Preparation method of crystal phase controllable titanium dioxide nanometer crystal
A technology of titanium dioxide and nanocrystals, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems that the phase ratio of anatase and rutile cannot be adjusted continuously, it is difficult to promote industrially, and the production cost is high, and it is easy to achieve process parameters The effect of control, easy industrial promotion, and short production cycle
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example 1~9
[0031] Dissolve 0.1 mol of butyl titanate in 1.5 mol of absolute ethanol, add dropwise a mixture of 1 mol of ethanol and 5 mol of water, stir at room temperature for 3 hours, then filter with suction and dry at room temperature to obtain amorphous titanium dioxide powder. Add a certain amount of nitric acid (10mL / g titanium dioxide powder) to the amorphous titanium dioxide powder, the concentration of nitric acid is 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 1.0mol / L, and stir at room temperature for 1 hours, hydrothermal crystallization at 180°C for 24 hours, suction filtration, washing, and drying to obtain titanium dioxide samples, which are respectively designated as samples 1-9.
example 10
[0033] The XRD patterns of samples 1-9 were measured on a Rigaku D / MAX-IIA diffractometer, and the peaks at 25.2, 38.7 and 48.0° belonged to the diffraction of anatase (101), (004) and (200) crystal planes, respectively , and the peaks at 27.4, 36.1, 41.2, and 54.3° are assigned to the diffraction of rutile (110), (101), (111) and (211) crystal planes, respectively. The proportion of anatase phase and rutile phase in titanium dioxide using the phase quantification formula x A =(1+1.26I R / I A ) -1 Calculate (C.C. Wang, J.Y. Ying, Chem. Mater., 1999; 11:3113), where x A is the proportion of anatase phase, I A and I R are the intensities of the diffraction peaks attributed to anatase and rutile, respectively, and the results are shown in Table 1.
example 11~12
[0035] Dissolve 0.1 mol of butyl titanate in 1.5 mol of absolute ethanol, add dropwise a mixture of 1 mol of ethanol and 5 mol of water, stir at room temperature for 3 hours, then filter with suction and dry at room temperature to obtain amorphous titanium dioxide powder. Add a certain amount of hydrochloric acid (20mL / g titanium dioxide powder) to the amorphous titanium dioxide powder, the concentration is 0.2, 0.3mol / L respectively, stir at room temperature for 1 hour, 180 ℃ hydrothermal crystallization for 24 hours, after suction filtration, Titanium dioxide samples were obtained by washing and drying, which were respectively recorded as samples 11 and 12, and the proportion of the anatase phase was determined by the method of Example 10.
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