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Condensed Matter and Interphases
Kondensirovannye Sredy i Mezhfaznye Granitsy https://journals.vsu.ru/kcmf/
Original articles
Original article
https://doi.org/10.17308/kcmf.2021.23/3306
New compounds Li3Ba2Bi3(XO4)8 (X = Mo, W): synthesis and properties
T. S. Spiridonova1 H, A. A. Savina12, Yu. M. Kadyrova13, E. P. Belykh3, E. G. Khaikina13
1Baikal Institute of Nature Management, Siberian Branch of the Russian Academy of Sciences, 6 Sakhyanova str., Ulan-Ude 670047, Republic of Buryatia, Russian Federation
2Skolkovo Institute of Science and Technology,
30 Bolshoy Boulevard, bld. 1, Moscow 121205, Russian Federation
3Dorji Banzarov Buryat State University (BSU),
24a Smolin str., Ulan-Ude 670000, Republic of Buryatia, Russian Federation Abstract
New compounds Li3Ba2Bi3(XO 4)8 (Х = Mo, W) were obtained by the ceramic technology. Those are the first representatives of the ternary molybdates and tungstates Li3Ba2R3(XO4)8 family, which contain different from the rare earth elements trivalent metal. The sequence of chemical transformations occurring during the Li3Ba2Bi3(WO4)8 formation has been established. The primary characterization of the obtained phases was carried out and their ion-conducting properties were studied. The synthesized compounds are shown to melt incongruently, isostructural to the lanthanide-containing analogues (structural type of BaNd2(MoO4)4, sp. gr. C2/c) and crystallize in the monoclinic crystal system with unit cell parameters а = 5.2798(1), b = 12.8976(4), c = 19.2272(5) A, b = 90.978(2)° (Х = Mo), а = 5.2733(2), b = 12.9032(4), c = 19.2650(6) A, b = 91.512(3)° (Х = W). Li3Ba2Bi3(XO4)8 are found to undergo the diffuse first-order phase transitions at 441°C (molybdate) and 527°C (tungstate), after that their conductivity reaches values of 10-3-10-4 S/cm.
Keywords: triple molybdates and tungstates, solid-state synthesis, powder X-ray diffraction study, thermal properties, ionic conductivity
Acknowledgements: the work was carried out in accordance with the state assignment of the BINM SB RAS and with partial support from the Russian Foundation for Basic Research (project No. 20-03-00533).
For citation: Spiridonova T.S., Savina A.A., Kadyrova Yu. M., Belykh E. P., Khaikina E. G. New compounds Li3Ba2Bi3(XO4)8 (X = Mo, W): synthesis and properties. Kondensirovannye sredy i mezhfaznye granitsy = Condensed Matter and Interphases. 2021;23(1): 73-80. https://doi.org/10.17308/kcmf.2021.23/3306
Для цитирования: Спиридонова Т. С., Савина А. А., Кадырова Ю. М., Белых Е. П., Хайкина Е. Г. Новые соединения Li3Ba2Bi3(XO4)8 (X = Mo, W): синтез и свойства. Конденсированные среды и межфазные границы. 2021;23(1): 73-80. https://doi.orgj/10.17308/kcmf.2021.23/3306
И Tatyana S. Spiridonova, e-mail: spiridonova-25@mail.ru © Spiridonova T.S., Savina A.A., Kadyrova Yu. M., Belykh E. P., Khaikina E. G., 2021
The content is available under Creative Commons Attribution 4.0 License.
T. S. Spiridonova et al.
Original articles
1. Introduction
Currently, the class of ternary molybdates includes more than 700 representatives, characterized by a large stoichiometric and structural diversity, and belongs to the most dynamically replenished groups of complex oxide compounds containing a tetrahedral anion and three different cations. Triple molybdates of different valence metals not only have a high material science potential, but also due to the wide possibilities of varying the elemental and quantitative compositions are convenient model objects for establishing genetic relationships in the series of composition - structure - properties of compound - properties of materials. A significant place among them is occupied by the family of triple molybdates obtained for all lanthanides and yttrium with the composition Li3Ba2R3(MoO4)8, belonging to the structure type BaNd2(MoO4)4 (sp. gr. C2/c, Z = 2) and related to scheelite. These compounds are shown to possess promising luminescent and generation properties [1-3], as well as the properties of solid electrolytes [1, 4]. In particular, the obtained results aimed at study of Li3Ba2R3(MoO4)8 (R = La, Gd, Y) doped with Eu3+, Tb3+, Er3+, Nd3+, indicate the prospects for their use as new photo- and IR-luminophores and laser materials [2, 5-7]. Since 2009, studies on the preparation of ternary tungstates of lithium-barium-lanthanides, isoformular and isostructural to the Li3Ba2Ln3(MoO4)8 which are, like them, are of great not only scientific but also practical interest started to appear [8-17]. Sizes and quality of grown crystals Li3Ba2Ln3(WO4)8 (Ln = La, Gd, Y) [9-12, 18] doped with Nd3+, Eu3+, Tm3+ and other ions, allowed proceeding to a detailed study of the optical-generation characteristics of these new highly efficient laser media. Ceramics Li3Ba2La3(WO4)8: Eu3+ [8] and Li3Ba2Gd3(WO4)8: Tb3+ [15] can be used as red and green luminophores, respectively.
In this study, the first representatives of the considered family of phases containing in their composition a different from the rare earth trivalent element - ternary bismuth - containing molybdate and tungstate of composition Li3Ba2Bi3(XO4)8 (X = Mo, W) were obtained by directed solid state synthesis. The primary characterization of the obtained compounds was carried out and their electrophysical properties were studied.
2. Experimental
Industrial reagents Li2MoO4, Li2WO4, XO3 (X= Mo, W), Bi2O3, BaMoO4, BaCO3 (chemically pure) were used as source components for the synthesis of Li3Ba2Bi3(XO4)8 (X = Mo, W). BaWO4 was obtained by annealing of the stoichiometric mixture of BaCO3 and WO3 (600-850 °C, 70 h), Bi2(MoO4)3 -by the reaction: Bi2O3 + 3MoO3 = Bi2(MoO4)3 (450500 °C, 50 h). Tertiary bismuth tungstate does not exist; it could not be obtained by the solid-state method, as it was shown in the literature data [19] and proved by our unsuccessful attempts to synthesize those. Therefore, in this case the source component was an oxide mixture of Bi2O3 and WO3. AXO4 (A = Ca, Sr, Cd, Pb; X = Mo, WAT), required to study of the possibility of realizing the considered structure in ternary molybdates and bismuth tungstates with complete or partial substitution of barium by another doubly charged cation, were obtained by the interaction of ACO3 (chemically pure and analytical grade) and XO3 by the reaction ACO3 + XO3 = AXO4+ CO2. The3 synthesis conditions were as follows: in case of Ca, Pb - 500-650 ° C, Sr - 500-750 ° C, Cd - 450-500 °C for 50-60 h; tungstates: Ca, Sr - 600-900 °C, Cd - 500-650 ° C, Pb - 500-750 °C for 70-80 h. The single-phase of the synthesized materials was monitored by powder X-ray diffraction analysis. The obtained compounds were identified by comparison with the ICDD PDF-2 database [20].
Powder X-ray diffraction analysis (XRD) was performed using a Bruker D8 ADVANCE diffrac-tometer (1CuKa, secondary monochromator, scanning step 0.02076°). Unit cell parameters of poly-crystalline samples Li3Ba2R3(XO4)8 (X = Mo, W) was calculated by the selection of an isostructural compound. Unit cell parameters were refined by the least squares method using the ICDD software package for preparation of the experimental standards. The Smith-Snyder F30 criterion was used as a validation criterion for X-ray patterns indexing [21].
Differential scanning calorimetry studies were carried out using NETZSCH STA 449C synchronous thermal analyser, V.
heat.(cool.)
= 10°/min.
For the ion-conducting properties investigation the ceramic discs Li3Ba2Bi3(XO4)8 (X = Mo, W) were prepared by pressing the powder at 1 kbar and annealing at 680 (X = Mo) or 730 °C (X = W) for 4 hours. The density of the obtained tablets was 90-95 % of the theoretical values. The
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disks were in diameter of 10 mm and thickness of 1.8 mm. In order to prepare electrodes, the surfaces of the disks were coated with colloidal platinum, followed by annealing at 660 (X = Mo) or 710 °C (X = W) for 1 hour. The electrical conductivity measurements of the samples were tested using an impedance meter "Z-1500J" at selected frequencies from 1 Hz to 1 MHz in the temperature range of 200-650 °C (X = Mo) and 300-700 °C (X = W) with heating and cooling rates of 2 deg./min.
3. Results and discussion
In the single-phase polycrystalline state, the triple molybdate Li3Ba2Bi3(MoO4)8 synthesized by annealing of stoichiometric mixtures of Li2MoO4, BaMoO4, and Bi2(MoO4)3 at 450-550 °C for 150 hi, analogous triple tungstate Li3Ba2Bi3(WO4)8 -300 hour annealing of Li2WO4, BaWO4, Bi2O3 and WO3, taken in a molar ratio of 3: 4: 3: 9, at 550700 °C (intermediate homogenization was carried out every 15-20 h).
According to powder XRD data (Fig. 1), the sequence of chemical transformations occurring during the formation of Li3Ba2Bi3(WO4)8 from a
stoichiometric mixture of oxides and tertiary tungstates, can be illustrated by the scheme [22]:
The formation of Li3Ba2Bi3(MoO4)8 most likely also proceeds through the stage of formation of a double lithium-bismuth compound, but due to the close temperature ranges of the formation of intermediate and final products, the appearance of LiBi(MoO4)2 in the reaction mixture was not recorded.
According to the differential scanning calorimetry (DSC) data, the obtained compounds melt incongruently at 756 (X = Mo) and 786 °C (X=W). In addition to BaWO4 and LiBi(WO4)2 and Bi2WO6 the presence of BaMoO4 and LiBi (MoO4)2, tungstate was revealed in the cooled melt of molybdate by XRD analysis.
Fig 1. Powder X-ray diffraction patterns of the reaction mixture Li2WO4+4BaWO4 + 3Bi2O3 + 9WO3, sequentially annealed at different temperatures
Condensed Matter and Interphases / Конденсированные среды и межфазные границы T. S. Spiridonova et al.
2021;23(1): 73-80 Original articles
Powder XRD patterns of Li3Ba2Bi3(XO4)8 (X = Mo, W) were indexed satisfactory under the assumption of isostructurality to lanthanide-containing analogues (in the case of molybdate F(30) = 217.1 (0.0035; 39), tungstate - F(30) = 162.3 (0.0047; 39)). The obtained crystallographic characteristics are shown in Table 1, the results of indexing of Li3Ba2Bi3(WO4)8 are shown in Table 2.
The possibility of realizing a similar structure in ternary bismuth molybdates and tungstates by replacing barium with another double-charged cation A2+ was investigated. However, attempts to synthesize Li3A2Bi3(XO4)8 (A = Ca, Sr, Cd, Pb) were unsuccessful. The compositions Li3Bax gA0 xBi3(MoO4)8 were obtained by the partial substitution of barium with strontium, cadmium,
Table 1. Crystallographic characteristics of Li3Ba2Bi3(XO4)8 (X = Mo, W), sp. gr. C2/c, Z = 2
Compound Unit cell parameters V, Â3
a, Â b, Â c, Â
5.2798(1) 12.8976(4) 19.2272(5) 90.978(2) 1309.12
5.2733(2) 12.9032(4) 19.2650(6) 91.512(3) 1310.38
Table 2. Indexing results of powder X-ray diffraction pattern for Li3Ba2Bi3(WO4)8
20 exp> VI0 d , Â exp h к l д = =20 - 20 , exp calc7 20 exp I/I0 d , Â exp h к l д = =20 - 20 . exp calc
9.191 31 9.6140 0 0 2 -0.014 35.032 1 2.5593 -2 0 2 -0.002
13.723 3 6.4475 0 2 0 -0.009 35.293 1 2.5410 -1 3 5 -0.004
16.539 2 5.3555 0 2 2 -0.013 35.447 16 2.5303 0 2 7 -0.006
18.163 2 4.8802 1 1 0 +0.001 35.527 1 2.5248 2 0 2 -0.008
18.417 18 4.8134 0 0 4 -0.004 35.900 2 2.4994 1 3 5 -0.003
18.637 14 4.7571 -1 1 1 -0.004 36.810 1 2.4397 2 2 0 -0.005
18.857 11 4.7021 1 1 1 -0.004 37.084 1 2.4223 -1 1 7 +0.004
19.501 5 4.5482 0 3 -0.010 37.322 1 2.4074 0 0 8 +0.001
20.184 5 4.3958 -1 1 2 -0.002 38.601 1 2.3305 -1 3 6 -0.014
20.592 1 4.3097 1 1 2 -0.005 38.814 1 2.3182 -1 5 0 +0.007
22.601 10 3.9309 -1 1 3 -0.003 39.056 1L 2.3044 -1 5 1 +0.000
23.032 6 3.8583 0 4 -0.002 39.168 2 2.2981 1 5 1 +0.000
23.148 8 3.8392 1 1 3 -0.004 39.268 3 2.2924 1 3 6 -0.006
25.650 66 3.4701 -1 1 4 +0.002 39.382 5 2.2861 2 0 4 -0.012
26.298 57 3.3861 1 1 4 -0.001 39.819 2 2.2620 2 2 3 -0.010
26.723 16 3.3332 -1 3 0 0.005 39.945 2 2.2551 0 2 8 -0.005
26.943 9 3.3065 0 2 5 -0.005 41.030 1 2.1980 -2 2 4 -0.004
27.059 86 3.2926 -1 3 1 -0.004 41.228 1 2.1879 -1 5 3 -0.006
27.219 100 3.2736 1 3 1 -0.009 41.384 2 2.1800 -1 1 8 -0.003
27.639 8 3.2248 0 4 0 -0.009 41.554 1L 2.1714 1 5 3 -0.011
28.032 11 3.1804 0 4 1 -0.009 41.879 2 2.1553 2 2 4 +0.000
28.172 51 3.1650 -1 3 2 -0.006 41.975 2 2.1506 0 6 0 +0.002
28.464 45 3.1331 1 3 2 +0.000 42.245 1L 2.1375 0 6 1 +0.006
29.167 97 3.0592 -1 1 5 -0.007 42.946 2 2.1042 1 3 7 -0.005
29.880 63 2.9878 1 1 5 -0.003 43.041 1 2.0998 0 6 2 +0.021
29.982 28 2.9779 -1 3 3 -0.002 43.083 3 2.0979 -1 5 4 -0.002
30.402 26 2.9377 1 3 3 -0.001 43.158 1 2.0944 0 4 7 +0.024
31.001 47 2.8823 0 4 3 -0.001 43.378 2 2.0843 -2 2 5 -0.001
31.097 61 2.8736 0 2 6 -0.001 44.391 25 2.0390 0 6 3 -0.003
32.998 8 2.7123 -1 1 6 +0.000 44.584 23 2.0306 0 2 9 -0.008
33.411 14 2.6797 0 4 4 -0.003 44.740 2 2.0239 2 4 1 -0.033
33.781 5 2.6512 1 1 6 -0.012 45.180 12 2.0052 -2 4 2 +0.005
33.985 61 2.6357 2 0 0 +0.000 45.395 2 1.9962 -1 5 5 +0.001
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End of Table 2
20 exp7 VI0 d , Â exp h к l Д = =20 - 20 exp calc7
45.581 15 1.9885 2 4 2 +0.001
45.881 3 1.9762 1 5 5 +0.009
46.136 21 1.9659 -2 2 6 +0.004
46.190 26 1.9637 0 6 4 +0.004
46.363 25 1.9568 -2 4 3 +0.003
46.948 22 1.9338 2 4 3 +0.001
47.077 2 1.9288 0 4 8 -0.014
47.147 9 1.9261 0 0 10 +0.006
47.311 17 1.9198 2 2 6 -0.006
48.018 6 1.8931 -2 4 4 +0.001
48.116 4 1.8895 -1 5 6 +0.000
48.447 3 1.8774 0 6 5 -0.008
48.680 5 1.8689 1 5 6 +0.003
48.771 7 1.8657 2 4 4 +0.004
49.270 11 1.8479 -2 2 7 -0.003
49.347 11 1.8452 0 2 10 -0.004
50.249 1 1.8142 -1 3 9 -0.006
50.481 9 1.8064 -1 1 10 -0.003
50.565 10 1.8036 2 2 7 -0.005
51.066 1 1.7871 1 3 9 -0.001
51.198 25 1.7828 -1 5 7 -0.001
51.391 11 1.7765 1 1 10 -0.003
51.829 24 1.7625 1 5 7 +0.000
52.069 2 1.7550 2 0 8 +0.012
52.558 22 1.7398 1 7 0 -0.007
52.746 8 1.7340 -1 7 1 -0.008
52.826 7 1.7316 1 7 1 +0.000
53.373 4 1.7151 -1 7 2 +0.008
53.558 2 1.7096 1 7 2 -0.001
53.665 2 1.7065 2 4 6 -0.004
54.601 1 1.6794 -1 3 10 -0.007
54.727 1 1.6759 1 7 3 +0.005
55.063 2 1.6664 -2 6 0 +0.005
55.270 7 1.6607 -1 1 11 -0.007
55.526 1 1.6536 0 4 10 0.002
55.627 8 1.6509 -3 1 4 -0.012
55.832 3 1.6453 -2 6 2 -0.045
56.021 2 1.6402 -1 7 4 -0.030
56.133 1 1.6372 2 6 2 -0.005
56.208 5 1.6352 1 1 11 -0.004
and lead in the single-phase state. The solubility limit in similar tungstates was less than 5%.
The ion-conducting properties of the obtained compounds were studied. It was established that Li3Ba2Bi3(XO4)8 undergo phase transformations at 441 (X = Mo) and 527 °C (X = W), which, based on the presence of temperature hysteresis in lg (aT)-(103/T) dependences in the heating -
Original articles
20 exp VI0 d , Â exp h к l Д = =20 - 20 , exp ca,c
56.460 8 1.6285 -2 2 9 -0.006
56.557 2 1.6259 -3 3 0 -0.029
56.627 11 1.6241 3 1 4 +0.009
56.810 4 1.6193 -2 6 3 -0.006
56.869 7 1.6177 3 3 1 +0.006
57.142 6 1.6106 -3 3 2 +0.009
57.309 4 1.6063 2 6 3 +0.000
57.464 8 1.6024 -3 1 5 +0.002
57.651 4 1.5976 3 3 2 +0.003
57.965 5 1.5897 2 2 9 +0.002
58.112 2 1.5860 -3 3 3 -0.001
58.229 7 1.5831 -2 6 4 +0.013
58.287 14 1.5817 -1 5 9 +0.011
58.557 2 1.5750 -2 0 10 +0.006
58.659 4 1.5725 -2 4 8 -0.007
58.727 4 1.5709 3 1 5 -0.013
58.893 13 1.5668 2 6 4 +0.011
59.043 10 1.5632 1 5 9 +0.000
59.148 1 1.5607 -1 3 11 +0.002
59.302 1 1.5570 0 2 12 -0.016
59.704 2 1.5475 -3 1 6 +0.001
59.972 1 1.5412 2 4 8 -0.006
60.070 3 1.5389 0 4 11 0.008
60.210 3 1.5357 -1 1 12 -0.001
60.459 7 1.5300 -2 2 10 +0.000
60.887 1 1.5202 2 6 5 +0.006
61.040 1 1.5168 0 6 9 -0.003
61.181 2 1.5136 1 1 12 +0.001
62.057 7 1.4943 2 2 10 +0.013
62.150 1 1.4923 -2 4 9 +0.005
62.274 1 1.4897 -1 5 10 -0.005
62.368 5 1.4876 0 8 5 -0.004
62.465 1 1.4856 3 3 5 +0.000
63.061 1 1.4729 1 5 10 +0.004
63.220 1L 1.4696 2 6 6 +0.035
63.908 2 1.4555 -1 3 12 +0.000
64.135 1 1.4508 -3 5 1 +0.008
64.475 1L 1.4440 0 2 13 +0.009
64.608 8 1.4414 0 8 6 +0.010
64.832 6 1.4369 0 4 12 +0.003
cooling cycle can be interpreted as the first order diffuse phase transitions. After the transition, the conductivity Li3Ba2Bi3(MoO4)8 reached values of 3.5 10-3 S/cm (640 °C) at Ea = 1.0 eV, Li3Ba2Bi3(WO4)8 - 2.7 10-4 S/cm (700 °C) at Ea = 0.8 eV. Temperature dependence of electrical conductivity of Li3Ba2Bi3(MoO4)8 as an example is shown in Fig. 2. The obtained interdependence
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of the active and reactive components of the electrical impedance for this compound (at temperatures before and after the phase transition), typical for ionic conductors with blocking electrodes is shown in Fig. 3.
4. Conclusions
Thus, the first compounds of Li3Ba2R3(XO4)8 (X = Mo, W) family were obtained with the structure of BaNd2(MoO4)4 (sp. gr. C2/c, Z = 2),
Z = 2), containing different from the rare earth elements a trivalent metal. The sequence of chemical transformations occurring during the synthesis of ternary tungstate of lithium, barium, bismuth from a stoichiometric mixture of tertiary tungstates and oxides was established. Crystallographic and thermal characteristics of Li3Ba2Bi3(XO4)8 (X = Mo, W) were determined and their ion-conducting properties were studied. It was shown that triple molybdates and tungstates
Fig. 2. The temperature dependence of the electrical conductivity for Li3Ba2Bi3(MoO4)8
Fig. 3. Nyquist plot for Li3Ba2Bi3(MoO4)8 at 673 K (a) and 813 K (b)
b
a
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Li3A2Bi3(XO4)8 (A = Ca, Sr, Cd, Pb; X = Mo, W) with the structure BaNd2(MoO4)4 are not formed.
Conflict of interests
The authors declare that they have no known competing financial interests or personal relationships that could have influenced the work reported in this paper.
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Information about the authors
Tatiyana S. Spiridonova, Leading Engineer, Laboratory of Oxide Systems, Baikal Institute of Nature Management, Siberian Branch of the Russian Academy of Sciences (BINM SB RAS), Ulan-Ude, Russian Federation; e-mail: spiridonova-25@mail.ru. ORCID iD: https://orcid.org/0000-0001-7498-5103.
AleksandraA. Savina, PhD in Chemistry, Researcher, Laboratory of Oxide Systems, Baikal Institute of Nature Management, Siberian Branch of the Russian Academy of Sciences (BINM SB RAS), Ulan-Ude and Skolkovo Institute of Science and Technology, Moscow, Russian Federation; e-mail: a.savina@skoltech.ru. ORCID iD: https://orcid.org/0000-0002-7108-8535.
Yulia M. Kadyrova, PhD in Chemistry, Researcher, Laboratory of Oxide Systems, Baikal Institute of Nature Management, Siberian Branch of the Russian Academy of Sciences (BINM SB RAS) and Senior Lecturer of the Department of General and Analytical Chemistry, Faculty of Chemistry, Dorji Banzarov Buryat State University (BSU), Ulan-Ude, Russian Federation; e-mail:yliychem@yandex.ru. ORCID iD: https://orcid. org/0000-0002-0106-8096.
Elena P. Belykh, Master's student, Faculty of Chemistry, Dorji Banzarov Buryat State University (BSU), Ulan-Ude, Russian Federation; e-mail:elena. belych1996@yandex.ru
Elena G. Khaikina, DSc in Chemistry, Head of Laboratory Oxide Systems, Baikal Institute of Nature Management, Siberian Branch of the Russian Academy of Sciences (BINM SB RAS) and Professor of the Department of Inorganic and Organic Chemistry, Faculty of Chemistry, Dorji Banzarov Buryat State University (BSU), Ulan-Ude, Russian Federation; e-mail: egkha@mail.ru. ORCID iD: https://orcid. org/0000-0003-2482-9297.
All authors have read and approved the final manuscript.
Received24 December2020; Approved after reviewing 15 January 2021; Accepted 15 March 2021; Published online 25 March 2021.
Translated by Valentina Mittova Edited and proofread by Simon Cox
