HF‐Free Solid‐State Synthesis of the Oxyfluoride Phosphor K₃MoOF₇:Mn⁴⁺

Abstract

K 3 MoOF 7 :Mn 4+ was synthesized through a facile twostep solid-state synthesis route without using HF. The first step was carried out in copper ampules, which were shut by welding, followed by the second step, a ball milling experiment. The sample was characterized by single-crystal and powder X-ray diffraction, EDX, and luminescence spectroscopy. K 3 MoOF 7 crystallizes in the triclinic space group P1 (no. 2). It features [a]

Synthesis and characterization of K5Sn2OF11

“…O2-Sn1-F1 98.3(2) O1-Sn2-F10 96.1(4) F1-Sn1-F5 170.4 (2) F7-Sn1-F1 83.2(2) O1-Sn2-F6 99.0(4) F9-Sn1-F3 171.1 (2) O2-Sn1-F9 97.4(2) F10-Sn2-F6 95.8(3) Ø 180 173.0 F7-Sn1-F9 84.7(2) O1-Sn2-F4 91.4(4) F1-Sn1-F9 91.4 2F6-Sn2-F4 90.0(3) O2-Sn1-F5 90.8 2O1-Sn2-F8 88.4(4) F7-Sn1-F5 87.6(2) F10-Sn2-F8 86.0(3) F10-Sn2-F4 169.6 3F9-Sn1-F5 90.4(2) F4-Sn2-F8 87.1(2) F6-Sn2-F8 172.1 4O2-Sn1-F3 90.8(2) F10-Sn2-F2 87.0(3) O1-Sn2-F2 171.0 3F7-Sn1-F3 87.0(2) F6-Sn2-F2 89.1(3) Ø 180 170.9 F1-Sn1-F3 90.9(2) F4-Sn2-F2 84. , and O1 are located at special positions on the Wyckoff site 4b, as well as F11 and F12. Furthermore, O2 is located on a special position (Wyckoff site 4a).…”

“…As a consequence, the structural motifs range from 0-dimensional (quasiisolated) units to 3-dimensional networks [1]. Octahedral units like [MoOF 5 ]in K 3 MoOF 7 [2], corner-sharing units like [Eu 2 O 10 F] 5in K 5 Eu 2 FSi 4 O 13 [3], and edge-sharing building blocks like [Ti 2 O 8 F 2 ] 10− in Ba 2 Ti 2 Si 2 O 9 F 2 are observed [4]. These units have a finite length.…”

K2SnOF4 and K2WO3F2 – different but similar

“…For oxidofluoridotungstanates different octahe-dral units have been reported in the literature, e.g., the [WO 4 F 2 ] 4− unit observed within Cs 2 WO 3 F 2 or Ba 2 WO 3 F 4 , the [WO 3 F 3 ] 3− unit observed within K 3 WO 3 F 3 , the [WO 2 F 4 ] 2− unit observed within K 3 HF 2 WO 2 F 4 and A 2 WO 2 F 4 (A = NH 4 , Na, Rb, Cs), and the [WOF 5 ] − unit observed within K 3 WOF 7 , Ag(WOF 5 ) 2 , and (XeF 2 )(WOF 4 ) [2][3][4][5][6][7][8][9][10][11][12][13]. Some of these units, as well as other oxidofluoridometallates exhibiting similar units, recently gained some attention because of the possibility for partial substitution with Mn 4+ which can produce materials exhibiting red luminescence upon blue light excitation [6][7][14][15][16][17][18]. Regarding the [WO 4 F 2 ] 4− unit, which has been observed within the compound Cs 2 WO 3 F 2 by Mattes and Förster, and within Ba 2 WO 3 F 4 by Wingefeld and Hoppe, the octahedral units are connected to infinite chains [2,8].…”

Mn(IV)‐Substituted Metal(II) Hexafluorido Metallates(IV): Synthesis, Crystal Structures, and Luminescence Properties

“…A two‐step route was reported for the syntheses of K 3 M OF 7 : Mn ( M =Mo, W). First, KHF 2 and M O 3 were first heated inside sealed Cu ampoules to obtain K 3 M OF 7 which were then ball‐milled together with K 2 MnF 6 to obtain the phosphors [15,16] . A synthesis of Li 2 SiF 6 : Mn that avoids usage as well as formation of HF was reported.…”