Ni6B22O39·H2O – extending the field of nickel borates

2017 ◽  
Vol 72 (12) ◽  
pp. 967-975 ◽  
Author(s):  
Martin K. Schmitt ◽  
Hubert Huppertz

AbstractNi6B22O39·H2O was synthesized in a high-pressure/high-temperature reaction at 5 GPa/900°C. It crystallizes in the orthorhombic space group Pmn21 (no. 31) with the lattice parameters a=7.664(2), b=8.121(2) and c=17.402(2) Å. The crystal structure is discussed with regard to the isotypic compounds M6B22O39·H2O (M=Fe, Co) and the structurally related phase Cd6B22O39·H2O. Furthermore, the characterization of Ni6B22O39·H2O via X-ray powder diffraction and vibrational spectroscopy is reported.

2011 ◽  
Vol 66 (2) ◽  
pp. 107-114 ◽  
Author(s):  
Stephanie C. Neumair ◽  
Johanna S. Knyrim ◽  
Oliver Oeckler ◽  
Reinhard Kaindl ◽  
Hubert Huppertz

The cubic iron hydroxy boracite Fe3B7O13OH・1.5H2O was synthesized from Fe2O3 and B2O3 under high-pressure/high-temperature conditions of 3 GPa and 960 °C in a modified Walker-type multianvil apparatus. The crystal structure was determined at room temperature by X-ray diffraction on single crystals. It crystallizes in the cubic space group F4̄3c (Z = 8) with the parameters a = 1222.4(2) pm, V = 1.826(4) nm3, R1 = 0.0362, and wR2 = 0.0726 (all data). The B-O network is similar to that of other cubic boracites.


2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.


2020 ◽  
Vol 75 (6-7) ◽  
pp. 597-603
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz

AbstractThe non-centrosymmetric scandium borate ScB6O9(OH)3 was obtained through a high-pressure/high-temperature experiment at 6 GPa and 1473 K. Single-crystal X-ray diffraction revealed that the structure is isotypic to InB6O9(OH)3 containing borate triple layers separated by scandium layers. The compound crystallizes in the space group Fdd2 with the lattice parameters a = 38.935(4), b = 4.4136(4), and c = 7.6342(6) Å. Powder X-ray diffraction and vibrational spectroscopy were used to further characterize the compound and verify the proposed structure solution.


2019 ◽  
Vol 74 (9) ◽  
pp. 685-692 ◽  
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz

AbstractThe title compound β-Eu(BO2)3 was synthesized in a high-pressure/high-temperature experiment at 4 GPa and 1473 K. The europium borate crystallizes in the orthorhombic space group Pnma (no. 62) with the lattice parameters a = 16.071(2), b = 7.440(4), and c = 12.362(5) Å. The structure is isotypic to the already known meta-borates β-RE(BO2)3 (RE = Y, Nd, Sm, Gd, Dy–Lu) and is built up of approximately triangular ribbons of BO4 tetrahedra. The compound was further characterized by X-ray powder diffraction, vibrational spectroscopy and shows a typical Eu3+ line emission upon excitation at 448 nm.


1996 ◽  
Vol 51 (8) ◽  
pp. 1099-1103 ◽  
Author(s):  
Thomas Berger ◽  
Klaus-Jürgen Range

Single crystals of Sr2(VO)2Si4O12 could be obtained by high-pressure high-temperature reaction of a SrSiO3/SiO2/V2O5 mixture in a modified Belt-type apparatus. The green crystals are orthorhombic, space group Cmcm, with a = 5.3139(3), b = 14.6281(7), c = 7.0329(4) Å and Z = 2. The structure comprises vierer single chains of SiO4 tetrahedra, the resulting Si4O12 units being connected by VO5 square pyramids. There is one short distance (V - O = 1.61 (1) Å) within the square pyramid, giving definite evidence to a (VO)2+ group with a V = O double bond.The crystal structure of microcrystalline Sr2(TiO)2Si4O12, obtained by high-pressure hightemperature reaction of a SrSiO3/SiO2/TiO2 mixture, was refined by the Rietveld technique. The compound (Cmcm, a = 5.3530(2), b = 14.4864(7), c = 7.0817(3) Å, Z = 2) is isostructural with the vanadium compound.


1977 ◽  
Vol 32 (5) ◽  
pp. 495-498 ◽  
Author(s):  
W. Muschick ◽  
Hk. Müller-Buschbaum

Single crystals of 1—x Ho2O3 : xCaO (x = 0.07), CaHoO2.5 (A) and Ca0.5Ho1.5O2.75 (B) were prepared by high temperature reaction and investigated with X-ray single crystal data. It can be shown that small amounts of CaO stabilize the monoclinic B-Typ of rare earth oxides. Phase (A) and (B) cannot be seen as a stabilized B-type crystal because they have an new crystal structure with space groupC22h–P 21/m, a = 656.6, b = 356.7, c = 529.4 pm, β = 92.3°; a = 650.2, b = 352.4, c = 584.5, β = 92.3°.


2017 ◽  
Vol 72 (1) ◽  
pp. 69-76 ◽  
Author(s):  
Daniela Vitzthum ◽  
Michael Schauperl ◽  
Klaus R. Liedl ◽  
Hubert Huppertz

AbstractOrthorhombic In3B5O12 was synthesized in a Walker-type multianvil apparatus under high-pressure/high-temperature conditions of 12.2 GPa and 1500°C. Its structure is isotypic to the rare earth analogs RE3B5O12 (RE=Sc, Er–Lu). In the field of indium borate chemistry, In3B5O12 is the third known ternary indium borate besides InBO3 and InB5O9. The crystal structure of In3B5O12 has been determined via single-crystal X-ray diffraction data collected at room temperature. It crystallizes in the orthorhombic space group Pmna with the lattice parameters a=12.570(2), b=4.5141(4), c=12.397(2) Å, and V=703.4(2) Å3. IR and Raman bands of In3B5O12 were theoretically determined and assigned to experimentally recorded spectra.


2010 ◽  
Vol 65 (10) ◽  
pp. 1206-1212 ◽  
Author(s):  
Almut Haberer ◽  
Reinhard Kaindl ◽  
Hubert Huppertz

The praseodymium orthoborate λ -PrBO3 was synthesized from Pr6O11, B2O3, and PrF3 under high-pressure / high-temperature conditions of 3 GPa and 800 °C in a Walker-type multianvil apparatus. The crystal structure was determined on the basis of single-crystal X-ray diffraction data, collected at room temperature. The title compound crystallizes in the orthorhombic aragonite-type structure, space group Pnma, with the lattice parameters a = 577.1(2), b = 506.7(2), c = 813.3(2) pm, and V = 0.2378(2) nm3, with R1 = 0.0400 and wR2 = 0.0495 (all data). Within the trigonal-planar BO3 groups, the average B-O distance is 137.2 pm. The praseodymium atoms are ninefold coordinated by oxygen atoms.


2006 ◽  
Vol 21 (7) ◽  
pp. 1700-1703 ◽  
Author(s):  
Junmin Yan ◽  
Xianfeng Ma ◽  
Wei Zhao ◽  
Huaguo Tang ◽  
Changjun Zhu ◽  
...  

In this work, a novel substitutional solid solution (W0.8Al0.2)C was synthesized by mechanically activated high-temperature reaction. X-ray diffraction was used for phase identification during the whole reaction process. Environment scanning electronic microscopy–field emission gun and energy dispersive x-ray were used to investigate the microstructure and the quantitative material composition of the specimen. (W0.8Al0.2)C was found to crystallize in the WC-type, and the cell parameters were a = 2.907(1) Å and c = 2.837(1) Å. The hardness of (W0.8Al0.2)C was tested to be 19.3 ± 1 GPa, and the density was 13.19 ± 0.05 g cm−3.


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