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The Crystal Structures of Namgp04, Na2camg(P04)2 and Nalsca13mgs(P04hs: New Examples for Glaserite Related Structures

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The Crystal Structures of Namgp04, Na2camg(P04)2 and Nalsca13mgs(P04hs: New Examples for Glaserite Related Structures by R. Olden bourg Verlag, Miinchen The crystal structures of NaMgP04, Na2CaMg(P04)2 and NalsCa13Mgs(P04hs: new examples for glaserite related structures J. Alkemper and H. Fuess * Technische Universitar Darmstadt, Fachbereich Materialwissenschaft, Petersenstr. 23, D-64287 Darmstadt, Germany Received October 2nd, 1997; accepted in revised form February 2nd, 1998 Abstract. Three phosphates with (NaMIIp04), composi- polymorphs of NaMgP04 were described (Kapralik, Po- tion have been synthesized and characterized structurally. tancok 1971; Majling 1973; U st'yantsev, Tretnikova, Ke- The low temperature modifications of NaMgP04 and lareva 1976). Na2CaMg(P04h crystallize in the orthorhombic space Brianite, Na2CaMg(P04h. the only intermediate phase group P2j2j2" and the monoclinic space group P21/c, re- in the system NaMgP04-NaCaP04 known by now, was spectively. The phase transitions at high temperature were first described by Fuchs, Olsen and Henderson (1967). investigated by thermal analysis and powder diffractome- Moore (1975) proposed isomorphism with merwinite try. The high-temperature modification of Na2CaMg(P04h (Ca3Mg(Si04h). Ust'yantsev and Tretnikova (1976) de- is isotypic with glaserite, K3Na(S04h as determined by tected a reversible phase transformation at 1113 K and an Rietveld refinement. NajsCa13MgS(P04)IS crystallizes in incongruent melting point at 1493 K. the trigonal space group R3m. The structures of all of Na4Ca4Mg21 (P04) IS, a quarternary oxide with a stoi- these phosphates can be related to the arrangement of ca- chiometry different from the general NaMIIP04 com- tions and phosphate tetrahedra in the glaserite structure. pounds, was synthesized and structurally characterized by Domanskii et al. (1982). Introduction Experimental Whereas the crystal chemistry of silicates of alkaline and alkaline earth metals has extensively been studied the A starting powder for the synthesis of NaMgP04-crystals knowledge of the crystal structures of the corresponding was obtained by heating an equimolar mixture of NaP03 phosphates is rather scarce. As some important biomate- and MgO to 1273 K, cooling to 873 K (5 Klmin) and rials are based on phosphate glass ceramics this lack of holding for 10 h. The powder contained a-NaMgP04, the information constitutes a considerable drawback for the low-temperature modification, and a small amount of further development of these materials (e.g. Vogel, Holand another phosphate, which could not be identified. This 1987; Schulz, Miehe, Fuess, Wange, Gotz 1994; Alkem- powder was then mixed with Na2Mo04 (1: I), heated to per, Fuess 1997). We therefore carried out a program to 1223 K and cooled slowly (10 K/h). After washing with synthesize and to characterize relevant phases which may water the powder contained platelike single crystals of occur in phosphate glass ceramics. a-NaMgP04. Single phase powders could be obtained In the system Na3P04-Ca3(P04h only the structure of by riddling these crystals. one ternary compound, NaCaP0 , was previously deter- 4 Na2CaMg(P04h single crystals were synthesized by mined (Olsen, Bunch, Moore 1977; Ben Amara, Vlasse, mixing NaP03, CaO and MgO in stoichiometric amounts Le FIem, Hagenmuller 1983 a). In the system with Na2Mo04, heating to 1073 K and cooling slowly to Na3P04 - Mg (P0 h three ternary phosphates were re- 3 4 773 K (5 K/h). The Na2Mo04 was removed by washing ported (Majling, Hanic 1976): NaMg (P0 4 4h, with water. In this way a powder with hexagonal Na4Mg(P04h and NaMgP0 . Whereas the structure of the 4 Na2CaMg(P04h- and rhombohedral NalsCaI3Mgs(P04)j8- first is completely known (Ben Amara et al. 1983b), the crystals was obtained. Single phase powders resulted from others were only identified by their powder diffraction pat- riddling the larger Na2CaMg(P04h-crystals. A suitable terns. Indexing for Na4Mg(P04h indicated tetragonal sys- crystal for structure determination had to be selected tem (Ghorbel, d'Yvoire, Dorernieux-Morin 1974) but carefully because the plates were often twinned. failed for NaMgP0 . Using thermal analysis and high-tem- 4 X-ray powder patterns were collected on a STOE perature powder diffraction, up to five high-temperature powder diffractometer in transmission geometry using CuK," I radiation. A position sensitive detector allowed fast * Correspondence author (e-mail: [email protected]) measurements. Structure refinements were performed by Rietveld analysis using FULLPROF (Rodriguez-Carvajal The final atomic coordinates and displacement parameters 1990) for phases with supposed or known structure. Phase are collected in Tables 2-4 I. transformations were observed in-situ using a high tempera- a-NaMgP04 crystallizes in the orthorhombic space tureattachment with Debye-Scherrer geometry. group P2,2,21• The phosphate tetrahedra are near! y re- The data acquisition for single crystal structure deter- gular. Mg is coordinated quadratic pyramidal by five mination was performed using a STOE-STADI-4 diffract- oxygen atoms with distances 1.97 A - 2.18 A. A sixth oxy- ometer with MoKa radiation (scan mode: 28/w = 1/1) at gen atom is shifted to a distance of 2.48 A-2.97 A. The 293 K. Due to the small size of the crystals, long measur- structure is closely related to that of maricite, NaFeP04 ing times and limitations in 28max were inevitable. The (Le Page, Donnay 1977), but there the Fe coordination is structure determination and the refinement were performed slightly distorted but centrosymmetric octahedral. This is with SHELX-86 and SHELXL-93, respectively. the main reason for the symmetry reduction from Pnma Phase transformation temperatures of powders were in the case of NaFeP04 to the subgroup P2,2,2j of detected with heating rates of 5 Klmin using a Setaram NaMgP04. differential scanning calorimeter. a-Na2CaMg(P04h is isotypic with merwmite, Ca2CaMg(Si04h as suggested by Moore (1975). Although Results I Additional material to this paper can be ordered referring to the The crystal structures of NaMgP04, no. CSD 408374 (NaMgP04), CSD 408373 (Na2CaMg(P04)2) and CSD 408372 (NaISCa13Mgs(P04)IS), names of the authors and cita- Na2CaMg(P04h and NalsCa13Mgs(P04hs tion of the paper at the Fachinformationszentrum, Karlsruhe, Ge- sellschaft fur wissenschaftlich-technische Information mbH, D-76344 The details of the single crystal structure data collection Eggenstcin-Leopoldshafen, Germany. The list of Fa/Fe-data is avail- and the structure determination are summarized in Table I. able from the author up to one year after the publication has appeared. Table 1. Details and results of single crystal a-NaMgP0 structure analysis of NaMgP04, 4 Na2CaMg(P04)2 and NalsCa13Mgs(P04)IS. Crystal colorless prism colorless hexagon colorless rhombohedron Crystal size 0.14 x 0.20 x 0.24 mm 0.20 x 0.20 x 0.07 mm 0.12xO.18xO.21 mm 1 I f1 9.35cm- 17.46 cm- 17.39 cm-I 28max 70° 70° 60° N (hkl) unique 3982 2792 1674 N (param )refined 190 128 135 Crystal system, SG orthorhombic, monoclinic, trigonal P212121 (No. 19) P21/c (No. 14) R3m (No. 166) a 8.828(2) A 9.120(3) A 15.811(3) A b 6.821(2) A 5.198(2) A 15.811(3) A c 15.250(4) A 13.370(4) A 21.499(4) A 90.78° 918.3(4) A3 633.8(4) A3 4644(4) A3 4 4 3 0.049 0.040 0.039 0.167 0.119 0.135 Table 2. Final atomic coordinates (- 104) 2 Atom x y c , U Un U U23 UI3 UI2 and displacement parameters (A . 103) for II 33 a-NaMgP0 . 4 Na(l) 1427(1) 2941(2) 5938(1 ) 8(1) 12(1) 9(1) -2(1) 0(1) -1(1) Na(2) 1494(2) 2196(2) 2617(1 ) 12(1) 17(1) 7(1)7 0(1) -1(1) -1(1) Na(3) 1484(2) 2324(2) -715(1) lI(1) 20(1) 9(1) 2(1) 0(1) 3(1) Mg(l) 4867(1 ) 4529(1 ) 2604(1 ) 7(1) 6(1) 6(1) -2(1) -2(1) 0(1) Mg(2) 4804(1) 415(1) 5960(1 ) 8(1) II (I) 8(1) 2(1) -3(1) -2(1) Mg(3) 4959(1 ) 247(1 ) 9218(1 ) 6(1) 13(1) 6(1) 3(1) -2(1) -2(1) P(I) 3204(1) 2184(1 ) 992(1) 2(1) 5(1) 3(1) 0(1) -1(1) -1(1) P(2) 3200(1) 2755(1 ) 7646(1 ) 3(1) 5(1) 2(1) 0(1) 0(1) 0(1) P(3) 3163(1 ) 2559(1) 4332(1 ) 3(1) 10(1) 3(1) 2(1) 0(1) 0(1) 0(1) 3845(2) 3964(3) 1476(1) 12(1) 5(1) 5(1) 0(1) -3(1) -2(1) 0(2) 3559(2) 4435(3) 4835(1) 8(1) II (1) 8(1) -2(1) -3(1) -2(1) 0(3) 3839(2) 4581(3) 8093(1) II (I) 9(1) 7(1) -3(1) -4(1) -4(1) 0(4) 1439(2) 2294(3) 1016(1) 3(1) 13(1) 7(1) 1(1) 1(1) 2(1) 0(5) 3805(2) 2157(3) 49(1) 6(1) 14(1) 5(1) -2(1) 1(1) 1(1) 0(6) 1439(2) 2861(2) 7665(1 ) 2(1) 5(1) 9(1) 0(1) -1(1) 0(1) 0(7) 3782(2) 2581(3) 3388(1 ) 7(1) 17(1) 4(1) 1(1) 2(1) 0(1) 0(8) 1404(2) 2347(3) 4334(1 ) 3(1) 12(1) 7(1) 2(1) 1(1) 3(1) 0(9) 3677(2) 939(3) 8160(1 ) II (I) 10(1) 10(1) 2(1) -4(1) 3(1) 0(10) 3666(2) 327(3) 1490(1) II (I) 5(1) 13(1) 1(1) -6(1) -1(1) 0(11) 3860(2) 817(3) 4810(1 ) 8(1) 13(1) 9(1) 4(1) -3(1) 1(1) 0(12) 3812(2) 2688(3) 6693(1 ) 6(1) 13(1) 6(1) -2(1) 2(1) 1(1) Table 3.
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