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Stahl 2014
Stahl 2014
Joachim Albrecht
Institute for Innovative Surfaces, FINO, Aalen University, Beethovenstraße 1, 73430 Aalen, Germany
(Received 5 June 2014; revised manuscript received 3 September 2014; published 19 September 2014)
The magnetic flux distribution arising from a high-Tc superconductor is detected and visualized using polarized
x rays. Therefore, we introduce a sensor layer, namely, an amorphous, soft-magnetic Co40 Fe40 B20 cover layer,
providing a large x-ray magnetic circular dichroism (XMCD). Temperature-dependent XMCD spectroscopy on
the magnetic layer has been performed. Exploiting the temperature dependence of the critical current density
of the superconductor we find a quantitative correlation between the XMCD signal and the in-plane stray field
of the superconductor. Magneto-optical Kerr effect experiments on the sensor layer can simulate the stray
field of the superconductor and hence verify the correlation. We show that the XMCD contrast in the sensor layer
corresponds to the in-plane magnetic flux distribution of the superconductor and can hence be used to image
magnetic structures in superconductors.
based on the magneto-optical Kerr effect, in which the place in a homogeneously in-plane magnetized quadrant of
superconductor is simulated by an external magnetic field. the square sample.
Finally, one of our first x-ray microscopy images of the double
layer is presented. The image pictures the magnetic domains
III. X-RAY SPECTROSCOPY EXPERIMENTS
of the superconductor which are mapped into the sensor layer
and visualized through the XMCD contrast of the Co L3 edge. The XMCD spectroscopy measurements were carried out
at the Helmholtz-Zentrum BESSY II in Berlin, Germany,
II. BASIC CONCEPT at the high photon flux Apple II type undulator beamline
UE56/2-PGM1, with variable photon energy and polarization
In Fig. 1 the critical state of a YBCO thin film is necessary for XMCD investigations. In order to measure in-
investigated by magneto-optical imaging with subsequent plane and out-of-plane magnetization components at various
numerical analysis. Figure 1(a) depicts the absolute value orientations of the external magnetic field, it is necessary to
of the critical current density and Fig. 1(b) the in-plane have a versatile experiment. We used a dedicated soft x-ray
component of the flux density distribution. The squared shape magnetic reflectometry end station built at the MPI for Metals
of the superconducting film leads here to the formation of Research, which allows nearly arbitrary field and sample
four current domains each having a constant current density orientations with high angular precision [27].
jc [25]. The in-plane components Bx of the magnetic flux Typically, the XMCD effect is defined as the difference
distribution are constant in each domain of constant current. in absorption between two measurements with a flipped
This can also be calculated by Bx = μ0 jc (d/2), with d being relative orientation of external field or beam polarization. Here,
the thickness of the superconductor [26]. This shows that in we extract the magnetic signal of the sensor layer CoFeB
thin-film geometry the in-plane components of a magnetic which is induced by the local current of the critical state
field generated by the critical current are proportional to the of the superconductor. Therefore, we designed a setup and
currents themselves. measurement routine. We prepared two different critical states
The method of magneto-optical imaging is sensitive to the in the superconductor with the supercurrent flowing clockwise
out-of-plane component of the magnetic flux distribution and and counterclockwise, respectively. In both cases an external
therefore a complex numerical inversion scheme is needed in magnetic field has been absent. Since the supercurrents create
order to obtain the critical current density [5]. This inversion a magnetic field, this field has opposite direction in these two
scheme would be redundant if the in-plane component was cases. These are labeled “north” and “south” in analogy to
measured. This fact is exploited by the following novel the north and south poles of a magnet. Without an external
measurement technique: The in-plane field component of the field during the measurements with circular polarized x rays
magnetic stray field of the superconductor magnetizes the the obtained magnetization is predominantly created by the
soft-magnetic sensor layer within the plane. A measurement critical state of the superconductor. With this measurement
of this local magnetic signal in the sensor layer allows sequence x-ray absorption spectra (XAS) of the Fe and Co
the reconstruction of the in-plane field component of the L2,3 edges at T = 38 K were obtained [Figs. 2(c) and 2(d)].
superconductor and with that of the critical current density. The setup has been chosen in order to apply an out-of-plane
Both Figs. 1 and 7 picture a sample with size 1 × 1 mm2 , external field to the superconductor and at the same time to
whereas the spectra are measured on a sample with the same measure the in-plane projection of the magnetization of the
geometry but a size of 5 × 5 mm2 . All three samples exhibit CoFeB layer. The angle of incident between the photons
the same square shape and have passed through the same and the sample surface was chosen to be = 70◦ . A sketch of
production process. Their characteristic properties have been the measurement geometry is given in Fig. 2(b); the position of
found to be very similar and hence comparable. The spot where the measurement is indicated by the orange spot in Fig. 1(b).
the x-ray spectroscopy measurements are taken is indicated in Note, the measurement configuration of = 70◦ between
Fig. 1(b) by an orange dot. The spectroscopy always takes the beam axis and the sample surface still provides as a main
component the in-plane magnetization of the CoFeB layer.
This becomes clear when considering the hysteresis loops of
the sensor layer shown in Fig. 2(a), measured at T = 300 K
using a Quantum Design MPMS SQUID magnetometer and
a NanoMOKE3. The in-plane (light and dark blue) and the
out-of-plane (green) magnetic moment of a CoFeB layer with
a thickness of 30 nm sputtered on YBCO with a thickness
of 100 nm is depicted. We find a soft-magnetic behavior
with clear in-plane easy axis. The in-plane hysteresis curve
exhibits a coercivity of about μ0 Hc = (2 ± 0.4) mT; above
approximately μ0 H = 3.5 mT the curve is saturated. The
FIG. 1. (Color online) Magneto-optical images of the critical slight variations between the two curves result from the fact
state of a YBCO thin film. The gray scale represents (a) the that the NanoMOKE measurement is local compared to the
absolute value of the critical current density jc and (b) the magnetic global magnetic moment of the superconducting quantum
flux distribution in the plane Bx , which is proportional to jc . The interference device (SQUID) curve. The measurement in a
orange point marks the spot for the in-plane x-ray spectroscopy corresponding out-of-plane geometry reveals magnetization
measurements which are always performed in the critical state. values that are about a factor of 10 smaller. An extensive
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FIG. 2. (Color online) (a) SQUID and MOKE hysteresis loops of 30 nm CoFeB on YBCO, in plane (dark and light blue) and out of plane
(green). The coercivity is μ0 Hc = (2 ± 0.4) mT and when saturation of the in-plane component is reached the magnetization is a factor of 10
larger compared to the out-of-plane part. The inset displays a wider range of magnetic field. N.B. Kerr rotation can be converted into absolute
values of the magnetization by comparing the curves from the two measurement methods. (b) Sketch of the measurement configuration in the
reflectometry end station: The magnet is oriented along the sample’s normal; the incoming beam is under an angle of = 70◦ towards the film
surface. The magnet is only used to induce current into the superconductor and is switched off during measurement. The magnetic fields for all
measurements originate from the superconductor. (c) and (d) Absorption spectra at the Fe and Co L2,3 edges at T = 38 K and Hext = 0. The
source of the magnetic field is the in-plane stray fields of the superconductor.
characterization of the samples used in this work can be found chosen here. Measurements have been done for both Fe and Co
in Stahl et al. [28]. and their analysis has yielded equivalent results. The curves
The difference between measurements of the north and for Fe (squares) and Co (triangles) follow the same shape.
south critical states is related only to the magnetization of A constant finite value is found for temperatures below T =
the element that has been measured. The XMCD obtained 55 K. Above T = 55 K the signal decreases continuously until
from the measurement of the Fe L2,3 edges shown in Fig. 2(c) it vanishes at 80 K < T < 90 K.
is depicted in Fig. 3(a). The same routine has been used at
different temperatures up to T = 90 K and the temperature-
dependent XMCD at the Fe L3 edge is shown in Fig. 3(b).
Above the critical temperature of the superconductor of Tc = IV. CORRELATION BETWEEN SENSOR LAYER
85 K the XMCD signal gets smaller than our measurement AND SUPERCONDUCTOR
sensitivity, clearly showing that the observed XCMD signal is In order to use XMCD measurements on the CoFeB
related to the superconducting state and that the ferromagnetic layer on top of the YBCO as a sensor for the magnetic
component itself does not significantly contribute to the flux density in the superconductor, a correlation between the
observed effect. XMCD values and the signal of the superconductor is needed.
The strength of the L3 edge XMCD effect represents the Figure 4(a) depicts the temperature-dependent measurement
projected magnetization along the photon beam direction of the critical state of the superconductor. At T = 6 K an
averaged over the photon beam spot size. N.B. The 70◦ angle external out-of-plane field of μ0 H = 300 mT has been applied
of incident has been corrected for the XMCD curves in Fig. 3 and subsequently removed. Then the temperature has been
but not for the XA spectra in Figs. 2(c) and 2(d). To extract increased until the critical temperature has been reached.
the absorption at the L3 edge the peak value of each XMCD The SQUID magnetization measurements yield the magnetic
curve has been divided by its peak value of the XA spectrum. moment m of the YBCO thin film. In the critical state of the
Hence, the XMCD value in percentage of the XAS spectrum superconductor this can be converted into the critical current
is plotted as a function of temperature in Fig. 3(c). N.B. This density via m = 12 V j × r d 3 r. Since the in-plane component
evaluation routine is equivalent to the analysis of the x-ray of the magnetic flux density Bx is proportional to jc [26] this
microscopy images following in Sec. V and therefore was has been plotted here directly.
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FIG. 3. (Color online) (a) XMCD signal from the Fe L2,3 edges
shown in Fig. 2(c). (b) XMCD signal of the Fe L3 edge at various
temperatures. (c) XMCD L3 edge of Co (red triangles) and Fe (black
squares) in percentage of the XAS value versus temperature. At T >
Tc both XMCD signals vanish, in region 2 (55 K < T < Tc ) there is
an increase with decreasing temperature, and at T < 55 K the signals
saturate (area 1).
FIG. 4. (Color online) (a) SQUID measurement of the magnetic
The temperature dependence of the critical current density moment of YBCO (green circles) converted to the in-plane com-
in a YBCO thin film is described as follows [29,30]: ponent of the magnetic flux distribution. The fit curve obtained by
using the model for the temperature dependence of the critical current
T s
jc (T ) ∝ Bx (T ) ∝ 1 − . (1) density [Eq. (1)] is shown as a red line. (b) XMCD L3 edge of Co
Tc (red triangles) and Fe (black squares) in percentage of the XAS
This formula is fitted to the data in Fig. 4(a) at temperatures value versus the in-plane field component of the stray field of the
superconductor. With the correlation B(T ) obtained from Fig. 4(a)
38 K < T < Tc with Tc = (84.82 ± 0.04) K and s = (1.213 ±
temperature can be converted into the magnetic flux density which
0.003). The measured data points and the curve are in
the superconductor provides at this temperature. The graph shows
accordance with each other within linewidth.
the correlation between the measured XMCD signal in the sensor
The temperature of the XMCD measurements can now be layer and the magnetic flux density of the superconductor. The data
converted into the flux density of the YBCO. The data shown is modeled by Eq. (2).
in Fig. 3(c) is plotted as a function of the in-plane flux density
in Fig. 4(b). The result is a direct and quantitative correlation
between the XMCD signal of the sensor layer and the flux
In order to verify the so obtained correlation between the
density of the superconductor.
XMCD signal and the flux density of the superconductor
In analogy to the calculations for magneto-optical sensor
additional measurements have been performed: The same
layers [10,31] the measured XMCD signal ξ proportional to
sample has been measured at room temperature in an ex-
the magnetization M as a function of the local magnetic field
ternal in-plane field. In this setup the flux density of the
H can be described by
superconductor is simulated by the external magnetic field.
1 H − Hc Hc N.B. The sensor layer material CoFeB has been measured to
ξ (H ) = ξs sin arctan + arctan .
2 Ha Ha be nearly temperature independent in the region 30 K < T <
(2) 300 K. When simulating the magnetic flux density provided
Here, the saturated XMCD signal is ξs = (6.99 ± 0.05)% of by the superconductor the procedure of the spectroscopy
the XAS, μ0 Hc = (1.90 ± 0.02) mT, and μ0 Ha = (0.67 ± measurements has to be considered: The superconductor has
0.03) mT. Hc and Ha are fitting parameters that correspond been prepared alternately in a positive and negative critical
to the coercive field and the anisotropy field, respectively. In state (called north and south). This means that the flux density
our case the values might slightly deviate owing to the fact that has been ±Bx .
the magnetization reversal runs along minor hysteresis loops. This scenario is realized via magneto-optical Kerr effect
The introduction of Hc is necessary because Hc /H cannot be (MOKE) measurements with a laser-NanoMOKE3. The setup
neglected in contrast to the magneto-optical case. provides an in-plane external magnetic field and an in-plane
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CLAUDIA STAHL et al. PHYSICAL REVIEW B 90, 104515 (2014)
taken at room temperature in zero external field after applying This requires the presence of appropriate probes that exhibit
and subsequently removing an external out-of-plane magnetic a dichroic signal. Therefore we fabricated optimally doped
field of μ0 Hext = 240 mT at T = 12 K. For comparison this high-Tc superconducting YBCO thin films with soft-magnetic
originally prepared critical state is pictured on the left obtained CoFeB covers as sensor layers directly on top. The magnetic
by magneto-optical imaging at T = 12 K in zero external field. flux density of the superconductor is mapped onto the
The magnetic domains of the superconductor are persistent in local magnetization of the magnetic layer. This magnetic
the sensor layer even above the critical temperature [28]. The signal is measured via XMCD spectroscopy as a function of
sample is comparable to the one shown in Fig. 1, but has temperature in zero external magnetic field. In this case, the
defects in order to show the abilities of the method. superconductor remains as the dominant origin of the magnetic
When comparing both images of the same sample in field. As a result the XMCD signal of the sensor layer can be
Fig. 7 the four domains of the flux density distribution of correlated to the in-plane flux density of the superconductor.
YBCO are visible as well as the domains due to scratches This allows the quantitative determination of the stray field
in the superconductor. The in-plane component of each of of superconductors via XMCD when one calibration point is
the four domains points in a different direction. The 90◦ obtained by a simple magneto-optical Kerr, Farady effect or
angle between the domains is visible in the form of one SQUID measurement. Based on these findings we performed
dark and one bright domain as well as two gray domains. room temperature magnetic x-ray microscopy on a comparable
The scratches are magnetized in the opposite direction as the sample, which had been prepared in the critical state of the
surrounding domain. This shows that XMCD microscopy of superconductor. The image visualizes that x-ray microscopy is
a magnetic sensor layer can map the magnetic flux density of capable of imaging the stray field domains of the superconduc-
a superconductor. Here, the measurement is not temperature tor, which are mapped into the sensor layer. Ongoing upgrades
dependent but spatially varying, which reveals the spatial of the microscopy setup will allow images at temperatures
distribution of the stray field of the superconductor. Since below the critical temperature reproducing the capabili-
Fig. 6 gives a monotonic and distinct correlation between ties of magneto-optical imaging while exceeding its spatial
the XMCD signal and the flux density, qualitative mapping resolution.
is possible. Quantitative analysis will also be possible if a
calibration measurement is taken by MOFE or in analogy to
magneto-optical imaging via a calibrated external field.
The capabilities of the microscope promise a further ACKNOWLEDGMENTS
increase in spatial resolution beyond the limits of the methods
based on visible light when all parameters are fully optimized, The authors appreciate the support by Iuliia Bykova, Birgitt
especially when low temperatures will be reached. Zada, and Willy Mahler and the whole team of BESSY II and
thank Helmholtz-Zentrum Berlin, Germany for the allocation
of synchrotron radiation beamtime. We are deeply grateful
VI. CONCLUSION
to Georg Christiani, Bernd Ludescher, and Patrick Walker
In conclusion, we present quantitative investigations of for fabricating these outstanding samples and thank Christian
the magnetic flux density in superconductors via XMCD. Wolter for technical support.
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