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H. Stiel, H. Legall
Hard x-ray spectroscopy
Funding: This project was founded by the Land
Berlin (ProFit) and EFRE.
Collaborations: Optigraph
GmbH, TU-Berlin,
IAP,
IfG, HZB-BESSY and PTB
Berlin
Investigations of the spectral properties
of Highly Oriented Pyrolytic Graphite (HOPG)
For x-ray spectroscopy in the keV range using ultrashort fs-pulses
emitting laser plasma sources or microfocus x-ray tubes efficient
collecting x-ray optics with high integral reflectivity and high
energy resolution are required. For this special purpose the diffraction
properties of thin Highly Oriented
Pyrolytic Graphite (HOPG) layers
were studied.
| Thin crystals
of HOPG are of particular interest for the use as dispersive
x-ray optics because their unique structure enables them to
be highly efficient in x-ray diffraction in an energy range
between 2 keV up to several 10 keV. HOPG is a mosaic crystal,
which consists of a large number of small crystallites (Fig.1).
The angular distribution of the crystallites, with plane orientations
off the normal axis to the surface, is called mosaic spread.
Mosaicity makes it possible that even for a fixed angle of
incidence to the crystal surface, an energetic distribution
of photons can be reflected, because each photon of this energetic
distribution can find a crystallite plane at the right Bragg
angle. On the other side, if the radiation is monochromatic
large accepting angle can be obtained. Therefore the mosaicity
is responsible for the dramatic increase of integral reflectivity
for mosaic crystals in comparison to perfect crystals. The
mosaicity also gives rise to mosaic focusing (parafocusing),
which further enhances the intensity in the image plane. In
addition thin crystals of HOPG give the opportunity
to realize crystal optics with arbitrary geometry by mounting
them adhesive on a polished mould of any shape. This enables
the design of crystal optics with high collecting efficiency. |
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Fig. 1: Experimental
setup.
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For investigation of the spectral properties a micro-focus x-ray
tube (IfG) with a source size of 50 µm was used and for recording
the reflected radiation a 16-bit deep depletion CCD camera (Roper
Scientific model PI-LCX 1300).
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Fig.2: The CCD-images
show the Cu Ka emission of a micro focus x-ray tube after
reflection by HOPG crystals in different distances and reflection
orders. |
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The spectral resolution of HOPG crystal
foils were investigated in two reflection orders of (002)
and (004). Images of the reflected Cu Ka radiation are shown
in Fig.2 for different distances. As can be seen in Fig.
2 the smearing of the Ka lines in the images remaines nearly
constant whereas the seperation of the lines increases.
Consequently the energy resolution increases with distance.
Due to increasing dispersion with distance constant contributions
to a smearing in the image plane, as e.g. source size and
penetartion depth can be neglected and the energy resolution
is then limited by the intrinsic broadening (darwin width
for perfect crystals) of the small crystallites in the mosaic
crystal. For the largest measured distance source-crystal
of 310 mm in (002)-reflection an energy resolution of E/deltaE=1800
was found at 8keV and in (004)-reflection a spectral resolution
of E/deltaE=2900. By rocking curve measurements the integral
reflectivity was determined to be 0.7e-3 rad in (002)-reflection,
which is about 10 times higher than that of Ge(111), while
in (004)-reflection an integral reflectivity of 0.08e-3
rad was estimated from the counts on the CCD.
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| Further enhancement
of energy resolution can be obtained if the intrinsic reflection
broadening is reduced. This is the case for a new kind of
pyrolytic graphite crystal provided by Optigraph
GmbH which is called Highly Annealed
Pyrolytic Graphite (HAPG).
In a comparison HAPG shows clearly better results in spectral
resolution. By rocking curve measurements an intrinsic width
of 27arcsec was obtained for HAPG crystals. On the other side
in the same manner as the intrinsic broadening was reduced
the intgral reflectivity of the HAPG crystals was reduced.
Measurements performed with different crystal thickness indicate
a reduction in mosaic spread for HAPG crystals. Latter is
favorable for high energy resolution because nearby a reduced
penetration depth an distance independent focusing error which
arises due to crystallites not aligned on the Rowland circle
is reduced too. Therefore with lower mosaic spread higher
spectral resolution limits can be reached with HAPG. Furthermore,
we found that the mosaic spread increases with crystal thickness
as well as the integral reflectivity on the cost of spectral
resolution (cp. Fig 4).
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Fig.3: Cross section
of the CCD-images measured for a thin HOPG crystal and for
spectroscopic application optimized HAPG crystal a distance
of F= 400mm..
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As mentioned above thin crystals of pyrolytic graphite
can be bent easily by mounting them on bent surfaces. That we have
done to investigate the influence of bending on the spectral resolution.
By bending crystals large collecting angles can be realized. Latter
is important if the signal is emitted in a large solid angle as
it is the case in laser plasma experiments. In Fig. 4 the measured
spectra for a 40 µm thick HAPG are shown. It can be seen that
bending seems not to affect the spectral resolution of the thin
pyrolytic graphite crystals.
Fig..4: CCD-images measured
for a flat HAPG crystals and and a bent HAPG film at a distance
of F=400 mm and a bending radius of 150mm.
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Von Hamos spectrometer
based on thin crystals of pyrolytic graphite
Spectrometer design
The spectrometer design can be different depending
on the desired field of application. If a broad energy range should
be covered and/or high collecting efficiency should be reached the
von Hamos geometry can be used. In this geometry a cylindrically
bent crystal focuses rays with different energy emitted from a point
source into different points on the cylinder axis, while in the
dispersion plane the curved crystal works like a flat crystal. The
position of the focal points on the cylinder axis depends on the
Bragg angle respectively on the photon energy of the radiation,
which is focused. Placing a CCD linear array in the cylinder axis,
with this scheme very compact spectrometer can be realized.

Fig..5:Von Hamos spectrometer.
Reported energy resolution with von Hamos spectrometer
ranges from 200 to 800 for HOPG in the first order reflection. However
there are some disadvantages of the von Hamos geometry. High spectral
resolution in a large spectral window results in spatially extended
image planes, exceeding the dimensions of commonly used electronic
detector systems. Additionally it is difficult to place a detector,
as e.g. commercially available cooled CCD-chips, on the axis of
the cylinder. Therefore we used a modified von Hamos geometry, in
which the CCD was placed perpendicular to the reflected radiation.
In this setup only a single photon energy is optimal focused on
the CCD. On the other side, test measurements have shown an only
sligthly reduction in spectral resolution for the used distances
F in our measurements. A picture of the spectrometer setup is shown
in Fig. 6. As can be seen, the design of the spectrometer allows
to adapt the spectrometer to an ultrafast
laser plasma X-ray source.

Fig. 6: Experimental setup (for photography
the shielding around the spectrometer was removed).
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