Methods of chemical analysis used to characterize battery materials

Jensen, K. J.; Streets, W. E.

doi:10.2172/5344713

Cited by 1 publication

(1 citation statement)

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“…The chemical analysis (14) yielded a value for the iron that was about 0.5-1% higher than that obtained by electron microprobe analysis, which can analyze individual grains and minimizes the contribution of the impurity phase. The metallographic examination showed the presence of an impurity phase that covered less than 5% of the area.…”

Section: Methodsmentioning

confidence: 86%

Neutron Diffraction Study of Electrochemically Synthesized Djerfisherite

Tani¹,

Mrazek²,

Faber³

et al. 1986

J. Electrochem. Soc.

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produces TaSi2 from the diffusion controlled interaction of silicon and Ta.~Si3.The three reactions combine and compete to determine the deposition stoichiometry, structure, and morphology; through these reactions, processing variables can greatly influence the microstructure of the deposited tantalum silicide. The interface roughness between the tantalum silicide and the polysilicon is determined by the competition between the displacement reaction and the silane reaction. In the absence of silane, TaC15 reacts readily with polysilicon to yield a rough interface between the phases. If silane is present in the reactor when the TaCl~ is introduced, the resultant interface between the silicide and polysilicon is much smoother. The grain size and pore density, the whisker density, the deposition rate, and the crystal structure are all strongly influenced by the tantalum chloride to silane ratio. The influence of temperature and total pressure are second-order contributors to the deposition rate and to the film characteristics. AcknowledgmentsWe would like to thank A. C. Adams and H. J. Levinstein for suggesting this work and for their continuing advice and encouragement during the program. Stimulating discussions with S. P. Murarka are also gratefully acknowledged. The special contribution of E. A. Dein to all phases of this program is acknowledged. We acknowledge the electron microscopy of R. V. Knoell, the RBS work of D.C. Jacobson, and the x-ray diffraction work of J. Vandenberg. Finally, we acknowledge the special insight that R. S. Wagner has given to the topic of whisker growth in CVD systems. ABSTRACTThe electrochemical synthesis of a synthetic form of the mineral djerfisherite produced sufficient material (4g) for neutron powder diffraction analysis. The data were collected on the time-of-flight neutron diffractometer at the Intense Pulsed Neutron Source Facility at Argonne National Laboratory. A crystallographic refinement of the neutron diffraction data by the Rietveld analysis technique showed an improvement in the atom coordinate positions by a factor of ten over prior x-ray powder diffraction data. In addition, the refinement indicates 23 iron atoms randomly distributed about 24 available sites such that the formula of the synthetic form of djerfisherite can be expressed as K~LiFez3S2~CI.) unless CC License in place (see abstract). ecsdl.org/site/terms_use address. Redistribution subject to ECS terms of use (see 138.251.14.35

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Section: Methodsmentioning

confidence: 86%