Physica C 433 (2006) 225233 www.elsevier.

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Experimental evidence for a dimensional crossover of the vortex ensemble in BSCCO (Bi1.8Pb0.4Sr1.8Ba0.2Ca2Cu3Ox) by multi-harmonic ac susceptibility measurements
V. Mihalache
a

a,*

, S. Popa a, D. Di Gioacchino b, P. Tripodi

b,c

, J.D. Vinko

National Institute of Materials Physics, Atomistilor 105 bis, Judet Ilfov, P.O. Box MG 7, 077125 Magurele, Romania b INFN-LNF, Via E. Fermi 40, 00044 Frascati, Italy c H.E.R.A., Corso della Repubblica 448, 00049 Velletri, Italy Received 11 October 2005; accepted 9 November 2005

Abstract We have studied a portion of HT phase diagram of the anisotropic Bi2223 bulk system using multi-harmonic ac susceptibility measurements (vn). Based on the behavior of the third harmonic modulus, jv3j, the irreversibility line (IL) was obtained from the onset of jv3j and an anomalous peak eect (PE) was observed. It has been shown that the anomalous peak is due to the crossover between a three-dimensional (3D) and a quasi-two dimensional (quasi2D) peculiarity of vortex dynamics, the crossover magnetic eld being Hcr % 0.1 T. The obtained portion of Birr(T) is well described by the melting line of the ux lattice. The 3D ux uctuation part (low eld and high temperature) is described by the nearly parabolic temperature dependence B = B0(Tc/T 1)n with n = 1.58 (sample 1) and n = 1.48 (sample 2). The other region (high eld and low temperature) is well described by the temperature dependence of the quasi-2D ux uctuations, T m H T 2D 1 b=ln B=Bcr 1=m corresponding to the weak interaction between panm cake vortices from adjacent planes. The 2D limit temperature was determined as T 2D 36:7 K (sample 1) and m T 2D 27:3 K (sample 2). m 2005 Elsevier B.V. All rights reserved.
PACS: 74.25.Dw; 74.25.Ha; 74.25.Nf; 74.72.Hs Keywords: Bi-based cuprates; Magnetic properties; Superconductivity phase diagrams

Corresponding author. Tel.: +40 21 4930047x193/+40 0745460105; fax: +40 21 4930267. E-mail address: vmihal@inm.ro (V. Mihalache).

0921-4534/$ - see front matter 2005 Elsevier B.V. All rights reserved. doi:10.1016/j.physc.2005.11.005

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1. Introduction The magnetic phase diagram of high-temperature superconductors (HTSC) exhibits an extraordinarily rich variety of phases [1]. Still controversial is the presence of a boundary, called the irreversibility line (IL), which separates a magnetically irreversible state, with a non-linear dissipative behavior, from a reversible region with a linear dissipative property. Some of the suggestions are based on a vortex glass formation [2] or on a ux lattice melting [3]. More recent studies investigating the irreversibility line have conrmed the presence of a predicted crossover characteristic value Hcr [4,5] in the dimensionality of the vortex uctuations [6,7]. The dimensional crossover 3D/2D has been observed experimentally in various HTSC systems including Tl2Ba2Cu3O10 (Tl2223) lms [8], YBa2Cu3O7+d thin lms [9], Bi2Sr2CaCu2O8 (Bi-2212) single crystals and Bi2Sr2CaCu2O8+d thin lms [6]. In layered superconductors [4,6] the increase of the magnetic eld causes a decoupling between the pancake-like vortices in adjacent CuO2 planes (3D to quasi-2D vortex lattice transition). Recently, numerical analysis conrmed a transition from ordered straight vortices to disordered decoupled vortices in layered superconducting material [10]. This transition has also been used to explain the presence of the second peak in the magnetization cycles [1012]. In fact the increase of the magnetic eld was accompanied by a sharp increase of the critical current density Jc (or a sharp increase of the pinning force) for a little span of the magnetic eld. The increase of Jc is due to the decoupling of the 2D pancake vortices that can easily adjust their positions on the defects, such as the dislocation networks [12], in the CuO2 planes. Hence there is a maximum in pinning [10], with respect to the previous weakly pinned 3D vortex line. In other words, the 3D2D transition lowers the linear dissipation losses and increases the non-linear (irreversible) dynamic processes. In highly anisotropic superconductors, such as BSCCO single crystals, a peak eect in which Jc shows a sharp increase is frequently observed as a function of increasing magnetic eld [1113]. The experimental results on the crossover transition were reported for textured c-axis oriented (Bi, Pb)2223-Ag tapes [7]

and for Bi1.7Pb0.3Sr2Ca2Cu3O [14], by means of magnetic measurements in the vicinity of the irreversibility line and dumping of mechanical oscillations, respectively. In this work, we have investigated the irreversibility line, the crossover transition and the peak eect in bulk Bi2223, using an ac multi-harmonic susceptibility apparatus [15]. This investigation was performed measuring the temperature dependence of the third harmonic susceptibility for different DC magnetic elds. The measurement was performed on bulk samples and evidenced dierent non-linear ux dynamics as well as a marked anomalous peak eect. In fact, a superconductor is characterized by a non-linear IV, so that its magnetization loop is strongly deformed (non-harmonic), comparatively to the elliptical magnetization loop shown by normal conductors with linear IV characteristics. The non-harmonic signal can be analyzed by means of Fourier series containing high-harmonic components. The measurement of higher harmonics, in particular the third harmonics, is an ecient method to depict the deformation of the magnetization loop and, as a consequence, a good tool for the analysis of the phenomena connected to the pinning processes, including the peak eect. In the case of PE, the magnetic loop has a steep deformation in a narrow range of dc magnetic eld, and is well characterized by the variation of the v3. The random orientation of the grains in bulk Bi2223 samples represents an apparent disadvantage. However, as will be shown in Section 2 paragraph, the susceptibility signal in our conditions of measurements mainly arises from the platelets oriented perpendicularly to the applied eld. Moreover, an advantage of our bulk samples is the clear separation between intra- and inter-granular vortex dynamics. Therefore, the study of the transition crossover dynamics was performed on a system consisting of decoupled Bi2223 plate-like crystals in bulk samples at relatively low elds. 2. Experimental Two samples with the same chemical composition Bi1.8Pb0.4Sr1.8Ba0.2Ca0.2Cu3Ox were prepared by using the standard solid-state reaction method.

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For sample 1, the Bi2O3, PbO, BaCO3, CaCO3 and CuO powders were mixed in the ratio Bi:Pb:Sr:Ba:Ca:Cu = 1.8:0.4:1.8:0.2:2:3. For sample 2 the following procedure of powder preparation for calcinations was used. Highpurity SrCO3, BaCO3, CaCO3, and CuO powders mixed in the ratio Sr:Ba:Ca:Cu = 1.8:0.2:2:3 were pressed in 9 9 3 mm3 pellets at 0.75 GPa which were treated at 947 C, this procedure being repeated and followed by a thermal treatment at 950 C. Bi2O3 and PbO powders were added to the obtained precursor, thus yielding the following ratio between the components Bi:Pb:Sr:Ba:Ca: Cu = 1.8:0.4:1.8:0.2:2:3. Samples 1 and 2 were calcinated in an alumina crucible at 815 C for 20 h in air, reground and pressed in 3 3 10 mm3 pellets at 0.75 GPa. The sintering thermal treatment of the pellets was performed in air at 848 C for 330 h and 320 h for samples 1 and 2, respectively. Every 110 h, sample 1 was quenched in air down to room temperature and then submitted again to the thermal treatment (848 C). According to XRD measurements sample 1 contains approximately 97% Bi-2223 phase, while sample 2 is single Bi-2223 phase without any trace of secondary or non-superconducting phases. The dimension of the samples was 5 3 2 mm3, the mean grain size being 58 lm for sample 1 and 1015 lm for sample 2. The ac susceptibilities including the higher harmonics were measured with a susceptometer based on double pick-up coils surrounded by a driven coil [15]. The sample was placed on a sapphire holder inserted in the pick-up coils. The temperature was measured with a platinum thermometer (PT100) in a good thermal contact with the sample. The whole assembly was cooled in zero magnetic eld (ZFC), in a thermally controlled He gas ow cryostat provided with an 8 T superconducting magnet. The temperature rate was 0.3 K/min, up to a temperature greater than the Tc value at zero eld, i.e., between 10 K and 120 K. The ac driving magnetic eld had an amplitude of 6 Oe and a frequency of f = 1070 Hz. The dc magnetic eld was swept from 0 to 1.5 T. The induced signal has been measured with a multiharmonic EG&G lock-in amplier. Both ac and

dc elds were applied parallel to the longest side of the sample. We avoided to grind the samples in order to study the isolated grains, because the grinding process may introduce defects into the grains (ssures, etc.) which can modify the pinning, and in this way can modify or even remove the anomaly (it is known that PE is a characteristic of the order-disorder transition in the vortex matter). Moreover the grinding produces non-homogeneity of the grain size. To prove that the signal in our measurements comes mainly from the platelets oriented perpendicular to the applied eld we measured a sample prepared in the following way. An as-grown sample, similar to sample 2 and prepared in the same conditions, was ground and the obtained powder was pressed at 3 GPa to diminish as much as possible the grain misalignment. The square shaped platelets were cut from the pressed material and superposed to make a cubic shaped sample. In Fig. 1, the v00 (T) dependence is shown for Hkab and H?ab measured in Hdc = 0.0128 T (Hac = 1 Oe). It is evident that the response in H?ab is more signicant than in Hkab. Therefore, for the conditions of the measurements used in this work on the bulk samples, our approximation in considering that the signal origin from the platelets

300

Hab
200

H = 0.0128 T
dc

H = 1 Oe
ac

" (a.u.)

f = 5500 Hz

100

H//ab
0 80 90 100 110 120

T (K)
Fig. 1. v00 (T) dependence for Hkab and H?ab measured in Hdc = 0.0128 T (Hac = 1 Oe). It is evident that the response in H?ab is more signicant than in Hkab.

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oriented perpendicular to the applied eld should not aect our results.

3. Results and discussion In Figs. 2A and 2B, the temperature dependence of the imaginary part of the rst harmonics v00 measured in the static magnetic eld in the 1 range 0 T > Hdc > 1.5 T is shown for samples 1 and 2, respectively. The clear separation of the inter- and intra-grain dissipation peaks due to the low values of the inter-grain critical current density (weak coupling) allowed us to scan also a portion of the irreversibility line for the grains. The v00 peak amplitude in respect to the applied 1 dc eld has a non-monotonic variation. A rapid drop around 0.07 T for sample 1 and around 0.1 T for sample 2 is observed. The decrease of the hysteretic cycle area for these eld values can be due to a contribution of both non-linear eects (pinning) and linear losses. To distinguish these two processes, an investigation of the higher harmonics is compulsory.
6.010-5

In Figs. 3A and 3B, the temperature dependence of the third harmonics module (jv3j) for two samples is shown. Increasing the magnetic eld, for sample 1, the amplitude of the third harmonics module has an unusual rise (jv3jmax) at Hdc = 0.1 T (Fig. 2A) while, for sample 2, around the same Hdc value, a signicant plateau is present before an abrupt decrease (Fig. 3B). (For higher elds jv3j is much smaller and, as a rule, is embedded in the inter-grain signal.) From Figs. 2 and 3 it is clear that some change in the vortex matter occurs, which could be due to a transition from an ordered to a disordered state [10] (like a 3D/2D transition [16]). To sustain the anomalous eects mentioned above, the peak amplitude of jv3jmax versus temperature has been plotted as a function of Hdc for both samples (Fig. 4). One can remark a peak for sample 1, and a plateau for sample 2, in the jv3jmax (Hdc) dependence. The peak as well as the plateau takes place in a very narrow Hdc range, indicating that around Bdc % 0.1 T a 3D/2D phase transition occurs which can be associated with the maximum of Jc (peak eect). At low elds the 3D

0.5T

0.1T 0.3T 0.07T

0.03T 0.002T

5.010-5

4.010-5

" (arb.unit)

3.010-5

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0.010 0

Sample 1 H ac = 6E-4T f = 1070 Hz

-1.010-5 50

60

70

80

90

100

110

Temperature (K)
Fig. 2A. v00 versus T for dierent dc elds (sample 1). Around Hdc = 0.1 T a rapid variation of the signal occurs. 1

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2.010 -4
sample 2 |H ac | = 6e-4T f = 1070 Hz

1.510 -4

"1 (arb.unit)

0.15T

0.1T

0.07T

0.03T

0T

1.010 -4

5.010 -5

0.010 0 50 60 70 80 90 100 110

Temperature (K)
Fig. 2B. v00 versus T for dierent dc elds (sample 2). Around Hdc = 0.07 T a rapid variation of the signal occurs. 1

1.210-5
0.5T 0.3T

Sample 1 H ac = 6E-4T f = 1070 Hz

0.15T 0.1T 0.07T 0.03T

0.002T

1.010-5

|X3 | (arb.unit)

8.010-6

6.010-6

4.010-6

2.010-6

0.0100 70

75

80

85

90

95

100

105

110

Temperature (K)
Fig. 3A. jv3j versus T for dierent dc elds (sample 1). Around Hdc = 0.1 T an increasing of the signal occur.

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5.010 -6

sample 2 |Hac | = 6e-4T f = 1070 Hz

0.15T 0.1T 0.07T 0.03T 0T

4.010 -6

| | (arb.unit)

3.010 -6

2.010 -6

1.010 -6

0.0100 70

75

80

85

90

95

100

105

110

Temperature (K)
Fig. 3B. jv3j versus T for dierent dc eld (sample 2). Around Hdc = 0.1 T a constant value of the signal (plateau) can realize.

110-5
sample 1 II peak sample 2

210 -5

| |(arb.unit) sample 2

| |(arb.unit) sample 1

510-6

110 -5

110-6

510 -6

0.0

0.1

0.2

0.3

0.4

0.5

0.6

Hdc (T)
Fig. 4. jv3j versus Hdc for samples 1 and 2. For Hdc = 0.1 T these curves show a peak for sample 1 and a plateau for sample 2.

vortex-pin center interactions are dominant and the vortices are poorly pinned [6]. The pinning strength decreases with the incrementing of the

magnetic eld due to the escalating of the in-plane vortex lattice stiness [17]. For Hdc % 0.1 T there is a sharp decoupling transition and the irreversibil-

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10 2 10 1 10 0 10 -1 10 -2 10 -3 10 -4 10 -5 10 -6 30
B irr(T) = B 0[1-(T/Tc )] n B 0 = 1.8T n = 1.58 Tc = 110K
2D B irr (T) = B cr exp{b[Tm /(T-Tm )] } B cr = 0.1T b = 2.1, =3.6 2D T m = 36.7K 2D

sample 1

B (T)

irr

40

50

60

70

80

90

100

110

Temperature (K)
Fig. 5A. IL line obtained from the onset of jv3j (T) (sample 1). The curve follows two dierent behaviors of the ux dynamic which are separates by the characteristic 3D/2D crossover.

ity response increases. At higher elds the eectiveness of the pinning decreases due to the increasing of the in-plane interactions. The crossover eld between 3D and quasi-2D dimension regimes follows the expression [4,5]: H cr % U0 =c2 d 2
15 2

T m is the elementary where U0 = 2.07 10 quantum ux, d is the spacing between adjacent groups of CuO2 layers and c is the anisotropy ratio, dened as c = nab/nc. The nab and nc are the superconducting ab-plane and c-axis coherence lengths, respectively. If one considered the inter layer spacing d = 18 A [18], Eq. (1) yields an anisotropy factor c % 80 for Hdc % 0.1 T. To conrm the validity of 3D/2D transition obtained from our analysis of the second peak eect we investigated the irreversibility line (IL) extracted from the onset of the jv3j for the two samples and have examined its behavior near Hdc % 0.1 T. The platelets in our polycrystalline samples are far from being clean so

we can assume that the irreversibility line is close to the melting line in the high temperature-low eld region, in this case IL can replace the ML and we shall also use Bm and Tm for the description of our experimentally obtained IL. In Figs. 5A and 5B, the plot of the log(Birr) versus T [6] is shown for samples 1 and 2, respectively. It is evident that the irreversibility line follows two dierent laws with temperature, separated by a crossover eld (Bcr). For Birr < Bcr, the region in which the nearly 3D-like vortex uctuations occur [3,6,19,20] we obtain a quite good t of the melting line with parabolic-like law: Bm T B0 T c =T 1n 2

where n = 1.58 for sample 1 and n = 1.48 for sample 2. The functional dependence of the IL is a representation of the ux lattice free energy [21]. Small thermal vortex uctuations render a value for n smaller than 2 [6].

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10 2
sample 2

10 1

10 0

B (T)

10 -1

10 -2

B irr(T) = Bcr exp{b[T m /(T-T m )] } B cr = 0.1T b = 6.2, =3 2D T m = 27.3K

2D

2D

irr

10 -3

10 -4

B irr(T) = B0[1-(T/Tc )] n B 0 = 1.6T n = 1.47 Tc = 107.7K

10 -5 30 40 50 60 70 80 Temperature (K) 90 100

Fig. 5B. IL line obtained from the onset of jv3j (T) (sample 2). The curve follows two dierent behaviors of the ux dynamic which are separates by the characteristic 3D/2D crossover.

IL line for Birr > Bcr, shows the same exponential behavior found in 2D ux lattice melting of coherent regions with weak Josephson interaction between adjacent layers [22]. We tted the low temperature data using this melting line approach described by the inverse formula [6] of the asymptotic deviation of Tm(H) from T 2D [23]: m T m H T 2D 1 b=ln B=Bcr m
1=m

2. These results t well with literature data, where T 2D $ 40 K was found using transport measurem ments on Bi2223/Ag tapes [25] and T 2D $ m 2830 K for Bi-2212 single crystal [26].

4. Conclusion In conclusion we have studied the multiharmonic ac susceptibility of the grains in Bi1.8Pb0.4Sr1.8Ba0.2Ca0.2Cu3Ox polycrystalline samples. Qualitative as well as quantitative behaviors of the third harmonic modulus that probes only the nonlinear losses (i.e., the pinning processes) have been studied. An unusual variation of jv3j (peak eect) at Hdc % 0.1 T was observed and a ux dynamics crossover on the IL at the same value has been found for both samples. The irreversibility lines follow two dierent behaviors upon increasing elds due to the thermal uctuations [1,28,29]. We analyzed them according to the general notions [1,4,27] which predict a characteristic

where b, m are constants and their values together with the formula for Birr(T) are shown in Figs. 5A and 5B. We obtained the crossover eld value Bdc % 0.1 T for both samples. It is remarkable to notice that the value of the crossover eld of our bulk Bi-2223 samples is close to those obtained in the literature for other Bibased HTS: 0.3 T [7] and 0.01750.1750 T [14], obtained on the textured Bi-2223, as well as 0.1 T on Bi-2212 single crystals [6]. In the strong eld region (B ) Bcr) the behavior of IL shows an asymptotic temperature [24] with value 36.7 K for sample 1 and 27.3 K for sample

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crossover that separates regions of 3D and 2D melting. Near Tc the melting line has been obtained by tting the experimental points with a quasi-parabolic temperature dependence (3D region) Birr = B0(Tc/T 1)n. For low temperatures Tm has been obtained by tting the data with a quasi-2D behavior, the asymptotic deviation of Tm(B) from T 2D has been used. m The behavior of the grain ux dynamics in BSCCO bulk has been measured using the accurate multi-harmonic susceptibility technique. The existence of the anomalous PE has been veried trough the analysis of the third harmonic modulus amplitude. At the same time the IL has been obtained using the onset of the same third harmonic modulus. Both these phenomena, PE anomaly and the behavior of IL, are compatible with the 3D/2D ux dynamic crossover.

Acknowledgements This work has been supported by the European Community Transnational Program (TARI) under contract number HPRI-CT-1999-00088 and by Romanian Ministry of Education and Research under Nucleu Programme.

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