# First order phase transition of the vortex lattice in twinned YBa2Cu3O7 single crystals in tilted magnetic fields

## I Introduction

During the last years, vortex physics in high-temperature superconductors has become a major topic of research. The main reason for this interest is that the interplay between thermal fluctuations, anisotropy and disorder determine the existence of several vortex phases in the magnetic phase diagram of these materials. These phases are separated by different kinds of thermodynamic transitions. In particular, it is now well established that in clean YBa<sub>2</sub>Cu<sub>3</sub>O<sub>7</sub> crystals the vortex solid transforms into a liquid through a first order phase transition . This thermodynamic transition shows up in the transport properties as a sharp drop or “kink” in the resistivity, $`\rho (T)`$, at the melting temperature $`T_m(H,\theta )`$ , and has an hysteretic behaviour both in temperature and field  which corresponds to a superheating of the solid phase .

When correlated disorder is present in the sample, as for example in twinned YBa<sub>2</sub>Cu<sub>3</sub>O<sub>7</sub> crystals, the transition transforms into second order  and occurs between a solid called Bose-Glass  and an entangled vortex liquid. The Bose-Glass phase, existing only within a small angular region around the direction of the correlated defects ($`\theta =0`$), is characterized by a universal behaviour of the non-linear and linear resistivity with well defined critical exponents . At the Bose- Glass transition temperature, $`T_{BG}(H,\theta )`$, the presence of correlated defects introduces changes in the thermodynamic properties of the mixed state that go beyond the mass anisotropy approximation. In contrast to $`T_m(H,\theta )`$ which smoothly follows the angular dependence given by the anisotropy, $`T_{BG}(H,\theta )`$ shows a sharp cusp around $`\theta =0`$. Within this small angular region, $`\rho (T)`$ has a smooth temperature dependence near the transition, while at larger angles a similar kink to that observed in untwinned crystals develops . Using the Lindeman criterion and the scaling rules for anisotropic superconductors  Kwok and co-workers  fitted the angular dependence of the temperature at which the kink occurred. This fit was interpreted as an indication of a recovery of the melting transition in the vortex system when the magnetic field was tilted away from the planar defect direction .

Using this interpretation, Langan et al. showed in a recent paper  that the kink in $`\rho (T)`$ is suppressed for fields larger than a certain field $`H^{}(\theta )`$. This behaviour is similar to that observed in untwinned crystals where a critical end point for the melting line has been identified , and gives support to the occurrence of a first order solid- liquid transition when the field is rotated away from the twin planes.

An interesting finding in oriented twinned crystals in inclined magnetic fields was done by Morré et al. , who showed that the transport properties of the liquid state at angles well beyond the so-called depinning angle, $`\theta _d`$, are quite different from those observed in clean samples. The depinning angle concept is commonly used in the literature to indicate the angle beyond which the twin boundaries becomes ineffective as a correlating potential. Morré et al. showed, however, that the twin boundary potentials continue to induce vortex velocity correlation even for $`\theta >>\theta _d`$. Their results demonstrated that the vortex liquid remains correlated in the field direction above the resistivity kink temperature. This behaviour is in sharp contrast to that observed in untwinned samples where the vortex velocity correlation in the field direction is lost at the melting temperature . The important difference between the characteristics of the two liquids was used to cast doubts about the interpretation of the resistivity kink in twinned crystals as a manifestation of a first order transition .

In order to investigate further the nature of the vortex solid-liquid transition in the presence of correlated defects at finite angles, we studied the vortex dynamics in YBa<sub>2</sub>Cu<sub>3</sub>O<sub>7</sub> crystals with oriented twin boundaries. We performed exhaustive transport measurements as a function of magnetic field, $`H`$, and angle, $`\theta `$, with respect to the twin boundary direction. Characterizing the resistivity kink near the transition by its width, we show that it remains almost constant as $`H`$ is increased until a field $`H^{}(\theta )`$ is reached. Below this field the V-I characteristics are non-linear and, what is more important, the resistive transitions are hysteretic. Moreover, our results indicate that the hysteresis corresponds to a superheating of the vortex lattice, in agreement with the results obtained by Charalambous et al.  Above $`H^{}`$ which scales as $`\epsilon (\theta )H^{}(\theta )`$, the kink width suddenly increases, the V-I characteristics become linear and the hysteresis disappears. We find that the resistivity kink height follows a universal behaviour when the reduced variable $`\epsilon (\theta )H`$ is used, in contrast to the results of Langan et al.. Our data together with those previously reported , lead us to conclude that when $`H`$ is tilted away from the direction of the twin planes the transition to the vortex liquid state, characterized by a steep jump in the resistivity, is indeed a first order phase transition. This transition occurs between a highly correlated vortex liquid  and a solid of unknown symmetry and therefore supports an interpretarion in therms of line-like melting  rather than a sublimation of the vortex lattice .

## II Experimental

We carried out transport measurements on YBa<sub>2</sub>Cu<sub>3</sub>O<sub>7</sub> single crystals with only one family of oriented twins. The crystals were grown using the self flux method . The fully oxygenated samples had typical dimensions $`1\times 0.3\times 0.01mm^3`$, critical transition temperatures $`T_c=93.2K`$, and transition widths $`\mathrm{\Delta }T_c0.6K`$. Four parallel contacts separated by 150$`\mu m`$ were made with silver epoxy over evaporated gold pads, resulting in contact resistances lower than 1$`\mathrm{\Omega }`$. The crystal was mounted onto a rotatable sample holder with an angular resolution better than $`0.05^{}`$ inside a commercial gas flow cryostat with an 18T magnet. The current was injected at $`45^{}`$ off the twin planes. Transport measurements were performed using conventional DC techniques. All resistivity measurements were made within the linear regime using a current density $`J3A/cm^2`$.

## III Results and Discussion

In Figure 1 we show the angular dependence of the temperature at which the resistivity of the crystal becomes zero within experimental resolution , at an applied magnetic field of 6T. Similar results were obtained for other applied fields. As clearly seen, there is a cusp at small angles which is indicative of the Bose-Glass phase, as has been recently demonstrated by Grigera et al. . In this paper we will concentrate on the investigation of the nature of the solid-liquid transition in the angular region away from that in which the Bose-Glass phase exists.

In Figure 2 we present $`R(T)`$ data for three different angles, as a function of the applied magnetic field. As can be seen, the transitions at low fields display a sharp drop to zero which we identify with the characteristic resistivity kink. Note that, for a fixed angle, the kink is washed out as the field is increased, an effect similar to that observed in ref.  and to that reported for untwinned crystals with the magnetic field applied parallel to the $`c`$-axis . In the case under study, the field value at which the transitions starts to broaden depends on the angle between $`H`$ and the correlated defects: the larger the angle, the larger the field at which the kink is washed out. This feature is more clearly seen in Figure 3 where, in order to quantify the above mentioned behaviour, we plotted the full width at half maximum (FWHM) of the temperature derivative, $`d\rho /dT`$, of the curves shown in Fig. 2 as a function of the applied field $`H`$. It can be seen that for $`\theta =23^{}`$ the transitions start to broaden at approximately $`H12T`$, while this field value is increased up to 14T for $`\theta =38^{}`$, and to almost 18T for $`\theta =58^{}`$. The values of the magnetic field at which the transitions start to broaden are independent of the criterion used for the definition of the transition width.

According to the scaling theory of Blatter et al. , in an anisotropic superconductor a physical magnitude which is a function of angle and field should scale as the product $`H\epsilon (\theta )`$, where the anisotropy factor $`\epsilon (\theta )=\sqrt{cos^2(\theta )+\gamma ^2sin^2(\theta )}`$, with $`\gamma ^2=m_c/m_{ab}`$. Such scaling for the FWHM, with $`\gamma =7`$, is shown in Figure 4, where we have also included data for other measured angles. Note that all curves collapse onto one and that the sudden increase of the transition widths occurs at the same reduced field $`H^{}=H\epsilon (\theta )11T`$ for all angles. The sudden change in the transition width is indicative of a corresponding change in the vortex dynamics below and above the characteristic field $`H^{}`$.

As is widely accepted, one of the most powerful tools to investigate vortex dynamics is the measurement of V-I characteristics. We performed such measurements in a temperature interval around the transitions for magnetic fields below and above $`H^{}`$. Typical results for the resistance as a function of the applied current at an angle $`\theta =23^{}`$ are shown in Figure 5. In panel (a) we plot the measurements for a field of 8T, lower than the critical field $`H^{}(23^{})`$. At low currents and high temperatures the vortex response is ohmic, changing to a non-linear behaviour as the temperature is reduced towards $`T_m=80.4`$. Note that in the intermediate temperature region, the R(I) curves have a characteristic s-shape. This feature, which has been reported in clean samples where a first order phase transition in the vortex lattice was identified , is characteristic of all the magnetic field region below $`H^{}(23^{})`$. It is more pronounced as $`H`$ is reduced, becoming less evident as $`H`$ approaches $`H^{}`$. Well above $`H^{}`$ the $`R(T)`$ curves are linear up to the maximum current that can be used without producing heating effects. In panel (b) we show the results for $`HH^{}(23^{})`$. Clearly, the vortex response is remarkably different from that shown in panel (a). In a wide range of applied currents the response is linear. Non-linearities developed at high currents and low temperatures and are due to vortex loop excitations . One may wonder if these non-linearities are a sign of a glass transition taking place at lower temperatures, a question that has also been raised concerning the nature of the transition above the critical point in clean crystals. If this were the case, the tails of the resistive transitions above the critical field should follow the scaling behaviour predicted by the theory , $`R(TT_g)^{\nu (z1)}`$. The analysis of our resistivity data in terms of this scaling yielded negative results. We cannot discard, however, the occurrence of the glass transition, since this negative results might be related to the voltage resolution we have in our experiments. Safar et al.  experimentally observed the above mentioned scaling in Bi<sub>2</sub>Sr<sub>2</sub>CaCu<sub>2</sub>O<sub>8+δ</sub> crystals by using SQUID picovoltimetry.

The extensive experimental results shown above display special features pointing towards the occurrence of a first order solid to liquid transition in the vortex lattice when $`H<H^{}`$. In order to consolidate this scenario, we have performed measurements to look for hysteretic behaviour in the resistive transitions. Due to experimental constrains, instead of searching for hysteresis in temperature, we performed such measurements at a fixed temperature (regulation better than 5 mK) and sweeping the magnetic field up and down. The results for an angle $`\theta =23^{}`$ and a measuring current $`I=50\mu A`$ are plotted in Figure 6. Panel (a) shows the data for $`TT^{}`$ where $`T^{}`$ is the temperature corresponding to the critical field at $`\theta =23^{}`$. The arrows indicate the sense in which the field was sweeped. Within experimental resolution no hysteresis is seen in this region. However, when the temperature is increased in such a way that $`T>T^{}`$ a clear hysteretic behaviour in the resistive transition develops, as can be seen in panel (b). It is important to mention that the width of the hysteresis is current independent between $`50`$ and $`100\mu A`$. When the applied current is increased above this value curve A shifts towards curve B and, at high enough currents (above $`150\mu A`$), the hysteresis is washed out. Following Charalambous et al.  we interpret this behaviour as indicative of a superheating of the vortex lattice.

In Figure 7 we compare the superconductor phase diagram for our sample with that obtained in a clean untwinned crystal . The inset show the raw H-T data, for different angles and the data at zero angle for the untwinned crystal. In order to take into account the anisotropy change as the angle between $`H`$ and the defects is changed, in the main panel we have used the corresponding scaling field $`H\epsilon (\theta )`$, while the reduced temperature scale $`t=T/T_c(H=0)`$ is used to account for the different critical temperature at zero field of both samples. The collapse of all data on one universal curve not only provides an impressive graphical view of our interpretation of the resistivity kink temperature in twinned samples as a melting temperature, but indicates that the presence of the twin boundary potentials does not modify this temperature. Later on we will come back to this point, continuing now with the anisotropy dependence of other physical quantities.

In clean crystals a relevant quantity related to the melting transition is the kink height at the melting temperature. It has been found to be angle and field independent , and this particular behaviour has attracted theoretical interest . In contrast, we have found that in $`45^{}`$ oriented twinned crystals, the kink height is angle and field dependent, an observation already reported in ref. . Since this quantity related to the occurrence of a first order phase transition which follows the anisotropy, we expect the kink height also to scale with it. In Fig. 8 we show such scaling. We have plotted the kink height measured at fixed angles and increasing the magnetic field (open symbols), together with measurements of the same quantity but at a fixed applied field (6T) and reducing the angle $`\theta `$(full symbols). Clearly all data collapse onto a universal curve. The behaviour reported by Langan et al. is distinctly different. The reasons for the lack of scaling in their data is related to the fact that their measurements at $`\theta =5^{}`$ were taken in an angular region were the dissipation at the transition is greatly reduced due to the effect of the twin planes on the vortex dynamics. This reduction is easily seen in $`V(\theta )`$ measurements where a dip in the dissipation occurs  for $`\theta 10^{}`$, an angle usually identified with $`\theta _d`$. One may wonder if this change in the vortex dynamics is a consequence of a corresponding change in the thermodynamic nature of the transition for $`\theta <\theta _d`$. This is certainly true when the Bose-Glass phase is reached since it has been demonstrated  that in this case the transition is second order. However, this phase exists  below $`\theta _{BG}2^{}`$, leaving a rather wide angular region ($`\theta _{BG}\theta \theta _d`$) where the full kink height develops (see e.g. ref. ). One interesting possibility  is that this angular region comprises a reentrant liquid phase separating the Bose-Glass from the vortex solid, in a similar way to what has been predicted to occur near $`H_{c1}`$ in clean samples in . In this case the resistive transitions below the developing kink should be linear due to an increased viscosity of the reentrant liquid phase as the temperature is lowered. Within this picture $`\theta _d`$ would be the angle below which the reentrant phase starts to develope. Another possibility is that the angular region between $`\theta _{BG}`$ and $`\theta _d`$) is governed by critical fluctuations of the Bose-Glass phase associated to the new thermodynamic variable $`H_{}=Hsin(\theta )`$. If this were the case the so-called depinning angle should be interpreted as the critical angle above which the first order solid-liquid transition sets in. Although a detailed analysis of the nature of the solid-liquid transition in this angular region is out of the scope of this paper, further investigation is underway to elucidate this interesting issue.

In the following, we would like to comment on a few important points concerning the $`HT`$ phase diagram shown in Fig. 7. The first one is related to the value of the critical field $`H^{}`$ compared to that of the untwinned sample. It is well known that in untwinned crystals this field has not a universal value. Its magnitude depends on the amount of point like disorder present in each crystal , the larger the disorder the lower the critical field. The results in Figure 7 which show $`H^{}H_S^{}`$ may therefore suggest that in tilted magnetic fields the presence of twin boundaries does not increase the amount of point like disorder. This suggestion seems to be corroborated by our measurements in another oriented twinned crystals and by the results shown in ref.  with a value of $`H^{}11T`$, similar to that obtained in our crystals.

The second remark is more fundamental since it is related to the nature of the solid and liquid vortex phases in the twinned crystal. In a recent paper Sasagawa et al.  suggested that the first order solid-liquid phase transition in the vortex system of high temperature superconductors, including the less anisotropic YBa<sub>2</sub>Cu<sub>3</sub>O<sub>7</sub>, corresponds to a vortex sublimation rather than a line melting. Within this scenario the vortex velocity correlation length in the field direction should vanish at the melting temperature because the vortex liquid phase is formed by uncorrelated pancakes. As already mentioned in the introduction, Morré et al. have shown , using the flux transformer contact configuration, that the vortex liquid in tilted magnetic fields mantains the vortex velocity correlation in the field direction even at rather large angles off the twin planes. Since we have concluded that the transition in tilted fields is indeed first order, their results imply that the solid transforms into a vortex liquid of correlated lines, contrary to what happens in clean samples. This has a two important implications: first the sublimation scenario proposed by Sasagawa et al.  does not hold for the melting transition in twinned crystals for tilted magnetic fields, and second, although the twin boundary potentials do not affect the melting temperature they play an important role in building up the vortex velocity correlation in the field direction. This last point indicates that the degree of correlation in the vortex liquid does not determine the nature of the thermodynamic transition. Therefore one may conclude that the liquid phase in clean and untwinned samples (in tilted magnetic fields) is essentially the same but with different dynamics due to the different vortex velocity correlation. On the other hand, it could also be possible that the nature of the liquid phase differs from that in untwinned samples. We speculate that for twinned crystals in tilted magnetic fields, the entangled vortex liquid might be formed by stair-like correlated lines which are stabilized by the twin boundary potential. Within this picture, the solid might have a complicated ordered structure also formed by stair-like vortices.

## IV Conclusion

We have shown that the vortex solid-liquid transition in twinned YBa<sub>2</sub>Cu<sub>3</sub>O<sub>7</sub> crystals for magnetic fields tilted away from the planar defect’s direction is first order. This thermodynamic transition is reflected in the transport properties as a sharp kink in the $`R(T)`$ curves at the melting temperature $`T_m(H,\theta )`$. The resistive transitions are hysteretic below a critical field that scales with the anisotropy of the material, with the hysteresis indicating a superheating of the solid phase. The correlated vortex liquid phase near the melting temperature could be probably formed by stair like entangled lines that maintain their vortex velocity correlation in the field direction due to the effect of the twin boundary potential. The structure of the vortex solid is unknown.

## V Acknowledgments

We acknowledge stimulating discussions and comments from F. De la Cruz. We thank J.Luzuriaga for a critical reading of the manuscript. This work is partially supported by ANPCyT, Argentina, PICT 97 No.03-00061-01116, and CONICET PIP 4207. E.O. and G.N acknowledge financial support from Consejo Nacional de Investigaciones Científicas y Técnicas.