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Superconductivity in Three-Layer Na0.3Coo2·1.3H2O

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Superconductivity in Three-Layer Na0.3Coo2·1.3H2O Superconductivity in three-layer Na0.3CoO2·1.3H2O M.L. Foo1, T. Klimczuk1,3, Lu Li2, N.P. Ong2, and R.J. Cava1 1 Department of Chemistry, Princeton University, Princeton NJ 08544, 2 Department of Physics, Princeton University, Princeton NJ 08544, 3 Faculty of Applied Physics and Mathematics, Gdansk University of Technology, Narutowicza 11/12, 80-952 Gdansk, Poland, The observation of superconductivity at 4.3 K in a new crystalline form of Na0.3CoO2·1.3H2O is reported. The new superconductor has three layers of CoO6 octahedra per crystallographic unit cell, in contrast to the previously reported two-layer superconductor. The three-layer cell occurs because the relative orientations of neighboring CoO2 layers are distinctly different from what is seen in the two-layer superconducting phase. This type of structural difference in materials that are otherwise chemically and structurally identical is not possible to attain on the layered copper oxide superconductors. The synthesis and stability of the new phase are described. Since the discovery of two-layer superconductor, this superconductivity near 4 K in superconductor is structurally distinct 1 Na0.35CoO2·1.35H2O , the physics of due to differences in the stacking of the electronic and magnetic systems based CoO2 sheets in the third dimension. The on layered triangular lattices, where the consequences of this kind of structural geometry frustrates long-range magnetic difference have not been pursued in the ordering at low temperatures, has been cuprate superconductors. The of great interest. The chemistry and observation of superconductivity at the structure of Na0.35CoO2·1.35H2O, which same critical temperature in both two- consists of two triangular cobalt oxide layer and three-layer sodium cobalt sheets per unit cell separated by spacer oxyhdrates suggests that the essential layers of water molecules and sodium physics of these superconductors will be ions, as well as its apparent balance well described by theoretical models that between magnetism and consider the magnetic and electronic superconductivity, are similar to the system to be essentially two-dimensional cuprate high Tc superconductors. Here in nature. we report the discovery of The parent phase of the original superconductivity in three-layer Na0.35CoO2·1.35H2O superconductor is Na0.30CoO2⋅1.3H2O, at a temperature of Na0.7CoO2, which is obtained by heating 4.3 K. Although essentially identical in sodium and cobalt oxides at 800 degrees chemical composition to the original in oxygen. The unit cell is built up by 1 two (2) sheets of edge-shared CoO6 atmosphere of flowing argon. The Na octahedra, which are rotated by 60 content of the product was verified by degrees with respect to each other. The neutron powder diffraction structural sodium ions, on two crystallographically analysis and Inductive Coupled Plasma distinct sites, are trigonal prismatic (P) (ICP) analysis to give the formula in coordination to the oxygen atoms, and Na0.30CoO2. The structural analysis, to hence the nomenclature P2 (prismatic, be reported elsewhere4, showed that the two layer) is used to describe the O3 structure type was fully maintained structure of Na0.7CoO2. A distinctly on deintercalation of the sodium. The different thermodynamic form of sodium bromine concentration employed to get cobalt oxide, NaCoO2, is obtained by the correct Na content to yield heating sodium and cobalt oxides at 500 superconductivity seems to be more 2 degrees in oxygen . NaCoO2, which is critical in the case of three-layer isostructural with α-NaFeO2, has three NaxCoO2 than in two-layer NaxCoO2. (3) sheets of edge shared CoO6 Figure 1 shows powder X-ray octahedra per unit cell, displaced Diffraction patterns (Cu Kα radiation) of laterally from each other. The sodium the three-layer compounds O3 NaCoO2, ions are only on one crystallographic Na0.30CoO2, and the “intermediate site, in octahedral (O) coordination to hydrate” of three-layer O3 Na0.30CoO2. the oxygen atoms, and hence the The overall chemical behavior of the nomenclature O3 (octahedra, 3 layer) is three-layer system on deintercalation of used to describe the structure of Na and intercalation of water is very NaCoO2. It is this three-layer similar to that observed in the two-layer octahedrally coordinated Na phase that sodium cobaltate. The c lattice parameter is the host compound for the new of O3 NaCoO2 expands on superconductor described here. The P2 deintercalation of Na to Na0.3CoO2, as is and O3 structures of NaxCoO2 are also seen on deintercalation of two-layer compared in figure 1. P2 Na0.7CoO2. Similar to the case for P2 O3 NaCoO2 was synthesized by Na0.7CoO2, an intermediate hydrate is an adaptation of the procedure used by obtained in the O3 system by drying a 3 Wiley and Cushing . A 15% excess of water washed sample of Na0.30CoO2 at NaOH pellets (EM Science, 97% room temperature. In the intermediate minimum purity) and stiochiometric hydrates (also called “monolayer amounts of Co metal sponge (Johnson hydrates”), the water molecules are in Matthey, Grade I) were mixed in a dense the same layer as the sodium ions, alumina crucible, followed by heating in increasing the c-axis of Na0.30CoO2 due O2 at 500 degrees for 12 h. The fused to their larger size. The new mixture was ground and annealed at 800 superconducting superhydrate (also degrees for 16 h in N2 to yield a gray called “bilayer hydrate”, two layers of crystalline powder. The powder was then water molecules are found between the finely ground and treated with Br2 CoO2 sheets) in the three-layer cobaltate concentration of 40x (1 x is the was synthesized by exposing anhydrous theoretical amount of Br2 needed to O3 Na0.30CoO2 to water vapor in a remove all the Na in NaCoO2) in humidity chamber with 100% relative CH3CN for 5 days. The product was humidity at room temperature for 1 to 6 washed in dry CH3CN and dried in an days. It may also be synthesized from 2 Na0.3CoO2 washed in water and superhydrates at low temperatures. The subsequently exposed to water vapor in a lowest temperature weight losses are 100% relative humidity chamber at room very similar, representing the temperature. We have found the former evaporation of surface water. The hump method to be the more satisfactory of the at intermediate temperatures represents two. the water loss on decomposition of the The hydration chemistry of the superhydrate to the intermediate hydrate. three-layer superconductor was studied From the weight loss observed, and the by Thermogravimetric Analysis (TGA). known formula of the intermediate The inset to figure 1 shows the change in hydrate, the formula for the weight for anhydrous three-layer superconducting superhydrate can be Na0.3CoO2 on exposure to a stream of determined to be Na0.30CoO2·1.3H2O (in wet oxygen at approximately 40% both cases). Looking carefully at the relative humidity. The gain in weight inset to figure 2 it is can be seen that that represents the uptake of water. X-ray the three-layer superconducting diffraction analysis of the product superhydrate decomposes to the showed it to be the intermediate hydrate intermediate hydrate at 35 degrees, five phase, yielding from the measured degrees lower than the decomposition weight gain a formula for the three-layer temperature of the two-layer intermediate hydrate of superconductor, indicating that it is even Na0.3CoO2·0.60H2O, in agreement with less thermally stable than that phase, the formula proposed for the essentially barely stable at ambient intermediate hydrate for the two-layer temperature. system5. Figure 2 shows the change in Extreme care must be taken in weight for the three-layer handling three-layer Na0.30CoO2·1.3H2O, superconducting Na0.3CoO2·xH2O as it decomposes fully to the superhydrate on heating very slowly in intermediate hydrate after about 6 flowing O2. The behavior on heating is minutes exposure to 40% relative generally quite similar to that of the two- humidity air at ambient temperature. X- layer superconductor, but with ray diffraction (XRD) characterization of significant differences. Water is lost in a three-layer Na0.30CoO2·1.3H2O was series of steps on increasing temperature. therefore carried out in a sample holder The lowest temperature weight losses that maintained the relative humidity represent the evaporation of intergrain around the sample at 100%. Figure 3 (surface) water, and the decomposition shows the XRD pattern of the three-layer of the superhydrate to the intermediate superconductor compared to that of the hydrate. The plateau in weight from 35 two-layer superconductor. As the o to approximately 50 C represents the distances between the CoO2 sheets of the stability region of the intermediate two superconductors are almost equal, hydrate Na0.3CoO2·0.60H2O. This defining the crystallographic c axis, the compound loses water in steps until first three (00l) peaks are found at the decomposition to Na0.5CoO2 and Co3O4 same diffracted angles for both phases. at 300oC. The inset to figure 2 compares However, on examining the higher angle the details of the weight loss peaks (inset), clear differences are seen characteristics of the two-layer and in the patterns, allowing unambiguous three-layer superconducting distinction between the two phases and 3 the purity of the synthesized three-layer characterization of the material indicated phase. The X-ray diffraction pattern can that the three-layer Na0.30CoO2·1.3H2O be indexed by the same R-3m space superconducting phase is present and group as the parent O3 NaCoO2 phase. single-phase to our experimental Clearly, the room temperature chemistry sensitivity for the duration of these performed on the three-layer O3 experiments. Therefore the chemical NaCoO2 host sodium cobalt oxide to changes that are taking place to yield the prepare the superhydrate superconductor observations in figure 4 do not involve does not provide sufficient energy to decomposition of the superconducting rotate the CoO6 octahedra from their phase but rather subtle structural or orientations in O3 NaCoO2, allowing the chemical changes.
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