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Study of Gas-Phase Reactions in TiO₂ Production and Functionalised Thin Films

Blackburn, B; (2017) Study of Gas-Phase Reactions in TiO₂ Production and Functionalised Thin Films. Doctoral thesis , UCL (University College London). Green open access

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Titanium dioxide (TiO₂) is a pigment used in the whitening of millions of products from paint to foodstuffs. Produced via purification of ores using the Chloride Process, the mined TiO₂ ore is chlorinated along with all of the impurities. The resulting TiCl₄ is a liquid at room temperature and can be separated from its impurities using distillation. V₂O₅, an impurity present in this ore is converted to vanadium oxytrichloride (VOCl₃) which is too similar in boiling point to TiCl₄ to separate via distillation and instead is removed via addition of an oil, which preferably binds to VOCl₃. This work, sponsored by Huntsman Pigments and Additives, seeks to better understand this reaction, as well as other aspects of the Chloride Process. This is achieved by analysing industrial samples as well as producing lab scale models for the process and investigating inorganic synthesis of analogous compounds [TiCl₄{CH₂(CO₂CH(CH₃)₂}₂] [1a], [(µ-O)(TiCl₃{CH₂(CO₂CH(CH₃)₂}₂)] [1b], [TiCl₄{CH₂(CO₂CH(C₆H₅)}₂] [2], [TiCl₄{C₂H₄(CO₂CH₃)}₂] [3], VOCl₃+glycerol tribenzoate [4], [VOCl₂(acac)] [5], [{VOCl₂(CH₂(CO₂Et)₂}4] [6] and [VOCl₂{C₂H4(CO₂Et)₂}]n [7] that were characterised via single crystal X-ray diffraction analysis (with the exception of 4) Alongside this study, multiple side projects were undertaken that sought to use some of the novel materials produced in materials synthesis, due to the useful nature of both TiO₂ and VO₂ in window coating applications, the abundance of oxygen in the products making them good contenders for metal oxide precursors. This included the deposition of TiO₂ /SiO₂ thin films for photocatalytic self cleaning applications, VO₂ thin films for energy saving windows and VC/VN particles for mechanical hardening applications. In addition, a new system for the in-situ study of high temperature gas phase inorganic reactions via mass spectroscopy was developed and used to study the reactivity of gaseous TiCl₄ and VOCl₃, as well as several other species including vanadium chloride, titanium isopropoxide and butyltin trichloride considered to be of greater interest to the field of thin film deposition.

Type: Thesis (Doctoral)
Title: Study of Gas-Phase Reactions in TiO₂ Production and Functionalised Thin Films
Event: University College London
Open access status: An open access version is available from UCL Discovery
Language: English
Keywords: Titanium dioxide, Vanadium, vanadium oxytrichloride, the chloride process, mass spectrometry, CVD, APCVD, AACVD, Photocatalyst, thin film, nanoparticles
UCL classification: UCL > Provost and Vice Provost Offices > UCL BEAMS
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of Maths and Physical Sciences
URI: http://discovery.ucl.ac.uk/id/eprint/1551605
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