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Lithium profiling using elastic recoil detection
analysis
Blake Jones*, Lyudmila V. Goncharova**
Department of Physics and Astronomy, University of Western Ontario, London, Ontario, N6A 3K7 Canada
*bjones82@uwo.ca,**lgonchar@uwo.ca
VI. Conclusions and References
We would like to thank Jack Hendricks for Tandetron operation.
Acknowledgements
I. Introduction
The analysis and depth profiling of light elements has always been
challenging. Due to their small atomic size and low mass, elements
such as H, He, and Li can be quite problematic to study in physical
targets. Conventional and very popular ion beam techniques such
as Rutherford Back Scattering (RBS) and Secondary Ion Mass
Spectrometry (SIMS) are ill equipped to deal with such issues. An
increasing occurrence of Li in battery and electronic technology
research has emphasized the need for a method of profiling and
detecting that is sensitive to light elements in a heavy matrix.
Elastic Recoil Detection Analysis (ERDA) is one such method.
ERDA was first used in 1976[1]
. Since then it has been offering an
accurate, non-destructive method for the investigation of light
elements in thin films.
II. Elastic Recoil Detection
Despite being an established ion beam technique, ERDA has not
been well developed for elements outside of hydrogen and its
isotopes. To improve the ease with which measurements can be
analyzed and to allow for quantitative data to be produced, a
standard and a well defined set of parameters needs to be
constructed tested.
III. Paramters IV. Results (continued)
IV. Results
1. L’Ecuyer, J., C. Brassard, C. Cardinal, et al. "An accurate and sensitive method for
the determination of the depth distribution of light elements in heavy
materials." Journal of Applied Physics. 47. (1976): 381. Web. 31 Oct. 2013.
<http://scitation.aip.org/content/aip/journal/jap/47/1/10.1063/1.322288>.
2. ISW Tandetron. 2013. Photograph. University of Western Ontario, London. Web. 31
Oct 2013. <http://www.isw.physics.uwo.ca/techniques/index.shtml>.
3. Arnold Bik, W.M, and F.H.P.M Habraken. "Elastic Recoil Detection." Reports on
Progress in Physics. 56. (1993): 859-902. Web. 31 Oct. 2013.
<(http://iopscience.iop.org/0034-4885/56/7/002)>.
4. ISW ERDA Chamber. 2013. Photograph. University of Western Ontario, London.
Web. 31 Oct 2013. <http://www.isw.physics.uwo.ca/techniques/index.shtml>.
5. Maas, Jos. Elastic Recoil Detection with Alpha Particles. Diss.
Universiteitsdrukkerij , 1998. Eindhoven: Universiteitsdrukkerij , 1998. Web.
<http://alexandria.tue.nl/extra2/9802039.pdf>.
6. Maas, Jos. Elastic Recoil Detection with Alpha Particles. Diss.
Universiteitsdrukkerij , 1998. Eindhoven: Universiteitsdrukkerij , 1998. Web.
<http://alexandria.tue.nl/extra2/9802039.pdf>. H. Jayatilleka, D. Diamare, M.
• ERDA shows great potential for quantitative Li analysis and
profiling. The initial results are promising and can likely be
improved upon with further experimentation.
• The use of Ni stopping foil instead of Al, and a higher incident
energy improved resolution of the Li peaks. It is probable that this
is a result of the increased stopping power of Ni. More
experimentation may indicate if peak resolution is always
correlated with foil stopping power.
• Surface H contamination does significantly affect the ERDA
spectra. However, the resolution is such that with SIMNRA the
profile and concentration of the contaminant can be found.
• Both spectra show good agreement with SIMNRA predictions.
• The sharp peak in both is due to hydrogen on the surface of the
target.
• The strong hydroscopic properties of LiCl means that a layer of
water forms very rapidly on its surface even in the vacuum of the
ERDA chamber.
• The less pronounced Li peak can is also present in both spectra.
Once again both spectra agree with SIMNRA predictions well.
The hydrogen peak is less pronounced in the LiNbO3 spectrums.
This is caused by the much weaker hydroscopic tendencies. In
addition, the targets were kept in vacuum conditions for six days
before measurements were taken.
Figure 2. Conventional setup for a
standard ERDA experiment. [3]
Figure 2. shows the typical
configuration used when
conducting standard ERDA
experiments. The grazing-
angle geometry allows for the
forward recoiling of target
species. A mono-energetic beam of ions
with masses greater than the atoms being
investigated is used to bombard a target sample.
The bombardment causes elements in the target matrix to be dislodged
(recoiled). The recoiled elements then travel through a stopping foil
with properties chosen so as to limit the transmission of elements that
are not of interest. After successfully transmitting through the foil, the
recoiled particles reach the detector where their energy is measured.
Figure 1. Tandetron
configuration at Interface
Science Western (ISW) [2]
Figure 3. ERDA chamber at
ISW. [4]
Figure 4. Schematic diagram of
energy loss due to stopping
power. [5]
Figure 5. The energy for the
scattered and recoiled particles
respectively. [6]
Depth profiling is made possible due
to the equations in Figure 5. which
compute the energy of the recoiled
particle immediately after the elastic
interaction between the incident ion
and an atom in the target matrix. As
well as knowledge of the stopping
powers of both the target and the
stopping foil.
Testing and developing a set of parameters that allow for accurate
data collection is an important part in further developing ERDA for
use in Li profiling.
Stopping Foil: Affects – Elemental peak resolution
– Transmission probabilities
Tests with Al and Ni foils were performed, the higher
stopping power of Ni produced better results.
Incident Ion: Affects – Which elements are recoiled.
Carbon ions were used for the incident beam. Oxygen are
another plausible choice. Carbon is sufficiently heavy to
recoil lithium but light enough not to recoil a host of unwanted
atoms.
Target: Affects – Li concentration.
– Other atoms possible of recoiling.
Several different targets were tried including LiCl, LiF,
Li2CO3 and LiNbO3
. LiNbO3 was deemed the most suitable for
a standard as it does not have strong hydroscopic tendencies
which create undesired H counts. It also has a prominent role
in electrical technologies.
Figure 6. ERDA spectrum of LiCl using a (a) 3.0 MeV
(b)3.4 MeV C+ beam and 1.899 µm Ni stopping foil.
a)
b)
a)
b)
Figure 7. ERDA spectrum of LiNbO3 using a a)3.6 MeV and
b) 3.8 MeV Carbon beam with 1.899 µM Ni stopping foil.
V. Advantages/Disadvntages
Advantages Disadvantages
• Non-destructive
• Good depth resolution
• Sensitive to light elements in a
heavy matrix
• Complementary with RBS
• Not quantitative for elements other
than Li isotopes.
• Only small amounts of literature to
compare results with.
• Uncertainty has a strong
dependence (3rd
order) on geometry.
Figure 7. ERDA spectrum of LiNbO3 using a a) 3.6 MeV and
b) 3.8 MeV Carbon beam with 1.899 µm Ni stopping foil.

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CAMBRPoster1

  • 1. Lithium profiling using elastic recoil detection analysis Blake Jones*, Lyudmila V. Goncharova** Department of Physics and Astronomy, University of Western Ontario, London, Ontario, N6A 3K7 Canada *bjones82@uwo.ca,**lgonchar@uwo.ca VI. Conclusions and References We would like to thank Jack Hendricks for Tandetron operation. Acknowledgements I. Introduction The analysis and depth profiling of light elements has always been challenging. Due to their small atomic size and low mass, elements such as H, He, and Li can be quite problematic to study in physical targets. Conventional and very popular ion beam techniques such as Rutherford Back Scattering (RBS) and Secondary Ion Mass Spectrometry (SIMS) are ill equipped to deal with such issues. An increasing occurrence of Li in battery and electronic technology research has emphasized the need for a method of profiling and detecting that is sensitive to light elements in a heavy matrix. Elastic Recoil Detection Analysis (ERDA) is one such method. ERDA was first used in 1976[1] . Since then it has been offering an accurate, non-destructive method for the investigation of light elements in thin films. II. Elastic Recoil Detection Despite being an established ion beam technique, ERDA has not been well developed for elements outside of hydrogen and its isotopes. To improve the ease with which measurements can be analyzed and to allow for quantitative data to be produced, a standard and a well defined set of parameters needs to be constructed tested. III. Paramters IV. Results (continued) IV. Results 1. L’Ecuyer, J., C. Brassard, C. Cardinal, et al. "An accurate and sensitive method for the determination of the depth distribution of light elements in heavy materials." Journal of Applied Physics. 47. (1976): 381. Web. 31 Oct. 2013. <http://scitation.aip.org/content/aip/journal/jap/47/1/10.1063/1.322288>. 2. ISW Tandetron. 2013. Photograph. University of Western Ontario, London. Web. 31 Oct 2013. <http://www.isw.physics.uwo.ca/techniques/index.shtml>. 3. Arnold Bik, W.M, and F.H.P.M Habraken. "Elastic Recoil Detection." Reports on Progress in Physics. 56. (1993): 859-902. Web. 31 Oct. 2013. <(http://iopscience.iop.org/0034-4885/56/7/002)>. 4. ISW ERDA Chamber. 2013. Photograph. University of Western Ontario, London. Web. 31 Oct 2013. <http://www.isw.physics.uwo.ca/techniques/index.shtml>. 5. Maas, Jos. Elastic Recoil Detection with Alpha Particles. Diss. Universiteitsdrukkerij , 1998. Eindhoven: Universiteitsdrukkerij , 1998. Web. <http://alexandria.tue.nl/extra2/9802039.pdf>. 6. Maas, Jos. Elastic Recoil Detection with Alpha Particles. Diss. Universiteitsdrukkerij , 1998. Eindhoven: Universiteitsdrukkerij , 1998. Web. <http://alexandria.tue.nl/extra2/9802039.pdf>. H. Jayatilleka, D. Diamare, M. • ERDA shows great potential for quantitative Li analysis and profiling. The initial results are promising and can likely be improved upon with further experimentation. • The use of Ni stopping foil instead of Al, and a higher incident energy improved resolution of the Li peaks. It is probable that this is a result of the increased stopping power of Ni. More experimentation may indicate if peak resolution is always correlated with foil stopping power. • Surface H contamination does significantly affect the ERDA spectra. However, the resolution is such that with SIMNRA the profile and concentration of the contaminant can be found. • Both spectra show good agreement with SIMNRA predictions. • The sharp peak in both is due to hydrogen on the surface of the target. • The strong hydroscopic properties of LiCl means that a layer of water forms very rapidly on its surface even in the vacuum of the ERDA chamber. • The less pronounced Li peak can is also present in both spectra. Once again both spectra agree with SIMNRA predictions well. The hydrogen peak is less pronounced in the LiNbO3 spectrums. This is caused by the much weaker hydroscopic tendencies. In addition, the targets were kept in vacuum conditions for six days before measurements were taken. Figure 2. Conventional setup for a standard ERDA experiment. [3] Figure 2. shows the typical configuration used when conducting standard ERDA experiments. The grazing- angle geometry allows for the forward recoiling of target species. A mono-energetic beam of ions with masses greater than the atoms being investigated is used to bombard a target sample. The bombardment causes elements in the target matrix to be dislodged (recoiled). The recoiled elements then travel through a stopping foil with properties chosen so as to limit the transmission of elements that are not of interest. After successfully transmitting through the foil, the recoiled particles reach the detector where their energy is measured. Figure 1. Tandetron configuration at Interface Science Western (ISW) [2] Figure 3. ERDA chamber at ISW. [4] Figure 4. Schematic diagram of energy loss due to stopping power. [5] Figure 5. The energy for the scattered and recoiled particles respectively. [6] Depth profiling is made possible due to the equations in Figure 5. which compute the energy of the recoiled particle immediately after the elastic interaction between the incident ion and an atom in the target matrix. As well as knowledge of the stopping powers of both the target and the stopping foil. Testing and developing a set of parameters that allow for accurate data collection is an important part in further developing ERDA for use in Li profiling. Stopping Foil: Affects – Elemental peak resolution – Transmission probabilities Tests with Al and Ni foils were performed, the higher stopping power of Ni produced better results. Incident Ion: Affects – Which elements are recoiled. Carbon ions were used for the incident beam. Oxygen are another plausible choice. Carbon is sufficiently heavy to recoil lithium but light enough not to recoil a host of unwanted atoms. Target: Affects – Li concentration. – Other atoms possible of recoiling. Several different targets were tried including LiCl, LiF, Li2CO3 and LiNbO3 . LiNbO3 was deemed the most suitable for a standard as it does not have strong hydroscopic tendencies which create undesired H counts. It also has a prominent role in electrical technologies. Figure 6. ERDA spectrum of LiCl using a (a) 3.0 MeV (b)3.4 MeV C+ beam and 1.899 µm Ni stopping foil. a) b) a) b) Figure 7. ERDA spectrum of LiNbO3 using a a)3.6 MeV and b) 3.8 MeV Carbon beam with 1.899 µM Ni stopping foil. V. Advantages/Disadvntages Advantages Disadvantages • Non-destructive • Good depth resolution • Sensitive to light elements in a heavy matrix • Complementary with RBS • Not quantitative for elements other than Li isotopes. • Only small amounts of literature to compare results with. • Uncertainty has a strong dependence (3rd order) on geometry. Figure 7. ERDA spectrum of LiNbO3 using a a) 3.6 MeV and b) 3.8 MeV Carbon beam with 1.899 µm Ni stopping foil.