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Thermal Transformation of (NH4)[Fe(AsO4)F] into the New Textural Porous Orthorhombic Fe(AsO4) Phase. Crystal Structures, Thermal Behavior, and Spectroscopic and Magnetic Properties.

โœ Scribed by Begona Bazan; Jose L. Mesa; Jose L. Pizarro; Jesus Rodriguez-Fernandez; Jorge Sanchez-Marcos; Anna Roig; Elies Molins; Maria I. Arriortua; Teofilo Rojo


Publisher
John Wiley and Sons
Year
2005
Weight
13 KB
Volume
36
Category
Article
ISSN
0931-7597

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โœฆ Synopsis


Iron

I 7100 Thermal Transformation of (NH 4 )[Fe(AsO 4 )F] into the New Textural Porous Orthorhombic Fe(AsO4) Phase. Crystal Structures, Thermal Behavior, and Spectroscopic and Magnetic Properties. -Light-green single crystals of (NH4)[Fe(AsO4)F] (I) are synthesized hydrothermally from FeCl3, As2O5, HF, and NH4OH (H2O, autoclave, 170 ยฐC, 5 d) and are converted to Fe(AsO4) (II) by heating at 525 ยฐC in air. Compound (I) crystallizes in the orthorhombic space group Pna2 1 with Z = 8 and compound (II) in the orthorhombic space group Imam with Z = 12 (single crystal XRD). The structure of (I) consists of a three-dimensional framework with chains formed by alternating FeO4F2 octahedra and AsO4 tetrahedra. The structure of (II) consists of a three-dimensional skeleton, constructed from sheets stacked along the [001] direction interconnected by chains of alternating vertex-sharing FeO6 octahedra and AsO4 tetrahedra. Transmission electronic microscopy indicates the existence of unconnected external and internal cavities. Magnetic measurements at low temperatures indicate the predominance of antiferromagnetic interactions with Nรฉel temperatures of 68.0 and 54.5 K for compounds (I) and (II), respectively. For both phases the existence of weak ferromagnetic components, giving rise to small hysteresis loops, is also detected at very low temperatures. -(BAZAN, B.; MESA*,


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