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Schneider, Hartmut

Publications and source records attributed to Schneider, Hartmut.

5 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Elucidating structural order and disorder phenomena in mullite-type Al{sub 4}B{sub 2}O{sub 9} by automated electron diffraction tomography

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along the b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Temperature-dependent structural studies of mullite-type Bi{sub 2}Fe{sub 4}O{sub 9}

We report on the temperature-dependent structural studies on the mullite-type Bi{sub 2}Fe{sub 4}O{sub 9} compound. The crystal structures were determined using both powder X-ray diffraction and single crystal neutron diffraction. The thermal expansion of the cell parameters from smallest to largest occurred in the order a<c<b; their expansion behavior was fit using either linear or nonlinear regression according to the region of choice. The anisotropic thermal expansion was monitored with respect to the expansion coefficients, anisotropy factor, and polyhedral geometry. At 900 K an abrupt change of the anisotropy factor is observed which correlates with a slope in the BiO{sub 6} polyhedral volume. At the same temperature the FeO{sub 4} tetrahedral distortion starts to increase. The temperature-dependent stereochemically activity of the Bi{sup 3+} 6s{sup 2} lone electron pair was probed by the absolute value of eccentricity parameter. This parameter shows a significant drop at around 773 K. Additionally, the average crystal size and micro-strain of the powder samples were studied. A healing of intrinsic defects is observed with respect to a decreasing micro-strain followed by crystal growth above about 900 K. The temperature-dependent infrared spectra were described in three distinct zones. Deconvolution of the absorption features between 370 cm{sup -1} and 1000 cm{sup -1} required nine fitted bands, and the decomposed Pseudo-Voigt elements were assigned to Fe-O stretching, Fe-O-Fe bending and O-Fe-O bending vibrations. The shift of the observed modes was described with respect to temperature. An effective linewidth parameter {Delta}corr was determined by autocorrelation analysis between 740 cm{sup -1} and 900 cm{sup -1} for each temperature-dependent spectrum. The break of the slope of {Delta}corr at about 773 K was interpreted as the change of some vibrational modes of the FeO{sub 4} tetrahedra. The intrinsic effects observed around 773 K are responsible for extrinsic parameter changes found around 900 K. - Graphical abstract: Temperature-dependent stereochemical activity (eccentricity |{Phi}{sub i}|) of the Bi{sup 3+} 6s{sup 2} lone electron pair directing in the non-bonded region of the Bi-O coordination in the Bi{sub 2}Fe{sub 4}O{sub 9} iron framework (given as polyhedra). Highlights: Black-Right-Pointing-Pointer Complex expansion-contraction mechanism explains anisotropic thermal expansion. Black-Right-Pointing-Pointer Bi 6s{sup 2} lone electron pair sphericity influences analyses by FTIR autocorrelation. Black-Right-Pointing-Pointer Intrinsic effects at 773 K are responsible for extrinsic parameter changes at 900 K.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Boron mullite: Formation and basic characterization

Graphical abstract: Display Omitted Highlights: ► Decrease of B-mullite formation temperature with increasing boron content. ► Decrease of lattice parameters b and c with increasing boron content. ► Significant reduction of thermal expansion (−15%) due to incorporation of boron. ► Decomposition of B-mullite at 1400 °C, long-term stability at 800 °C. -- Abstract: A series of boron doped mullites (B-mullite) was prepared from single-phase gels with initial compositions based on a 1:1 isomorphous substitution of Si by B, starting from a 3:2 mullite composition (Al{sub 4.5}Si{sub 1.5}O{sub 9.75}). A high amount of boron (>10 mol.%) can be incorporated into the crystal structure of mullite where it most likely replaces Si. In situ phase formation of B-mullites was studied with high temperature X-ray diffraction and thermal analysis. A decrease of the formation temperature for B-mullite with increasing boron content was observed. With increasing boron content lattice parameters b and c significantly decrease, while no systematic evolution of a is observed. Long annealing at 1400 °C results in decomposition of B-mullite to boron free mullite and α-alumina. At 800 °C B-mullite appears to be stable over a period of at least 12 days. The mean thermal expansion coefficient was reduced by 15% upon incorporation of boron which makes the material technologically interesting.

36 MATERIALS SCIENCE↗