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Preparation method and application of hollow silica/titania microspheres with in-situ carbon-doped hierarchical structure

A hierarchical structure, silicon dioxide technology, applied in the manufacture of hybrid/electric double layer capacitors, hybrid capacitor electrodes, etc., can solve problems such as poor photoelectric performance

Active Publication Date: 2018-06-01
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing methods of preparing silica / titania composites through sol-gel and co-hydrolytic condensation still have limitations such as excitation under ultraviolet light and poor photoelectric properties.

Method used

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  • Preparation method and application of hollow silica/titania microspheres with in-situ carbon-doped hierarchical structure
  • Preparation method and application of hollow silica/titania microspheres with in-situ carbon-doped hierarchical structure
  • Preparation method and application of hollow silica/titania microspheres with in-situ carbon-doped hierarchical structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Put 72g of deionized water, 8g of styrene and 0.16g of potassium persulfate into a 150mL four-necked bottle, and at a stirring speed of 350rpm, pass nitrogen gas to remove the air for about 20 minutes, then place in a constant temperature water bath at 70°C . After reacting for 1.5 hours, under the protection of nitrogen, inject 1.2g of VTC / deionized water mixture (the volume ratio of VTC to deionized water is 1:1) into the reaction bottle with a micro-injector. One injection per hour (10 μL per injection), and then two injections, one injection per hour, each injection is (50 μL). Then the remaining solution was injected every 3 minutes (10 μL) until all the remaining VTC was injected. After the injection was completed, the polymerization was extended for about 12 hours to make it fully polymerized. After the polymerization is completed, the polymer is suction-filtered, washed and separated with a water-based microporous membrane (0.22 μm), and finally monodisperse ca...

Embodiment 2

[0053] Preparation of Hierarchical Carbon-Doped Hollow Silica / Titania (SiO 2 / C-TiO 2 ).

[0054] CPS / SiO2 2 Preparation: In a 100mL four-neck flask, add 3.2g of CPS template and disperse it in 40mL of ethanol, control the temperature of the system at 50°C, add 3mL of ammonia water with a mass fraction of 25% as a catalyst, slowly add 0.8g of CPS under mechanical stirring After reacting for 4 hours, add 0.2mL allyltriethoxysilane under nitrogen protection, react for 6 hours, cool to room temperature, centrifuge, wash and dry to prepare functional CPS / SiO 2 Core-shell microspheres; such as figure 2 ;

[0055] CPS / SiO2 2 / CPS synthesis: In a 100mL four-neck flask, add 2g CPS / SiO 2 And dispersed in 40mL of ethanol, under the protection of nitrogen and mechanical stirring, the reaction temperature was raised to 50°C, then 2g of styrene monomer and 0.02g of initiator AIBN were added, and the temperature was raised to 70°C. After reacting for 1.5h, add dropwise a mixture of ...

Embodiment 3

[0059] Preparation of Hierarchical Carbon-Doped Hollow Silica / Titania (SiO 2 / C-TiO 2 ).

[0060] CPS / SiO2 2 Preparation: In a 100mL four-neck flask, add 3.2g of CPS template and disperse it in 40mL of ethanol, control the temperature of the system at 50°C, add 3mL of ammonia water with a mass fraction of 25% as a catalyst, slowly add 0.8g of CPS under mechanical stirring After reacting for 5 hours, add 0.2mL allyltriethoxysilane under nitrogen protection, react for 6 hours, cool to room temperature, centrifuge, wash and dry to prepare functional CPS / SiO 2 Core-shell microspheres;

[0061] CPS / SiO2 2 / CPS synthesis: In a 100mL four-neck flask, add 2g CPS / SiO 2 And dispersed in 40mL of ethanol, under the protection of nitrogen and mechanical stirring, the reaction temperature was raised to 50°C, then 2g of styrene monomer and 0.02g of initiator AIBN were added, and the temperature was raised to 70°C. After reacting for 1.5h, add dropwise a mixture of 0.75g of DMC and 0.75...

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Abstract

The invention provides a preparation method and application of in-situ carbon doped hierarchically structured hollow silicon dioxide / titanium dioxide microspheres. The preparation method includes following steps that: monodispersed cationic submicron polystyrene core-shell structural microspheres are prepared; step 2, functional CPS(cationic submicron polystyrene core-shell structural microsphere) / SiO2(silicon dioxide) core-shell structural microspheres are prepared; step 3, CPS / SiO2 / CPS microspheres are prepared; step 4, a CPS / SiO2 / CPS / TiO2 (titanium dioxide) precursor is prepared; and step 5, the in-situ carbon doped hierarchically structured hollow silicon dioxide / titanium dioxide microspheres are prepared. According to the preparation method of the invention, the monodispersity, TEOS and TBT (tetrabutyl titanate) sedimentation and catalytic hydrolysis rates of two layers of cationic templates, so that the uniform self-assembly of the surfaces of the cationic templates can be realized, and therefore, the in-situ carbon doped hierarchically structured hollow silicon dioxide / titanium dioxide microspheres can be prepared.

Description

technical field [0001] The invention relates to a simple preparation technology of a novel supercapacitor electrode material, in particular to a preparation method and application of a hollow silicon dioxide / titania microsphere with an in-situ carbon-doped hierarchical structure. Background technique [0002] As a new generation of energy storage devices, supercapacitors are widely used in hybrid electric vehicles, mobile devices and storage backup systems due to a series of advantages such as high power storage performance, good charge and discharge process, and excellent cycle life ( X.Lu, M.Yu, G.Wang, T.Zhai, S.Xie, Y.Ling, Y.Tong, Y.Li.H-TiO 2 @MnO 2 / H-TiO 2 @C Core–Shell Nanowires for High Performance and Flexible Asymmetric Supercapacitors. Adv. Mater. 2013, 25, 267–272). In order to meet the growing demand for next-generation portable and smart energy storage devices, a large number of scientific and technological workers have focused on the study of new high-per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G11/24H01G11/30H01G11/46H01G11/86
CPCY02E60/13
Inventor 张颖曹顺生陈娟荣常俊程黎傅行礼
Owner JIANGSU UNIV
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