Phase transitions in the ferroelectric crystals CH 3 NH 3 5 Bi 2 Cl 11 and CH 3 NH 3 5 Bi 2 Br 11 studied by the nonlinear dielectric effect P. Szklarz, 1 M. Galązka, 2 P. Zieliński, 2,3 and G. Bator 1, * 1 Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw, Poland 2 The H. Niewodniczański Institute of Nuclear Physics PAS, Radzikowskiego 152, PL-31-342 Kraków, Poland 3 Cracow University of Technology, Institute of Physics, ul. Podchorążych 1, 30-084 Kraków, Poland Received 23 February 2006; revised manuscript received 19 July 2006; published 13 November 2006 The real part of the complex electric permittivity at low frequencies and at several biasing fields between 0 and 5 10 5 V/mhas been measured in ferroelectric crystals CH 3 NH 3 5 Bi 2 Cl 11 MAPCBand CH 3 NH 3 5 Bi 2 Br 11 MAPBBin the temperature range covering the temperature of the ferroelectric phase transitions. Comparative measurements for the known triglycine sulphate NH 2 CH 2 COOH 3 H 2 SO 4 crystal have been used as a test of the validity and of possible errors in the determination of the ferroelectric equation of state by the method applied. The estimates of the critical parameters T C , , and then have been evaluated for MAPCB and MAPBB on the basis of the Widom-Griffiths scaling hypothesis. Complementary pyroelectric measurements of the spontaneous polarization providing the critical exponent are in accordance with the parameters obtained. DOI: 10.1103/PhysRevB.74.184111 PACS numbers: 77.22.-d, 75.40.Gb, 72.20.Ht I. INTRODUCTION Measurement of the electric susceptibility in a biasing constant field is sometimes called nonlinear dielectric effect NDE. 1,2 It is a convenient method of studying ferroelectric phase transitions, especially those of second order. The ap- plication of the biasing electric field then allows one to scan the region of the critical point in a two-dimensional temperature-field space. Generally, the temperature depen- dence of the electric susceptibility measured in this way has the form of an asymmetric bell-like curve with a maximum which shifts towards higher temperatures with increasing bi- asing field. Far below and far above the phase transition region the curves tend to constant values corresponding to the low- and high-temperature limit susceptibilities, respec- tively. Consequently, such curves are concave—i.e., have negative second derivative close to the maximum—and convex—i.e., have positive second derivative in the low- and high-temperature limits. Thus, there are at least two points of vanishing second derivative on every such curve, one below or to the left toand one above or to the right tothe maximum. The points are called inflection points. It has been shown by the present authors 3,4 that for materials obeying the scaling-invariant equation of state there are in fact from one to three inflection points below the maximum depending on the values of the critical exponents and . In particular there is always an inflection point exactly at the critical tem- perature for the classical mean-fieldexponents =1 and = 1 2 . What precedes the susceptibility is meant to be the static one. In practice, however, only ac data are available in most cases. Then, the low-frequency limit—i.e., that far below the normal dielectric absorption peak—of the real part of the complex electric susceptibility can be taken into account. Rigorously it is impossible to come too closely to the critical point because the dielectric absorption peak moves towards zero frequency when the critical point is approached. The effect is known as critical slowing down, which corresponds to the relaxation time going to infinity. As a consequence, any experimental frequency becomes too large to be consid- ered as the static limit. Moreover, the thermal conductivity tends to zero at the critical point so that the time needed to attain the thermal equilibrium after supplying a portion of heat to the system becomes infinite. Therefore, any experi- mental rate of changes of temperature is too rapid close enough to the critical point. No physical quantity measured in such conditions then corresponds to the thermal equilib- rium. Related to the zero of thermal conductivity is also the phenomenon of passing from isothermal to adiabatic susceptibility. 5 The use of a biasing field, which drives the system out of the critical point, allows one to evade all the described ef- fects of the critical slowing down. Staying at a distance from the critical point in the temperature-field plane makes the dielectric absorption peak always lie at a finite frequency. Then, the low-frequency limit of the real susceptibility is, at least in principle, always possible to attain. The present pa- per deals with such a low-frequency electric susceptibility. We use the frequency independence of the real part of the susceptibility as a test of staying at the low-frequency limit because this corresponds to the practically vertical part of the Cole-Cole plot. 6 As described in Sec. III and in Refs. 713 the analysis of the data obtained in the NDE allows one to determine, through so-called scaling invariants, all the pa- rameters of the equation of state compatible with the scaling hypothesis. Such an analysis has been done for the known ferroelectrics TGS, TGSe, GPI, and DMAGaS. 7,8,11 In the present work the scaling equations of state are established for the CH 3 NH 3 5 Bi 2 Cl 11 MAPCBand CH 3 NH 3 5 Bi 2 Br 11 MAPBBcrystals. These are relatively new materials belonging to the familiy of halogenoanti- monates IIIand halogenobismuthates IIIRef. 14or imi- dazolium tetrafluoroborate Ref. 15. Particularly interesting are the recently synthesised methylammonium salts MAPCB Ref. 16and MAPBB Ref. 17. Both of them show qua- sirigid anionic sublattices and orientationally disordered cat- PHYSICAL REVIEW B 74, 184111 2006 1098-0121/2006/7418/1841117©2006 The American Physical Society 184111-1