel
100
Measurement of a copper on silicon test
50
structure (made at Fraunhofer Institute for
Reliability and Microintegration).
185
190
195
200
A & B: 100 µm stripes, distances: 300/200/100 µm;
Pixel
C & D: 67 µm stripes, distances: 200/135/67 µm;
Fitted signal of a sharp boundary between
E:
10 µm stripes, distances: 30/20/10 µm
stainless steel and tin-solder; resolution ≈139 µm.
(radiation protection limit)
First results of ores
High-Speed PIXE proton energy:
Eudialyte ore:
4
whole sample area under detector
6
5
2
12 mm
12
Intensity [Counts]
≤ 4.2 MeV
Beam size:  2-3 mm is extended to 12 x 12 mm² (simultaneous analysis of
1
200
200
Beam current: ≤ 400 nA
Schematics 6 MV accelerator @ HZDR.

100
100
Counts
6 MV Tandem accelerator
10 m

50
50
10
8
12.5 cm
6
5
10
15
25
20
Energy [keV]
Eudialyte Bearing Urtite, Lovozero, Kola Peninsula, Russia; left: sample with indicated beam spot;
right: sum spectra of all pixel over 23 min; inset: elemental distribution map; 6.4 x 106 events;
sample spot size: 12 x 12 mm².
1m
Left: schematics of the end station of the High-Speed PIXE beamline; right: beam diagnostic &
analysis chamber.
1) quadrupol lens, 2) beam extension system, 3) beam diagnostic chamber, 4) X-ray colour camera,
5) analysis chamber, 6) lock for sample transfer.
Nepheline ore:
12
X-ray Colour camera

12 cm
X-ray sensitive CCD-camera
(CCD = charge-coupled device)


8.6 cm
10
8
6
69696 pixel on 12.6 x 12.6 mm² area
5
Simultaneous detection of an energyeach pixel
lateral resolution
1:1 optics
15
X-ray colour camera with 1:1 test
optics.[3]
Ø 19 mm
Acknowledgements
Thanks to BMBF, SPRITE, BAM,
6:1 optics
staff @ Ion Beam Centre @ HZDR,
Lateral resolution
Picture size
Distance optics to
sample
50 µm
20
25
Nepheline ore, Kiya Shaltiv, Kemerowo Obl., Siberia, Russia; left: sample with indicated beam spot;
right: sum spectra of all pixel over 70 min; inset: elemental distribution map; 2.2 x 107 events;
sample spot size: 12 x 12 mm².
”colour camera“
Special capillary optics
10
Energy [keV]
resolved (160 eV Mn Kα) X-ray spectrum for

12 mm
Intensity [Counts]
3
3
10 µm
12 x 12 mm²
1.2 x 1.2 mm²
< 10 mm
0.8 mm
and M. Hartig (Dreebit).
Capillary bundle 1:1 optics.[3]
References
82 mm
Sketch of 6:1 optics.[3]
[1] S. Akhmadaliev et al., Nucl. Instr. Meth B 294 (2013) 5-10.
[2] O. Scharf et al., Analyt. Chem. 83 (2011) 2532 -2538.
[3] IFG Institute for Scientific Instruments (Berlin).
René Ziegenrücker | Helmholtz Institute Freiberg for Resource Technology | Department of analytics | [email protected] | www.hzdr.de/hif