Hydrothermal Synthesis and Crystal Structure of a (Ba0.54K0.46

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Hydrothermal Synthesis and Crystal Structure of a (Ba0.54K0.46)4Bi4O12 Double-Perovskite Superconductor with Onset of the Transition Tc ∼ 30 K Md Saiduzzaman,† Hikaru Yoshida,† Takahiro Takei,† Sayaka Yanagida,† Nobuhiro Kumada,*,†,‡ Masanori Nagao,† Hisanori Yamane,§ Masaki Azuma,⊥ Mirza H. K. Rubel,∥ Chikako Moriyoshi,¶ and Yoshihiro Kuroiwa¶ Downloaded via NOTTINGHAM TRENT UNIV on August 30, 2019 at 22:44:21 (UTC). See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.

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Center for Crystal Science and Technology, University of Yamanashi, 7-32 Miyamae-cho, Kofu 400-8511, Japan Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan ⊥ Laboratory for Materials and Structures, Tokyo Institute of Technology, 4259 Nagatsuta, Midori, Yokohama 226-8503, Japan ∥ Department of Materials Science and Engineering, University of Rajshahi, Rajshahi 6205, Bangladesh ¶ Department of Physical Science, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima, Hiroshima 739-8526, Japan §

S Supporting Information *

Ba1−xKxBiO3 (x = 0.35) perovskite via a hydrothermal method at 180 °C with Tc ∼ 22 K.14 Recently, our research group hydrothermally synthesized a Na-incorporated (A-site) BKBObased superconducting double perovskite, (Na0.25K0.45)(Ba1.00)3(Bi1.00)4O12, at 220 °C with Tc ∼ 27 K.10 Later, we hydrothermally synthesized12 another double perovskite, (K1.00)(Ba1.00)3(Bi0.89Na0.11)4O12, at 240 °C with a higher Tc of ∼31.5 K by incorporating the same element (Na) at the other site (B site) of BKBO. The above-mentioned superconducting double perovskites10,12,18 were prepared by using NaBiO3·nH2O as the starting material. While KBiO3 was used for the synthesis of our new BKBO double-perovskite superconductor, this is the first reported superconducting BKBO that has a double-perovskite-type structure. This double perovskite BKBO has superconducting properties with Tc ∼ 30 K, which is higher than that of the previously reported14 BKBO simple perovskite (Tc ∼ 22 K) prepared via hydrothermal reactions. Although the Tc value of this new bismuthate is still low compared to that of cuprate superconductors,19 this material allows us to explore the relationship between superconductivity and long-range ordering. The discovery of this BKBO superconductor also represents a significant advancement for exploring new or additional Bi-based hightemperature superconductors via hydrothermal reactions and is likely to have broad interest in inorganic chemistry. We compare the synthesis conditions and superconducting properties of our previously reported10−13,18 hydrothermally synthesized BKBO-based perovskite superconductors in Table S1. Herein, we describe the hydrothermal synthesis procedure of a new Bi-based double perovskite, (Ba0.54K0.46)4Bi4O12, superconductor with crystal structure refinement and superconducting properties including magnetic susceptibility, electrical resistivity, and isothermal magnetization as well as firstprinciples calculations.

ABSTRACT: A new superconducting double perovskite was successfully synthesized by a low-temperature hydrothermal reaction at 240 °C. The crystal structure refinement of this double perovskite was done by singlecrystal X-ray diffraction, and it had a cubic unit cell of a = 8.5207(2) Å with space group Im3̅m (No. 229). This superconducting double-perovskite chemical composition was estimated by electron probe microanalysis and was similar to the refined data. The superconducting transition temperature of the double perovskite was ∼30 K; the electrical resistivity began to fall at ∼25 K, and zero resistivity occurred below 7 K. Moreover, temperaturedependent resistivity under various magnetic fields and isothermal magnetization measurements ensured the nature of a type II superconductor for the sample. Finally, the metallic nature of the material was investigated by a first-principles study.

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ince its discovery, a Cu-free Bi-based superconducting simple cubic Ba1−xKxBiO3 (BKBO, x = 0.4)1 perovskite (ABO3) with Tc ∼ 30 K has attracted much research interest2−9 to increase its transition temperature (Tc) by partial replacement of the A and/or B site(s).10−13 Not only the incorporated elements but also the starting materials, reaction temperature, and synthesis route influence the superconducting properties of BKBO perovskites.10−17 Generally, BKBO-based perovskites are prepared by solid-state reactions,1,2 hydrothermal reactions,10−14 and high pressure.8,15−17 Previously, our research group18 hydrothermally synthesized a superconductive BKBO-based double perovskite, (Ba0.75K0.14H0.11)BiO3·nH2O, at 180 °C with Tc ∼ 8 K. However, the superconducting properties of this compound were difficult to determine because it had less than a 1% superconducting volume fraction. Later, Zhang et al. synthesized another superconductive simple cubic © XXXX American Chemical Society

Received: June 14, 2019

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DOI: 10.1021/acs.inorgchem.9b01768 Inorg. Chem. XXXX, XXX, XXX−XXX

Communication

Inorganic Chemistry

In the crystal, the A site was partly filled by Ba and K atoms, and the B site cannot be occupied by either a Ba or K atom because of their larger ionic radii. Thus, Bi atoms completely filled the B site. The final chemical composition (Ba0.54K0.46)4Bi4O12 of the cubic double-perovskite structure was estimated from single-crystal XRD refinement data and was approximately close to the composition (Ba0.57K0.43)4Bi4O12 obtained from electron probe microanalysis (EPMA). The detailed crystal data, structural parameters, and Uaniso (Å2) are summarized in Tables S2− S4, respectively. In addition, iodometric titration data ensured the presence of a mixed Bi valence (Bi5+ and Bi3+) in the sample, and the mean Bi valence was found to be 4.41, which was close to that obtained from the EPMA data. The lattice parameter derived from single-crystal refinement was a = 8.5207(2) Å, which was similar to that of (K 1.00 )(Ba1.00)3(Bi0.89Na0.11)4O12 [a = 8.52933(2) Å] of the superconducting double perovskite12 but slightly smaller than the (Na0.25K0.45)(Ba 1.00)3(Bi1.00)4O12 lattice parameter [a = 8.5493(5) Å] because of the lower Bi valence (4.35) of this reported10 sample. The crystal structure of the double perovskite (Ba0.54K0.46)4Bi4O12 had two different A sites (2a and 6b), as depicted in Figure 3, similar to earlier reports of super-

Figure 1a shows the X-ray diffraction (XRD) pattern of the hydrothermally prepared sample at 240 °C was indexed as a

Figure 1. (a) XRD pattern of the (Ba0.54K0.46)4Bi4O12 sample, (b) SEM image, and (c) elemental mapping.

cubic cell (space group Im3̅m, No. 229), which resembled that of double-perovskite oxides.10,12,20−22 However, samples synthesized at 180, 200, and 220 °C also exhibited a doubleperovskite structure, as presented by the XRD patterns (Figure S1), but there were fewer particles with a large cubic shape than the sample synthesized at 240 °C (Figure S2). Moreover, the observed superconducting transition temperature (Tc) and the diamagnetic signals of samples prepared at 180, 200, and 220 °C were also lower and inferior compared to those of the sample prepared at 240 °C (Figure S3). Thus, only the large cubic crystals have superconducting properties, and the small cubic crystals were responsible for the shoulder peaks that appeared on the synchrotron powder X-ray diffraction (SPXRD) pattern. The sample synthesized at 260 °C was unfavorable for obtaining a perovskite structure because of impurity phases (Figure S1). Elemental mapping (Figure 1b,c) showed that a large cubic particle of ∼18 μm exhibited uniform arrangements of the Ba, K, Bi, and O atoms in the microscopic range. Rietveld refinement of the powder sample was performed considering that the double-perovskite-type (A′A″)4B4O12 phase had the same symmetric space group (Im3̅m, No. 229) as that mentioned in earlier reports.10,12 However, it was very difficult to achieve good fitting using the SPXRD data of the powder sample by the Rietveld refinement method because of the presence of a significant number of shoulder peaks (Figure 2) in the double-perovskite structure, which led to a higher Rwp (16%) value. Thus, we refined the large cubic single crystal based on single-crystal XRD, which has been shown to possess superconducting properties. The R1 and wR2 values of the refinement were 0.0078 and 0.0136 (all data), respectively.

Figure 3. Crystal structure of the double perovskite (Ba0.54K0.46)4Bi4O12 sample. The Bi makes a corner-sharing (BiO6) octahedral at the 8c site.

conducting double perovskites.10,12 In the structure, the 2a and 6b sites were randomly occupied by Ba and K; the 6b sites were partly occupied by both Ba and K with a 50%−50% distribution, and the 2a sites were occupied by Ba (67.3%) and K (32.7%). Moreover, the Ba/K−O distance at the 2a site was 3.013(17) Å, while at the 6b site, it was 3.01(17) Å. The Ba/ K−O distances were 3.0285(8) and 3.0434(8) Å for Ba0.6K0.4BiO3 and Ba0.63K0.37BiO3 simple perovskites, respectively,1,23 which were slightly higher than that of our synthesized sample. The Bi−O bond distance of 2.130(6) Å was lower compared to that of the simple BKBO perovskites1,23 [2.141(6) and 2.152(6) Å for Ba0.6K0.4BiO3 and Ba0.63K0.37BiO3] because of the higher K content.24 The Bi−O bond length of our synthesized double perovskite is close to those of previously superconducting double perovskites [2.137(16) Å for (Na 0.25 K0.45 )(Ba 1.00 )3 (Bi1.00) 4O 12 and 2.134(3) Å for (K1.00)(Ba1.00)3(Bi0.89Na0.11)4O12].10,12 The temperature dependence of the magnetic susceptibility graph is displayed in Figure 4 for the (Ba0.54K0.46)4Bi4O12 sample, in both the zero-field-cooled (ZFC) and field-cooled (FC) processes with H = 10 Oe. The shielding volume fractions were measured from the magnetization unit (emu) utilizing the density, obtained from the refinement data. The

Figure 2. Refinement pattern for the highest Tc sample from the SPXRD data. Up and down ticks indicate the locations for the doubleperovskite structure (Ba0.54K0.46)4Bi4O12 and the simple perovskite (Ba0. 96Bi0. 86O2. 59(OH)0.41, respectively. B

DOI: 10.1021/acs.inorgchem.9b01768 Inorg. Chem. XXXX, XXX, XXX−XXX

Communication

Inorganic Chemistry

temperature range of 250−25 K, in which the temperature dropped at ∼25 K and zero resistivity (T0c ) was attained at a comparatively low temperature of ∼7 K. This semimetallic behavior of the resistivity could be due to the high-pressure pressing and/or grain boundaries, which was also noticed in earlier reports.10−13 However, the density of states (DOS) calculations (Figure 6a) showed a metallic behavior with dispersion bands crossing

Figure 4. Direct-current magnetic susceptibility on the temperature dependence for the (Ba0.54K0.46)4Bi4O12 sample in an external magnetic field of 10 Oe.

shielding volume fraction of ∼121% obtained at 5 K, with a marked drop at approximately ∼30 K, is called onset of the transition. Tmag is similar to Tmag from simple BKBO perovskite c c prepared by solid-state reactions.1 On the other hand, the FC curve related to a Meissner signal of ∼15% at 5 K is considerably less than the ZFC value. The variation between the ZFC and FC data may be due to the strong vortex pinning during the FC process.10−13 The Meissner volume fraction (∼15% at 5 K) 25,26 and/or large shielding volume fraction12,13,27 indicate bulk superconductivity, which exceeds 100% perhaps by not including the demagnetization effect.26,27 The diamagnetic signal curves for both the FC and ZFC processes of our synthesized sample are not typical curves compared with other superconducting BKBO-based perovskites,10−13 which could be attributed to the presence of two polycrystalline phases. We assumed that another polycrystalline phase could be hydrothermally prepared in a nonsuperconducting simple perovskite phase (30 wt %), Ba0. 96Bi0. 86O2. 59(OH)0.41.28 This kind of irregular ZFC curve was also observed for rare-earth-doped CaFe2As2 and Ca intercalates of MoS2 superconductors,29,30 probably because of the mixed superconducting and nonsuperconducting phases. Samples synthesized at 180, 200, and 220 °C also displayed shielding volume fractions of approximately 9%, 46%, and 60% at 5 K with onsets of the transition Tmag of c approximately 8, 26.5, and 28 K, respectively (Figure S3). Figure 5a shows the temperature dependence of the electrical resistivity ρ(T) of a pellet sample. The resistivity curve displays a semimetallic nature resembling that of other BKBO-based superconducting double perovskites10,12 over the

Figure 6. (a) Band structure and (b) TDOS and PDOS of the (Ba0.54K0.46)4Bi4O12 sample.

the Fermi level (EF), similar to previously reported BKBObased single- and double-perovskite superconductors.10−13 In Figure 6b, from partial DOS (PDOS), we observe hybridization among the O 2p and Bi 6s and 6p orbitals crossing EF, which agrees well with calculation of the reported superconducting single- and double-perovskite compounds.10−13 Participation of the O 2p orbital is larger compared to that of the Bi 6s and 6p orbitals. However, the Ba 4d and K 4s and 3p orbitals have a trivial contribution in the total DOS (TDOS) at EF of the material. Therefore, the major contribution of TDOS at EF originates from the O 2p and Bi 6s and 6p orbitals, with little contribution from the Ba 4d and K 4s and 3p states. The observed T0c at a low temperature of ∼7 K contrasted with onset of the transition Tonset at ∼25 K could be explained c in terms of the fraction of superconducting clusters present in the prepared sample. The same circumstance was noticed in earlier superconducting double perovskites.10,12 Figure 5b presents the magnetic field dependence of the superconducting nature over an external magnetic field measured in the range 2−10 kOe for the highest Tc sample. It is observed that, with increasing magnetic field, onset of the transition Tconset gradually decreases, but the superconducting nature persists up to a maximum value (10 kOe). This nature provides additional proof of the bulk superconductivity as well as the characteristics of a type II superconductor with a behavior similar to that previously observed for superconducting double perovskites.10,12 Isothermal magnetization (MH) curves of the highest Tc sample recorded from 3 to 35 K (Figure S4) indicated type II superconducting behavior with a lower critical field Hc1 = 119 Oe at 3 K. However, the upper critical field Hc2 was not clearly detected, perhaps because of the existence of an impurity phase (nonsuperconducting) in the hydrothermally prepared sample. At high temperatures (600 °C), this compound completely loses its superconducting properties (Figure S5), probably because of thermal decomposition, leading to impurity phases

Figure 5. (a) Temperature dependence of the electrical resistivity ρ(T) for the (Ba0.54K0.46)4Bi4O12 pellet sample. (b) Resistivity curves under various applied fields in the range from 2 to 10 kOe for the same sample. C

DOI: 10.1021/acs.inorgchem.9b01768 Inorg. Chem. XXXX, XXX, XXX−XXX

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ACKNOWLEDGMENTS The SPXRD experiments at SPring-8 were conducted with permission of the Japan Synchrotron Radiation Research Institute (Proposal 2018A1189). This research work was jointly supported by JSPS KAKENHI Grant 17H03388 and a research project of Materials and Structure Laboratory, Tokyo Institute of Technology.

observed in the SPXRD (Figure S6a). This thermal decomposition started above 300 °C (Figure S6b), and the mass loss was associated with the evaluation of O 2 corresponding to the reduction of Bi5+ to Bi3+ because pentavalent bismuthates are thermally unstable at high temperature.31−33 In summary, for the first time, we report a doubleperovskite-type BKBO superconductor. Structural refinement of the material was done by single-crystal XRD. The shape of the particles was cubic, with a mixture of large- and small-sized particles. The temperature-dependent magnetic susceptibility and electrical resistivity analysis revealed onset of the transition Tmag at ∼30 K and Tonset at ∼25 K. Further, zero resistivity c c occurred under 7 K. The metallicity of the BKBO double perovskite was ensured from band-structure calculations.

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REFERENCES

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ASSOCIATED CONTENT

S Supporting Information *

The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.inorgchem.9b01768. Experimental and computational details, list of hydrothermally synthesized superconducting BKBO-based single and double perovskites with their superconducting properties, all samples’ XRD patterns, SEM images, magnetic susceptibility of all samples, single-crystal data, structural parameters, anisotropic atomic displacement parameters, isothermal magnetization curves, dc magnetic susceptibility at 600 °C, SPXRD patterns at different temperatures, and TG curve (PDF) Accession Codes

CCDC 1860903 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, or by emailing [email protected], or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336033.

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Communication

AUTHOR INFORMATION

Corresponding Author

*E-mail: [email protected]. Phone: +81-55-220-8615. Fax: +81-55-220-8270. ORCID

Md Saiduzzaman: 0000-0001-8003-9914 Takahiro Takei: 0000-0002-5624-2899 Sayaka Yanagida: 0000-0002-4719-5023 Nobuhiro Kumada: 0000-0002-0402-5809 Masanori Nagao: 0000-0002-1139-7838 Hisanori Yamane: 0000-0002-7931-5210 Masaki Azuma: 0000-0002-8378-321X Present Address ‡

N.K.: Center for Crystal Science and Technology, University of Yamanashi, 7-32 Miyamae-cho, Kofu 400-8511, Japan. Author Contributions

The manuscript was written by M.S. with discussion from all the authors. All authors have given permission to the final manuscript. Notes

The authors declare no competing financial interest. D

DOI: 10.1021/acs.inorgchem.9b01768 Inorg. Chem. XXXX, XXX, XXX−XXX

Communication

Inorganic Chemistry (16) Khasanova, N. R.; Izumi, F.; Kamiyama, K.; Yoshida, K.; Yamamoto, A.; Tajima, S. Crystal Structure of the (K0.87Bi0.13)BiO3 Superconductor. J. Solid State Chem. 1999, 144, 205−208. (17) Kim, D. C.; Baranov, A. N.; Kim, J. S.; Kang, H. R.; Kim, B. J.; Kim, Y. C.; Pshirkov, J. S.; Antipov, E. V.; Park, Y. W. High pressure synthesis and superconductivity of Ba1−xKxBiO3 (0.35 < x < 1). Phys. C 2003, 383, 343−353. (18) Jiang, H.; Kumada, N.; Yonesaki, Y.; Takei, T.; Kinomura, N.; Yashima, M.; Azuma, M.; Oka, K.; Shimakawa, Y. Hydrothermal Synthesis of a New Double Perovskite-Type Bismuthate, (Ba0.75K0.14 H0.11)BiO3·nH2O. Jpn. J. Appl. Phys. 2009, 48, No. 010216. (19) Cava, R. J.; Batlogg, B.; van Dover, R. B.; Murphy, D. W.; Sunshine, S.; Siegrist, T.; Remeika, J. P.; Rietman, E. A.; Zahurak, S.; Espinosa, G. P. Bulk superconductivity at 91 K in single-phase oxygen-deficient perovskite Ba2YCu3O9−δ. Phys. Rev. Lett. 1987, 58, 1676. (20) Ganguli, A. K.; Grover, V.; Thirumal, M. New double perovskites having low dielectric loss: LaBaZnTaO6, LaSrZnNbO6 and Ba2Zn0.5Ti0.5TaO6. Mater. Res. Bull. 2001, 36, 1967−1975. (21) Chaillout, C.; Durr, J.; Escribe-Filippini, C.; Fournier, T.; Marcus, J.; Marezio, M. Structure determination of a new perovskite phase in the BaKBiNaO system. J. Solid State Chem. 1991, 93, 63−68. (22) Subramanian, M. A. Ordered Perovskites Containing Pentavalent Bismuth: Ba(Bi0.75M0.25)O3 and Ba(Bi0.67M0.33)O3. J. Solid State Chem. 1994, 111, 134−140. (23) Antipov, E. V.; Khasanova, N. R.; Pshirkov, J. S.; Putilin, S. N.; Bougerol, C.; Lebedev, O. I.; Van Tendeloo, G.; Baranov, A. N.; Park, Y. W. The Superconducting Bismuth-Based Mixed Oxides. J. Low Temp. Phys. 2003, 131, 575−587. (24) Antipov, E. V.; Khasanova, N. R.; Pshirkov, J. S.; Putilin, S. N.; Bougerol, C.; Lebedev, O. I.; Van Tendeloo, G.; Baranov, A. N.; Park, Y. W. The superconducting bismuth-based mixed oxides. Curr. Appl. Phys. 2002, 2, 425−430. (25) Nagamatsu, J.; Nakagawa, N.; Muranaka, T.; Zenitani, Y.; Akimitsu, J. Superconductivity at 39 K in magnesium diboride. Nature 2001, 410, 63−64. (26) Jiang, S.; Xing, H.; Xuan, G.; Wang, C.; Ren, Z.; Feng, C.; Dai, J.; Xu, Z.; Cao, G. Superconductivity up to 30 K in the vicinity of the quantum critical point in BaFe2(As1−xPx)2. J. Phys.: Condens. Matter 2009, 21, 382203. (27) Takenobu, T.; Ito, T.; Hieu Chi, D.; Prassides, K.; Iwasa, Y. Intralayer carbon substitution in the MgB2 superconductor. Phys. Rev. B: Condens. Matter Mater. Phys. 2001, 64, 134513. (28) Jiang, H.; Kumada, N.; Yonesaki, Y.; Takei, T.; Kinomura, N. Hydrothermal synthesis of a new perovskite-type bismuth oxide: Ba0. 96Bi0. 86O2. 59(OH)0.41. J. Ceram. Soc. Jpn. 2009, 117, 214−216. (29) Jung, S. G.; Shin, S.; Jang, H.; Kang, W. N.; Han, J. H.; Mine, A.; Tamegai, T.; Park, T. Manipulating superconducting phases via current-driven magnetic states in rare-earth-doped CaFe2As2. NPG Asia Mater. 2018, 10, 156−162. (30) Zhou, M.; Li, X.; Yang, L.; Dong, C. Synthesis, crystal structure and superconducting properties of calcium intercalates of MoS2. J. Solid State Chem. 2018, 258, 131−137. (31) Saiduzzaman, M.; Yanagida, S.; Takei, T.; Moriyoshi, C.; Kuroiwa, Y.; Kumada, N. Hydrothermal Synthesis, Crystal Structure, and Visible-Region Photocatalytic Activity of BaBi2O6. ChemistrySelect. 2017, 2, 4843−4846. (32) Saiduzzaman, M.; Yanagida, S.; Takei, T.; Kumada, N.; Ogawa, K.; Moriyoshi, C.; Kuroiwa, Y.; Kawaguchi, S. Crystal Structure, Thermal Behavior, and Photocatalytic Activity of NaBiO3·nH2O. Inorg. Chem. 2018, 57, 8903−8908. (33) Saiduzzaman, M.; Takei, T.; Yanagida, S.; Kumada, N.; Wakazaki, S.; Das, H.; Kyokane, H.; Azuma, M.; Moriyoshi, C.; Kuroiwa, Y. Hydrothermal Synthesis of Pyrochlore-Type Pentavalent Bismuthates Ca2Bi2O7 and Sr2Bi2O7. Inorg. Chem. 2019, 58, 1759− 1763.

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DOI: 10.1021/acs.inorgchem.9b01768 Inorg. Chem. XXXX, XXX, XXX−XXX