Effects of magnetic impurities on upper critical fields in ...
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Effects of magnetic impurities on upper critical fields in
the high-Tc superconductor La-doped CaFe2As2
Soon-Gil Jung1, Soohyeon Shin1, Harim Jang1, Pavlo Mikheenko2, Tom H Johansen2, and
Tuson Park1
1Center for Quantum Materials and Superconductivity (CQMS) and Department of Physics,
Sungkyunkwan University, Suwon 16419, Republic of Korea
2Department of Physics, University of Oslo, P.O. Box 1048 Blindern, 0316 Oslo, Norway
E-mal: [email protected]
Fax: +82 31 290 7056
Abstract
We investigate the effects of magnetic impurities on the upper critical field (μ0Hc2) in La-doped
CaFe2As2 (LaCa122) single crystals. The magnetic field dependency of the superconducting transition
temperature (Tc) for LaCa122 is rapidly suppressed at low fields up to ~1 kOe despite its large μ0Hc2(0)
value on the order of tens of Tesla, resulting in a large positive curvature of μ0Hc2(T) near Tc. The
magnetization hysteresis (M − H) loop at temperatures above Tc shows a ferromagnetic signal and the
M(H) value rapidly increases with increasing magnetic field up to ~1 kOe. Taken together with the linear
suppression of Tc with the magnetization in the normal state, these results suggest that the large upward
curvature of μ0Hc2(T) near Tc in La-doped CaFe2As2 mainly originates from the suppression of
superconductivity due to the presence of magnetic impurities.
PACS numbers: 74.25.Op, 74.62.Dh, 74.70.Xa, 74.81.-g
keywords: La-doped CaFe2As2, upper critical field, magnetic impurity
1. Introduction
Since the discovery of Fe-based superconductors with a superconducting (SC) transition
temperature (Tc) of 26 K [1], interesting results have continued to be reported, such as high SC
transition temperature in an electron-doped FeSe monolayer (Tc > 100 K) [2] and in rare-earth
(RE) doped CaFe2As2 (Tc ~ 49 K) [3, 4]. Electron-doped CaFe2As2 (Ca122) compounds with RE
elements (RE: La, Ce, Sm, Pr, Nd) as dopants, show the highest Tc values among AFe2As2 (A:
Ca, Sr, Ba, Eu) compounds [5, 6]. The compounds have different Tc - dopant concentration
phase diagrams distinguishing between hole and electron doping, compared to high-Tc cuprates,
where hole doping usually induces a higher Tc than electron doping [7, 8]. The origin of the
higher Tc in electron-doped Ca122 is still under debate because of their large inhomogeneity and
non-bulk superconductivity [9-12].
Understanding the mechanism of the high Tc in Fe-based superconductors is critical to
achieving room temperature superconductivity. Together with the critical current and SC
transition temperature, the upper critical field (μ0Hc2) is one of the most important
superconducting parameters that can provide information on the pairing mechanism [13-14].
The μ0Hc2(T) of RE-doped Ca122 shows a remarkable upward curvature near Tc, which could be
explained by the two-band theory, Ginzburg-Landau phenomenology, and the Werthamer-
Helfand-Hohenberg (WHH) model [14-19]. However, its origin is still contradictory and needs
to be clarified. Despite the large μ0Hc2(T) on the order of tens of Tesla, a fast decrease of Tc at
low fields is difficult to explain [15, 16, 20-23]. It has been reported that there exists a large
inhomogeneity of superconducting phases and filamentary superconductivity in these materials
[9, 10, 12], which in turn could strongly affect the Tc.
Here, we report on the upper critical fields of the La-doped Ca122 single crystals and
discuss a plausible origin of the large suppression of Tc at low fields. Magnetotransport
measurements show a rapid decrease of Tc with magnetic fields up to ~1 kOe, which is
consistent with the ferromagnetic-like magnetization hysteresis (M − H) loops measured at
temperatures above Tc. M(H) shows a strong field dependence up to ~1 kOe and is then
saturated at higher magnetic fields, indicating that the rapid decrease of Tc at low fields is
closely associated with the destruction of superconductivity by ferromagnetic impurities in the
La-doped Ca122 system.
2. Experimental
La-doped Ca122 single crystals were synthesized by using the FeAs self-flux method [20, 22].
First, the binary FeAs precursor was prepared by reacting Fe powder (99.998%, Alfa Aesar)
with As lumps (99.999%, Alfa Aesar). Then, Ca (granules 99.5%, Alfa Aesar), La (rods 99.9%,
Alfa Aesar), and the FeAs precursor were put into an alumina crucible at a ratio of (Ca,
La):FeAs = (0.8, 0.2):4 and sealed in an evacuated quartz tube. Next, the ampoule was heat-
treated at 1,180 °C for 24 h and then slowly cooled to 960 °C at a rate of 4 °C/h. Finally, the
furnace was turned off and cooled down to room temperature naturally. Through this process,
we obtained ~18% La-doped Ca122 (LaCa122) single crystals with plate-like shapes. The
composition ratio of the synthesized LaCa122 crystals was determined by employing energy-
dispersive spectroscopy (EDS).
Two small pieces of LaCa122 single crystals, LaCa122-A and LaCa122-B, were used in this
study with sizes of 1.50 0.45 0.045 mm3 and 1.17 0.46 0.074 mm3, respectively. The
superconducting phase transition of LaCa122-A is quite sharp compared to that of LaCa122-B,
and LaCa122-A shows a clear two-step superconducting transition. The temperature
dependencies of the in-plane electrical resistivity in magnetic fields were measured by using a
standard four-probe technique and the measurements were performed using a physical property
measurement system (PPMS 9T, Quantum Design). Magnetization hysteresis (M − H) loops
were measured by using a magnetic property measurement system (MPMS 5T, Quantum Design).
In order to probe the homogeneity of the crystals, magneto-optical imaging was performed at 4 K
after field cooling for the relatively large-sized La-Ca122 crystals.
3. Results and discussion
Figures 1(a) and 1(b) show the temperature dependencies of the in-plane electrical resistivity
(ρab) and magnetization (M) for the LaCa122-A and LaCa122-B crystals, respectively.
LaCa122-A sample reveals a shaper SC transition than LaCa122-B in the ρab(T), as presented in
figure 1(a), where ρab(T) is normalized by its value at 46 K for comparison for each sample. The
SC transition widths (ΔTc) for LaCa122-A and -B are 5.0 and 9.3 K, respectively, where the
width was determined from a resistivity decrease from 90 to 10% of the normal state value at Tc.
When plotted on a semi-logarithmic scale, as shown in the inset in figure 1(a), the two-step SC
transition is clearly observed in LaCa122-A, which is commonly seen in RE-doped Ca122
superconductors [9-12, 20, 24].
Difference is also observed in the Meissner effect for LaCa122-A and -B samples as shown
by the temperature dependencies of magnetization (M) in figure 1(b). The stronger temperature
dependency of the zero-field cooled (ZFC) M values for LaCa122-B indicates more rapid
suppression of the SC volume with increasing temperature compared to LaCa122-A. An
increase of the field cooled (FC) M with decreasing temperature and the positive magnetization
values at low temperatures imply that LaCa122-B contains ferromagnetic-like impurities [25,
26].
The temperature dependencies of the in-plane resistivity (ρab) of LaCa122-A and -B in
different magnetic fields are shown in figures 2(a) and (c), respectively, where the magnetic
fields were field was applied perpendicular to the ab plane. The SC transition for both samples
becomes much broader even in a small magnetic field of 100 Oe. This rapid suppression of
superconductivity by small fields is observed up to 0.1 T and then, the SC suppression rate is
reduced as the magnetic field increases towards 9 T. Figures 2(b) and (d) present the field
dependencies of ρab(T) on a semi-logarithmic scale, revealing a long tail with another SC
transition for both LaCa122-A and -B. The two-step SC phase transitions can be attributed to the
inhomogeneously distributed high-Tc phases that are surrounded by the low-Tc or non-SC
phases [9-12].
Figures 3(a) and 3(b) show the upper critical fields (μ0Hc2) as a function of temperature for
LaCa122-A and B, respectively. Because both samples have a broad SC transition, μ0Hc2(T)
was obtained by using three different criteria of ρ90%, ρ50%, and ρ10% of the normal-state
resistivity value near the Tc for each magnetic field. Significant positive curvature near Tc is
observed for all cases and is linked to the rapid decrease of Tc in low magnetic fields. The two-
band or multiband theory has been broadly used to describe the positive curvature in μ0Hc2(T)
[13, 14, 19, 27]. The Werthamer-Helfand-Hohenberg (WHH) model has been previously
applied to estimate μ0Hc2(0), for which the upward curvature was not taken into account [16, 21-
23]. In this study, the μ0Hc2(T) values for both samples were fitted by using the empirical
formula μ0Hc2(T) = μ0Hc2(0)[1 - (T/Tc)2]n, where the best fits (solid lines) were obtained with
similar n values for both compounds: n(ρ90%) = 2.48 and 2.45, n(ρ50%) = 2.84 and 2.90, and
n(ρ10%) = 3.28 and 3.21 for LaCa122-A and B, respectively. The large n values for the ρ10%
criterion are related to the fast decrease of Tc as the magnetic field increases. High-field
experiments are required for more precise investigation of μ0Hc2(T) for RE-doped Ca122
compounds.
The upper critical field of LaCa122 is plotted against 1−(T/Tc)2 on a logarithmic scale in
figure 4(a), where μ0Hc2 shows a slight deviation from the linear dependence below 1 kOe. As
shown in figure 4(b), the SC transition width defined as the difference between 90% and 10% of
the normal-state resistivity value at Tc, ΔTc = Tc(ρ90%) –Tc( ρ10%), rapidly increases up to ~1 kOe.
Both crystals show similar field dependencies of ΔTc(H) although their ΔTc values at zero field
are very different: 5.0 K and 9.3 K for LaCa122-A and -B, respectively. Figures 4(c) and 4(d)
representatively show the M − H loops at 2 and 50 K for LaCa122-A and -B, respectively. At
50 K, which is higher than Tc, both compounds show ferromagnetic (FM) behavior. The FM
signal for LaCa122-A is relatively small compared to the large SC signal at 2 K. In contrast, the
FM signal for LaCa122-B is comparable to the SC signal at 2 K and strongly distorts measured
magnetization loop, which is a superposition of the FM and SC signals [28-30]. The field-
dependent M value at 50 K for LaCa122-B rapidly increases with magnetic field up to ~1 kOe
and then is almost saturated. This FM-like behavior is probably responsible for the small hump
developed at 1 kOe in the M − H curve at 2 K, as indicated by the arrows [31]. These results
suggest that the significant upward curvature in μ0Hc2(T) near Tc is mainly caused by the FM ic
impurities related to Fe or the undoped Ca122 phase, because ferromagnetic ordering can act as
a strong pair-breaking source in superconductors [10, 32-34].
Support of the importance of magnetic impurities for understanding the unusual behaviour
of upper critical field with temperature is given by figure 5(a). It shows that Tc’s for both
crystals are almost linearly decreases as function of the magnetization value at 50 K. Here we
used M at 50 K because it represents magnetic impurities only. Even though the relative
impurities contribution to the M − H loops for LaCa122-A is much smaller than for LaCa122-B
(see figure 4), the widening of superconducting transition with field is similar for both crystals.
Figure 5(b) shows the SC transition width ΔTc as a function of the normalized magnetization on
a logarithmic scale. The field-induced increase in the transition width ΔW follows a power-law
with the same exponent α = 0.520.05 for both crystals, ΔW = ΔTc(H) − ΔTc(0) ∝ Mα. Further
experimental and theoretical study is necessary to properly understand if the power-law
behavior is accidental or reflects the nature of the competition between superconductivity and
magnetism of impurities.
Magneto-optical imaging (MOI) was performed to visualize magnetism of the LaCa122
crystals. Figures 6(a) and (c) show optical images for both faces of the LaCa122 crystal and (b)
and (d) show MOI images of the crystal in the superconducting state, respectively. The latter are
remnant-state MOI images at 4 K after a field cooling procedure, and the brightness of in the
image represents the local density of trapped by superconductor flux. The images demonstrate
that the crystals are not uniform. The distinct nearly rectangular dark area in the right part of the
MO images shows a region, in which flux trapping is very weak. Note that the MO image
presented in figure 6(d), which is the image taken from the other side of the crystal shown in
figure 6(b), has the same dark region resulting likely from magnetic impurities. Apparently, this
particular region is weakly or non-superconducting throughout the entire sample thickness.
These MOI results are consistent with earlier reports in which RE-doped Ca122
superconductors were inhomogeneous and even that the high Tc could not be of bulk origin [9-
11, 35]. Our MOI study confirms bulk origin of superconductivity. Moreover, areas of
different contrast could be identified as having magnetic impurities. The similar weak contrast
is present at elevated temperatures, where superconductivity is suppressed (not shown). This is
in agreement with the role of magnetic impurities revealed by the M − H results.
4. Conclusions
In conclusion, we studied the upper critical field of La-doped Ca122 single crystals, in
which a significant positive curvature in μ0Hc2(T) is observed near Tc. The regime (μ0H 1 kOe),
where superconducting transition is strongly influenced by magnetic field, corresponds to that in
the magnetization in the normal state, where the M − H loops show ferromagnetic-like behavior
and M is almost saturated for μ0H ≥ 1 kOe. The observation of the linear relationship between
characteristic temperatures of superconducting transition and the normal-state magnetization
emphasizes that the fast increase of the width of superconducting transition at small magnetic
fields, which is typically ascribed to multiband effects in other Fe-based superconductors, may
originate from the magnetic impurities that suppress the Cooper electron pairing in the high-Tc
phase of the La-doped Ca122 superconductors. The results of magneto-optical study are in
agreement with these conclusions.
Acknowledgements
This work was supported by the National Research Foundation (NRF) of Korea by a grant
funded by the Korean Ministry of Science, ICT and Planning (No. 2012R1A3A2048816). S.-G.
Jung was also supported by the Basic Science Research Program through the National Research
Foundation of Korea (NRF) funded by the Ministry of Education (NRF-
2015R1D1A1A01060382).
Figure Captions
Figure 1. (a) Temperature dependence of the in-plane resistivity (ρab) of LaCa122-A (black) and
B (red), where ρab(T) is normalized by the resistivity value at 46 K for comparison. The semi-
logarithmic plot of (a) presented in the inset shows broad and clearly two-step SC transitions in
LaCa122-B. (b) Zero-field cooled (ZFC) and field cooled (FC) dc magnetization (M) at 2 Oe for
LaCa122-A and -B, where M(T) curves are normalized by the ZFC magnetization value at 2 K.
0 10 20 30 40 50
-0.9
-0.6
-0.3
0.0
0 10 20 30 40 500.0
0.2
0.4
0.6
0.8
1.0
FC
ZFC
M(T
)/M
(2 K
)
T (K)
LaCa122-A
LaCa122-B
2 Oe
LaCa122-A
LaCa122-B
(b)
ab(T
)/
ab(4
6 K
)
T (K)
(a)
0 10 20 30 40 50
1E-3
0.01
0.1
1
ab(T
)/
ab(4
6 K
)
T (K)
Figure 2. Temperature dependence of the in-plane resistivity (ρab) of LaCa122-A ((a) and (b))
and LaCa122-B ((c) and (d)) at different magnetic fields. The resistivitiy is plotted in (a) and (c)
on a linear scale and in (b) and (d) on a semi-logarithmic scale. Even though the upper critical
fields are large in both crystals, the SC transition is strongly suppressed by relatively low
magnetic field on the order of 0.1 T.
0.1
1
10
100
0 10 20 30 40 50
0.1
1
10
100
ab (c
m)
9 T
0 T
9 T
0 T
0 T
0.01 T
0.05 T
0.1 T
0.2 T
0.5 T
1 T
3 T
5 T
7 T
9 T
0 T
0.01 T
0.05 T
0.1 T
0.2 T
0.5 T
1 T
3 T
5 T
7 T
9 T
(c) LaCa122-B
(a) LaCa122-A
0 T
T (K)
9 T
9 T
(d) LaCa122-B
(b) LaCa122-A
ab (c
m)
0 T
0
20
40
60
80
ab (c
m)
0 10 20 30 40 500
60
120
180
ab (c
m)
T (K)
Figure 3. Temperature dependencies of the upper critical field (μ0Hc2) for (a) LaCa122-A and (b)
LaCa122-B. The upper critical field μ0Hc2(T) values were obtained using three different criteria
of resistivity: ρ90%, ρ50%, and ρ10%, which correspond to 90, 50, and 10% of the normal-state
resistivity value near Tc, respectively. Irrespective of the criteria, both crystals show a large
upward curvature in Hc2(T) near Tc. The solid lines are plotted based on the phenomenological
relationship of μ0Hc2(T) [1 − (T/Tc)2]n.
0 10 20 30 400
5
10
15
20
0
5
10
15
20
90%
50%
10%
0H
c2 (
T)
T (K)
(b)
LaCa122-B
LaCa122-A
90%
50%
10%
0H
c2 (
T)
(a)
Figure 4. (a) The upper critical field, μ0Hc2(T), of LaCa122-A (open circles) and -B (solid circles)
plotted as a function of 1−(T/Tc)2 on a logarithmic scale. (b) The SC transition width (ΔTc(H) −
ΔTc(0)) is shown as a function of the magnetic field, where the width rapidly increases at low
magnetic fields up to ~1 kOe. Here, ΔTc(H) = ρ90%(H) − ρ10%(H). The M − H loops for
LaCa122-A and -B are shown in (c) and (d), respectively. Ferromagnetic-like behavior for both
samples is observed in the M − H curves at 50 K, which is more clear for LaCa122-B.
0.01 0.1 1
0.01
0.1
1
10
0 2 4 60
2
4
6
8
-15 -10 -5 0 5 10 15
-2
-1
0
1
2
-15 -10 -5 0 5 10 15
-1.0
-0.5
0.0
0.5
1.0
A B
90%
50%
10%
0H
c2 (
T)
1-(T/Tc)
2
LaCa122-A
LaCa122-B
T
c(H
) -
Tc(0
) (K
)
0H (T)
2 K
50 K
M (10
-4 e
.m.u
.)
0H (kOe)
1 kOe
2 K
50 K
(d) LaCa122-B(c) LaCa122-A
(b) (a) LaCa122
M (10
-4 e
.m.u
.)
0H (kOe)
1 kOe
Figure 5. Relationship between width of superconducting transition and magnetization (M) of
the sample in normal state. (a) The decrease of characteristic temperature at which resistance is
50% of its value at Tc with corresponding magnetization value at 50 K. The open and solid
circles are for LaCa122-A and -B, respectively. The magnetization value is normalized by its
value at 5 kOe, M(H)/M(5kOe). Dashed lines show linear fits to the points. (b) The SC
transition width ΔW as a function of normalized magnetization at 50 K plotted in double
logarithmic scale. Here ΔW = ΔTc(H) − ΔTc(0). ΔW(M) follows a power-law with the same
exponent of 0.52 for both compounds, i.e., ΔW∝M0.520.05. Solid lines are results from the
power-law fits.
Figure 6. Optical ((a) and (c)) and magneto-optical ((b) and (d)) images of LaCa122 crystals.
The magneto-optical (MO) image in (b) corresponds to the optical image in (a), while the MO
image in (d) corresponds to the optical image in (c). The MO images were obtained at 4 K after
field cooling and the degree of brightness represents the local density of flux trapped in
superconductor, indicating that the crystal is inhomogeneous to some extent.
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