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AssigneePt Spe Subco LLC
InventorsJason Allen REPAC, Serpil Gonen WILLIAMS, Selina Thomas MONICKAM, Robert J. WIACEK
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The preparation of monodispersed TiO2 nanocrystals with nanocrystal size between 1-30 nm is described herein. These TiO2 nanocrystals are used to prepare dispersions into solvents, formulation into monomers, oligomers, and polymers, and nanocomposites from the resulting formulations. Dispersions of nanocrystals can be formed in various solvents at high loading, high transmittance, and low viscosity. Formulations incorporating these nanocrystals and a matrix material are highly stable, where the resulting nanocomposites have high refractive index and are optically transparent in the visible wavelengths, with very little or no scattering.
A method of preparing TiO2 nanocrystals, comprising converting a precursor of titanium dioxide into TiO2 nanocrystals in a solvent, wherein the majority of the solvent is not water, wherein the converting comprises 1) mixing the precursor of titanium dioxide in the solvent to provide a reaction mixture, and 2) heating the reaction mixture at a reaction temperature, e.g., about 180° C. to about 250° C., about 200° C. to about 210° C., for a period of time to provide the TiO2 nanocrystals.
A method of preparing TiO2 nanocrystals having an average particle size of greater than 4 nm but less than 50 nm (such as about 10 nm to about 25 nm or about 4 nm to about 20 nm) as measured by TEM, the method comprising 1) adding a precursor of titanium dioxide and water in a solvent to provide a reaction mixture, and 2) heating the reaction mixture at a reaction temperature of about 180° C. to about 250° C. (e.g., about 200° C. to about 210° C.) for about 10 minutes to 5 hours (e.g., 20 minutes to 1 hour, or 1-5 hours) to provide the TiO2 nanocrystals, wherein the molar ratio of the precursor of titanium dioxide to water ranges from about 1:0.3 to about 1:3, such as about 1:0.5 to about 1:2.5, about 1:0.5 to about 1:1, about 1:1 to about 1:1.5, about 1:1.5 to about 1:2, about 1:2 to about 1:2.5.
A nanocrystal dispersion comprising at least partially capped TiO2 nanocrystals and a solvent, wherein the at least partially capped TiO2 nanocrystals are present in an amount of greater than 30%, e.g., greater than 40%, greater than 50%, greater than 60%, or greater than 70%, such as about 40%, about 50%, about 60%, about 70%, about 80%, or any ranges between the recited values, such as about 40-70%, about 30-80%, about 50-80%, etc., by weight of the dispersion.
A nanocomposite formulation comprising 1) at least partially capped TiO2 nanocrystals;
A nanocomposite film comprising at least partially capped TiO2 nanocrystals and at least one monomer, oligomer and/or polymer, wherein the at least partially capped nanocrystals are present in an amount greater than 50%, such as greater than 60%, greater than 70%, greater than 80%, or greater than 90%, such as about 55%, about 60%, about 70%, about 80%, about 90%, or any ranges between the recited values, such as about 55-90%, about 60-90%, about 70-90%, by weight of the nanocomposite.
Dependencies are inferred from the claim text.