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Graded porous honeycomb nickel oxide microsphere and preparation method thereof

A hierarchical porous and honeycomb-shaped technology, applied in the direction of nickel oxide/nickel hydroxide, etc., can solve the problems of high cost, high energy consumption, cumbersome preparation process, etc., and achieve the effects of saving production energy, improving production efficiency and short reaction time

Active Publication Date: 2020-06-26
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Usually, the synthesis methods of mesoporous nickel oxide mainly include silica hard template method, carbon hard template method and other methods, but the preparation process of the above methods is relatively cumbersome, requires multi-step processing, and has high energy consumption, high cost, and easy to pollute the environment; The currently reported microspherical nickel oxide generally has difficulties such as easy agglomeration and difficult size control.
However, it is more challenging to simultaneously control the microsphere morphology and make it have tunable microsphere size and tunable mesopore size.

Method used

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  • Graded porous honeycomb nickel oxide microsphere and preparation method thereof
  • Graded porous honeycomb nickel oxide microsphere and preparation method thereof
  • Graded porous honeycomb nickel oxide microsphere and preparation method thereof

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preparation example Construction

[0025] The invention provides a preparation method of hierarchical porous honeycomb nickel oxide microspheres, comprising the following steps:

[0026] Mix nickel sulfate hexahydrate, urea, water and glycerin to obtain a mixed solution;

[0027] performing a hydrothermal reaction on the mixed solution to obtain a precursor product;

[0028] The precursor product is calcined to obtain the hierarchical porous honeycomb nickel oxide microspheres.

[0029] The invention mixes nickel sulfate hexahydrate, urea, water and glycerol to obtain a mixed solution.

[0030] In the present invention, the mass ratio of nickel sulfate hexahydrate to urea is preferably (0.24-0.28):(0.06-0.60), more preferably (0.25-0.26):(0.48-0.60).

[0031] In the present invention, the volume ratio of glycerol to water is preferably (0-18):(36-18), more preferably 1:35, 1:5, 1:2 or 1:1.

[0032] In the present invention, the ratio of the total solid mass of nickel sulfate hexahydrate and urea to the total...

Embodiment 1

[0043] Dissolve 0.263g of nickel sulfate hexahydrate into 36mL of deionized water at room temperature to obtain a green clear solution, then add 0.48g of urea to the above solution and stir well. The synthesized mixture was transferred to a Teflon-lined stainless steel autoclave and hydrothermally heated at 140 °C for 1 h. After the hydrothermal reaction was completed, the green product was collected by centrifugation after cooling to room temperature, washed three times with deionized water and absolute ethanol, and dried in an oven at 60°C for 12 hours to obtain a green product (precursor product). In order to remove residual intermediate products, the sample was heat-treated in a tube furnace at 400°C for 20 hours to collect hierarchical porous honeycomb nickel oxide microspheres, named NiO-1, with a specific surface area of ​​131.1 m 2 / g.

Embodiment 2

[0045] Dissolve 0.263g of nickel sulfate hexahydrate in 35mL of deionized water at room temperature to obtain a green clear solution, then add 0.48g of urea to the above solution, add 1mL of glycerol and stir until uniform. The above liquid was transferred to a polytetrafluoroethylene-lined stainless steel autoclave, and hydrothermally heated at 140°C for 1 hour. After the hydrothermal reaction was completed, the green product was collected by centrifugation after being cooled to room temperature, washed three times with deionized water and absolute ethanol, and dried in an oven at 60°C for 12 hours to obtain a green product. The resulting product was heat-treated in a tube furnace at 400°C for 20 hours, and the porous honeycomb nickel oxide microsphere product was collected, named NiO-2, with a specific surface area of ​​135.6m 2 / g.

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Abstract

The invention provides a preparation method of hierarchical porous honeycomb nickel oxide microspheres, and belongs to the field of micro-nano material preparation. In the hydrothermal reaction of thepresent invention, in the first stage of the growth process, glycerol and Ni<2+> in a reaction system form coordination, and react with CO3<2-> and OH<-> generated by urea hydrolysis to form a primary core; in the second stage of the growth process, the original primary core is adsorbed by a chelating agent of glycerol and nickel, is used as an end-capping reagent to adjust the form by reducing the surface energy, and finally is converted into a highly symmetrical flower-shaped structure; and in a urea-glycerol mixture system, the adopted non-surfactant organic small molecule glycerol template contains more hydroxyl groups, glycerol is firstly gathered through the hydrogen bond effect, then a mesoporous structure is formed through the interaction of the hydrogen bond and the hydroxyl group of the urea hydrolysis inorganic phase, and finally the hierarchical porous honeycomb-shaped nickel oxide microspheres are obtained through calcination.

Description

technical field [0001] The invention relates to the technical field of preparation of micro-nano materials, in particular to a hierarchical porous honeycomb nickel oxide microsphere and a preparation method thereof. Background technique [0002] Stoichiometric nickel oxide is a good insulator, but oxygen is always in excess in practice, and nickel oxide usually behaves as a p-type semiconductor with a bandgap energy of 3.6-4.0eV. Due to the advantages of high natural abundance, low toxicity, low environmental impact and strong stability, nickel oxide has received extensive attention in recent years. For example, nickel oxide nanostructure materials are used as electrode materials because of their high specific capacitance and low resistance, which can be used to manufacture high-energy and power supercapacitors; they are also promising candidates for making resistive random access memories. material due to its display of high-speed, low-voltage, high-stability, and reliable...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/04
CPCC01G53/04C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2006/12C01P2006/16C01P2006/17C01P2004/34
Inventor 耿旺昌徐诗露闫毅张秋禹
Owner NORTHWESTERN POLYTECHNICAL UNIV
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