Sea-urchin-shaped nanometer nickel silicate hollow sphere and preparation method thereof

A nano-silicic acid and sea urchin-like technology, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve complex and changeable factors affecting synthesis conditions, difficult control of sample shape and particle size, and relatively high requirements for fine operation. Advanced problems, to achieve the effect of low price, non-denaturation and good repeatability

Inactive Publication Date: 2015-12-09
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Soft templates mainly use biological templates, organic macromolecules, and surface active substances as templates. The reaction system is unstable, the particle size distribution is uneven, and the product often contains a certain proportion of solid balls; the sol-gel method uses metal organic alkoxides, This raw material is difficult to prepare and expensive; and the hydrothermal synthesis method has relatively high environmental requirements for the reaction. The generation of the compound has a great influence, the repeatability of the product is poor, the influencing factors of the synthesis conditions are complex and changeable, and the operation refinement requirements are high
At present, it is generally believed that the use of ultrasound to prepare nanomaterials is related to its cavitation. Its biggest advantage is that the reaction can be carried out at room temperature and the reaction time is short. However, although the ultrasonic method is simple and easy, the shape and particle size of the prepared samples are difficult Control; the spray drying method can precipitate the solute in a short time, the preparation process is continuous, and the operation is simple, but this method is limited by many factors, such as solution viscosity, atomizer efficiency and heating temperature, etc.

Method used

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  • Sea-urchin-shaped nanometer nickel silicate hollow sphere and preparation method thereof
  • Sea-urchin-shaped nanometer nickel silicate hollow sphere and preparation method thereof
  • Sea-urchin-shaped nanometer nickel silicate hollow sphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Ultrasonic disperse 0.5g of silica balls (particle size about 120nm), 1.3g of urea and 0.2g of nickel nitrate hexahydrate in 40mL of deionized water, pour it into the core of a polytetrafluoroethylene reactor and place it in a 105°C Heated in an oven for 12 hours, cooled naturally to room temperature, centrifuged and washed the obtained product with deionized water and absolute ethanol, and dried at 70°C for 10 hours to obtain a nickel salt / SiO2 core-shell structure. The SEM picture is as follows: figure 1 shown;

[0030] 2) Weigh 0.05g of the product prepared in step 1) and disperse it in 40ml of NaOH solution with a pH of 12, pour it into the hydrothermal reaction

[0031] In the kettle, heat at a constant temperature of 160°C for 12 hours, cool naturally to room temperature, wash the obtained product by centrifugation with deionized water and absolute ethanol, and dry at 60°C for 12 hours;

[0032] 3) The product obtained in step 2) was calcined in air at 200° C....

Embodiment 2

[0034] 1) Ultrasonic disperse 1.2g of silica balls, 1.7g of urea and 0.1g of nickel nitrate hexahydrate in 40mL of deionized water.

[0035] The obtained solution was poured into the polytetrafluoroethylene reactor core, and heated in an oven at 120°C for 10 hours, cooled to room temperature naturally, and the obtained product was centrifugally washed with deionized water and absolute ethanol, and then heated at 80°C Dry for 7 hours;

[0036] 2) Weigh 0.05g of the product obtained in step 1) and disperse it in 40ml of Na with a pH of 12 2 CO 3 / NaOH solution, pour water

[0037] In a thermal reaction kettle, heat at a constant temperature of 200°C for 10 hours, cool naturally to room temperature, wash the prepared product with deionized water and absolute ethanol, and dry it at 80°C for 7 hours;

[0038] 3) The product obtained in step 2) was calcined in air at 400° C. for 1.5 h to prepare sea urchin-shaped nano-nickel silicate hollow spheres.

Embodiment 3

[0040] 1) Ultrasonic disperse 1.5g of silica balls, 1.3g of urea and 0.07g of nickel nitrate hexahydrate in 35mL of deionized water.

[0041] Pour the obtained solution into the core of a polytetrafluoroethylene reactor and place it in an oven for 8 hours at 150°C, cool it down to room temperature naturally, wash the obtained product centrifugally with deionized water and absolute ethanol, and dry it at 160°C for 5 hours ,, the nickel salt / SiO2 core-shell structure is obtained, and its SEM picture is as follows figure 2 shown;

[0042] 2) Weigh 0.10g of the product prepared in step 1) and disperse it in 40ml of KOH solution with a pH of 13, and pour it into a hydrothermal reaction kettle

[0043] , 100°C constant temperature hydrothermal reaction for 12h, naturally cooled to room temperature, the prepared product was washed with deionized water and absolute ethanol, and dried at 100°C for 6h;

[0044] 3) The product obtained in step 2) was calcined in air at 350° C. for 2 h...

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Abstract

The invention discloses a sea-urchin-shaped nanometer nickel silicate hollow sphere and a preparation method thereof. An appropriate quantity of silicon dioxide spherules and an appropriate amount of urea, soluble nickel salt and deionized water are added into a hydrothermal reaction kettle core, react for certain time inside a drying oven at the constant temperature of 80-150 DEG C and then are naturally cooled to indoor temperature; the prepared product is subjected to centrifugal washing and drying, an appropriate quantity of NaOH solutions and the product are together added into a hydrothermal reaction kettle and placed at the constant temperature of 100-200 DEG C to be subjected to hydrothermal reaction for certain time, and the product is subjected to centrifugal washing and drying and then calcined at certain temperature to prepare the sea-urchin-shaped nanometer nickel silicate hollow sphere. The prepared nickel silicate hollow sphere is tested by an X-ray diffractometer, a scanning electron microscope and a transmission electron microscope and is in a sea urchin shape, the wall of the sphere is quite thin, the specific surface area is large, particle size distribution is even, and the nickel silicate hollow sphere can serve as a material for manufacturing an electrochromic device and an electrode material for manufacturing a super capacitor.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and in particular relates to a sea urchin-shaped nano-nickel silicate hollow sphere and a preparation method thereof. Background technique [0002] Nano-nickel salt has unique properties in electricity, magnetism and catalysis. In recent years, its application in supercapacitors, gas sensors, electrochromic materials, etc. has attracted the attention of researchers, and it is a very promising function. Sexual inorganic materials. The shape and size of nanomaterials have a direct impact on their functionality, and the current research on nano-nickel salts is mainly focused on nanorods, nanosheets, nanowires, nanofibers, etc., and there is little research on its nanohollow spherical shape. [0003] At present, the chemical methods for preparing hollow nanospheres mainly include template method (including soft template and hard template), sol-gel method, hydrothermal synthesis method, etc., a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/20B82Y30/00B82Y40/00
Inventor 王金敏赵聪聪李太良
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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