Rutile titanium dioxide nanoparticles and ordered acicular aggregates of same
AssigneeCristal Inorganic Chemicals Switzerland Ltd
InventorsGuoyi Fu, Mark B. Watson
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Abstract
Ordered acicular aggregates of elongated TiO2 crystallites which resemble nano-sized flower bouquets and/or triangular funnels, and process for their preparation by thermally hydrolyzing a soluble TiO2 precursor compound in aqueous solution in the presence of a morphology controlling agent selected from carboxylic acids and amino acids.
Claims12
A method for preparing calcined rutile TiO2 nanoparticles from rutile TiO2 nanoparticles which are aggregates of elongated TiO2 crystallites comprising:
- (a) forming an aqueous solution of a soluble titanium compound at a titanium concentration of from 0.5 to 1.0 moles per liter, optionally in the presence of a mineral acid;
- (b) introducing a morphology controlling agent or a mixture of said morphology controlling agents selected from (i) an a-hydroxy carboxylic acid of the formula R—CH(OH)COOH, (ii) an a-hydroxy carboxamide of the formula R—CH(OH)CONH2 or (iii) an α-amino acid of the formula R—CH(NH2)COOH, wherein said R group in each formula is an alkane, alkene, alkyne, arene, or cycloalkane group having 6 or more carbon atoms, into the solution at an acid- or carboxamide-to-titanium molar ratio of from 0.02 to 0.2 while simultaneously heating the solution to a temperature in the range of from 60° C. to 80° C. with constant stirring;
- (c) introducing TiO2 seeds into the stirred solution at a seed-to-TiO2 molar ratio of from 0.0005 to 0.0015 and maintaining the stirred solution including said TiO2 seeds at a temperature in the range of from 60° C. to 80° C. for a period of from one to 3 hours;
- (d) elevating the temperature of the stirred solution from step (d) to a value of from 100° C. to the refluxing temperature of the aqueous solution and maintaining said temperature for a period of from 2 hours to 4 hours to form a reaction product;
- (e) cooling the reaction mixture which results from step (e) to room or ambient temperature;
- (f) optionally neutralizing the reaction mixture;
- (g) separating and drying the reaction product;
- and
- (h) calcining the reaction product.
Calcined rutile TiO2 nanoparticles which are produced by calcining rutile TiO2 nanoparticles which are ordered acicular aggregates of elongated TiO2 crystallites having a thickness in the range of from 3 nm to 5 nm in which one end of each of said elongated TiO2 crystallites are joined into a cluster such that the opposite ends of each of said elongated TiO2 crystallites extend outwardly in the shape of a nano-sized funnel structure having a diameter of about 50 nm and a height in the range of from 50 nm to 100 nm.
Dependencies are inferred from the claim text.