Preparation of new Ba[sub 4]M[sub 3]S[sub 10] phases (M = Zr, Hf) and single crystal structure determination of Ba[sub 4]Zr[sub 3]S[sub 10]

Journal Article · Mon Mar 01 04:00:00 EST 1993 · Journal of Solid State Chemistry; (United States)

DOI:https://doi.org/10.1006/jssc.1993.1080· OSTI ID:6309453

Chen, Baihao; Eichhorn, B W ^[1]; Wong-Ng, W ^[2]

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1. Univ. of Maryland, College Park (United States)
2. National Inst. of Standards and Technology, Gaithersburg (United States)

Two new Ruddlesden-Popper Ba[sub n+1]M[sub n]S[sub 3n+1] compounds where M = Zr, Hf and n = 3 have been prepared in good yield from BaS, M, and S in a BaCl[sub 2] flux at 1,050[degrees]C. The structures comprise triple layer perovskite slabs separated by double BaS layers. The single crystal structure of Ba[sub 4]Zr[sub 3]S[sub 10] revealed Zr-S distances of 2.493(3) [Angstrom] (average) with one long Zr-S contact of 2.562(5) [Angstrom] for the distal bond of the ZrS[sub 6] octahedron at the perovskite/double BaS interface. The Ba-S contacts average 3.52(1) [Angstrom] inside the perovskite blocks and range between 3.084(5) and 3.552(1) [Angstrom] in the double BaS layers. Crystal data for Ba[sub 4]Zr[sub 3]S[sub 10] (25[degrees]C) are a = 7.0314(5) [Angstrom], b = 7.0552(7) [Angstrom], c = 35.544(7) [Angstrom], Z = 4, D[sub calc] = 4.038 g/cm[sup 3], orthorhombic, space group Fmmm, R(F) = 0.038, R[sub w](F) = 0.058. Single crystals of Ba[sub 4]Hf[sub 3]S[sub 10] were indexed on an orthorhombic cell with a = 6.989(3) [Angstrom], b = 7.022(2) [Angstrom], and c = 35.428(8) [Angstrom] but the structure was not refined due to poor quality data. 16 refs., 1 fig., 4 tabs.

• OSTI ID: 6309453
• Journal Information: Journal of Solid State Chemistry; (United States), Journal Name: Journal of Solid State Chemistry; (United States) Vol. 103:1; ISSN 0022-4596; ISSN JSSCBI
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
360202* -- Ceramics
Cermets
& Refractories-- Structure & Phase Studies
ALKALINE EARTH METAL COMPOUNDS
BARIUM COMPOUNDS
BARIUM SULFIDES
CHALCOGENIDES
CHEMICAL REACTION YIELD
CRYSTAL LATTICES
CRYSTAL STRUCTURE
HAFNIUM COMPOUNDS
HAFNIUM SULFIDES
LATTICE PARAMETERS
LAYERS
MINERALS
ORTHORHOMBIC LATTICES
OXIDE MINERALS
PEROVSKITE
PEROVSKITES
REFRACTORY METAL COMPOUNDS
SULFIDES
SULFUR COMPOUNDS
TRANSITION ELEMENT COMPOUNDS
YIELDS
ZIRCONIUM COMPOUNDS
ZIRCONIUM SULFIDES