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Hard Xray Directional Dark Field
Hard Xray Directional Dark Field
X-ray absorption contrast imaging has been widely used deviation as a dark-field signal (see the Supplemental
in medical diagnostics and material science. Phase-contrast Material [12]). Recently, an alternative method has been
imaging can further enhance the sensitivity for samples proposed to extract the dark-field image using only a few
with weak absorption. X-ray dark-field imaging, which is images [13], Nevertheless, the spatial resolution of this
related to the subpixel structural anisotropy or variations in method is poor, and the directional dark-field information is
the electron density in samples on length scales smaller not accessible. In this Letter, we describe a new algorithm
than the detector resolution, provides complementary to extract the directional dark-field signal from the maxi
mechanisms to reveal subtle features of the material under mum correlation coefficient by applying normalized
study [1], Even though dark-field imaging is well known in cross-correlation algorithms. We demonstrate that pixelwise
visible light and electron microscopy, it has taken nearly analysis of dark-field images can be performed by scanning
a century after the discovery of x rays for it to be realized a phase object in only one dimension (ID).
in the x-ray regime. Initially, it was demonstrated using When an object consisting of high-spatial-frequency
analyzer crystals [2], but the dark-field signal was weak due features is placed into a coherent or partially coherent
to the low bandpass (~10-4) of crystal optics. Over the last photon beam, a speckle pattern is generated by the combi
decade, dark-field imaging has increased in popularity after nation of numerous waves of the same frequency but with
successful demonstrations using grating interferometry different phases and amplitudes. In the x-ray near-field
[3-5]. Directional dark-field imaging shows great potential region (z < 2nqd/X, where X is the wavelength, £ is the
for the application in mammography, emphysema diagnosis, coherence length, and d is the average pore size of the
and material study [6-8]. Recently, the edge-illumination membrane or scattering particle), the speckle size does not
technique was also successfully used to detect the dark-field depend on the distance from the phase membrane or the
signal with incoherent illumination [9,10], However, most x-ray energy [14,15], This remarkable property allows the
existing dark-field imaging techniques involve complicated near-field speckle to access x-ray scattering information in
optical elements, such as perfect crystals, precision gratings, the low-g region, thereby enabling investigation of inho
or sophisticated masks. To overcome these limitations, the mogeneous systems [16], The key idea behind using phase
x-ray near-field speckle technique was demonstrated to membranes is to act as a high-frequency wave front marker
retrieve the dark-field image by scanning a simple phase and enable the geometrical path of each ray to be uniquely
object (a membrane or abrasive paper) [11], Unfortunately, tracked as it passes through the sample. When a phase
this approach is time consuming as two-dimensional (2D) membrane is scanned along the horizontal (vertical) direc
raster scans involve acquiring a large number of images. tion xp (yp), the intensity signal 1(1, m) in each pixel (/, m) in
Furthermore, it is not appropriate to treat the standard the detector plane oscillates as a function of xp (yp). The
amplitude of the speckle pattern depends on the degree of
coherence of the x-ray beam [17], which is degraded by
small-angle scattering by the specimen, thereby broadening
Published by the American Physical Society under the terms of
the Creative Commons Attribution 3.0 License. Further distri the speckle pattern. Variation in the intensity of the speckle
bution o f this work must maintain attribution to the author(s) and pattern due to this broadening can, therefore, be used to infer
the published article’s title, journal citation, and DOI. the change in beam coherence induced by the specimen.
The fundamental principle of the method presented here is to v(l , m) can then be used to calculate the local wave front
evaluate the maximum correlation coefficient distribution radius of curvature, which is related to the wave front
for each pixel with its neighboring pixel from a stack of gradient [11,19]. The maximum value of the correlation
speckle images captured with and without the specimen. To coefficient is reduced if the difference of the coefficient
analyze such a coherence change quantitatively, the intensity an between two nearby pixels increases due to strong
oscillation for pixel (l, m) in a Fourier series is distortion of the speckle pattern. The relative decrease of
the correlation coefficient due to the specimen can be used to
N quantify the loss of the coherence, and the normalized
I (l ,m ,x p) = ^ a \ ( l , m ) e x ^ [ b hn(l,m)xp + (phn(l,m)\, maximum correlation coefficient M / m can be defined as
n =0
N = (4)
I(l>m,yp) = Y ^ a vn(l,m)exp[bvn{l,m)yp + (pvn(l,m)},
n =0 where s and r denote the sample and reference beams,
(1) respectively.
Dark-field image contrast increases when the maximum
where h and v denote horizontal and vertical scans, and n correlation coefficient M reduces due to internal inhomo
is the order of the Fourier series. For simplicity, only geneity in the specimen. As mentioned above, grating
the vertical scan case is discussed below, and we drop the interferometry is treated as a special case of the speckle-
subscripts h and v to aid clarity. an, bn, and cpn are the based technique. Hence, the normalized maximum corre
appropriate Fourier coefficients. The values of all coeffi lation coefficient M for the proposed technique is analogous
cients depend on the order number and the pixel position. to the fringe visibility V for grating interferometry. The
As described in Ref. [11], grating interferometry can be dark-field signal D can be defined via the relation [20]
considered as a special case only if Eq. (1) is approximated to
first order. In this instance, the constant bx is related to the D = —21ogM. (5)
analyzer grating period, and the amplitude coefficients a0,
Although several physical phenomena can contribute to
a x, and phase shift cpx can be retrieved by performing ID
the reduction of the correlation coefficient, we consider
discrete fast Fourier transforms for each pixel [18]. Speckle-
only the two dominant phenomena: small-angle scattering
based imaging can be understood as a general case where
and second-order differential phase contrast [21]. In par
all orders are included to adequately describe the observed
ticular, the internal electron density fluctuations in the
speckle intensity oscillations. For vertical scanning mode,
specimen produce small-angle x-ray scattering, which, in
the coefficients bn for neighboring pixels (/, m) and (/, m!)
turn, distorts the speckle pattern. The second-order differ
are approximately equal, whereas the differences in coef
ential phase contrast from a specimen is often observed
ficients an can be quantified by the correlation coefficient
under illumination using a partially coherent x-ray beam.
y(l ,m,yp). This is typically performed at every step by
The speckle pattern abruptly changes around the edges of
subtracting the mean and dividing by the standard deviation
the specimen, creating an interference pattern. Hence, the
of the respective signals:
contribution from the second-order differential phase con
trast is also included in the calculation of the correlation
I{l,m , y p) - I ( l , m , y p ) coefficients.
r { l m , y p)
A/(Z, m ,y p) The principle of the technique presented was validated
I(l,m',yp) - I ( l , r r i , y p) with experimental measurements at the Diamond Light
P) Source’s B 16 Test beamline [22], X-rays with an energy of
®— W ^) — 21 keV were selected from the bending magnet source
using a silicon double-crystal monochromator. A schematic
where I and A7 are the mean and standard deviation of the
of the experimental setup is shown in Fig. 1. The specimen
signals, respectively, (g> is the cross-correlation operation,
was mounted on a motorized stage located 47 m from
and the correlation coefficient y(l, m, yp) ranges from —1 to
the x-ray source. A membrane was mounted on a two-
+1. The maximum value of the correlation coefficient dimensional piezoelectric stage installed 100 mm down
(M/m) is unity, and occurs when the corresponding coef stream of the specimen. The distance between the specimen
ficients a„ are the same between 1(1, m, yp) and 1(1, m! , yp). and detector was 1000 mm. Images of the speckle pattern
This implies that only a phase shift is involved between the were collected using a high-resolution x-ray camera com
two signals. Here, the phase shift v(l, m ) can be assumed to posed on a PCO 4000 CCD detector and a microscope
be the same for all orders, and the phase shift coefficient for objective with a Ce-doped YAG scintillator. Two stacks of
the two signals can be written as images, with and without the specimen, were acquired
by scanning the membrane transverse to the x-ray beam
(pn(l,m') = (pn(l,m) + v(l,m) (3) for the horizontal and vertical dark-field images. As a
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1 3 4
FIG. 4 (color online), (a) Absorption image, vertical (b), and horizontal (c) dark-field images of a bar-pattern phantom. Two-times
magnified and contrast-optimized parts of the absorption image [(d),(f)] and directional dark-field image [(e),(g)]. (d),(e) and (f),(g)
show the horizontal and vertical bar patterns with a 2 /mi line width, respectively. The scale bar is equal to 0.2 mm.
significantly enhanced contrast compared to a conventional primarily perpendicular to the axial direction creating the
absorption image. observed contrast [4], In Fig. 4(b), vertical scattering is
A bar-pattern phantom was selected to demonstrate the clearly visible for the horizontal lines, while they are hardly
applicability of the dark-field technique for the study of noticeable in the horizontal dark-field images [Fig. 4(c)].
strongly ordered systems. This phantom is composed of In contrast, the vertical lines in Fig. 4(b) show much less
two 3 x 3 mm2 chips, which contain several line and point contrast than in Fig. 4(c). Therefore, the speckle scanning
patterns with features of 1 to 10 /<m wide. In order to show technique provides directional dark-field images and gives
the capability to inspect the porosity at a subpixel length insight into the orientation of the edges, fibers, or cracks in
scale, a lOx microscope objective was chosen to provide an the specimen. By looking closely at the sections of the
effective pixel resolution of 3.6 x 3.6 pm 2 by 4 x 4 pixel images [enclosed by the square regions in Figs. 4(a)—(c))],
binning. A sheet of silicon carbide abrasive paper with a dramatically different behavior in 'the absorption and
average particle diameter of 18.3 /mi was used so that the scattering information for the two directions is observed.
speckle pattern could be resolved by the detector. Exposure The lines in the marked square in Fig. 4(a) are not present
time for each image was 2 s, and 100 images for each stack, in the absorption image [Figs. 4(d) and 4(f)] since the line
with and without the sample, were acquired by scanning width is only 2 /mr, which is smaller than the detector pixel
the membrane transverse to the x-ray beam. In the conven size. In contrast, the scattering signals of these thinner lines
tional absorption image, Fig. 4(a), lines and points with are clearly visible in the corresponding dark-field images
thickness greater than 4 /mi are visible with lower contrast. [Figs. 4(e) and 4(g)],
Figures 4(b) and 4(c) represent the vertical and horizontal In summary, we have demonstrated that the speckle
dark-field images, respectively. As expected, the two direc scanning technique can be used for directional dark-field
tional dark-field images provide complementary informa imaging with pixel size spatial resolution, which enables one
tion. In principle, a locally strongly oriented sample scatters to detect fine structures in materials. The technique requires
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only moderate x-ray beam coherence and a simple exper [6] S. Schleede etal., Proc. Natl. Acad. Sci. U.S.A. 109, 17880
imental setup compared to the other dark-field imaging ( 2012).
techniques. In addition, quantitative scattering information [7] V. Revol, C. Kottler, R. Kaufmann, A. Neels, and A.
can potentially be derived from the dark-field signal. Dommann, J. Appl. Phys. 112, 114903 (2012).
[8] K. Scherer et a l, PLoS One 9, e93502 (2014).
Moreover, the proposed approach o f using a ID scan is
[9] M. Endrizzi, P. C. Diemoz, T. P. Millard, J. Louise Jones,
highly desirable for rapid and reduced-dose x-ray imaging
R. D. Speller, I. K. Robinson, and A. Olivo, Appl. Phys.
since it is much quicker than the conventional standard
Lett. 104, 024106 (2014).
deviation method employing a 2D raster scan. Furthermore, [10] F. A. Vittoria, M. Endrizzi, P. C. Diemoz, U. H. Wagner,
ID scanning enables directional x-ray dark-field imaging of C. Rau, I. K. Robinson, and A. Olivo, Appl. Phys. Lett. 104,
anisotropic samples. The technique can be employed for the 134102 (2014).
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properties. The technique further benefits from providing 063813 (2012).
both the dark-field image and the differential phase-contrast [12] See Supplemental Material at http://link.aps.org/
image simultaneously from the same data set [11], As the supplem ental/10.1103/PhysRevLett.ll4.103901 for com
phase contrast and the dark-field images provide comple parison between the proposed technique and the previous
method using standard deviation. An example is also given
mentary information, a more detailed characterization of the
to demonstrate that dark-field and phase contrast images can
sample is achieved (see the Supplemental Material [12]).
provide complementary information over the absorption
The method is equally applicable for the inspection of
image.
biomedical and material science samples. [13] I. Zanette, T. Zhou, A. Burvall, U. Lundstrom, D. H.
This work was carried out with the support o f Diamond Larsson, M. Zdora, P. Thibault, F. Pfeiffer, and H. M. Hertz,
Phys. Rev. Lett. 112, 253903 (2014).
Light Source Ltd. The authors are grateful to Sebastien
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Berujon from ESRF for fruitful discussion and Simon
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