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Hydrothermal preparation method for NiS2 with controllable shape

A morphological and hydrothermal technology, applied in nickel sulfide, nanotechnology and other directions, can solve the problems of high production cost, flammable, explosive, and volatile, and achieve low production cost, low human toxicity, and narrow particle size distribution. Effect

Inactive Publication Date: 2012-08-15
SHENYANG LIGONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, this method uses a large amount of toxic organic substances such as benzene, pyridine, ethylenediamine, and ethylene glycol as a reaction solvent, which is flammable, explosive, and volatile, harmful to the human body, and the production cost is relatively high.

Method used

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  • Hydrothermal preparation method for NiS2 with controllable shape
  • Hydrothermal preparation method for NiS2 with controllable shape
  • Hydrothermal preparation method for NiS2 with controllable shape

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of NiS with different shapes and particle sizes by hydrothermal method 2 method, the steps are as follows:

[0035] Press Ni 2+ / S 2 o 3 2- =1 (molar ratio), weigh a certain amount of NiCl 2 ?6H 2 O and Na 2 S 2 o 3 ?5H 2 O, moved to a 100ml Teflon-lined autoclave. Then add distilled water to fill up to 80% of the total capacity of the reactor, place it on a magnetic stirrer and stir for 10 minutes to fully dissolve the solid. Then the reaction vessel was sealed and allowed to react at a constant temperature of 140°C for 12h. After the reaction kettle was naturally cooled to room temperature, the obtained product was washed several times with distilled water and ethanol, separated by centrifugation, and dried at 60°C to obtain a black product.

[0036] attached figure 1 and 2 XRD pattern and SEM pattern of the product, respectively. Both illustrate that the above-mentioned preparation product is NiS 2 , and its shape is spherical, which is re...

Embodiment 2

[0038] Preparation of NiS with different shapes and particle sizes by hydrothermal method 2 method, the steps are as follows

[0039] Prepare NiS by the step of embodiment 1 2 , The different reaction conditions are: the reaction time is 6h and 24h respectively. attached image 3 and 4 The SEM pictures of the two products are respectively, they show that the product NiS 2 The morphologies of both are spherical, indicating smoothness, but the particle diameters of the two are different, about 1μ and 5μ respectively.

[0040] This example illustrates that NiS with a spherical shape can be prepared by adopting the technology of the present invention. 2 . In conjunction with Example 1, this example emphasizes that by changing the synthesis conditions, the product NiS 2 The particle size is adjusted.

Embodiment 3

[0042] Preparation of NiS with different shapes and particle sizes by hydrothermal method 2 method, the steps are as follows

[0043] Prepare NiS by the step of embodiment 1 2 , The different reaction conditions are: the reaction temperature is 180°C. attached Figure 5 and 6 They are the XRD pattern and SEM pattern of the product respectively, both of which indicate that the above-mentioned prepared product is NiS 2 , The particle morphology is nearly quadrilateral flake, the side length is 1~2μ, and the thickness is 300~500nm. The quadrilateral flake particles are stacked in a nearly spherical form.

[0044] This example illustrates that the technology of the present invention can be used to prepare phase-pure and nearly quadrilateral plate-like NiS 2 . Compared with Example 1, this example also illustrates that by changing the synthesis conditions, the product NiS 2 shape control.

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Abstract

The invention discloses a hydrothermal preparation method for NiS2 with a controllable shape, and the method mainly comprises the following steps of: mixing nickel salt, a sulphur source and a complexing agent in a certain molar ratio, transferring the mixture into a high-pressure reactor, adding distilled water, and stirring to adequately dissolve soluble solids; adjusting the pH value of the reaction system, sealing the reactor, and reacting at a certain temperature; and washing the obtained product by use of distilled water and ethanol respectively, centrifugally separating, and drying. The hydrothermal preparation method for NiS2 with a controllable shape disclosed by the invention has the advantages of being simple in operation by using a hydrothermal method, moderate in reaction condition, narrow in particle size distribution, high in product purity, easy in industrial production, and the like. The particle shape and size of NiS2 can be controlled by adjusting the synthesis conditions such as hydrothermal reaction temperature, reaction time, complexing agent type and pH value, and the prepared NiS2 can be approximately-cube-shaped, spherical, sheet-shaped and the like. Compared with a solid-state reaction method, an ultrasonic spray pyrolysis method, a gamma-ray irradiation method and an organic solvent hot method, the NiS2 prepared by the hydrothermal method has the advantages of being low in reaction temperature and equipment demand, less in toxicity on a human body, high in safety factor, low in production cost, capable of meeting the requirements of energy conservation and emission reduction, and the like.

Description

[0001] technical field [0002] The invention belongs to the technical field of hydrothermal synthesis materials, and specifically relates to the preparation of NiS with different shapes (near cube, spherical or flake, etc.) and / or particle sizes by hydrothermal method. 2 . Background technique [0003] NeS 2 It is an important class of inorganic functional materials, and the outer electron layer structure of the sulfur atom is 3s 2 threesome 4 , d orbitals can also participate in bonding under certain conditions, thus making NiS 2 Exhibit special optical, electrical, magnetic and catalytic properties. NeS 2 It is a pyrite structure, when pressurized to 32kPa at 22°C, NiS 2 It gradually transitions from an insulating state to a metallic state, showing metal conductivity, having the properties of a semiconductor material, and can exhibit weak ferromagnetism or antiferromagnetism at different temperatures. At the same time, it can interact with Ag 2 S is compounded int...

Claims

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Application Information

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IPC IPC(8): C01G53/11B82Y40/00
Inventor 曹晓晖孟锦宏陈威宏杨少华林保山
Owner SHENYANG LIGONG UNIV
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