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Method for preparing hollow ball of sulfide and oxide of nickel

A chalcogenide and hollow sphere technology, applied in binary selenium/tellurium compounds, nickel oxide/nickel hydroxide, nickel sulfide, etc., can solve the problem of difficulty in synthesizing nickel disulfide crystals, and achieve easy operation and experimental scheme. Simple, low-equipment effect

Active Publication Date: 2013-04-24
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there have been few reports on nickel disulfide so far, partly because it is difficult to synthesize nickel disulfide crystals with a single phase, let alone nickel disulfide with regular morphology (Adv.Fun.Mater.,2002.12 (4): p.277-285)
And there are few literature reports about the conversion technology between nickel chalcogenides and their oxides

Method used

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  • Method for preparing hollow ball of sulfide and oxide of nickel
  • Method for preparing hollow ball of sulfide and oxide of nickel
  • Method for preparing hollow ball of sulfide and oxide of nickel

Examples

Experimental program
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Embodiment 1

[0025] Embodiment 1, the preparation of nickel disulfide hollow sphere

[0026] Weigh 0.5mmol hexahydrate and nickel nitrate into a 50ml reactor with 20ml deionized water, then add 2mmol L-cysteine ​​and 0.5mmol urea, ultrasonicate at room temperature, and then put the reactor into 140 °C heating for 24 hours, filtering and washing to obtain nickel disulfide hollow spheres.

Embodiment 2

[0027] Embodiment 2, the preparation of nickel sulfide and nickel oxide hollow spheres

[0028] The obtained nickel disulfide is respectively roasted at 350-450° C. and 650-800° C. for 1 hour to obtain nickel monosulfide and nickel oxide hollow spheres respectively.

Embodiment 3

[0029] Embodiment 3, the preparation of nickel diselenide and nickel ditelluride hollow spheres

[0030] 0.5mmol nickel disulfide powder is put into the reactor that has the hydrazine hydrate of 20ml, then add 1mmol selenous acid and 0.5mmol tellurous acid respectively, heat 24 hours under 140 ℃ of conditions, filter, wash to obtain disulfide Nickel selenide and nickel ditelluride hollow spheres.

[0031] Synthetic nickel chalcogenides and oxide hollow spheres such as Figure 1-6 As shown, it shows that the hollow nanospheres have a uniform diameter of about 2 microns and a shell thickness of 60-150 nanometers.

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Abstract

The invention discloses a method for preparing a hollow ball of sulfide and oxide of nickel. The method comprises the following steps: (1), adopting ultrasonic or mechanical stirring to disperse nickel nitrate, L-cysteine and urea uniformly in deionized water; (2), transferring the mixed liquid into a reaction kettle, and reacting for 8 to 48 hours at a temperature of 140 DEG C to obtain a nickel disulphide hollow ball; (3), calcinating nickel disulphide at different temperatures to obtain hollow balls of nickel monosulfide and nickel oxide respectively; and (4), under hydrothermal condition, reacting nickel disulphide with selenium source and tellurium source respectively for 4 to 48 hours at a temperature of 140 DEG C to obtain hollow balls of nickel diselenide and nickel telluride. According to the method, raw materials are cheap, easy to obtain, and convenient to compound; the required devices are simple; no pollution is caused in the production process; and the large scale production can be realized rapidly.

Description

technical field [0001] The present invention relates to a kind of preparation technology of transition metal chalcogenide compound group and oxide hollow sphere, particularly a kind of preparation and preparation of nickel sulfide, nickel disulfide, nickel diselenide, nickel ditelluride and nickel oxide hollow sphere its transformation technology. Background technique [0002] Since the properties of the material are not only affected by the chemical composition of the material, but also by the shape and size of the material (Angew.Chem.Int.Ed., 2006.45(21):p.3414-3439). Nano / micro hollow spheres refer to a class of materials with special structures ranging in size from nanometers to micrometers. Their properties are very different from those of bulk materials, because the hollow part of such materials can accommodate a large number of guest molecules or large-sized guests, resulting in some peculiar effects. Due to the characteristics of low density, large specific surfac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11C01G53/04C01B19/04B82Y40/00
Inventor 刘小鹤马炜周科朝邱冠周
Owner CENT SOUTH UNIV
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