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5Condensed Matter and Interphases (Kondensirovannye sredy i mezhfaznye granitsy)
Original articles
DOI: https://doi.org/10.17308/kcmf.2020.22/2967 ISSN 1606-867X
Received 31.07.2020 eISSN 2687-0711
Accepted 15.08.2020 Published online 30 September 2020
Synthesis and characterisation of ternary molybdates AgZn,R(MoO4)5 (R = In, Fe)
© 2020 I. Yu. KotovaHa, T. S. Spiridonovaa, Yu. M. Kadyrovaa, A. A. Savinab
aBaikal Institute of Nature Management, Siberian Branch of the Russian Academy of Sciences, 6, Sakhyanova str., 670047 Ulan-Ude, Republic of Buryatia, Russian Federation
bSkolkovo Institute of Science and Technology,
30, Bolshoy Boulevard, bld. 1, 121205Moscow, Russian Federation
Abstract
An important role in the study and the obtaining of new phases with valuable physical and chemical properties is taken by ternary compounds with a tetrahedral anion containing various combinations of mono- and multivalent cations, including ternary molybdates and tungstates. Silver ternary molybdates AgA3^(MoO4)5 with the NaMg3In(MoO4)5 structural type (triclinic crystal system, space group PI, Z = 2) are of particular interest and have a high ion conductivity (10-3-10-2 S/cm). In this regard, the aim of this work was to reveal the possibility to form similar compounds in silver, zinc, indium, and iron molybdate and tungstate systems and to determine the effect of the nature of tetrahedral anion and three-charged cations on their obtaining and properties.
Polycrystalline samples were synthesized using a ceramic technology and studied by differential thermal (DTA) and X-ray diffraction analysis (XRD).
The research resulted in obtaining a new ternary molybdates AgZn3R(MoO 4)5 (R = In, Fe) crystallising in the triclinic crystal system (space group PI, Z = 2). The sequence of chemical transformations that occur during the formation of these compounds, their crystallographic and thermal characteristics were determined. Unit cell parameters for the indium compound are as follows: a = 6.9920(4), b = 7.0491(4), c = 17.9196(9) Á, a = 87.692(5), p = 87.381(5), g = 79.173(5)°; and for the iron compound: a = 6.9229(3), b = 6.9828(4), c = 17.7574(8) Á, a = 87.943(4), p = 87.346(5), g = 78.882(5)°. It was established that silver-containing ternary zinc tungstates with indium and iron with a similar structure are not formed. Keywords: ternary molybdates, silver, tungsten, solid-state synthesis, X-ray diffraction analysis (XRD), thermal properties. Funding: The study received financing within the framework of state order No. 0339-2019-0007 to the Baikal Institute of Nature Management, Siberian Branch of the Russian Academy of Sciences. It was partially funded by the Russian Foundation for Basic Research (project No. 16-03-00510 a).
For citation: I. Yu. Kotova, T. S. Spiridonova, Yu. M. Kadyrova, A. A. Savina Synthesis and characterisation of ternary molybdates AgZn3R(MoO4)5 (R = In, Fe). Kondensirovannye sredy i mezhfaznye granitsy = Condensed Matter and Interphases. 2020; 22(3): 336-343. DOI: https://doi.org/10.17308/kcmf.2020.22/2967
Kl Irina Yu. Kotova, e-mail: [email protected]
l@ ® I The content is available under Creative Commons Attribution 4.0 License.
1. Introduction
Currently, a lot of attention is paid to searching, synthesising, and extending the range of application of complex oxide compounds, and using them to develop new materials with functionally relevant properties.
An important role in the study and the obtaining of new phases with valuable physical and chemical properties is given to ternary compounds with a tetrahedral anion containing various combinations of mono- and multivalent cations, including ternary molybdates and tungstates. One of the largest families within this class of compounds are molybdates with one-, two-, and three- charged cations. Silver NASICON-like rhombohedral phases Ag1-xA1-xR1[x(MoO4)3 (A = Mg, Co, R = Al, Sc; A = Mg, R = In) [1 -4] and the triclinic AgA3R(MoO4)5 (A = Mg, R = Cr, Fe, Ga; A = Zn, R = Ga; A = Fe11 , R = Fe111; A = Mn, R = Al, Cr, Fe, Sc, In) [5-10] are of particular interest due to a high ionic conductivity (10-3-10-2 S/cm) [4, 7, 10]. Both structural types occur in systems where two- and three-charged cations tend to have octahedral coordination and the radius of the three-charged cation does not exceed 1 Â.
The characteristic features of the phase formation in systems, where the considered phases are formed are shown in Fig. 1 (by the example of Ag2MoO4-MgMoO4-In2(MoO4)3 [3]). The subsolidus structure of this system is determined by the formation of the NASICON-type ternary molybdates AgMgIn(MoO4)3 (S1) and AgMg3In(MoO4)5 (S2) without any visible homogeneity regions along the section AgIn(MoO4)2-MgMoO4. The phase of variable composition Ag Mg In (MoO^ (S1) is formed along the sectionAgMgIn(MoO4)3-In2(MoO4)3 and is an omission solid solution based on the ternary molybdate AgMgIn(MoO4)3 where homogeneity region is up to x = 0.6.
According to X-ray diffraction analysis (XRD), triple molybdates AgA3R(MoO4)5 are isotypical to NaMg3R(MoO4)5 R = In, Al (triclinic crystal system, space group PI, Z = 2 [11,12]).
Crystals were obtained and their structure was determined for AgMg3R (MoO4)5 ( R = Cr, Fe), AgMnII3(MnIII0 26Al0 74)(MoO4)5, Ag090AlL06Co2.94(MoO4)5, and AgFe^Fe^MoO^ [5-8]. The data from the X-ray powder patterns obtained by a full-profile analysis (Rietveld
method) [13] were used to refine the crystal structures of AgM3Ga(MoO4)5 (M = Mg, Zn) [9, 10].
Research was conducted to reveal a possibility to form similar compounds in silver, zinc, indium, and iron molybdate and tungstate systems and to determine the effect of the nature of tetrahedral anion and three-charged cations on their obtaining and properties.
2. Experimental
The source components were molybdates and tungstates of silver, zinc, and indium iron molybdate obtained by annealing of the stoichiometric mixtures of AgNO3 (analytical reagent grade), ZnO (chemically pure grade), In 2O3 (extra-pure grade), Fe(NO3)3-9H2O (analytical reagent grade), MoO3 (chemically pure grade), and WO3 (chemically pure grade) at 350-450 °C (Ag2MoO4), 500-700 °C (ZnMoO4), 400-800°C (In2(Mo O4)3,300-700 °C (Fe2(MoO4)3), 480-520 °C (Ag2WO4), 650-850 °C (ZnWO4), 700-900 °C (In2(WO4)3). The single-phase of synthesised products was monitored by X-ray analysis and in some cases by thermographic analysis. The synthesised compounds were identified by comparing with the results of previous studies and the ICDD PDF-2 database [14-17].
AgZnR(3O4)5 (R = In, Fe; Э = Mo; R = In, Э = W) samples were prepared from molybdates and tungstates, taken in stoichiometric proportions. Ag2WO4, ZnWO4 WO3 and Fe(NO3)3-9H2O were
A a Mnfl
Fig. 1. Scheme of subsolidus phase relations in the Ag2MoO4-MgMoO4-In2(MoO4)3 system (Sj -Ag^MgJn^MoO^, S2 - AgMg^nCMoO^) [3]
used to synthesize AgZn3Fe(WO4)5, in this case heat treatment started with 350°C.
The mixtures were gradually annealed in air with increments of 20-50 °C (in some cases 5-10°C) starting from 400-450 °C (for molybdates) and 550-600 °C (for tungstates), and finishing before they started to melt with intermediate homogenisation after 20-30 hours. The heat treatment time at each temperature was 30-70 hours. The phase composition of the sintered products was monitored by XRD before the annealing temperature was increased.
X-ray studies of polycrystalline products were carried out using a Bruker automated powder diffractometer D8 Advance (1CuKa, scanning step 0.02076°) and Thermo ARL (1CuKa, scanning step 0.02°). a
Crystallographic characteristics of polycrystalline samples were determined based on isostructural compound data. Unit cell parameters were refined by the least-squares method using ICDD software package to prepare experimental standards. Smith-Snyder criterion F30 [18] was used as a validation criterion for XRD pattern indexing.
Thermoanalytical investigations were performed using a NETZSCH STA 449 F1 Jupiter device (Pt-crucible, heating rate 10 deg/min in a flow of argon).
3. Results and discussion
According to the XRD, the sequence of chemical transformations that occur during the formation of AgZnR(MoO4)5 (R = In, Fe) from a stoichiometric mixture of molybdates can be described in the following scheme:
Ag2MoO4
ZnMoO4
^(MoO4)
Ag R (M0O4 )2 ^ ZnMoO4
AgZn3 R (M0O4 )5 ^ AgZn3 R (M0O4 )5
The primary product of the solid-phase interaction between Ag2MoO4, ZnMoO4 and R2(MoO4)3 (R = In, Fe) is double molybdate AgR(MoO4)2. An increase in temperature to 470-500 °C (R = In) and 420-450°C (R = Fe) leads to the formation of AgZn3R(MoO4)5 in the reaction mixture. In the single-phase state, these compounds were obtained at 650-700 °C (R = In) and 600-650°C (R = Fe). The heat treatment time was 100-120 h. Further annealing only resulted in a better formation of the ternary molybdate structure.
As an example, Fig. 2 shows the AgZn3Fe(MoO4)5 X-ray diffraction pattern.
X-ray diffraction analysis revealed that AgZn3R (MoO4)5 synthesised compounds
2d, degree
Fig. 2. X-ray diffraction pattern for ternary molybdate AgZn3Fe(MoO4)5
are isostructural to each other and to the previously obtained NaMg3R(MoO4)5 [11,12] and AgA^MoO^ [5-10].
The structural features of the considered group of ternary molybdates are that MoO4 tetrahedra and pairs and triplets of (A, R)O 6-octahedra connected along the edges share common vertices and form three-dimensional frameworks. Silver cations disordered over three closely-spaced positions are located in large frame voids.
Crystallochemical analysis of the inner space of the frame revealed the presence of channels located along the a axis, connected with channels along the c axis which contributes to increased ionic conductivity experimentally confirmed in
the case of AgA3R(MoO4)5 (AR = MgAl, MnAl, MnGa) [7,10].
The indexing results of AgZn3R (MoO4)5 (R = In, Fe) powder patterns are shown in Table 1, and their crystallographic characteristics are shown in Table 2 (it also contains previously published data for an isostructural gallium analogue). It is evident that the parameters a, b, and c and the volume of AgZn3R(MoO4)5 unit cells decrease with a decreasing radius of the triply-charged cation.
Thermal characteristics of AgZn3R(MoO4)5 were defined. All phases melt incongruently. The indium compound has the highest thermal stability, with a decrease in the size of the three-charged cation in In3+ - Fe3+ - Ga3+ (rR3+= 0.80, 0.65,
Table 1. Indexing results for AgZn_R(MoO4)s (R = In, Fe) X-ray diffraction patterns
hkl AgZn3In(MoO4y AgZn3Fe(MoO4)5**
20 exp7 I/I0 d , Â exp A = 20 exp 20calc, 20 exp I/I0 d , Â exp A = 20 exp 20calc,
1 2 3 4 5 6 7 8 9
0 0 2 9.878 3 8.95 +0.001 9.966 2 8.87 +0.002
0 1 0 12.929 1L 6.842 -0.014
1 0 0 12.900 9 6.857 -0.010 13.024 6 6.792 +0.009
1 0 1 13.633 1 6.490 +0.005 13.769 1L 6.426 +0.001
-1 0 1 13.989 1 6.326 +0.000 14.148 1L 6.255 -0.002
0 0 3 14.841 2 5.964 +0.001 14.990 1L 5.905 -0.014
0 1 2 15.957 1 5.550 -0.034 16.105 1 5.499 +0.015
1 0 2 -0.001 +0.005
0 -1 2 16.448 1L 5.385 -0.015 16.550 1L 5.352 +0.008
1 1 1 16.874 1 5.250 -0.010 17.027 1L 5.203 -0.022
-1 -1 1 17.370 1L 5.101 +0.027
1 0 3 19.300 1L 4.595 +0.019 19.508 1L 4.547 -0.009
-1 -1 2 19.643 1L 4.516 +0.007 19.779 2 4.485 +0.007
-1 1 0 19.824 1 4.475 +0.005 20.095 1L 4.415 -0.007
0 0 4 +0.009
-1 0 3 20.080 1L 4.418 +0.005 20.291 1L 4.373 +0.007
-1 1 1 20.459 1L 4.337 +0.009
1 1 3 21.549 2 4.120 +0.004 21.751 2 4.083 +0.009
1 -1 2 22.161 5 4.008 -0.002 22.390 6 3.968 +0.005
-1 -1 3 22.789 1 3.899 +0.012
1 0 4 23.306 3 3.814 -0.013 23.507 2 3.781 -0.002
0 1 4 +0.003 23.575 1 3.771 +0.010
0 -1 4 24.017 2 3.702 -0.001 24.190 3 3.676 +0.004
-1 0 4 24.147 4 3.683 +0.002 24.397 1 3.645 +0.003
0 0 5 24.857 100 3.579 +0.005 25.088 100 3.547 +0.002
-1 1 3 25.243 11 3.525 +0.009
1 1 4 25.120 3 3.542 -0.011 25.361 4 3.509 -0.004
0 2 0 25.734 3 3.459 -0.007 25.997 1 3.425 +0.000
Continuation of Table. 1
1 2 3 4 5 6 7 8 9
2 0 0 25.949 51 3.431 -0.003 26.235 52 3.394 +0.003
0 2 1 26.055 35 3.417 -0.004 26.346 28 3.380 +0.002
2 0 1 26.233 10 3.394 +0.001 26.516 10 3.359 +0.004
0 -2 1 26.366 10 3.378 +0.006 26.622 11 3.346 +0.002
-1 -1 4 26.532 5 3.357 +0.019 26.735 3 3.332 +0.010
1 2 0 26.606 7 3.348 -0.023 26.790 1 3.325 +0.007
-2 0 1 +0.016 26.917 4 3.310 +0.007
1 2 1 26.806 16 3.323 -0.006 27.036 12 3.295 +0.002
2 1 1 26.948 2 3.306 -0.006 27.169 2 3.280 +0.011
-1 -2 1 27.303 21 3.264 -0.002 27.503 12 3.240 +0.002
0 2 2 +0.009 27.640 2 3.225 +0.001
-2 -1 1 27.473 2 3.244 +0.001 27.700 2 3.218 +0.008
1 0 5 27.634 2 3.225 +0.006
0 1 5 27.675 4 3.221 -0.005 27.983 6 3.186 +0.006
0 -2 2 27.931 6 3.192 -0.007 28.164 3 3.166 +0.004
1 2 2 +0.007 28.202 2 3.162 +0.005
2 1 2 28.070 2 3.176 -0.011 28.303 1 3.151 +0.010
1 -1 4 28.135 2 3.169 -0.010 28.378 2 3.142 +0.004
-2 0 2 28.188 1 3.163 +0.004 28.504 1 3.129 +0.010
-1 1 4 28.263 1 3.155 -0.010 28.637 9 3.115 -0.011
0 -1 5 28.430 11 3.137 -0.006 +0.002
-1 -2 2 28.887 1 3.088 +0.009 29.101 1L 3.066 -0.002
-2 -1 2 29.088 7 3.067 -0.012 29.314 5 3.044 +0.007
1 1 5 29.168 1L 3.059 -0.037
0 2 3 29.400 3 3.036 -0.002 29.767 3 2.999 -0.002
2 0 3 29.502 1 3.025 -0.001 +0.035
2 1 3 30.002 7 2.976 -0.005 30.270 5 2.950 +0.004
0 -2 3 30.267 1L 2.951 -0.013 30.502 1L 2.928 -0.001
-1 -1 5 30.708 2 2.909 -0.003 30.950 1L 2.887 -0.011
-1 2 0 31.020 1 2.881 -0.007 31.416 1L 2.845 -0.011
-1 -2 3 31.244 2 2.860 -0.001 31.454 2 2.842 +0.002
-1 2 1 31.372 16 2.849 -0.003 31.785 14 2.813 +0.002
-2 -1 3 31.679 1L 2.822 +0.012
2 -1 1 31.474 6 2.840 -0.010 31.859 2 2.807 -0.010
1 -1 5 31.944 2 2.799 -0.013 32.223 1 2.776 -0.011
0 2 4 32.167 3 2.780 -0.002 32.556 6 2.748 +0.015
2 0 4 32.231 5 2.775 +0.001 -0.005
0 1 6 32.642 1 2.741 +0.000
1 2 4 32.552 10 2.788 -0.005 32.883 5 2.722 +0.009
2 -1 2 +0.018 32.926 2 2.718 +0.027
1 -2 2 32.722 5 2.735 +0.006 33.085 4 2.705 +0.002
-2 1 2 33.384 1 2.682 +0.007
2 2 0 33.127 1 2.702 +0.013 +0.012
0 -2 4 33.224 17 2.694 -0.008 33.473 9 2.675 +0.002
2 2 1 +0.018 33.506 4 2.672 +0.006
1 1 6 33.488 1 2.674 -0.010 33.822 1L 2.648 -0.006
-2 0 4 +0.012 33.863 1 2.645 +0.013
-2 -2 1 33.823 8 2.268 -0.013 34.060 4 2.6301 +0.000
The end of the Table. 1
1 2 3 4 5 6 7 8 9
2 2 2 34.120 5 2.626 -0.012 34.398 2 2.6050 +0.002
-1 -2 4 34.203 2 2.619 +0.002 34.434 1 2.6024 +0.003
-2 -1 4 34.398 1 2.605 -0.012
-1 2 3 -0.002 34.873 1L 2.5706 +0.004
2 -1 3 +0.005 34.788 1L 2.5767 -0.002
1 -2 3 34.709 1L 2.582 -0.017 35.041 1L 2.5587 +0.006
-2 1 3 34.926 1L 2.567 +0.011 35.407 1L 2.5331 +0.004
0 0 7 35.064 1L 2.557 +0.016 -0.001
-1 -1 6 +0.018
2 0 5 35.519 10 2.525 -0.011 35.854 7 2.5025 -0.002
2 2 3 35.643 1 2.517 +0.046 36.002 1 2.4925 +0.009
1 2 5 35.711 1 2.512 +0.039 36.139 1 2.4834 +0.000
2 1 5 35.790 1L 2.507 +0.018 +0.011
-1 1 6 36.257 1L 2.4756 -0.009
0 -2 5 36.679 1 2.4481 -0.001 36.968 1 2.4296 -0.011
2 -1 4 36.899 2 2.4340 -0.030 37.233 1L 2.4129 +0.025
-1 2 4 +0.001 37.438 1 2.4002 -0.022
-2 0 5 36.963 11 2.4299 +0.001 37.367 8 2.4046 +0.007
1 -2 4 37.269 4 2.4107 +0.001 37.638 1 2.3879 -0.009
-2 -2 3 +0.005 37.514 1 2.3955 +0.024
-2 1 4 37.545 1L 2.3936 -0.007
-1 -2 5 37.672 1L 2.3858 -0.015
-2 -1 5 37.831 1 2.3761 +0.005 38.165 1 2.3561 -0.003
2 2 4 37.912 3 2.3712 -0.002 38.269 1 2.3499 -0.003
-1 0 7 38.013 1 2.3652 -0.003
1 1 7 38.455 1L 2.3390 +0.000
1 3 1 38.884 1 2.3142 -0.018
0 3 0 39.464 1L 2.2815 -0.028
3 1 1 39.113 1 2.3012 +0.034
0 2 6 39.212 6 2.2956 -0.004 39.702 3 2.2684 -0.002
2 0 6 +0.005 39.605 4 2.2737 -0.013
3 0 0 39.361 4 2.2872 -0.004 39.816 5 2.2621 -0.007
1 2 6 +0.034 +0.015
3 0 1 39.479 2 2.2807 +0.009 39.937 2 2.2556 -0.003
1 3 2 39.619 1L 2.2729 +0.018
-3 -1 1 40.053 1L 2.2493 -0.007
2 -1 5 40.251 1L 2.2387 +0.020
-3 0 1 39.896 5 2.2578 -0.003 40.360 2 2.2329 -0.003
-2 -2 4 +0.013 40.185 1 2.2422 +0.009
-1 2 5 40.499 2 2.2255 -0.013
0 3 2 40.015 4 2.2513 +0.002 -0.004
0 0 8 40.289 5 2.2367 +0.004 40.680 5 2.2161 -0.008
0 -2 6 40.529 3 2.2240 +0.008 40.851 1 2.2072 -0.007
* F30 = 83.2 (0.0075, 48) " F = 96.4 (0.0066, 47)
Table 2. Crystallographic characteristics of AgZn3R(MoO4)5 (R = In, Fe, Ga)
R a, Â b, Â c, Â a° ß° V, Â3
In 6.9920(4) 7.0491(4) 17.9196(9) 87.692(5) 87.381(5) 79.173(5) 866.13
Fe 6.9229(3) 6.9828(4) 17.7574(8) 87.943(4) 87.346(5) 78.882(5) 841.08
Ga [10] 6.9037(3) 6.9639(4) 17.7147(8) 88.107(4) 87.440(4) 78.982(4) 834.87
Fig. 3. A general view of AgZn3Ga(MoO 4)5 structure [10]
0.62 E for CN = 6 respectively [19]) the melting temperature decreases (832°C - 777°C - 644°C).
Despite similar values for Mo (VI) and W (VI) sizes (0.41 and 0.42 E for CN = 4, respectively [19]), ternary tungstates with a similar structure apparently do not exist. All our attempts to obtain AgZn3R(WO4)5 triclinic phases (variation by thermal treatment and heat treatment modes) did not lead to any positive results, which is probably due to a significantly lower susceptibility of W (VI) (as compared to Mo (VI)) to tetrahedral coordination [20].
4. Conclusions
Thus, the possibility to form silver, zinc, and indium (iron) ternary molybdates and tungstates, of the NaMg3In(MoO4)5 structural type (triclinic crystal system, space group PI, Z = 2) were studied for the first time. New ternary molybdates AgZn3R(MoO4)5 (R = In, Fe) were obtained. The sequence of chemical transformations that occur during their synthesis from a stoichiometric mixture of molybdates was determined. The crystallographic and thermal characteristics of synthesized compounds were identified. The frame structure of this group of phases containing connected cavities, the defective
positions of silver cations, their low and open coordination can contribute to the increased Ag-ion conductivity of the received compounds. It was established that such phases do not form in tungsten systems.
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
Irina Yu. Kotova, 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, Russian Federation; e-mail: [email protected]. ORCID iD: https://orcid.org/0000-0003-3829-6516.
Tatiyana S. Spiridonova, Lead 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: [email protected]. ORCID iD: https://orcid.org/0000-0001-7498-5103.
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), Ulan-Ude, Russian Federation; e-mail: [email protected]. ORCID iD: https://orcid.org/0000-0001-7569-6233.
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 Researcher, Skolkovo Institute of Science and Technology, Moscow, Russian Federation; e-mail: [email protected]. ORCID iD: https://orcid.org/0000-0002-7108-8535.
All authors have read and approved the final manuscript.
Translated by Irina Charychanskaya
Edited and proofread by Simon Cox
