Structural and NMR study of the lithiated defect thiospinels Li/sub x/Cu/sub 0. 07/(Ti/sub 2/)S/sub 4/ (0 < x < 2)
Journal Article
·
· J. Solid State Chem.; (United States)
Oxidative extraction of copper from the normal thiospinel Cu(Ti/sub 2/)S/sub 4/ followed by chemical lithiation of the resulting defect thiospinel enabled the metallic, lithiated defect thiospinels Li/sub x/Cu/sub 0.07/(Ti/sub 2/)S/sub 4/ (0 < x < 2) to be prepared with high purity and chemical homogeneity. X-ray and neutron powder diffraction studies of Li/sub x/Cu/sub 0.07/(Ti/sub 2/)S/sub 4/ ( < x < 2) showed that lithium insertion into Cu/sub 0.07/(Ti/sub 2/)S/sub 4/ is topotactic and that the inserted lithium occupies only the 16c-octahedral sites of the thiospinel framework at all lithium compositions. Static and MAS /sup 7/Li NMR spectra of Li/sub x/Cu/sub 0.07/(Ti/sub 2/)S/sub 4/ (O < x < 2) exhibited a single resonance with a small chemical shift relative to lithium acetate dihydrate at all lithium compositions; the chemical shift increased linearly with increasing lithium content x. The /sup 7/Li NMR spectra showed the onset of quadrupolar line broadening and a Knight-shift anisotropy for x greater than or equal to 0.9; these effects are probably due to interactions between lithium ions on neighboring edge-sharing 16c sites.
- Research Organization:
- Univ. of Texas, Austin (USA)
- DOE Contract Number:
- W-31109-ENG-38
- OSTI ID:
- 6255564
- Journal Information:
- J. Solid State Chem.; (United States), Journal Name: J. Solid State Chem.; (United States) Vol. 77:2; ISSN JSSCB
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
ALKALI METAL COMPOUNDS
ALKALI METAL ISOTOPES
CHALCOGENIDES
CHEMICAL SHIFT
COPPER COMPOUNDS
COPPER SULFIDES
CRYSTAL DOPING
CRYSTAL STRUCTURE
DISPERSIONS
ISOTOPES
LIGHT NUCLEI
LITHIUM 7
LITHIUM COMPOUNDS
LITHIUM ISOTOPES
LITHIUM SULFIDES
MAGNETIC RESONANCE
MIXTURES
NUCLEAR MAGNETIC RESONANCE
NUCLEI
ODD-EVEN NUCLEI
RESONANCE
SOLID SOLUTIONS
SOLUTIONS
STABLE ISOTOPES
SULFIDES
SULFUR COMPOUNDS
TITANIUM COMPOUNDS
TITANIUM SULFIDES
TRANSITION ELEMENT COMPOUNDS
400201* -- Chemical & Physicochemical Properties
ALKALI METAL COMPOUNDS
ALKALI METAL ISOTOPES
CHALCOGENIDES
CHEMICAL SHIFT
COPPER COMPOUNDS
COPPER SULFIDES
CRYSTAL DOPING
CRYSTAL STRUCTURE
DISPERSIONS
ISOTOPES
LIGHT NUCLEI
LITHIUM 7
LITHIUM COMPOUNDS
LITHIUM ISOTOPES
LITHIUM SULFIDES
MAGNETIC RESONANCE
MIXTURES
NUCLEAR MAGNETIC RESONANCE
NUCLEI
ODD-EVEN NUCLEI
RESONANCE
SOLID SOLUTIONS
SOLUTIONS
STABLE ISOTOPES
SULFIDES
SULFUR COMPOUNDS
TITANIUM COMPOUNDS
TITANIUM SULFIDES
TRANSITION ELEMENT COMPOUNDS