Doctoral Dissertations

Keywords and Phrases

Epoxide; Fluorinated electrolyte; Neutron reflectometry; Sol-gel; Solid electrolyte interphase; Vanadia


"This dissertation focuses on the synthesis and characterization of vanadium oxide nanomaterials and neutron-transparent Li-ion battery electrolytes.

Vanadium oxide gels were synthesized via the epoxide-assisted gelation of VOCl3 using epichlorohydrin in ethanol. This represents the first epoxide-assisted gelation developed for vanadium oxide gels and serves as a potential economical replacement for the fabrication of vanadium oxide gels via the hydrolysis of vanadium alkoxides. Though epoxide-assisted gelation has been demonstrated for a number of transition metal oxides, the gelation mechanism observed here for VOCl3 appears to be unique.

While investigating the electrochemical and structural properties of lithium vanadates, it became desirable to perform in situ neutron diffraction with electrochemical cycling. The inability to perform these experiments prompted the development of a series of perfluorocarboxylate esters which could potentially serve as neutron-transparent electrolyte solvents and help enable in situ neutron scattering characterizations. Electrochemical studies were carried out on Si anodes, and the solid-electrolyte-interphase was studied both ex situ and in situ. Results indicate that these electrolyte solvents improve neutron scattering data when used in place of standard deuterated carbonates and provide insight into fluorinated components proposed for next-generation electrolytes"--Abstract, page iv.


Winiarz, Jeffrey G.
Leventis, Nicholas

Committee Member(s)

Dawes, Richard
Sotiriou-Leventis, Chariklia
Kaiser, Helmut
Taub, Haskell



Degree Name

Ph. D. in Chemistry


United States. Army Research Office
National Science Foundation (U.S.)
Oak Ridge Institute for Science and Education
Missouri University of Science and Technology. Materials Research Center
Bayer Corporation


Various sources provided student and material support: the Army Research Office (W911NF-14-1-0369), the National Science Foundation through a University of Missouri Neutron Scattering IGERT Traineeship (grant DGE-1069091), the U.S. Department of Energy, Office of Science, Office of Workforce Development for Teachers and Scientists, Office of Science Graduate Student Research (SCGSR) program, administered by the Oak Ridge Institute for Science and Education for the DOE under contract number DE‐AC05‐06OR23100, the Missouri S&T Materials Research Center, and Bayer Corporation


Missouri University of Science and Technology

Publication Date

Fall 2015

Journal article titles appearing in thesis/dissertation

  • Economical synthesis of vanadia aerogels via epoxide-assisted gelation of VOCl3
  • A study of perfluorocarboxylate ester solvents for lithium ion battery electrolytes
  • Evaluating the solid-electrolyte-interphase formed on silicon electrodes: a comparison of ex situ X-ray photoelectron spectroscopy and in situ neutron reflectometry


xiv, 149 pages

Note about bibliography

Includes bibliographic references.


© 2015 Tyler Martin Fears, All rights reserved.

Document Type

Dissertation - Open Access

File Type




Subject Headings

Vanadium oxide -- Synthesis
Nanostructured materials
Epoxy compounds
Lithium cells
Photoelectron spectroscopy

Thesis Number

T 10820

Electronic OCLC #


Included in

Chemistry Commons