Amorphous photonic crystal schemochrome material based on black titanium dioxide and silicon dioxide composite and preparation method of amorphous photonic crystal schemochrome material

[0035] 2)SiO2 2 Preparation of microspheres

[0036] Drop the ethanol solution of ethyl orthosilicate into the ethanol solution of ammonia water, make the concentration of ammonia water 0.1-0.6mol/L, and the concentration of ethyl orthosilicate 0.4-1.2mol/L, stir the reaction, centrifuge after the reaction is completed, Washed and dried to obtain SiO 2 microsphere powder;

[0037] 3) B-TiO 2 /SiO 2 material preparation

[0038] Weigh SiO according to the mass ratio of 1:(0.1~1) 2 Powder and B-TiO2 Powder, according to the ratio of (1 ~ 2) g: 50ml SiO 2 The powder was dissolved in ethanol, and then the corresponding B-TiO was added 2 The powder is ultrasonically dispersed for a certain period of time after being stirred for 2 hours, and dried at room temperature after sufficient reaction to obtain an amorphous photonic crystal structural color material based on black titanium dioxide and silicon dioxide with a photocatalytic effect.

[0039] In step 1), the grinding time is 1-3 hours, the reaction temperature is 250-400° C., and the holding time is 0.5-4 hours. The washing was performed by cross-washing with deionized water and absolute ethanol four times, and drying at room temperature. Nano powder refers to nano microspheres between 20-50nm.

[0040] Step 2) in, reaction temperature is 25~50 ℃, SiO 2 The particle size of the microspheres is between 180-400nm.

[0041] In step 3), the stirring speed is 600r/min, and the sufficient reaction time is 2-12h for ultrasonic dispersion.

[0042] Example 1

[0043] An amorphous photonic crystal structural color material with photocatalytic effect based on the composite of black titanium dioxide and silicon dioxide and a preparation method thereof, comprising the following steps:

[0044] 1) Black TiO2 2 (B-TiO 2 ) Preparation of nanoparticles

[0045] Weigh P25(TiO 2 ) and NaHB 4 , ground with an agate mortar, mixed evenly, heated up to 380°C at a heating rate of 7°C/min, heat-treated at 380°C in vacuum for 3 hours, and cooled naturally. After the reaction was completed, cross-wash with deionized water and ethanol four times, and dry at room temperature to obtain B-TiO 2 Nano powder.

[0046] 2)SiO2 2 Preparation of microspheres

[0047] Drop the ethanol solution of ethyl orthosilicate into the ethanol solution of ammonia water, so that the concentration of ammonia water is 0.1mol/L, and the concentration of ethyl orthosilicate is 0.8mol/L. Stir and react at 36°C for 4 hours. After the reaction is completed, centrifuge, Washing and drying to obtain SiO with a diameter of 320nm 2 powder of microspheres;

[0048] 3) B-TiO 2 /SiO 2 material preparation

[0049] Weigh SiO at a mass ratio of 1:1 2 Powder and B-TiO 2 Powder, according to the ratio of 2g:50ml SiO 2 The powder was dissolved in ethanol, and then the corresponding B-TiO was added 2 The powder is stirred for 4 hours, then ultrasonically dispersed for 8 hours, fully reacted and then dried at room temperature to obtain an amorphous photonic crystal structure color material based on black titanium dioxide and silicon dioxide with photocatalytic effect.

[0050] Samples of the amorphous photonic structural color material with photocatalytic effect prepared in this embodiment are as follows: figure 1 As shown, the green powder has a pastel tint. like figure 2 It is its X-ray diffraction pattern, and the diffraction angles 2θ=25.28°, 36.95°, 48.05°, 53.89°, 55.06°, 62.69°, 68.76° correspond to TiO 2 (101), (103), (200), (105), (204) and (116) crystal faces, due to the SiO formed by the sol method 2 is amorphous, which proves that the sample is pure anatase phase TiO 2 Nanoparticles and SiO 2 blending; image 3 The UV-Vis diffuse reflectance spectrum shows that B-TiO 2 /SiO 2 It can absorb ultraviolet light and part of visible light before 400nm, and a reflection peak appears at 525nm, which is consistent with the relationship between the microsphere particle size and wavelength of the Bragg diffraction law, and 248nm corresponds to the green light band in the visible light range (480-560nm) ; Figure 4 is the B-TiO prepared in Example 1 2 Nanopowder, it can be seen from the figure that the black titanium dioxide nanoparticles are between 20-50nm. Figure 5 For the obtained B-TiO of embodiment 1 2 /SiO 2 It can be seen from the SEM image that B-TiO exists between the smooth silica microspheres with uniform particle size. 2 Nano ion, SiO 2 The introduction of the black titanium dioxide provides attachment sites, improving the B-TiO 2 dispersion and specific surface area. exist Figure 5 The Fourier transform in the inset shows the B-TiO obtained after the composite of black titanium dioxide and silicon dioxide 2 /SiO 2 It is an amorphous photonic crystal structure with long-range disorder and short-range order. Image 6 For the B-TiO obtained in Example 1 2 /SiO 2 Photocatalytic degradation diagram of rhodamine B, B-TiO obtained after composite of black titanium dioxide and silicon dioxide 2 /SiO 2 After 60min under ultraviolet light, the degradation rate of RhB reached 83%. It can be seen that the introduction of black titanium dioxide not only absorbs coherently scattered light in white silica and displays color, but also improves the photocatalytic performance, realizing the one-step synthesis of soft-colored amorphous photonic structural color materials with photocatalytic effect.

[0051] Example 2

[0052] 1) Black TiO2 2 (B-TiO 2 ) Preparation of nanoparticles

[0053] Weigh P25(TiO 2 ) and NaHB 4 , ground with an agate mortar, mixed evenly, heated up to 250°C at a heating rate of 7°C/min, heat treated in vacuum at 250°C for 2 hours, and cooled naturally. After the reaction was completed, cross-wash with deionized water and ethanol four times, and dry at room temperature to obtain B-TiO 2 Nano powder.

[0054] 2)SiO2 2 Preparation of microspheres

[0055] Drop the ethanol solution of ethyl orthosilicate into the ethanol solution of ammonia water, so that the concentration of ammonia water is 0.2mol/L, and the concentration of ethyl orthosilicate is 0.4mol/L. Stir and react at 25°C for 6h. After the reaction is completed, centrifuge, Washing and drying to obtain SiO with a diameter of 180nm 2 powder of microspheres;

[0056] 3) B-TiO 2 /SiO 2 material preparation

[0057] Weigh SiO at a mass ratio of 1:0.1 2 Powder and B-TiO 2 Powder, according to the ratio of 1g: 50ml SiO 2 The powder was dissolved in ethanol, and then the corresponding B-TiO was added 2 The powder is stirred for 2 hours, then ultrasonically dispersed for 10 hours, fully reacted and dried at room temperature to obtain an amorphous photonic crystal structure color material based on black titanium dioxide and silicon dioxide with photocatalytic effect.