Hard X-ray microanalysis with parabolic refractive lenses [Elektronische Ressource] / vorgelegt von Marion Kuhlmann

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Hard X-Ray Microanalysis with Parabolic Refractive Lenses.Von der Fakult¨ at fur¨ Mathematik, Informatik und Naturwissenschaftender Rheinisch Westf¨ alischen Technischen Hochschule Aachenzur Erlangung des akademischen Gradeseines Doktors der Naturwissenschaften genehmigte Dissertationvorgelegt vonDiplom-Physikerin Marion Kuhlmannaus Bramsche.Berichter: Universit¨ atsprofessor Dr. B. LengelerUniversit¨ Dr. H. Luth¨Tag der mundlic¨ hen Prufung:¨ 13. August 2004Diese Dissertation ist auf den Internetseiten der Hochschulbibliothek online verfugbar.¨Contents1 Introduction 12 Optics for Hard X-Rays 32.1 InteractionofX-RayswithMatter........................ 32.2 FocusingOpticsforHardX-Rays......................... 92.3 ParabolicRefractiveLensesasHardX-RayOptic................ 102.3.1 HistoricalNote............................... 102.3.2 Design.................................... 112.3.3 PrincipalGeometries............................ 123 Parabolic Refractive Lenses: Properties 153.1 ParabolicShape .................................. 153.2 SurfaceRoughnes................................. 163.3 FocalLength.................................... 173.4 TransmisionandGain............................... 183.5 EffectiveandNumericalAperture ........................ 203.6 DepthofFieldandDepthofFocus. 203.7 Resolution...................................... 203.8 Chromatic Aberration 213.9 ExampleExperiment................................
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01 janvier 2004

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Hard X-Ray Microanalysis with Parabolic Refractive Lenses.
Von der Fakult¨ at fur¨ Mathematik, Informatik und Naturwissenschaften
der Rheinisch Westf¨ alischen Technischen Hochschule Aachen
zur Erlangung des akademischen Grades
eines Doktors der Naturwissenschaften genehmigte Dissertation
vorgelegt von
Diplom-Physikerin Marion Kuhlmann
aus Bramsche.
Berichter: Universit¨ atsprofessor Dr. B. Lengeler
Universit¨ Dr. H. Luth¨
Tag der mundlic¨ hen Prufung:¨ 13. August 2004
Diese Dissertation ist auf den Internetseiten der Hochschulbibliothek online verfugbar.¨Contents
1 Introduction 1
2 Optics for Hard X-Rays 3
2.1 InteractionofX-RayswithMatter........................ 3
2.2 FocusingOpticsforHardX-Rays......................... 9
2.3 ParabolicRefractiveLensesasHardX-RayOptic................ 10
2.3.1 HistoricalNote............................... 10
2.3.2 Design.................................... 11
2.3.3 PrincipalGeometries............................ 12
3 Parabolic Refractive Lenses: Properties 15
3.1 ParabolicShape .................................. 15
3.2 SurfaceRoughnes................................. 16
3.3 FocalLength.................................... 17
3.4 TransmisionandGain............................... 18
3.5 EffectiveandNumericalAperture ........................ 20
3.6 DepthofFieldandDepthofFocus. 20
3.7 Resolution...................................... 20
3.8 Chromatic Aberration 21
3.9 ExampleExperiment................................ 22
4 Beryllium Lenses: Properties and Performance 25
4.1 Improvements due to Beryllium . . . 26
4.2 MaterialQualityandShapeControl....................... 30
4.3 Comparison of Beryllium Lenses and Aluminium Lenses . ........... 3
5 Beryllium Lenses: Methods and Applications 35
5.1 ImagingandMicroscopy.............................. 35
5.2 FocusingandMicroprobing............................ 40
5.3 Tomography..................................... 41
5.3.1 ScanningTomography 42
5.3.2 MagnifyingTomography.......................... 4
5.4 HardX-RayLithography ............................. 46
5.5 MicroSmalAngleX-RayScatering....................... 49
5.6 BeamConditioning................................. 50
5.7 RefractiveLensesforX-RayFreElectronLasers................ 50
5.8 ComparisonandOutlook ............................. 51CONTENTS
6 XANES Microtomography 53
6.1 X-RayAbsorptionFineStructure(XAFS).................... 53
6.2 TheGoal:XANESMicrotomography....................... 57
6.3 ExperimentalImplementation........................... 57
6.4 ResultsofXANESMicrotomography 58
6.4.1 Feasibility Test ............................... 58
6.4.2 CatalystScience.............................. 62
6.4.3 BiologicalandEnvironmentalScience.................. 64
6.5 Conclusions..................................... 67
7 Nanofocusing 69
7.1 DesignandManufacturingofNanofocusingLenses............... 69
7.2 ExperimentalImplementation........................... 73
7.3 NFLCharacterization............................... 74
7.4 FirstNanofocusingResults . 76
7.5 NanofocusingLenses:SummaryandOutlook.................. 82
8 Summary 83
A The Choice of Lens Material A1Chapter 1
Introduction
Since their discovery by Wilhelm Conrad Ron¨ tgen in 1895 X-rays have been used in analytical
applications. Most common, X-rays are known as medical diagnostic tools due to their ability
to non-destructively pass through matter which cannot be penetrated by visible light.
Beside this, many physical analysis methods rely on the properties of X-rays. Hard X-rays
cover the energy range from about 1000 eV to 200 keV, which correspond to a large part of
the spectrum of electronic and a few nuclear transitions in atoms. Therefore, the elemental
composition of a sample can be analyzed by its emitted fluorescence radiation. Likewise
absorption spectroscopy can describe the chemical state and the short range environment of
˚ ˚an element. Further, the hard X-rays wavelengths of 10A to 0.05A allow to study the structure
of condensed matter, as they are in the range of characteristic interatomic distances. This is
the foundation of X-ray crystallography.
As powerful as these analytical methods may be, many applications need a focused X-ray
beam. Especially, heterogeneous samples and complex structures benefit from the higher
spatial resolution of a micro focused beam. Some focusing optics are able to implement high
resolution imaging. For soft X-rays, full field and scanning microscopy have been realized by
means of Fresnel zone plates as optical elements. However most optics (like mirrors, multi
layers, capillaries, Fresnel zone plates, and Bragg-Fresnel optics) become less efficient with
higher X-ray energies.
This thesis follows the development of microscopy, micro probing, and micro diffraction in the
hard X-ray range based on parabolic refractive lenses. Obviously, refractive lenses for visible
light are most successful. But the weak refraction and strong absorption of hard X-rays in
matter make the realization of refractive lenses difficult. The first refraction experiment by
R¨ ontgen led to the conclusion that there are non refractive lenses for X-rays. Since then,
the concept have been controversially discussed and was mainly considered as unrealistic.
Highly brilliant X-ray sources and advanced instrumentation are the foundation for the first
experiment, which used refractive X-ray lenses, by Snigirev, et al., in 1996. The aperture
of refractive lenses for hard X-rays is comparable to their radius of curvature. Therefore,
spherical refractive lenses suffer from aberration and are not appropriate for microscopy and
other imaging applications. Parabolic refractive hard X-ray lenses have solved this problem.
A full field hard X-ray microscope which used a stack of parabolic refractive aluminium lenses
was first implemented in 1999 by Lengeler, et al.
To improve the imaging application of parabolic refractive lenses and to enhance the mean-
ingful energy range beryllium lenses have been developed. Their benefits for analytical appli-
12 CHAPTER 1. INTRODUCTION
cation are outlined in the chapters 4 and 5.
Microanalysis with hard X-rays has benefited from the high brilliance of 3rd generation syn-
chrotron radiation sources. The experiments were carried out at the European Synchrotron
Radiation Facility ESRF in Grenoble, France, and at the Advanced Photon Source APS at
Argonne National Laboratory, USA. The next generation of synchrotron radiation sources
will be the X-ray free electron laser XFEL, whose spectral brilliance is expected to be sev-
eral orders of magnitude higher than that of present synchrotron radiation sources. Beryllium
refractive lenses will probably allow microanalysis despite the high power of these new sources.
Arranging the individual lenses in a stack gives the refractive X-ray lenses a high degree of
flexibility concerning choice of energy and spot size. In that way, standard small angle scatter-
ing experiments were improved. Also, parabolic beryllium lenses were used in implementing
XANES microtomography. This combination of near edge absorption spectroscopy with two
dimensional scanning microscopy allows to examine the chemical state and the local environ-
ment of a given atomic species in a virtual slice through a sample without really cutting it.
The opportunities of this powerful approach are outlined in chapter 6.
The demand for X-ray microprobes with still smaller spot size is growing. For this reason
nanofocusing refractive lenses have been designed in Aachen. A prototype made out of silicon
is presented in chapter 7. With this first nanofocusing hard X-ray lens we were able to enhance
the results of fluorescence nanotomography experiments and nanodiffraction, already. In the
near future focusing of hard X-rays with refractive lenses below 100 nm is a realistic goal,
opening the way to study biologic cells and structures of nanotechnologic devices.Chapter 2
Optics for Hard X-Rays
The interaction of X-ray with matter is discussed in this chapter. Then, hard X-ray optics will
be introduced, followed by a general presentation of refractive lenses, including their design
concept, the choice of material, and their classification as hard X-ray optic.
2.1 Interaction of X-Rays with Matter
At a boundary between vacuum to matter X-rays are refracted and reflected. Inside the
matter they are attenuated by absorption and scattering. If the material has a periodic
structure diffraction can occur. Further, inhomogeneities in the material generate small angle
scattering.
The propagation of an electromagnetic wave in matter depends on its wavelength λ and on
the material to interact with. Different phase velocities for different materials are expressed
by the index of refraction n [1].
n=1− δ + iβ. (2.1)
The refraction is described by the real part 1-δ whereas the attenuation of X-rays in matter
is described by β.
visible light X-rays
θ θn = 1 n = 1
1
11 1
θn > 1 n = 1-δ+iβ2 θ 2 2
2
Figure 2.1: Refraction at the boundary between vacuum and matter for visible light and
for X-rays according to Snell’s law, equation (2.2). In contrast to visible light, X-rays are
refracted away from the surface normal.
34 CHAPTER 2. OPTICS FOR HARD X-RAYS
Refraction: the change in direction of

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