Crystal growth experiments in the systems Ni₂MSbO₆ (M = Sc, In) using chemical vapour transport reactions: Ni₂InSbO₆ and NiSb₂O₆ crystals in the millimetre range

Abstract

Endothermic chemical vapour transport (CVT) reactions of Ni 2 MSbO 6 (M = Sc, In), using a temperature gradient T of 1313 → 1233 K and HgCl 2 , HgBr 2 , PtCl 2 or TeCl 4 as transport agents, led to growth of Ni 2 InSbO 6 single crystals in the millimetre range, whereas in the case of Ni 2 ScSbO 6 an incongruent dissolution of the solid in the source region was observed, leading to the formation of single crystals of the ternary phase NiSb 2 O 6 in the sink region. The crystal structures of the obtained crystals were refined from single crystal X-ray data with high precision [Ni 2 InSbO 6 : R3, Z = 3, a = 5.21640(10)Å, c = 14.0142(3)Å, 1279 structure factors, 33 parameters, R[F 2 > 2σ (F 2 )] = 0.0189; NiSb 2 O 6 : P4 2 /mnm, Z = 2, a = 4.63910(10)Å, c = 9.2182(2)Å, 500 structure factors, 19 parameters, R[F 2 > 2σ (F 2 )] = 0.0145]. Ni 2 InSbO 6 crystallizes in a corundum-related structure, NiSb 2 O 6 in the trirutile structure type. Spontaneous polarization and the ferroelectric transition temperature were estimated from the atomic arrangement and cation displacement along the polar axis in Ni 2 InSbO 6 . Magnetic measurements on Ni 2 InSbO 6 evidence an antiferromagnetic transition near T N = 74 K, with significant magnetic frustration.

Local and long-range order and the influence of applied magnetic field on single-crystalline NiSb2O6

“…A handful of publications describe [10][11][12][13] investigations of polycrystalline NiSb 2 O 6 . This investigation adds to the current level of knowledge through magnetization, specific heat, and thermal expansion measurements of singlecrystalline NiSb 2 O 6 .…”

Lattice and magnetic dynamics in the polar, chiral, and incommensurate antiferromagnet Ni2InSbO6

“…No frequency shifts more than 2 cm −1 were observed in angular-resolved measurements which rules out the presence of oblique modes observed for, example, in BiFeO 3 [5]. We suppose that the absence or smallness of the frequency shifts could be due to a small value of the electric polarization 6 µC cm −2 of Ni 2 InSbO 6 [31] in comparison with other polar systems where angular dispersion shifts were clearly observed [52,53].…”

“…Single crystals were grown by the chemical vapor transport method. The powder samples of Ni 2 InSbO 6 were synthesized by solid-phase reaction technique and put into evacuated tube with PtCl 2 as a transport agent [31]. The tube was placed for two weeks in horizontal furnace with temperatures of 1080 • C and 1000 • C for source and growth sides of the tube, respectively.…”

“…Despite being a chiral, Ni 2 InSbO 6 belongs to the achiral trigonal space group R3 (#146, Z = 3 in hexagonal cell) which was determined using the X-ray diffrac-tion [21,31]. According to the group theoretical analysis 18 modes are expected which are simultaneously active in the infrared (IR) and Raman processes according to Eq.…”

Metamagnetic transitions and magnetoelectric responses in a chiral polar helimagnet Ni$_2$InSbO$_6$

“…Single crystals of Ni 2 InSbO 6 were grown by the chemical vapor transport method with use of PtCl 2 as the transport agent 21 . The c-plane was easily grown, resulting in plateshaped crystals.…”