AXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

AXO DRESDEN GmbH- Applied X-ray Optics and High Precision Deposition • Development and production of multilayer X-ray optics• Complex 1- and 2-dimensional X-ray optical systems• Synchrotron optics from EUV to hard X-rays• Monochromators for XRF• High precision deposition by means of magnetron sputter
deposition (MSD), large area pulsed laser deposition (LA-PLD)
and dual ion beam deposition (DIBD) technologies• Application and teaching in X-ray diffraction (XRD),
X-ray reflectometry (XRR) and X-ray fluorescence (XRF)

HIGH PRECISION DEPOSITION

X-RAY OPTICAL SYSTEMSAXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

MULTILAYER X-RAY OPTICS

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und PräzisionsbeschichtungHigh Precision Deposition Techniques:
Magnetron Sputter Deposition (MSD)
Large Area Pulsed Laser Deposition (LA-PLD)
Dual Ion Beam Deposition (DIBD)• High precision deposition of
nanometer single and multilayers• Accuracy and homogeneity in thepicometer range• Multilayer stacks for a wide variety
of applications• Constant and graded thickness
distributions• Deposition on rectangular or roundsubstrates (typical dimensions: 8 inch
diameter or 500 mm length)

Dual beam large area pulsed laser deposition
plasma plumes caused by the interaction of
focussed ns-laser pulses and the target surface

Application of nanometer single undmultilayers for X-ray optics
Synchrotron

Polarizers

Multilayer optics
TlAP, PET, …

Crystal optics
0.01 nmλ0.1 nm

1 nm
L-lines (Br..Ca)

Ni,Co,
Fe, O

10 nm

K-lines (Si..Be)

W Kα

Ag Kα
In Kα
Ag Kß
Sn Kα

Mo Kα
Mo Kß

Cr Kα
Co Kα, Co Kß
Cu Kα
Ga Kα, Ga Kß

P Kα
S Kα
Si Kα

Na Kα
Mg Kα
Al Kα

C Kα

B Kα

Si Lα
Be Kα

Plasmasources,EUV

N Kα

Laboratory
sourcesE

O Kα

Sample fluorescence
100 keV

AXO DRESDEN GmbH

10 keV

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

1 keV

100 eV

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Parallel Beam X-ray Optics

High precision 60 mm parallel beam optics on
prefigured substrate (right) and on flat substrate,
which are glued and bend after deposition (left)

Generation of a monochromatic parallel beamin one dimension

Parallel beam X-ray optics are opticalcomponents with a graded multilayer
deposited on a substrate having aparabolic shape in beam direction.
These optical devices convert (in one
dimension) a divergent incoming
beam into a parallel one, or vice-versa
an incoming parallel beam into a
focusing one.
In order to obtain high efficiency, thed-spacing of the multilayer has to bevaried from the front end to the rearend of the optics in correspondence
to the aspheric curvature. Either the
X-ray source or the detector (ordetector slit) may be placed at the
optics focal distance, for primary or
secondary side applications,
respectively.

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Spectral lines

Y

p
y=
2

/
p
0

p
2

M

e
lin
ro
g

th

X

m

n
f=
th
g

m

b

x

a
P
=


)
f(x

e
lfo
a
c

X
F

r
a
lb
e

d
i
w
=
b

tfh

x
,L
(p


d
2
=

f

f
e

F

X

in
)s
x
(

Cr, Co, Cu, Ga, Mo, Ag(others on request)

Mean Reflectivity R > 70 %MonochromacyK1 + K2 or K

Divergence ≤ 0.03°(40 m source width)

Mirror length

L = 40...100 mm(on customer’s request)

X- ray source
geometry
Parallel beamwidth bline focus
dependent on mirror
length, geometry and
X-ray wavelength

Typical b values

1.5 mm (Cu-K, L = 60 mm)
1.0 mm (Mo-K, L = 100 mm)

Geometry

typical focal length(source - mirror center)
L = 60 mm, xm = 100 mm

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Convex Parallel Beam Optics

Outstanding Feature
Increase of the parallel beam photon
flux in combination with a focusing
optic by reduction of beam width bcompared to conventional parallel
beam optics
Convex curved parallel beam multilayer
optics of various geometries for thegeneration of a compressedmonochromatic parallel beam in one
dimension

Spectral lines

Cr, Co, Cu, Ga, Mo, Ag(others on request)

Mean reflectivity R > 70 %AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

MonochromacyK1 + K2 or K

Mirror length

typical values:
20 mm – 40 mm(others on request)

X-ray source
geometryline focus

Geometrycustomized

Oct-09Siegfried-Rädel-Straße 31
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www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Focusing X-ray Optics

ngth L
Mirror le

Y

Xm

0

F1

F2

X

Generation of a monochromatic focusing
beam in one dimension

Parallel beam and focusing X-ray
optics with various geometries

Spectral lines

Focusing X-ray optics are artificial
optical components with a 1dimensional lattice deposited ona substrate.

Mean reflectivity R > 70 %These optical devices convert
a divergent incoming beam into
a focusing one. To obtain highefficiency, the d-spacing of thelattice has to be changed fromthe front end to the rear end of
the optics.
The device needs to have an
elliptical figure of curvature to
produce a focusing beam. The
focus of the X-ray source islocated in one of the two focal
points of the ellipse.

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Cr, Co, Cu, Ga, Mo, Ag(others on request)

MonochromacyK1 + K2 or K

Mirror length

typical values:
L = 40 mm … L = 80 mm(on customer’s request)

X-ray source
geometryline focus

Focal line width b dependent on spectral
line, geometry andmirror length
Geometrycustomized

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Monochromators for XRF
and Synchrotron Applications
reflectivity [%]

100
80
60
40

0

Monochromatization of X-rays by meansof a nanometer multilayer stackmaterial system Ni/C

20
0

20

40

60

energy [keV]

Reflectivity of a Ni/C multilayer (d = 4.0 nm) in the
spectral range between 8 keV ... 70 keV(Measurement: G. Falkenberg, Hasylab at DESY)

Monochromators are optical devices
with a 1-dimensional multilayer
deposited on a substrate. To obtainhigh efficiency, the d-spacing of themultilayer is constant from the frontend to the rear end of the monochromator. A plane figure is required
for the monochromator.
Depending on the application either
high resolution or high flux multilayer monochromators can be
fabricated.

Spectral range< 50 eV – 100 keVMaterial systems

optimized on wavelength
or on customer’s request

Typical sizes

500 mm in lengthor 8 inches diameter

Resolution

0.25 % < E/E < 2 %(periodic multilayers)
E/E > 5% on request(aperiodic multilayers)

0

10

Thickness
homogeneity

-1

10

al
tic
re ivityoteth flec
re

-3

10

-4

10

%
00
r1

Ge

111

Si

111

-5

Crystals

10

Applications

Be

110

High-Z
Low-Z
ML's(Mirrors)

o
it f
lim

high-resolution ML's

Integrated reflectivity

-2

10

ak
pe

depth-graded ML's

forbidden area

-6

10

-6

10

-5

10

-4

10

-3

10

-2

10

-1

10

0

10



Energy resolution and divergence of hard x-ray
multilayer monochromators (*)

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtungd/d < 0.02%
monochromators forlaboratory X-ray sources
and for synchrotrons,
optimized for highreflectivity or tailored
resolution
polarizers in the soft X-ray
range (O-K, Fe-L, Ni-L)(*) Ch. Morawe et al.- ESRF – Grenoble (F)Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Monochromators
for X-ray Fluorescence Analysis
Analysis of Light Elements (Be...Cl)High resolution multilayer
Monochromators (2d = 3.02 nm)
vs. TlAP crystals (2d = 2.59 nm)
TLAP
W/B4C Multilayer

120

Mg K

Intensity a. u.

100

80

60

Al K

Si K
40

20

0
7

8

9

10

Wavelength (Angström)

Performance of high resolution
W/B4C multilayers and TlAP crystals
for the detection of Si, Al and Mg

W/B4C

TlAP

Si Kα1,2
peak intensity[kcps]
P/B ratio

31.3
55.6

39.1
129.2

37.6
58.4

36.8
213.7

107.8
65.0

103.5
207.0

Al Kα1,2
peak intensity[cps]
P/B ratio

Performance of high resolution
multilayers (IWS30)* at the Si K-Linein comparison to W/B4C multilayers and
TlAP (Thallium biphtalate) crystals.
W/B4C

IWS30

TlAP

d [nm]

1.51

1.55

1.295

Order

1st

1st

1st

E [keV]

1.74

1.74

1.74

R [%]

21

26

ca. 25

E/E

309

404

ca. 400

Mg Kα1,2
peak intensity[cps]
P/B ratio

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung(*) in cooperation with Fraunhofer IWS, Dresden

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

ASTIX-c2- dimensional Parallel Beam
X-ray Optics

Collimating 2- dimensional X-ray optics
in a modified Montel geometry (1)for the generation of 2- dimensional
high intense parallel X-ray beams• Typical length 60 mm - 150 mm• Application with all typical types of X-ray
sources (rotating and fixed anodes, liquid
metal jet and micro focus X-ray tubes)• Typical parallel beam width:
1 mm2 ≤ b2 ≤ 5 mm2• Wavelengths: Cr, Co, Cu, Ga, Mo, Ag…
• High precision vacuum mirror housing

ASTIX-c: collimating geometry

Parallel beam profile for
Mo K radiation
I > 107 cps(low power μ-source)b2  1 mm2High precision vacuum mirror housings for
ASTIX optics(1) M. Montel - „The X-Ray Microscope with Catamegonic RoofShaped Objective“ in: X-ray Microscopy and Microradiography,
Vol.5, 1957,pp 177 - 185

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

ASTIX-f
2- dimensional Focusing
X-ray Optics

Focusing 2-dim. X-ray optics in a
modified Montel geometry (1)for the generation of 2-dimensional
high intense focused X-ray beams• Typical length 60 mm - 150 mm• Application with all typical types of X-ray
sources (rotating and fixed anodes, liquid
metal jet and micro focus X-ray tubes)• Typical spot diameter<30 μm … 500 μm• Convergence: customized• Wavelengths: Cr, Co, Cu, Ga, Mo, Ag, …
• High precision vacuum mirror housing

ASTIX-f: focusing geometry

High Flux Optics

Profile of diffracted beam between optics
and focal point (f2 = 310 mm)• high flux (HF) at sample position

focal point f2• high integrated pixel intensity

I > 109 cps(rotating anode)Ø  200 μm

High Resolution Optics• small spot size at sample position• high resolution (HR) in the detector
plane(1) M. Montel - „The X-Ray Microscope with Catamegonic RoofShaped Objective“ in: X-ray Microscopy and Microradiography,
Vol.5, 1957,pp 177 - 185

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

ASTIX-fApplication of Different Typesof Optics to a Lysozyme Sample
High Flux Optics

High Resolution Optics
Advantages of HR optics
Small spot size at sample position
High resolution (HR) in detector plane

Advantages of HF optics
High integrated pixel intensity
High flux (HF) at sample positionice

Lysozyme sample
Measured with HR optics

Nonius X-ray generator
Cu K radiation
Marresearch dtb andmar345 imaging plate detector

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Twin Mirror Arrangement

A new quality in inin-house X-ray
reflectometry
Special features• Easy and fast sample alignment
Twin Mirror Arrangement consisting of primary
mirror with housing (left) and secondary mirror
with housing, beam tube and detector slit holder(right).

reflectometry (Cu K )
graded Ni/C-multilayer

7

10

6

intensity [cps]10

sample stage position
H=+200μm
H=0
H=-200μm

5

10

4

10

3

10

2

10

1

10

2.5

5

7.5

10

12.5

15

17.5

2 [degree]

X-ray reflectometry: Independence of peakintensities and angular positions at threedifferent stage heights

Setup of Twin Mirror Arrangement (TMA)

Upgrades available for all common X-ray
instruments (for example Cr, Co, Cu, Ga,
Mo, Ag K or K, W Lor L radiation)
Geometries on customers‘ request• No influence of sample displacement
errors up to 200 μm on peak position
and intensity• Sample alignment within 10 seconds• Dynamic range of more than 7 ordersof magnitude(cross intensity I > 3 . 109 cps)
• Low divergence ( Cu K :  < 0.03° )• Detectable thin film thicknesses
between 2 nm and 270 nm

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Twin Mirror Arrangement

Twin Mirror Arrangement consisting of primary
mirror with housing (left) and secondary mirror
with housing, beam tube and detector slit holder(right).

A new quality in X-ray diffractometry –secondary parallel beam optics

Better resolution than soller slits
because of a more than two times
lower angular acceptance(Cu K :  < 0.03°)600a) TWIN MIRRORS

600b) BRAGG-BRENTANO geometry

Quartz triplet
400

intensity / cps

intensity / cps

400

200

0
67.00

67.50

68.00



• Increased S/N-ratio due to sample
fluorescence suppression• Transmission higher than 60%• Fits best to primary parallel beam
optics• Parallel beam geometry:- simplified sample preparation- increased accuracy

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Quartz triplet

Cu K
Cu K

68.50

69.00

Cu K
Cu K

200

0
67.00

67.50

68.00

68.50

69.00



Powder diffraction measurement in the
angular range of the quartz triplet inparallel beam geometry (TMA) (a) and
BRAGG-BRENTANO geometry (b)Superior K suppression:
I(Cu K1) : I(Cu K) > 1.000.000 : 1(– 2 – scan at Si (400) wafer)Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Thin Film XRF Reference Samples

X-ray fluorescencereference sample with up
to 7 different elements ona silicon nitride membrane(above), PEEK sample
holder (below).

Energy spectra of three 7-element reference samples. The energy
range from ~2 keV to ~40 keV is covered with peaks of comparable
intensity.
Advantages of Thin Film XRF reference samples:• Absorption free standard: no matrix
correction necessary• Substrate thickness of 100 nm / 200 nm permits
transmission measurements and leads to low
background from the substrate• Mass depositions in the range of ng/mm²(1-3 atomic layers) permit quantification
without the need to interpolate fromhigher values• Uncertainty  1 ng/mm² (1 atomic layer)• Wide selection of non-overlapping XRFlines, exact calibration curve with many
points over a large energy range
Mass deposition of the elements on the• Signal strength easily adjustable byreference sample with corresponding
thickness, similar intensity for all elements
fluorescence emission line energies.
• High degree of uniformity & homogeneity(better than 1% for the full sample area)
Element
Mass
Emission Lines (eV)• Application for adjustment of confocal
μ-XRF possible(ng/mm²)KL• Wide range of available elements(standard and tailored compilations)Pb
7.61±0.96
85335
10541
La

11.01±0.62

33298

4649

Pd

1.8±1.0

21123

2838

Mo

1.32±0.40

17444

2293

Cu

2.84±0.35

8040

930

Fe

5.04±0.87

6401

747

Ca

19.31±1.10

3691

341

Si

Substrate

1740

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Lateral homegeneity measured by XRF μ-beammapping (1.2x1.2 mm² with 2.8x12 μm² beam)of La and Cu, and XRF large area mapping(15x15 mm² with 0.8x0.4 mm² beam) of La andCu (from left to right)
Oct-09Siegfried-Rädel-Straße 31
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+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Teaching Tool
for X-ray Reflectometry
Concept of sample selection:
one interface bulk material / airsingle layer with two interfacesmultilayer system with many interfaces

reflectivity

100

simulation
measurement

10-2
10-4
silicon substrate
10-6
0
0.5

1

1.5

2

2.5

/°

reflectivity

100

simulationd(Ni)=29.9nm
measurement

10-2
10-4
10-6
0

substrate and Ni-layer
0.5

1

1.5

2

2.5

/ °

100
reflectivity

X-ray reflectometry (XRR) is an essential
technique for non-destructive characterizationof surfaces, interfaces and thin films in thenanometer range. The Dresden University ofTechnology (TUD) Institute of Structural
Physics (Nanostructural Physics - Prof. Dirk C.
Meyer) offers an advanced practical course in
X-ray reflectometry.
The
samplescharacterizedintheseexperiments are now available as a complete
teaching tool in cooperation of TUD with AXO
DRESDEN GmbH and FhG IWS. The scope ofdelivery also comprises an elaborated
introduction in the basic principles of X-ray
reflectometry and a commented trail guidance
together with some protocols of students ofthese practical course of Dresden University ofTechnology as examples.
The set consists of three silicon substrates of
40x20 mm² size, one without coating, onewith a thin single Ni-layer (d  30 nm) and one
with a 10-period Ni/C-multilayer (mean period
thickness d  4nm). The films are deposited byPulsed Laser Deposition (PLD).
The specular reflected intensity is measured asa function of grazing incident angle. Eachmeasurement shows a characteristic pattern.
Basic principles of total external reflexion andthe interference of reflected and diffracted
X-rays in a layer stack can be discussed. Layer
thicknesses and interface roughnesses are
determined by selected simulation programs
that are on a CD delivered with the sample
set.

simulation
N=10, d=4.08nm
measurement

10-2
10-4
10-6
10-8
0

Ni/C multilayer
1

2

3
/°

4

5

6

Simulation programs for quantitative analysis ofexperimental data are available as freeware [1].
Simulations of presented measurement werecarried out using the program IMD.
[1] D.L. Windt, IMD - Software for modeling theoptical properties of multilayer films, Computersin physics 12, 360-370 (1998).
More information:
http://www.physik.tu-dresden.de/isp/nano/lehre.php

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Oct-09phone: +49(0)351-83391-3249
Siegfried-Rädel-Straße 31
www.axo-dresden.de+49(0)351-83391-3314 contact@axo-dresden.deD-01809 Heidenau · Germany fax:

AXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

AXO DRESDEN GmbH - Applied X-ray
Optics and High Precision Deposition was founded as a Spin-off by employeesof the Fraunhofer Institute Material andBeam Technology Dresden (IWS) with aparticipating share of the Fraunhofer
Society.

To deliver our customers an optimum
high quality solution we are working inclose collaboration with the Fraunhofer
IWS, further Fraunhofer Institutes, theUniversity of Technology Dresden as wellas with other national and international
research institutions.

Our production program contains both
single X-ray optics and complex X-ray
optical systems to generate highintensity collimated or focussed
monochromatic X-ray beams, special
customized depositions and applicationsin X-ray reflectometry and diffraction.

More than 18 years of experience in thefields of high precision deposition anddesign, development and application ofmultilayer X-ray optics guarantees ourclientele effective and customized
solutions in the fields of X-ray optics andhigh precision deposition.

A wide assortment of flat and curved
X-ray optics are available that can beused with the common types of X-ray
sources with respect to wavelength,
construction and focus geometry.

We are looking forward to answer yourquestions and inquiries.

AXO DRESDEN is develops and applies
various high precision deposition
techniques for the production of
nanometer single and multilayers
showing sub-nanometer precision.

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deAXO DRESDEN GmbH Applied X-ray Optics Röntgenoptik und Präzisionsbeschichtung

Die AXO DRESDEN GmbH ist ein Spin-Off
aus dem Fraunhofer Institut fürWerkstoff- und Strahltechnik (IWS)
Dresden unter Beteiligung ehemaliger
IWS-Mitarbeiter und der Fraunhofer
Gesellschaft.
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AXO DRESDEN entwickelt und benutzt
unterschiedliche, sich ergänzende
Präzisionsbeschichtungsverfahren, mit

AXO DRESDEN GmbH

Applied X-ray Optics · Röntgenoptik
und Präzisionsbeschichtung

Oct-09Siegfried-Rädel-Straße 31
phone: +49(0)351-83391-3249
www.axo-dresden.deD-01809 Heidenau · Germany fax:
+49(0)351-83391-3314 contact@axo-dresden.deX-Ray analytical application of multilayer X-ray optics
R. Dietsch*, Th. Holz*, G. Falkenberg*** AXO DRESDEN GmbH, Siegfried-Rädel-Str. 31, 01809 Heidenau, Germany; contact@axo-dresden.de** HASYLAB at DESY, Notkestr. 85, 22603 Hamburg, Germany
Ag K parallel beam optics for X-Ray diffraction

ASTIX-f – Optics for micro focusing
Advantages of the ASTIX-solution
Symmetric spot geometry in the focal plane even forhighly asymmetric source dimensions
Improved lateral and temporal homogeneity

Goal• covering a large q-range up to 20 Å-1 in the reciprocal space (0.1° < 2 < 160°)• high penetration depth also in metal samples• reduced influence of sample fluorescence, displacement errors and sample transparency in parallel beamgeometry with secondary monochromator

Wide variety in spot dimension of less than 30μm tomore than 300μm on fixed anode and micro focus Xray tubes depending on multilayer system,
deposition and geometry parametersexperimental setup:
Diffractometer XRD 3003
(GE-IT) for samples up to
200 mm x 200 mm or 8“ and for measurements up
to 2= 160°

Typical mirror length up to 150 mm
Beam path and monochromatization of a focusing
ASTIX-f system

Improved P/B ratio due to reduced scattered
backgroundylid crystal

ylid crystal

XRD measurements of LaB6 powder sample (50kV / 25mA)
100

measuredreflexinf - 1.84

ASTIX 150 and ASTIX 100 with vacuum mirror housing
AMH100 and AMH150659

 <100μm

653

P/B ratio

5.5

Rint

81.29

0.014

1.83 - 1.44

825

822

6.9

58.25

0.015

980

977

8.2

38.88

0.020

979

962

8.1

34.94

0.021

1.12 - 1.03

875

871

7.3

23.01

0.027

1.03 - 0.97

719

718

6.0

21.79

0.028

0.97 - 0.91

Symmetric shape of secondary focal spots with  <100μm up to > 300 μm measured at fixed anode tubes (Cu) coupled withASTIX-f (marcam images)

averageredundancy

1.44 - 1.24
1.24 - 1.12

 >300μm

kept
reflex

609

608

5.1

16.75

lin intensity [cps]

10 2

443

443

3.7

12.35

0.041

276

276

2.3

10.48

0.041

0.83 - 0.78

178

177

1.4

9.43

0.038

inf - 0.78

6543

6507

5.4

35.15

0.018

8
6
4
95

96

97

98

99

100

2 [degree]

30

20

40

60

80

X
Z

34

log. intensity [cps]

FWHM

36

FWHM
(2) = 0.029°

10 3

10 2

FWHM / µm

26

9

20
0

1

2

3

4

5

Position at optical axis / mm

6

7

(b)

Si 111

24
22

38

(a)

10 1

28

36

Parallel beam profile without (a) and with sample (b) in
the beam path (LaB6* capillary  500 μm)

32
30

34

100

XRD measurementof single crystal Si111 reflection

10 4

40

32

2 [degree]* data of ylid single crystal diffraction by courtesy of Oxford Diffraction

38

0.11°

2 [degree]

Table: Results of data collection (YLID crystal); completeness > 99% *)Modular X-ray system (micro source + ASTIX-f optics) applicable both for standard XRD (powder diffraction / SCD) and microdiffraction

FWHM

50

10 1

0.033

0.91 - 0.87
0.87 - 0.83

lin. intensity [cps]Resolution
Åarrangement 2:
Fixed anode tube (Mo) coupled with
HOPG*

log. intensity [cps]10 3arrangement 1:
μ-source (Mo) coupled with ASTIX-f*

102 [degree]

11

Results:• intensity > 108 cps• I(Ag K) : I(Ag K) > 10.000• beam divergence   0.015° (<60 arcsec)• improved P/B ratio due to suppression of other characteristic
emission lines (Ag K)• low background intensity level ( <5 cps)
• reflexions up to 2 = 100° detected at LaB6

FWHM < 30 μm
FWHM < 150 μm
Geometry 300/100:
 28 μm x 21 μm
I  2.5 x 106 cps

Geometry 100/300:
  150 μm
I  7.5 x 106 cps

Multilayer Monochromators for Synchrotron Applications

Mo K Microfocus X-ray source (spot  50 μm @ 30 W) and ASTIX-f100

Application :from EUV to hard X-rays (< 50 eV – 100 keV)
Material systems: optimized on wavelength and bandwidth
on customers’ request
Dimensions:
up to 8“ diameter or up to 500 mm in length
Thickness homogeneity: d < 0.002 nm for d = 1 nm (d/d < 0.2%)
Resolution:
0.25% < E/E < 10%

μ-focus MoK source coupled with ASTIX-f (a) vs. X-ray tube + HOPG + capillary (b)Stability of Ni/C multilayer2 = 4°-40°

STOE –powder diffraction system

2 = 40°-70°

LaB6 powder sample / capillary  250 μm
time: 3 min / Image plate detector
experimental
setup:
spot size :conv. angle:(a)
150 μm3 mradIlluminated areas:(b)
300 μm7 mrad(a)(b)

Results with ASTIX-f:• highly symmetric spot at sample position• low background intensity• twice the flux density in a 150 μm spot
• nearly the same peak intensity with reduced illuminated sample volume• higher resolution (K1+2 splitting)• increased P/B ratio with ASTIX-f solution• higher efficiency due to μ-source applicationwater cooled
Ni/C (IWS): d = 3.38 nm
100 layers
 = 0.45
E/E = 210-2
deposited on Si-mirrors (Zeiss)
size 120×30×10 mm3energy range: 3-8 keV and 10-100 keV

Ni/C
W/B4C

Mo/Si

Combination of sealed X-ray source with ASTIX-c (L=60) for Cr K
Cr K sealed tube X-ray source(spot 1.2x0.4 / 1.2kW)
and ASTIX-c 60  / 150

WH 1: close to source

Geometry /150:
Beam profile:   105μm (FWHM)
I > 1 x 106 cps (Cr K)Long distance focussing
Measurement up to 2 > 160°

IUCr 2008

Results:
Ni/C multilayer used as DMM (HASYLAB at DESY)
Physical life: 1.5 a / effective 4 months
Energy range: 12 keV, 18 keV, 40-60 keV / water cooling
Vacuum: base pressure 1 x 10-6 mbar
Results of Cu K reflectometry: No remarkable decrease of reflectedpeak intensities at both multilayers
WH1: increase of mean period thickness about 0.15 nm
Higher heat load at mirror WH1 up to a temperature of approx. 200°C

WH 2

Application and characteristics of Ag K multilayer X-ray optics
Th. Holz*, R. Dietsch*, N. Mattern*** AXO DRESDEN GmbH, Siegfried-Rädel-Str. 31, 01809 Heidenau, Germany; contact@axo-dresden.de** Leibnitz Institute for Solid State and Material Research (IfW) Dresden, Helmholtzstrasse 20, 01069 Dresden, Germany; n.mattern@ifw-dresden.de
Motivation for Ag K parallel beam mirror setup

Characteristics of Ag K TMA

Covering of a large q-range up to 20 Å-1 in the reciprocal space ( 0.1° < 2 < 160° )High penetration depth in metallic samples
Reduced influence of sample fluorescence, displacement errors
and sample transparency in parallel beam geometry with secondary monochromator

XRD measurement of LaB6 powder sample
Generator: 50 kV, 25 mA

Experimental setup - Twin Mirror Arrangement (TMA)

3

(b)

10

100

lin. intensity [cps]

(b)
2

(a)

8
6
4

95

96

97

98

99

100

2 [degree]

(a)

1

10

20

40

60

log. intensity [cps]

32

34

36

38

2 [degree]

80

100

Result:• intensity  108 cps• I(Ag K) : I(Ag K) > 10.000• beam divergence of = 0.015° (<60 arcsec)• improved P/B ratio due to suppression ofother characteristic emission lines (Ag K)• low background intensity level (<5 cps)
• reflections up to 2 = 100° detected for LaB6FWHM
(2) = 0.029°

103

102

1

10

Parallel beam geometry (twin mirror arrangement -TMA)- schematic view -30

Parallel beam profile without and with sample inthe beam path
(LaB6* capillary  500 μm)

Si 111104• high intensity and low divergence• no influence of sample displacement and transparency
on peak position for reflectometry and X-ray diffraction• superior K suppression• sample fluorescence suppression• easy and fast sample alignment

0.11°

2 [degree]

XRD measurementof single crystal Si111 reflection

TMA - the parallel beam concept with

FWHM

50

LaB6

step width: 0.005°
time/step: 10s

experimental setup:
diffractometer XRD 3003 (GE- inspection technology)
for samples of up to 200 mm x 200 mm (  8“) andfor measurements from starting at 0° (reflectometry) up to 2 = 160° (diffraction)

lin intensity [cps]log. intensity [cps]10

9step width: 0.002°
absorber: Cu 0.2mm
time/step: 1s

10112 [degree]* LaB6 powder sample was kindly provided by Huber Diffraktionstechnik GmbH

Results

Measurements with Ag K (E = 22.2 keV) and Synchrotron (E = 119 keV)sample: Pd40Cu30Ni10P20
locked coupled 2:1 scan: 2° < 2 < 160° ; (2) = 0.1 ° ; t = 45 s

14
12

S (q)

[S (q) -1 ] * q

E = 22.2 keV
E = 119 keV

42

E = 22.2 keV
E = 119 keV

10
8
6
4
2

105

0
-2
2

4

6

8

-4

10 12 14 16 18 20 22 24

2

4

6

8

10 12 14 16 18 20 22 24-1-1

q [Å ]q [Å ]

88
E = 22.2 keV
E = 119 keV

6

E = 22.2 keV
E = 119 keV

64

PDF (r)G (r)log. intensity [cps]

0

2

4
2

0

0

-2
2

4

6

8

10

r [Å]

12

14

16

18

20

2

4

6

8

10

12

14

16

18

20

3

10

2

10

x10

r [Å]

The TMA allows to cover the reciprocal space up to 20 Å-1 . The dynamic range of measured intensities is about
two orders of magnitude. The low brillance of laboratory X-ray sources limits the correlation determination to
the first shells with distances up to 10 Å.
The coincidence between synchrotron and TMA measurements with Ag K radiation is clearly visible. A
distinction between individual correlation lengths in the PdCuNiP alloy is not possible and was not the aim of
this experiment.

Acknowledgements:
The authors are indepted to N. Huber for providing the LaB6 capillary sample and to
Dr. H. Borrmann (MPI-Dresden) and Dr. M. Schuster (SIEMENS AG Munich) for helpful discussions andtheir suggestion for starting the work on Ag K multilayer parallel beam optics.

RQ13, 2008

4

10

101

5

10

15

20

25

-1

q = 4**sin()/ [A ]Summary:• Using the TMA, diffraction measurements can be done up to 2=160° to cover a large q-range in reciprocal space• The intensity on laboratory X-ray sources is limited, but resolution is comparable up to 10 Å-1 .
• The second multilayer mirror on the diffracted beam side increases the P/B ratio.
Sample fluorescence can be suppressed.
• The low divergence and the small beam width of 0.5mm could allow a local 1dim mapping of structural gradients

High Resolution and High Flux Multilayer Monochromators
for Synchrotron Application
Reiner Dietsch*, G. Falkenberg**, Th. Holz*, D. Weissbach** AXO DRESDEN GmbH, Siegfried-Rädel-Str. 31, 01809 Heidenau, Germany; contact@axo-dresden.de** HASYLAB at DESY, Notkestrasse 85, 22603 Hamburg, Germany
Motivation
Depending on the application either high flux or high resolution multilayer monochromators areused in synchrotron applications to characterize the structural and morphological parameters ofcompact materials and thin films. The required beam characteristics which mostly depend on thereal sample can be realized by various X-ray optical systems that produce either low divergence(high resolution) or high intensity beams. The actual developments tend to the design ofcustomized systems using one or two dimensional beam shaping multilayer X-ray optics, multilayer
monochromators or the combination of multilayer optics with other types of X-ray optics. A closeinterrelation of design, deposition, characterization and application is required to produce thesetailored systems. To fabricate either high reflectance or tailored resolution multilayer X-ray optics
both the material combination and the layer stack morphology have to be optimized. In particularhigh resolution is realized by a combination of low-Z / low-Z materials or by low-Z / high-Z layer
stacks having very thin high-Z absorber layers in the sub-nm range. Because the multilayer
resolution is determined by the number of active layer pairs, stacks with more than 500 periods
have to be deposited, for example. To guarantee maximum performance an optimum high precision
deposition technology has to be applied for each specific material combination. To realize theserequirements complementary high precision deposition technologies such as magnetron sputtering,large area pulse laser deposition and dual ion beam deposition technologies with a reproducibility.
and long term stability in the sub-nanometer range have to be installed.

Overview of reflecting hard x-ray optics(*)
010

forbidden area

ti
ore
the

for

it
l li m
ca

ti
ec
refl
ak
pe

y
vit

(3)
(2)

-3

Ge

-4

111

Si

111

-5

Crystals

10

Be

110

depth-graded ML's

10

10

•Homogeneity: 99.8 % (80 mm) 99.5 % (40 mm)• Cu K-reflectivity of a Ni/C-Multilayerd = 3.0 nm:
R = 68 %• run-to-run stability:
99.5 %(1)high-resolution ML's

Integrated reflectivity

-2

10

0%
10

Large Area Pulsed Laser Deposition•Homogeneity: 99.9% (6“ diameter)•Cu K reflectivity of a Mo/Si-system:
R > 60% (Cu K / d = 2.0 nm)•run-to-run stability:
99.9%

High-Z
Low-Z
ML's(Mirrors)-1

Magnetron sputtering system

Characterization of a Double Multilayer Monochromators (DMM) bymeans of rocking scan measurements in the energy range between 8 keV
and 21 kev at DORIS: Experimental Setup

Integrated reflection coefficient vs. energy resolution

10

High Precision Multilayer Deposition Techniques:
Combination of Large Area Pulsed Laser Deposition andMagnetron Sputter Deposition

-6

10

-6

10

-5

10

-4

10

10

-3

-2

-1

10

10

0

10


( )

* Ch. Morawe et al. ESRF - Grenoble (F)Comparison of spectral resolution of W/B4C, Mo/Si and Ni/C DMM
1:Spectral resolution (/tg in %) of W/B4C, Mo/Si and Ni/C DMM in the
spectral range between 8 keV and 21 keV

W/B4C multilayer (**)
d = 1.5 nm
Ep = 12 keV
 (FWHM) = 0.046°

2:

8 keV
12 keV
15 keV
18 keV
21 keVd = 2.98 nm
 (FWHM) = 0.09°

3:
Ni/C multilayerd = 3.34 nm
Ep = 12 keV
 (FWHM) = 0.14°

W/B4C
0.46
0.49
0.56
0.61
0.66

Mo/Si
0.96
0.89
0.92
0.95
1.07

Relative integrated intensity of W/B4C, Mo/Si and Ni/C DMM normalized
to a Si (111) double monochromator in the spectral range between 8 keV
and 21 keV

Mo/Si multilayer
Ep = 12 keV

Ni/C
1.65
1.70
1.78
1.83
2.13

8 keV
12 keV
18 keV
21 keV

Ni/C
40
20.7
30.3
33.5

W/B4C
4.3
2.4
4.4
4.9

Mo/Si
7.9
12.0
27.6
9.2

Summary:• Multilayer monochromators with different spectral resolution in the range
between /tg = 0.5% … 2% can be fabricated by means of complementaryhigh precision deposition techniques such as LA-PLD and magnetron sputtering.
• To guarantee an optimum performance special material combinations have to be
selected depending on the wavelength and considering the absorption edges.
• The increase of integrated intensity in comparison to Si (111) monochromators
corresponds with a decrease of spectral resolution.

(**) N. Chkhalo, IPM Nizhny Novgorod

SRI 2006

Influence of X-ray optical systems and sample characteristics on the angularresolution of X-ray reflectometry measurements with Cu Kradiation
T. Holz*, M. Schuster**, T. Böttger****AXO DRESDEN GmbH, Siegfried-Rädel-Str. 31, D-01809 Heidenau, Germany, contact@axo-dresden.de**SIEMENS AG, CT MM 7, Otto-Hahn-Ring 6, D-81739 Munich, Germany***Fraunhofer Institute Material and Beam Technology (IWS), Winterbergstr. 28, D-01277 Dresden, Germany

Motivation-1

Reflectivity

10=0.030°

-3

10

-4

10

-5

10

-6

10

-7

10

0

22.35

Reflectivity

Mo/Si multilayer stack

-2

10

1E-4

22.40

/°

22.45

2

6

N*d = 414 nm 0.01

1E-3

1E-5

1E-4
1E-5
3.8

4.0

4.4

4.2

4.4

Göbel Mirror (GM)limits in layer thickness determination

4.6
4.6

4.8

5.0

8

10

0.1

N*d = 270 nm

0.01

4

/°

22.50

Reflectivity

Intensity

beam divergence

The concept presented here
overcomes the shortcomings ofconventional systems. By coupling aparallel beam multilayer mirror to achannel cut monochromator, asignificantly lower beam divergence ata still high beam intensity can beachieved.

010

Ge(022)0.1

Advanced solution

X-ray reflectometry  = 0.154nm (Cu K)The determination of film thicknesses from thickness oscillations (Kiessig fringes)
with specular X-ray reflectometry (XRR) is limited by (i) the absorption of X-rays inthe film, (ii) the divergence and (iii) the monochromacy of the incident beam incase of ideal lateral thickness homogeneity. A prerequisite for the resolution of
thickness oscillations of films thicker than 250 nm with Cu K is a small beam
divergence and a high beam intensity. In commercial XRR systems and in literature,various solutions have been given comprising (1) direct beam optics, (2) Göbel
mirror optics, (3) channel cut monochromators and (4) secondary
monochromators. These beam optics, however, suffer either from a large
divergence or a low intensity.

5.2

1E-4

1E-3

1E-5

1E-4
1E-5
3.8

2 / °

4.0

4.2

4.4
4.4

4.6
4.6

4.8

5.0

5.2

2 / °

22.35

/°

22.40

20.70

22.45

0.1

/°

20.80

20.85

22.35

4.6

1E-4

4.2

4.4

1E-3

4.6

4.8

5.0

5.2

1E-5

N*d = 414 nm

22.50

22.35

4.4

4.6

4.0

4.2

4.4

4.6

4.8

5.0

1E-3

1E-5
3.8

5.2

/°

22.45

22.50

1E-4

1E-5

4.4

4.6

1E-3

1E-5

4.4

4.6

1E-4

4.0

4.2

4.4

2 / °

4.6

4.8

5.0

1E-5
3.8

5.2

2 / °

N*d = 415 nm

22.40

0.01

1E-4

1E-5
3.8

2 / °

22.45

1E-4

1E-4

4.0

/°

0.01

Reflectivity

4.4

Reflectivity

1E-5

22.40

Ge(022)

0.1

1E-4

0.01

1E-3

FWHM
 = 20“

0.1

1E-4

Reflectivity

20.75

0.1

0.01

1E-5
3.8

Ge(022)FWHM
 = 14“Reflectivity

Intensity
22.30

GM + COMP VC

Ge(022)FWHM
 = 26“Intensity

Ge(022)FWHM
 = 15“GM + EXP VC

Intensity

GM + asymmetric CC

Intensity

Result:GM + symmetric CC

4.0

4.2

4.4

4.6

4.8

5.0

5.2

2 / °

N*d = 414 nm

N*d = 414 nm

GMsym.CCasym.CC

EXP VCCOMP VC

intensity after primarybeam optics [cps]3 * 109

1.3 * 108

1.5 * 108

1.7 * 108

3.9 * 107

beam width [mm]

0.8

0.55

0.55

2.2

0.15

intensity after sample
reflection (Ge022) [cps]2.1 * 108

1.0 * 108

6.4 * 107

1.4 * 108

2.2 * 107

divergence Ge(022)*

0.030°

0.0037°0.0070°0.0035°0.0052°GM
Göbel mirror
CCchannel-cut monochromator
VC
V-cut monochromator
EXP
beam expander
COMP beam compressor* We estimated the divergence from the measured FWHM by using a 12” Darwin widthof Ge(220) symmetrical Bragg reflection.

Summary

The resulting beam properties have been characterized by rocking curves on a Ge(022) reflection from a perfect single-crystalline germanium
sample and -2scans on multilayer samples of various layer stack thicknesses.
Compressing and expanding V-cut Ge(022) crystal monochromators (VC) are compared with standard symmetric and asymmetric channel cut
monochromators (CC). The results on the beam width, divergence and intensity are summarized in the table above.
Beam width and angular resolution can be tuned by the beam optics. Layer stack thicknesses of more than 400 nm can be analyzed with a
combination of a parallel beam Göbel mirror and a CC/VC [1, 2]. The resolution of Kiessig fringes is best for the expander VC yielding adivergence of 0.0035° at a gross beam intensity of 140 Mio. cps using a long fine focus Cu tube (2.2 kW) at 40 kV / 40 mA.
The ideal lateral homogeneity better than d/d = 0.1% and the accurate periodicity of the layer stack do not obliterate oscillations andtherefore meet the requirements of high resolution X-ray reflectometry.

Fraunhofer

XTOP 2004

Institute
Material andBeam Technology

References:[1] DPG Spring Meeting 2004, Regensburg,
08-11.03.2004[2] D. Korytar, priv. communication andproviding CC monochromators.
Contact:
Thomas Holz, Tel: +49 (0)351-833913250
Reiner Dietsch, Tel: +49(0)172-8420546

Multilayer X-ray optics with high precision deposition
M. Krämer*, R. Dietsch*, Th. Holz*, D. Weißbach*, St. Braun***
AXO DRESDEN GmbH, Siegfried-Rädel-Str. 31, 01809 Heidenau, Germany; contact@axo-dresden.de** Fraunhofer IWS, Winterbergstr. 28, 01277 Dresden, Germany

High precision deposition

ASTIX optics

DIBD

Combination of complementary high precision
deposition technologies:- Magnetron Sputtering (MSD)- Large-Area PLD (LA-PLD)- Dual Ion Beam Sputter Deposition (in cooperation with IWS)

Small angle X-ray scattering: ASTIX optics – modified
Montel geometry for the generation of 2-dim. highintense focused or collimated X-ray beams

Features of ASTIX-f optics:• symmetric spots in focal plane even for highly asymmetric source dimensions• better lateral & temporal homogeneity of beam profile in the focal plane• wide variety in spot dimension from <30 μm to more than 300 μm with fixed
anode tubes depending on multilayer system, deposition and geometry parameters• imaging properties are more independent of source dimension
in beam path direction (take-off angle effects)• typical length up to 150 mm• improved P/B ratio due to low background
ASTIX 150 and ASTIX 100 withvacuum mirror housing

MSD

Typical multilayer systems:
MSD: W/Si, Mo/Si, Pd/B4C, …
DIBD: Ni/B4C, C/C, a-C, …
PLD: Ni/C, C/C, a-C, …

C/C

Ni/C

with reciprocal space image of electron diffraction

Background reduction
μ-focus MoK source coupled with ASTIX-f (red curve) vs. X-ray tube + HOPG + capillary (blue)

Mo/Sismooth interfaces

2 = 40°-70°

X-ray Mirror Geometries- nearly same peak intensity &reduced illuminated sample volume- higher resolution (K1+2 splitting) &reduced background intensity with ASTIX-f
 2 times higher flux density
 half of the total flux in the focal spot

2D

1D

- Side-by-side optical systems:-- Montel (c)-- ASTIX (d)- Kirkpatrick-Baez arrangement (e)- Single bounce mirrors (f)Parallel beam optics:- Twin mirror arrangement (a)- Goebel Mirror (b)
(a)

(c)

2 = 4°-40°

Diffraction patterns of an ylid crystal:
Improved P/B ratio due to reduced scattered background.
Arrangement 1 (left): fixed anode tube (Mo) with HOPG
Arrangement 2 (right): μ-source (Mo) with ASTIX-f(e)

Microspots
(b)

(d)

(f)

20000 data points

Radiation Focal length f2 Spot size
Cr K150 mm 105 μm
90 mm
< 100 μm
Cu K

Ag K
Mo K

100 mm
100 mm 40 μm< 25 μm

25 μm step size 2D (right) and5 μm step size linear (below)
X-ray absorption scan of a Cu
SEM grating (400 lines/inch)with a 40 μm diameter Ag K
beam. A Moiré pattern isvisible in the 2D scan.
The ~60 μm grating structure
can be clearly resolved.

Microscope images (below) of the Cu SEM gratingwith an illustration of the beam spot size.
95.000Parallel beam for X-ray reflectometry
-TWINs – High resolution mirror setup for reflectometry (XRR)

I0 > 10 cps (Cu K)80.013° (45 arcsec)
beam divergence
600 nm resolution
without channel cut
log. intensity a.u.

Reflectivity scan of a W/Si ML withresolved Kiessig fringes of ~0.01°
total layer stack thickness:d = 2.9 nm, N = 200

N*d = 580 nm

Cu K
0.5

1

1.5

2

2.5

3

lin norm. intensity

Cu K
0.007

0.006

0.005

0.004

4.25

COST Salamanca 2009

4.5

4.75

 [degree]

5

3.5

4

 [degree]

0.008

5.25

4.5

5

5.5

6

6.5

The optimized combination of
low divergence multilayer
optics and reflectometry X-ray
tube yields to a divergence ofless than 50 arcsec (compared to
110 arcsec in standard TMA) inthe parallel beam. So it ispossible to measure total thinfilm thicknesses up to 600 nm
without channel cut
monochromators in the beampath. An improved P/B ratio isachieved due to suppression ofother characteristic emission
lines (Cu K) and sample
fluorescence radiation. So adynamic range of more than 7orders of magnitude can becovered.
-Twins combine the highintensity and brillance of amultilayer mirror system with ahigh resolution comparable tochannel cut systems.

beam
scan direction

Intensity / cps

90.00085.00080.000

Grating constantd =1500 μm / 24 = 62.5 μm

75.00070.000
64,5

65,0

65,5

66,0

66,5
Y / mmμ-XRF
Modular X-ray system (micro source +ASTIX-f optics) applicable both forstandard XRD (powder diffraction / SCD)
and micro diffraction
Mo K μ-focus X-ray source (spot  50 μm, 30 W) and ASTIX-f100:
μ-XRF spot  < 30 μm at 30 W
Application:• Scanning μ-XRF by monochromatic excitation• Combination of scanning μ-XRD and μ-XRF# with courtesy of Prof. B. Kanngiesser, TU Berlin,
Institute for Atomic Physics and Teacher Training, Berlin, Germany

67,0

67,5

68,0

Nanometer thin films as XRF reference samples
M. Krämer1, R. Dietsch1, D. Weißbach1, G. Falkenberg2, R. Simon3, U. Fittschen4,5, T. Krugmann5
1 AXO DRESDEN GmbH, Siegfried-Rädel-Str. 31, 01809 Heidenau, Germany; contact@axo-dresden.de.
.

2 HASYLAB at DESY, Notkestr. 85, 22603 Hamburg, Germany

3 Institute for Synchrotron Radiation, FZ Karlsruhe, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein, Germany
4 Chemistry Division, Los Alamos National Laboratory, P.O. Box 1663 Mail Stop

K484, Los Alamos, NM 87545, USA

5 Institute for Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg, Germany

Introduction

Homogeneity

Schematic of XRF thinfilm reference samples
Metal layers (1-10nm)- Absorption free standard – nomatrix correction needed

Substrate (foil, membrane)- Wide range of suitableelements- Selection of non-overlapping
X-ray fluorescence lines

Applications:- Quality assurance in XRF set-ups:alignment, optimization, calibration,
minimum detection limits- Confocal setups: depth resolution,
detector capillary calibration

Fabrication- Signal strength easilyadjustable by layer thickness,comparable intensity for all
elements- High degree of uniformity andhomogeneity possible (PVD)

polymer foil

ANKA FLUO-Beamline, KIT, Karlsruhe, Germany (shown here)
Beamline L, HASYLAB at DESY, Hamburg, Germany
μ-XRF Eagle III, Los Alamos National Laboratory, USA

Radiation energy:

9.5 keV, 25 keV, 26 keV, 28 keV synchrotron; 20 kV laboratory

Scanning area:
Probe/Beam size:

0.3x0.3 mm2 up to 15x15 mm2
μm2 range up to mm2 range

Elements scanned:

Si, Ca, La, Fe, Cu, Pb, Mo, Pd (La and Cu shown here)

Homogeneity:

Deviation < 1% over the entire scanned area
SF2 26 keV

S10 9.5 keV

μ beam mapping(2.3 μm x 6 μm)

Large area map

μ beam sampling(2.3 μm x 6 μm)

μ beam „mapping“(2.8 μm x 12 μm)

Cu Kα

Cu Kα

Cu Kα

Cu Kα

Cu Kα

silicon nitride membrane
1.2mm

1.4mm

15mm

10mm

30mm

1.4mm

50mm

SF1 26 keV
Large area map(0.8 mm x 0.4 mm)

15mm

Multielement samples were
fabricated by PVD methods
such as Magnetron
Sputtering (MSD), Ion Beam
Sputtering (IBS) and Pulsed
Laser Deposition (PLD).

Radiation source:
Advantages:

5mm

La Lα

La Lα

La Lα

La Lα

La Lα

Polymer foils and silicon
nitride membranes wereused as ultrathin substrates.

Energy spectrum
Sum spectra of the reference samples were measured at various Xray sources. It can be seen that comparable characteristic emission
lines of six to seven elements are well separated in the energy scale.

Concentrations
Chemical Analysis(University of Hamburg)

Sum spectra of thesamples SF1 (black),
SF2 (blue), RF4 (red)measured at 40 keV
at HASYLAB
Beamline L

Foils were digested by HNO3 / H2O2
and a Mars Microwave digestion
device. Elements were determinedusing a Ciros CCD ICP-OES
instrument (Spectro).

XRF Analysis(ANKA, Karlsruhe and
HASYLAB/DESY, Hamburg)
Sum spectra were calculated fornumerous area mappings.
Elemental concentrations were
determined by ab initio
calculations with instrumental
parameters.

Sum spectrum of sample
S10 measured at ANKAFLUO beamline(25 keV, 0.1x0.1 mm²)

Comparison of calculated deposition amounts (Aim)and measurement results of different analysis
methods (XRF and ICP-OES) for three identicalreference samples (SF1, SF2, S100). Most target
values were achieved and reproducible.

Results
Sum spectrum of sample RF4
measured at an Eagle
laboratory μ-XRF with Rh
tube (20 kV) at Los Alamos
National Laboratory- Successful production of multi-element reference samples.
- High degree of homogeneity and reproducibility.
- Low X-ray absorption (below 2% in standard SF1 for E > 3 keV).
- Large spectral range without line overlap, emission lines have similar intensities.
- Membrane substrates withstand high radiation dose.

connected withICXOM-2009