Physica C 369 (2002) 232–235 www.elsevier.com/locate/physc Temperature, field and current dependence of the flux creep activation energy in bulk MgB2 D. Botta a, A. Chiodoni a, R. Gerbaldo a, G. Giunchi b, G. Ghigo a, L. Gozzelino a, F. Laviano a, B. Minetti a, E. Mezzetti a,* a INFM––U.d.R Torino-Politecnico; INFN––Sez. Torino; Politecnico di Torino, c.so Duca degli Abruzzi 24, 10129 Torino, Italy b Edison S.p.A., Foro Buonaparte 31, 20121 Milan, Italy Abstract In this paper we investigate the behavior of the flux creep activation energy as a function of T, B and J in the temperature range from 4 K up to Tc . The experimental methodology is mainly based on ac susceptibility measurements at different frequencies and applied field, though some dc measurements are referred to along the discussion. A new analysis method is employed in the framework of the flux creep theory to explore the full range of temperature. It turns out that the key energy scale U0 ðT ; BÞ at any external field exhibits a peak. The main outcome of the study is that the peak values are laying along the dc irreversibility line (IL) curve, while the points where U0 ¼ 0 match the ac IL. Then these two curves divide the phase diagram in three reference regions to be investigated in details. Ó 2001 Elsevier Science B.V. All rights reserved. Keywords: Flux creep activation energy; Flux pinning; Flux-line lattice dynamics; Magnesium diboride The recent discovery of the superconductor MgB2 [1] has aroused great interest and intensive studies have been carried out on this material, as prepared in different laboratories [2]. One of the main issues concerning MgB2 is the determination of its flux-pinning properties, because the motion of the vortices (flux creep) over the pinning barriers induces dissipation and sets the limiting critical current density Jc . The interest is driven by the need to understand the basic pinning mechanisms, * Corresponding author. Address: Department of Physics, Politecnico di Torino, c.so Duca degli Abruzzi 24, 10129 Torino, Italy. Tel.: +39-011-564-7314/7349; fax: +39-011-5647399. E-mail address: mezzetti@polito.it (E. Mezzetti). as well as by the practical requirement to enhance Jc [3,4]. In this paper we investigate the flux creep activation energy and its dependence on temperature, field and current density. Aiming at obtaining the most general information about the pinning properties of our samples, we present a new analysis of the pinning energy in the whole temperature range, from 4.2 K up to the critical temperature. The main results reported in the paper are based on ac susceptibility measurements at different frequencies and dc magnetic fields. High density MgB2 bulk pellets were prepared starting from the elemental compounds B (99.5% of purity) and Mg (99.9% of purity), after their reaction in a sealed stainless steel container, lined with a Nb foil. The thermal treatment was 0921-4534/01/$ - see front matter Ó 2001 Elsevier Science B.V. All rights reserved. PII: S 0 9 2 1 - 4 5 3 4 ( 0 1 ) 0 1 2 4 8 - 5 D. Botta et al. / Physica C 369 (2002) 232–235 Fig. 1. SEM of the MgB2 pellet. In the inset a magneto-optical image is reported (l0 Hext ¼ 89 mT; T ¼ 35 K): bright regions indicate presence of magnetic field, while dark regions indicate shielded zones. Black lines mark the sample edge. performed for 2 h in the range of 850–950 °C. The superconducting transition temperature is Tc ¼ 38:9 K, with DTc ¼ 0:3 K [5]. The apparent absence of magnetic granularity up to temperatures very close to Tc was checked by means of a magneto-optical analysis (inset of Fig. 1): despite the polycrystalline nature of the material, clearly visible in the scanning electron microscopy (SEM) picture reported in Fig. 1, the flux enters the sample in a single crystal like fashion, with a Bean profile [5]. The ac susceptibility measurements have been performed on a disk-shaped sample (diameter ¼ 2:93 mm; thickness ¼ 0:34 mm) with l0 Hac ¼ 0:13 mT, at different frequencies (2, 10, 110, 1000, 5000 and 10 000 Hz) and dc magnetic fields (0, 0.125, 0.25, 0.5 and 1 T). Fig. 2 shows the characteristic effects of the dc external magnetic field l0 Hext on the ac susceptibility: as l0 Hext is increased, the transition broadens and shifts towards lower temperatures. The real part of the first harmonic susceptibility were analysed in the framework of the Clem and Sanchez model for the case of a thin sample in a transverse field [6,7] in order to obtain the critical current density in the whole (T ; B; m) range. Fig. 3 shows the critical current density as a function of temperature, at l0 Hext ¼ 0:5 T and for different values of the frequency. Irreversibility lines (ILs) have been determined by both ac and dc methods, by means of the onset 233 Fig. 2. Ac susceptibility as a function of temperature, at different values of the external magnetic field. of the third harmonic component of the susceptibility and from the closing up of the hysteresis cycles, respectively. Critical current values are analysed in the framework of a thermally activated flux creep model: flux lines jump to neighbouring states over the energy barrier U via thermal activation. The mean relaxation time is given by the Arrhenius law: s ¼ s0 expðU =kT Þ ð1Þ where s0 is the relaxation time scale. In the framework of the collective creep model one can assume the very general relation [8]: l 1 Jc U ðT ; B; J Þ ¼ U0 ðT ; BÞ 1 ð2Þ l J where U0 is a characteristic energy scale, Jc is the critical current density in the absence of thermally activated creep processes and the exponent l is a characteristic of the particular flux dynamics. Eq. (2) becomes U ðJ Þ ¼ U0 lnðJc =J Þ as l ! 0. The experimental critical currents (Fig. 3) exhibit a noticeable dependence on the frequency. This characteristic can be considered the signature of creep effects that can be introduced into a critical state model by considering a frequencydependent ‘‘critical current’’ Jc ðT ; B; mÞ [9]: kT m0 ln Jc ðT ; B; mÞ Jc ðT ; BÞg U0 ðT ; BÞ m 234 D. Botta et al. / Physica C 369 (2002) 232–235 Fig. 3. Critical current density as a function of temperature, at l0 Hext ¼ 0:5 T and for different values of the frequency. where the function gðxÞ reflects the relaxation of the flux profile during the time 1=m. This expression incorporates Eq. (1), with s ! 1=m and s0 ! 1=m0 . By assuming Eq. (2), it becomes 1=l lkT m0 ln Jc ðT ; B; mÞ ¼ Jc ðT ; BÞ 1 þ ð3Þ U0 ðT ; BÞ m Jc ðT ; BÞ Jc ðT ; B; m ¼ m0 Þ represents the critical current density in absence of flux creep, while J Jc ðT ; B; mÞ can be interpreted as the effective critical current density when thermally activated processes are present. Eq. (3) could be used to determine U0 and l, if the value of m0 is known. However, in order to minimize numerical instabilities, we adopted the following equivalent approach. At any fixed value of temperature and external field we independently determine from the experimental data the ratio Jcexp ðT ; B; mÞ J Jcexp ðT ; B; m0 Þ Jc and the value of the activation energy U ðT ; B; J Þ ¼ kT ln s m0 ¼ kT ln s0 m as deduced from Eq. (1). To obtain general information about the pinning properties of our samples, we did not assume any a priori functional dependence of the pinning energy on temperature and field. At any given value of T and B, we fit the data U vs. J =Jc by means of Eq. (2), with U0 and l Fig. 4. Typical U vs. J =Jc fit of experimental data by means of Eq. (2) (see text) at fixed value of the external magnetic field (l0 H ¼ 0:25 T) and temperature (T ¼ 25 K). as fitting parameters (a typical example is reported in Fig. 4). We assumed m0 ¼ 10 kHz, as driven from a detailed v00 -peak analysis on the same sample, reported in a recent paper [4]. It turns out that the value of m0 is significantly lower than that usually reported for HTSs [9]. As already pointed out above, the main result of this approach is the determination of the activation energy U in the whole temperature range, at different values of the external magnetic field. The main feature of the energy scale parameter U0 ðT ; BÞ is the presence of a sharp peak, dividing the temperature range into two distinct regions (Fig. 5). It turns out that the peak position exactly corresponds, in a temperature–field phase diagram, to the IL, determined in the same sample by a dc method, i.e. by the closing-up point of the hysteresis cycles (Fig. 6). The exponent l maintains a nearly constant value (in the range from 1.4 to 2.2), up to temperatures close to the U0 peak. Above this temperature it drops to very low values, resulting in a logarithmic dependence of the energy activation on the current. In the high temperature region (above the peak) the present analysis is in good agreement with the results we reported in Ref. [4], obtained by a different approach based on the v00 -peak analy2 a sis, where we assumed U ¼ U 0 ½1 ðT =Tx Þ . Here a and Tx are field-dependent parameters. Tx repre- D. Botta et al. / Physica C 369 (2002) 232–235 Fig. 5. Activation energy scale U0 , determined as a fit parameter (see Fig. 4) by the procedure described in the text, as a function of temperature for different values of the external magnetic field. Dotted lines represent the extrapolation used to determine the temperature where U0 ¼ 0. 235 the power-law decrease of the pinning energy U0 with temperature, notwithstanding the different analysis method. In the low-temperature region (below the peak), the U0 curves at a fixed external field are increasing functions of temperature (it is worthwhile to remind that along these curves the internal field, i.e. the average number of vortices, is not constant). This result takes one back to U ðT Þ dependences obtained for YBCO in Ref. [10]. Some insight into the vortex matter behavior in correspondence of the two regimes, below and above the U0 peak, are provided by the comparison between the features observed in the U0 ðT ; BÞ curves and the ILs, as evaluated by ac and dc methods (Fig. 6). In particular, as already pointed out, the points of the U0 peaks exactly match the dc IL, while the points where U0 ðT Þ ¼ 0 match the ac IL. Therefore the results point toward the presence of three main regions in the vortex–phase diagram, all of them in a context of relatively weak pinning: the first one (I) is characterized by a pinning energy increasing with T up to the dc IL, the second one (II) by a pinning energy collapsing toward zero at the ac IL, the third one (III) corresponding to a reversible region with unpinned vortices. References Fig. 6. Vortex–phase diagram determined by the comparison among different independent analysis: onset of the third harmonic susceptibility (IL ac), hysteresis cycles (IL dc), U0 ðT ; BÞ features (see Fig. 5). Dotted lines are guides for eye. sents the temperature at which U ¼ 0. In the framework of the present analysis, if we extrapolate the U0 ðT Þ curves, it results that the T ðU0 ¼ 0Þ points are fully consistent with previous Tx values. It is important to emphasize that the Tx values of the present and of the previous analysis exactly match the IL, as determined by ac methods [4] on the same sample are shown (Fig. 6). A qualitative agreement is also found with the results reported by Qin et al. [3] for what concerns [1] J. Nagamatsu, N. Nakagawa, T. Muranaka, Y. Zenitali, J. Akimitsu, Nature 410 (2001) 63. [2] C. Buzea, T. Yamashita, Supercond. Sci. Technol. 14 (2001) R115. [3] M.J. Qin, X.L. Wang, H.K. Liu, S.X. Dou, Phys. Rev. B 64 (2001) 060505. [4] G. Ghigo, D. Botta, A. Chiodoni, R. 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