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Abstract
Optimum conditions for the growing of single crystals of NaMn(PO3)3 compound have been selected. Complete X-ray diffraction analysis has been performed to study synthesized polyphosphate Li2Mn(PO3)4. Structure of the double phosphate belongs to the orthorhombic crystal system, space group Р212121, lattice parameters: a = 14.446(2), b = 14.463(2), c = 14.522(3) Å, V = 3034 Å3, Z = 16, Rhocalc. = 2.757 g/cm3. Structural features of synthesized phosphate have been determined. The compound has been studied using XRD/RSA, DTA and IR spectroscopy techniques along with complete chemical analysis. The crystalline structure of novel double phosphate NaMn(PO3)3 has been determined using X-ray diffraction method. X-ray diffraction analysis of white crystals with rhomboidal habit having size of 0.1 × 0.019 × 0.2 mm has been performed using Siemens P3/PC diffractometer under molybdenum radiation with graphite monochromator. As a result of experiment, 3018 reflections (within 0 ≤ h ≤ 11; 0 ≤ k ≤ 11; -12 ≤ l ≤ 0) have been obtained, of which 2133 independent reflections with F > 4δ(І) have been used for calculations. The integrated intensity has been measured using 2 θ : θ method over the range of angles 4.88 ≤ θ ≤ 50.14 at scan rate of 2–28 degrees per minute. Crystalline lattice parameters have been refined according to 36 reflections within the range of angles 16.0 ≤ θ ≤ 32.0. The final value of the divergence factor is Rw = 0.0547. The crystallization range of new double phosphate NaMn(PO3)3 has been determined in the melts of Na2O–P2O5–Mn2O3 system at a temperature range of 650–900 0С. Furthermore, optimum conditions for the growing of single-crystals of the compound with high yield (over 45 % of weight) have been selected, the series of their physical and chemical properties have been studied and the melting point of the compound has been determined -850 0С. A complete XRD of the synthesized polyphosphate NaMn(PO3)3 has been performed and the special features of its structure have been defined: statistically disordered alkali metal atoms with a characteristic coordination number (6); the record period of repetition of tetrahedra [PO4] in the polyphosphate chains of the structure is 24; the framework of the compound contains “tunnels”, that can be used and modified. These results stimulate further research of the compound and creation of materials on its basis.
References
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