Dependence of the specific heat of Na x CoO 2 · yH 2 O/D 2 O on sodium and water concentrations R. Jin, 1, * B. C. Sales, 1 S. Li, 2 and D. Mandrus 1,2 1 Condensed Matter Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, USA 2 Department of Physics and Astronomy, The University of Tennessee, Knoxville, Tennessee 37996, USA Received 1 June 2005; published 26 August 2005 We report specific heat measurements down to 0.4 K on the layered oxide Na x CoO 2 · yH 2 O/D 2 O with 0 x 0.74 and y = 0 and 1.4. For the nonhydrated system y =0, the electronic specific heat coefficient N and the Debye temperature D vary nonmonotonically with x, both displaying minima when x is close to 0.5. This indicates a systematic change of the electronic and vibrational structures with Na content. For both hydrated and deuterated systems x = 0.35 and y = 1.4, the specific heat reveals a sharp peak with C p 45.5 mJ/mol K at T c mid 4.7 K and an anomaly at T x 0.8 K. While the origin of the latter is not clear, the former corresponds to the superconducting transition. With the application of magnetic fields up to 14 Tesla, T c decreases gradually but T x remains more or less unchanged. The implication of these results is discussed. DOI: 10.1103/PhysRevB.72.060512 PACS numbers: 74.25.Bt, 74.20.Rp, 74.25.Jb, 74.90.+n There is growing evidence that the strong electron- electron correlation in layered Na x CoO 2 is responsible for some of its anomalous physical properties such as its “colos- sal” thermopower 1,2 and possibly superconductivity in its hy- drated form. 3 Although it is a good metal with high electrical conductivity for a wide Na-doping range except for x = 0.5, both local-density approximation LDAcalculations 4 and experimental work 5 indicate that the itinerant bands of Na x CoO 2 are very narrow with W U, where W is the band width and U is the effective on-site Coulomb interaction. This implies a high value of the density of states DOSat the Fermi level. However, all specific heat data reported so far reveal a weak or moderate enhancement of electronic specific heat coefficient N for both hydrated and nonhy- drated cases compared to the value from the LDA band structure. 4,6–9 In these reports, the N value was obtained by analyzing specific heat data above 2 K for x in the range of 0.3–0.8. It is possible that the extracted N value does not represent that for T 0 K. On the other hand, recent calcu- lations, using the LDA+ U method, suggest that the strength and effect of Coulomb interactions are reduced with decreas- ing x. 10 One would thus expect a variation of N with x. On the experimental side, the electronic properties of hy- drated and nonhydrated Na x CoO 2 have not been systemati- cally studied as a function of composition. While the phase diagram shown in Ref. 11 is constructed from electrical transport and magnetic measurements for 1 / 3 x 3/4 and water content y = 1.4, little is known about how the thermo- dynamic properties vary with both x and y. Of particular importance is the specific heat behavior in the superconduct- ing state of the system, which can provide key information about the superconducting pairing symmetry. In this paper, we report the low-temperature specific heat of Na x CoO 2 · yH 2 O/D 2 O with 0 x 0.74 and y =0 and 1.4. Single crystals of Na x CoO 2 were used for specific heat measurements. Starting with Na 0.74 CoO 2 single crystals grown using a flux method, 12 crystals with smaller x were obtained by chemical deintercalation as described in Ref. 6. By controlling the deintercalation time, we obtain single crystals with x 0.72 and 0.48, as determined from measure- ments of the c-axis lattice parameter using the calibration curve in Ref. 11. However, it is known that the above tech- nique cannot extract all Na from Na x CoO 2 . In order to obtain CoO 2 x =0with the hexagonal structure, we extract all Li from LiCoO 2 powders using NO 2 BF 4 as described in Ref. 13. Polycrystalline samples of Na 0.35 CoO 2 and superconduct- ing Na 0.35 CoO 2 · 1.4H 2 O/D 2 O were prepared following a procedure similar to that described in Ref. 14. Specific heat measurements were carried out using a physical property measurement system PPMSfrom Quantum Design. In Fig. 1a, we present the temperature Tdependence of the specific heat C p for Na x CoO 2 with x 0.74, 0.72, 0.48, 0.35, 0. Note that C p varies monotonically with T be- tween 0.4 and 10 K and the curve tends to move upward with increasing x. For easy analysis, we replot the data as C p / T vs T 2 as shown in Fig. 1b. If the specific heat is due to electrons and phonons only, it is expected that C p / T will be a linear function of T 2 at low T. While this is true for CoO 2 x 0between 0.4 and 10 K, C p / T clearly deviates from linearity below 2 K for samples with x 0. The low- T upturn indicates that an additional contribution sets in that increases with decreasing T. Similar behavior was reported previously and was attributed to a Schottky effect. 7 Thus, for FIG. 1. aTemperature dependence of the specific heat C p for single crystalline Na 0.74 CoO 2 filled circles, Na 0.72 CoO 2 unfilled circles, Na 0.48 CoO 2 crosses, polycrystalline Na 0.35 CoO 2 filled diamonds, and CoO 2 unfilled diamondsbetween 0.4 and 10 K. Shown in bis the replot of the data as C p / T vs T 2 , and the solid curves are the fits of experimental data to Eq. 1. PHYSICAL REVIEW B 72, 060512R2005 RAPID COMMUNICATIONS 1098-0121/2005/726/0605124/$23.00 ©2005 The American Physical Society 060512-1