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Optimization of the conditions in the molten salt hydrate assisted synthesis method of TiO2

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Title
Optimization of the conditions in the molten salt hydrate assisted synthesis method of TiO2
Name (type = personal)
NamePart (type = family)
Huang
NamePart (type = given)
Chenfeng
NamePart (type = date)
1994-
DisplayForm
Chenfeng Huang
Role
RoleTerm (authority = RULIB)
author
Name (type = personal)
NamePart (type = family)
Tsilomelekis
NamePart (type = given)
George
DisplayForm
George Tsilomelekis
Affiliation
Advisory Committee
Role
RoleTerm (authority = RULIB)
chair
Name (type = corporate)
NamePart
Rutgers University
Role
RoleTerm (authority = RULIB)
degree grantor
Name (type = corporate)
NamePart
School of Graduate Studies
Role
RoleTerm (authority = RULIB)
school
TypeOfResource
Text
Genre (authority = marcgt)
theses
OriginInfo
DateCreated (encoding = w3cdtf); (keyDate = yes); (qualifier = exact)
2020
DateOther (encoding = w3cdtf); (qualifier = exact); (type = degree)
2020-05
CopyrightDate (encoding = w3cdtf); (qualifier = exact)
2020
Language
LanguageTerm (authority = ISO 639-3:2007); (type = text)
English
Abstract (type = abstract)
With the current transition in energy usage and concern for the environment, a primary goal is to find renewable and environmentally friendly catalysts with high activity and efficacy. To achieve this, advanced catalytic properties, such as high surface area, high acidity and low band gap energy, are of the utmost importance for heterogeneous catalysts. TiO2 is one promising metal dioxides with good mechanical structure, prevalent in both Lewis and Bronsted acid sites, low band gap energy, non-toxicity and cost effectiveness. Synthesis of TiO2 is itself not particularly novel. Sol-gel, hydrothermal, physical vapor deposition, and microwave methods have been widely studied for the production of titania. However, synthesis of TiO2 via molten salt hydrates (MSHs) have limited exposure in the open literature. In MSH, ion-water interaction is optimized and water-water interactions are minimized; by changing ratios of water/salt and salt/precursor, modification of the structure, morphology and chemical properties of synthesized materials can be achieved. Therefore, the project was undertaken in order to understand how the MSH system affects crystalline growth and to synthesize TiO2 with desirable catalytic properties.

In this work, Titanium Isopropoxide (TTIP) was utilized as the precursor, using a MSH-assisted sol-gel method to synthesize TiO2 with varying properties by changing the ratio of water/LiBr and LiBr/TTIP. In order to understand the effect of the MSH system, XRD, N2-BET, Raman, SEM, UV-vis and TPD-MS techniques were applied to characterize these samples. Likewise, TiO2 phase transformation was observed to investigate thermal stability. Samples were calcined at different temperatures ranging from 400 to 600┬░C to observe phase transformation in TiO2 using Raman; XRD was further used to quantify preponderance of anatase, brookite and rutile phases and to identify phase transition. Since TiO2 serves as a semiconductor and photocatalyst, electronic spectroscopy was taken for all samples to measure the band gap energy via the Kubelka-Munk equation. To gain further insight into the potential of TiO2 as a material for acid-catalyzed reaction, identification and quantification of Lewis and Bronsted acid sites was conducted by pyridine and 2,6-dimethylpyridine TPD-MS.

The results show that all samples exhibit anatase and brookite phases. Utilizing Raman and XRD methods, it was found that brookite changes to anatase, which further transforms to rutile. Band gap energy of MSH TiO2 was measured to be much lower than that of commercial anatase, brookite or even rutile. Moreover, a unique decreasing trend of band gap energy with increasing salt/TTIP ratio was observed. Based on results from TPD-MS, MSH TiO2 is comprised of both Lewis and Bronsted acid sites, though these sites vary in quantity and strength. SEM images show MSH TiO2 have flake-like morphology, and the thickness of these flakes decreases slightly with increasing ratios of salt/TTIP. BET surface area of some samples reaches to 200 m2/g, which is much higher than that of commercial anatase. These promising properties highlight the potential of using MSH TiO2 in future research and industrial applications, such as photocatalysis and alkylation reactions.
Subject (authority = LCSH)
Topic
Titanium dioxide -- Synthesis
Subject (authority = RUETD)
Topic
Chemical and Biochemical Engineering
RelatedItem (type = host)
TitleInfo
Title
Rutgers University Electronic Theses and Dissertations
Identifier (type = RULIB)
ETD
Identifier
ETD_10881
PhysicalDescription
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application/pdf
InternetMediaType
text/xml
Extent
1 online resource (ix, 43 pages) : illustrations
Note (type = degree)
M.S.
Note (type = bibliography)
Includes bibliographical references
RelatedItem (type = host)
TitleInfo
Title
School of Graduate Studies Electronic Theses and Dissertations
Identifier (type = local)
rucore10001600001
Location
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NjNbRU
Identifier (type = doi)
doi:10.7282/t3-knyr-9873
Genre (authority = ExL-Esploro)
ETD graduate
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RightsDeclaration (ID = rulibRdec0006)
The author owns the copyright to this work.
RightsHolder (type = personal)
Name
FamilyName
Huang
GivenName
Chenfeng
Role
Copyright Holder
RightsEvent
Type
Permission or license
DateTime (encoding = w3cdtf); (qualifier = exact); (point = start)
2020-04-29 11:52:56
AssociatedEntity
Name
Chenfeng Huang
Role
Copyright holder
Affiliation
Rutgers University. School of Graduate Studies
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License
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Author Agreement License
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I hereby grant to the Rutgers University Libraries and to my school the non-exclusive right to archive, reproduce and distribute my thesis or dissertation, in whole or in part, and/or my abstract, in whole or in part, in and from an electronic format, subject to the release date subsequently stipulated in this submittal form and approved by my school. I represent and stipulate that the thesis or dissertation and its abstract are my original work, that they do not infringe or violate any rights of others, and that I make these grants as the sole owner of the rights to my thesis or dissertation and its abstract. I represent that I have obtained written permissions, when necessary, from the owner(s) of each third party copyrighted matter to be included in my thesis or dissertation and will supply copies of such upon request by my school. I acknowledge that RU ETD and my school will not distribute my thesis or dissertation or its abstract if, in their reasonable judgment, they believe all such rights have not been secured. I acknowledge that I retain ownership rights to the copyright of my work. I also retain the right to use all or part of this thesis or dissertation in future works, such as articles or books.
Copyright
Status
Copyright protected
Availability
Status
Open
Reason
Permission or license
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2020-05-06T12:47:07
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2020-05-06T12:47:07
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