Inorganic nanocrystalline vesicular microspheres and their photochemical synthesis and application
An inorganic nano, vesicle-like technology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of time-consuming and laborious, limited wide application, etc., achieve good enhancement effect, mild preparation method conditions, good catalysis The effect of hydrogen production performance and stability
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Embodiment 1
[0047] A method for preparing inorganic nanocrystalline vesicle-like microspheres that is easy to obtain, with controllable size and shell structure, comprising the following steps:
[0048] At room temperature, a toluene solution of 50uL 7-(12-mercaptododecyloxy)-2hydro-chromen-2-one with a concentration of 4mM was added to the surface of 3nm gold nanoparticles modified by oleylamine molecules. In the toluene solution, the mass of the gold nanoparticles is 1 mg, and the volume of the toluene solution is 4 mL. After the mixture was sonicated for 30 min, about 30 mL of ethanol was added and washed twice by centrifugation. The ratio of mercaptan and oleylamine on its surface was determined to be 1:3 by XPS. Finally, the obtained solid was dispersed in 400 uL of toluene, and then poured into 3.6 mL of acetone. Immediately use ultraviolet light on the mixture, the wavelength of ultraviolet light is 300-400nm, irradiate in the air for about 30 minutes, and at the same time pass i...
Embodiment 2
[0052] Repeat Example 1, the difference is only that the 3nmAu nanocrystals are changed to 3nmCdSe quantum dots, the resulting vesicle microsphere structure and size distribution are as follows Figure 4 As shown in A and 4B, it was applied to the photocatalytic hydrogen production experiment.
[0053] In two 50mL quartz tubes, add catalyst and 1.68gNa 2 S·9H 2 20 mL of O and 0.25 M Na 2 SO 3 The aqueous solution, the catalysts added to two quartz test tubes are 10mg water-soluble CdSe quantum dots and 10mg vesicular microspheres respectively. Nitrogen was passed through the two quartz test tubes for 30 minutes to exclude oxygen and sealed with a rubber stopper, and the tubes were illuminated for 1 hour under stirring. The light source was a 300W xenon lamp, and ultraviolet light with a wavelength of less than 400nm was filtered out. Determination of hydrogen production with Shimadzu GC-2014 gas chromatograph, such as Figure 5 As shown in A. Repeat the above experiment,...
Embodiment 3
[0056] Repeat embodiment 1, its difference is only to change acetone into butanone. The morphology and size distribution of the vesicular microspheres of the obtained Au nanocrystals are as follows: Figure 8 As shown in A and 8B, its morphology has good uniformity, and its size is 115.6±17.0nm. Figure 9 As shown, it indicates that the sample is a multi-shelled vesicle structure.
[0057] The vesicular microspheres were applied to the surface plasmon-enhanced Raman (SERS) detection, and the enhancement effect was compared with that of monodisperse nanocrystals as the substrate. Figure 10 can be found in rhodamine B (RhB, 10 -5 mol / L) is the probe molecule, on the monodisperse gold nanoparticle substrate, only 1647cm -1 The Raman peak at the wave number is detected, and more than five Raman peaks can be detected when the gold nanocrystalline vesicular microspheres are used as the substrate, which are located at 1199cm -1 ,1278cm -1 ,1357cm -1 ,1505cm -1 and1648cm -1 ,...
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