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RAPID COMMUNICATIONS

PHYSICAL REVIEW B 78, 220505R 2008

Determination of anisotropic Hc2 up to 60 T in Ba0.55K0.45Fe2As2 single crystals

M. M. Altarawneh, K. Collar, and C. H. Mielke


MPA-NHMFL, Los Alamos National Laboratory, Los Alamos, New Mexico 87545, USA

N. Ni, S. L. Budko, and P. C. Canfield


Department of Physics and Astronomy, Ames Laboratory US DOE, Iowa State University, Ames, Iowa 50011, USA
Received 28 July 2008; revised manuscript received 22 September 2008; published 16 December 2008
The radio frequency penetration depth was measured in the superconductor Ba0.55K0.45Fe2As2 under
pulsed magnetic fields extending to 60 T and down to 14 K. Using these data we are able to infer a Hc2T, H-T
phase diagram, for applied fields parallel and perpendicular to the crystallographic c axis. The upper critical-
field curvature is different for the respective orientations, but they each remains positive down to 14 K. The
upper critical-field anisotropy is moderate, 3.5 close to Tc, and drops with the decrease in temperature,
reaching 1.2 at 14 K. These data and analysis indicate that i Ba0.55K0.45Fe2As2 anisotropy diminishes with
temperature and has an unusual temperature dependence and ii Hc2T = 0 for this compound may easily
approach fields of 75 T.

DOI: 10.1103/PhysRevB.78.220505 PACS numbers: 74.70.Dd, 74.25.Dw, 74.25.Op, 74.25.Fy

c
The discovery of relatively high-temperature supercon- trapolation of the Hc2c T and Hc2 T curves to lower tem-
ductivity in several families of FeAs-based compounds1,2 has perature indicates that values between 75 and 80 T are
raised hope in both basic and applied physics circles. likely in this material.
Whereas these materials present intriguing questions about Single crystals of Ba0.55K0.45Fe2As2 were grown in pre-
mechanism, lying as they do near a confluence of structural cisely the manner described in Ref. 8. For these crystals the
and magnetic phase transitions,14 they also hold out the potassium content was directly measured by wavelength dis-
promise of not only high Tc values but also apparently ex- persive x-ray spectroscopy and was found to have an average
tremely high Hc2 values as well. RFeAsO1xFx compounds value of 0.45 with a 0.07 standard deviation from layer to
have been shown to have Hc2T curves that can be reason- layer.8
ably extrapolated to low-temperature Hc20 values in excess Radio frequency rf contactless penetration depth mea-
of 100 T.5,6 Although in some cases anisotropic Hc2 data can surements were performed on the single-crystal sample in a
be inferred from magnetization measurements on polycrys- 60 T pulsed field magnet with a 10 ms rise time and a 40 ms
talline samples,7 to date, the lack of sizable single crystalline extended decay. The rf technique was used as it has proven
RFeAsO samples has prevented thorough determinations of to be a sensitive typically 1 part per 1000 resolution and
anisotropic Hc2T curves over extended field ranges. accurate method for determining the upper critical field in
Fortunately, methods for growing single crystals of super- anisotropic superconductors.9 A radio frequency probe based
conducting Ba1xKxFe2As2,8 and subsequently the Sr and on a commercially available integrated circuit IC proximity
Ca analogs, were readily developed based on the fact that the detector was used to establish a high stability tank circuit
AFe2As2 compounds are true intermetallics and are amenable oscillator. The IC delivers a voltage proportional to the tank
to conventional metallic solution growth techniques. The circuit voltage. The fundamental resonant frequency is ap-
availability of large single crystals allows for the determina- proximately 28 MHz at Tc. The technique is highly sensitive
tion of anisotropic Hc2T data. Initial anisotropic magnetore- to small changes 1 5 nm in the rf penetration depth9
sistivity data collected on Ba0.55K0.45Fe2As2 show that when the sample is in the superconducting state. As the mag-
there is a very minor suppression of Tc even for 14 T.8 Ex- netic field increases, the probe detects the transition to the
trapolations of Hc2T plots inferred from these data to T normal state by tracking the shift in resonant frequency pro-
= 0 K suggest that Hc2T for this discovered superconductor portional to the penetration depth, i.e., = fR2 / f 0rs, where
may easily exceed 70 T, and interpolation of the data indi- R is the detection coil radii, rs is the sample radii, f 0 is the
cates that the upper critical-field anisotropy parameter, fundamental frequency, and f is the frequency shift9. The
c
= Hc2 / Hc2c , is approximately 3.5 close to Tc. Higher-field IC voltage is mixed with an intermediate frequency IF, and
data are clearly required in both cases to improve our under- the difference frequency is extracted by using a low-pass
standing and to place the extrapolation of Hc2T on firmer filter at 1.9 MHz. This simple rf technique allows for the
footing. frequency shift to be recorded with a digitizing oscilloscope
In this Rapid Communication we present anisotropic at a rate of 80 ns/point 12.5 MHz for a duration of 100 ms
high-frequency susceptibility measurements on single crys- 1.25 Msamples/channel. A simple peak-finding algorithm
tals of Ba0.55K0.45Fe2As2 grown in the same manner as runs on the raw data to calculate the frequency shift as a
those used to collect the initial H 14 T data.8 We are able function of time. The time-dependent frequency is then cor-
to extend Hc2T curves to significantly higher magnetic related with the applied magnetic field yielding a frequency
fields and lower temperatures. As a result we find that i vs magnetic-field plot see Figs. 1 and 2.
varies in a continuous manner from a relative maximum of A small 0.55 0.55 0.014 mm3 single crystal was
3.5 near Tc to a value of 1.16 near 14 K and ii the ex- chosen as larger 1 mm cross-section samples tend to ex-

1098-0121/2008/7822/2205053 220505-1 2008 The American Physical Society


RAPID COMMUNICATIONS

ALTARAWNEH et al. PHYSICAL REVIEW B 78, 220505R 2008

2.0 80
Sensing Coils
0H c 0H c
1.9
Applied Field 10.0K
c 12.0K
14.0K
0H || c
16.0K 60
1.8 17.0K
Sample
18.0K
19.0K
Frequency Shift (MHz)

20.0K
1.7 21.0K
22.0K

Hc2 (T)
2.0
10K 23.0K 40
3

Frequency Shift(MHz)
24.0K

(Hc2 c / H
25.0K (From Hc2 )
1.6
26.0K Zero Field Cooling Curve
27.5K 1.8

27.0K
28.0K 2
1.5

c2||c
28.5K 20

)
29.0K 1.6
29.5K
30.0K
1.4 31.0K
32K 31.5K 5 10 15 20 25 30 35

32.0K Temperature (K)


0
1.3 0 5 10 15 20 25 30
0 10 20 30 40 50 60 70
Magnetic Field (T) Temperature (K)

FIG. 1. Color online Frequency shift as a function of magnetic FIG. 3. Color online Anisotropic Hc2T for

field applied perpendicular to the crystallographic c axis at different Ba0.55K0.45Fe2As2 single crystals. Circles indicate the Hc2c and
temperatures from 10 to 32 K. The arrow indicates the approximate squares Hc c2 . Inset: the rf zero-field cooling curve for
Hc2 point for the 24 K field pulse and the linear guides used for Ba0.55K0.45Fe2As2 single crystals on the left axis and temperature-
dependent anisotropy of Hc2 : = Hc
c
determination of the point. Inset: the schematic diagram of the rf c2 / Hc2 as determined from the
sensing coil and sample for the 0H c configuration. fits to the Hc2 data on the right axis.

placed in a circular detection coil 0.8 mm in diameter.


hibit signs of heating due to eddy currents induced in the
The sample and probe were cooled down to liquid-helium
sample, caused by the pulsed field. Our results show no hys-
temperatures inside of a double-walled nonmetallic cryostat
teresis hence no measurable heating during the pulse, indi-
with 500 Torr of helium exchange gas. The onset of the
cating a good thermal anchor was established with the bath.
superconducting transition is clearly observed as a resonant
To determine the upper critical-field anisotropy the single
frequency shift near 32 K in zero applied magnetic field
crystal was measured in two orthogonal sample orientations:
shown in the inset of Fig. 3. In the second orientation H
with the applied field parallel to the conducting planes per-
parallel to the c axis Fig. 2 a flux-compensated figure
pendicular to the crystallographic c axis see inset of Fig. 1
eight detection coil set 0.7 mm diameter each was placed
and with the applied field normal to the conducting planes
with its symmetry axis parallel to the applied magnetic field.
parallel to the crystallographic c axis see inset of Fig. 2.
The compensated nature of the detection coil was necessary
Alignment accuracy was within approximately 2. For ap-
to minimize induced voltages feeding back into the rf IC.
plied field perpendicular to the c axis Fig. 1 the sample was
The sample was placed on the top surface of one side of the
counterwound coil pair. This configuration has weaker cou-
Figure of Eight Sensing Coils pling to the sample 50%, resulting in a smaller but still
easily resolvable frequency shift. The temperature was stabi-
0H || c
1.41
14K
lized with a conventional proportional-integral-derivative
Applied Field b 15K PID temperature controller with an accuracy of 0.1 K.
a 16K
17K The criterion for determining the point at which the Hc2
Frequency Shift (MHz)

Sample 18K
1.40 19K transition occurs requires consistency, and no one method is
31K 20K
21K
entirely unambiguous. However, the rf penetration depth
22K
23K
technique has demonstrated a high degree of agreement with
1.39
24K accepted thermodynamic methods9 and as a contactless
25K
26K method avoids problems with contact lead problems that can
27K
28K be detrimental to transport measurements in pulsed magnetic
29K
1.38
14K 30K fields. In addition the rf technique has the advantage of being
31K more sensitive with several-orders-of-magnitude faster time
response, hence making it suitable for millisecond duration
pulsed magnetic fields when compared to specific heat, for
0 20 40 60
Magnetic Field (T)
example. Our method, for determining a consistent Hc2
point in the f vs 0H data shown in Figs. 1 and 2, is based
FIG. 2. Color online Frequency shift as a function of magnetic on identifying the point at which the slope of the rf signal in
field applied along the crystallographic c axis at different tempera- the transition region intercepts the slope of the normal-state
tures from 14 to 31 K. Inset: the schematic diagram of the rf sensing background. The justification is simply that the high-field
coil and sample for the 0H c configuration. data above Hc2 show a smooth close-to-linear magnetic-

220505-2
RAPID COMMUNICATIONS

DETERMINATION OF ANISOTROPIC Hc2 UP TO 60 PHYSICAL REVIEW B 78, 220505R 2008

field dependence. In this region the rf probe is sensitive to To summarize, we have measured the anisotropic Hc2T
the normal-state magnetoresistance of the sample and detec- curves for Ba0.55K0.45Fe2As2 down to 14 K and up to 60 T.
tion coil. Below Hc2 the suppression of the superconducting We find i a nonlinear temperature dependence of the Hc2
state with increasing field leads to a field-dependent fre- anisotropy of Ba0.55K0.45Fe2As2, although there is at
quency shift that results in a clear slope change in the data present no direct evidence for superconducting layer decou-
see Figs. 1 and 2. The Hc2 value is determined for each pling, and ii Hc2T = 0 for this compound may easily ap-
subsequent fixed temperature magnetic-field pulse producing
the H-T plot see Fig. 3. proach fields of 75 T or above. Higher-field measurements
The shapes of the upper critical-field curves for the par- will be required to determine the lower-temperature parts of
allel and perpendicular orientations clearly do not manifest the full temperature dependence of these remarkably large
the same temperature dependence. The anisotropy parameter Hc2T curves. On the other hand, perhaps even further
inset of Fig. 3 varies accordingly. Estimates of the aniso- physical insight will be drawn from careful studies of the
tropic coherence length at 14 K, based solely on the vortex angular dependence of Hc2T for fields below 50 T. Rota-
flux density argument, yield c0 34 in-plane and tions from H c to H 100 and H 110, as well as in-plane
c0 29 interlayer since c = 0 / 2Hc2 c
and c rotations studies, should reveal a wealth of details about this
c 10
= 0 / 2cHc2 . Decoupling of the superconducting layers modest and temperature-dependent upper critical-field aniso-
would occur when cT becomes less than the c-axis spac- tropy.
ing, c 13 for Ba0.55K0.45Fe2As2.8 To estimate the zero-
temperature coherence length, we note that T is approxi- We would like to thank James Brooks for valuable scien-
mated by Ginzburg-Landau GL theory, i.e., T 0 / 1 tific discussion. Work at the Ames Laboratory was supported
t1/2 where t = T / Tc. From c14 K above, c0 K is by the U.S. Department of Energy, Basic Energy Sciences
about 21.5 . Hence although the critical-field anisotropy under Contract No. DE-AC02-07CH11358. M.M.A was sup-
appears to decrease at lower temperatures, there is no simple ported in part by NSF under Contract No. DMR 0602859
argument based on estimates of the temperature-dependent
through the research grant of James Brooks of Florida State
coherence lengths to support a dimensional crossover in the
temperature range of this experiment. Increased magnetic- University. K.C. was supported in part by the NNSA/DOE
field intensities exceeding 75 T will be required to fully map research under Grant No. DE-FG52-06NA26193 of Stan
out the lower-temperature critical-field phase diagram. Tozer of Florida State University. Work at National High
The anisotropy of Hc2 in Ba0.55K0.45Fe2As2 is also re- Magnetic Field Laboratory-Pulsed Field Facility, Los Ala-
ported in Ref. 11 by measurement of the electrical resistivity mos National Laboratory was supported by NSF Division of
of samples from a different origin. The work presented here Materials Research through Contract No. DMR-0654118, the
differs from Ref. 11 in that a double hump appears in the U.S. Department of Energy, and the State of Florida. Ad-
cooling data in Ref. 11. This artifact may be due to multiple vances in contactless penetration depth technology are cred-
crystalline phases or a doping inconsistency. Our crystals ited to Los Alamos National Laboratory Contract No.
manifest a single and continuous superconducting transition LDRD-DR20070013. Los Alamos National Laboratory is
shown in the inset of Fig. 3. operated by LANS LLC.

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