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Preparation method for chestnut-shaped copper sulphide hollow micron sphere composed of nanosheets

A nano-sheet, copper sulfide technology, applied in copper sulfide and other directions, to achieve the effect of high specific surface free energy, less agglomeration and damage, and large specific surface area

Inactive Publication Date: 2013-04-24
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, soluble copper salt, ethylenediamine (en), CS 2 As a raw material, the method of preparing chestnut-shaped copper sulfide hollow microspheres composed of nanosheets by hydrothermal-inverted microemulsion-interfacial reaction method has not been reported in the literature.

Method used

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  • Preparation method for chestnut-shaped copper sulphide hollow micron sphere composed of nanosheets
  • Preparation method for chestnut-shaped copper sulphide hollow micron sphere composed of nanosheets
  • Preparation method for chestnut-shaped copper sulphide hollow micron sphere composed of nanosheets

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh 8.52g CuCl 2 2H 2 Dissolve O with deionized water, add 6.69mL of ethylenediamine (en) copper chloride and ethylenediamine, the ratio of the amount of copper chloride to ethylenediamine is 1:2, transfer to a 100mL volumetric flask, and dilute to 100mL with deionized water 0.5mol / L[Cu(en) 2 ] 2+ solution.

[0031] (2) Mix 2.26mL octylphenol polyoxyethylene (9) ether (Triton X-100), 2.08mL n-hexanol and 35mL cyclohexane with 2mL 0.5mol / L [Cu(en) 2 ] 2+ The solution is mixed (ω=30, P=4.5), and the volume of cyclohexane is 8.1 times of the volume of octylphenol polyoxyethylene (9) ether and n-hexanol. Heating to 50°C, and stirring vigorously for 10 minutes to obtain a uniform [Cu(en) 2 ] 2+ inverse microemulsion. Then, add 0.18mL CS to the inverse microemulsion 2 (CS 2 The amount of the substance is 1.5 times that of ethylenediamine), and stirred evenly to obtain a mixed solution. The mixture was injected into a Teflon-lined reactor, and reacted at 120°...

Embodiment 2

[0035] (1) Weigh 7.48g CuSO 4 ·5H 2 Dissolve O with deionized water, add 5.02mL ethylenediamine (en) (the ratio of the amount of copper sulfate to ethylenediamine is 1:2.5), transfer to a 100mL volumetric flask, and dilute to 100mL 0.3mol with deionized water / L[Cu(en) 2 ] 2+ solution.

[0036] (2) Mix 3.39mL octylphenol polyoxyethylene (9) ether (Triton X-100), 2.04mL n-butanol and 32mL isooctane with 2mL 0.3mol / L [Cu(en) 2 ] 2+ The solutions are mixed (ω=20, P=4.0), and the volume of isooctane is 6 times of the sum of volumes of octylphenol polyoxyethylene (9) ether and n-butanol. Heating to 40°C, and stirring vigorously for 20 minutes to obtain a uniform [Cu(en) 2 ] 2+ inverse microemulsion. Then, add 0.13mL CS to the inverse microemulsion 2 (CS 2 The amount of the substance is 1.8 times that of ethylenediamine), stirred evenly to obtain a mixed solution. The mixed solution was injected into a polytetrafluoroethylene-lined reactor and reacted at 125°C for 6 hours...

Embodiment 3

[0040] (1) Weigh 19.32g Cu(NO 3 ) 2 ·3H 2 Dissolve O with deionized water, add 11.78mL ethylenediamine (en) (the ratio of the amount of copper nitrate to ethylenediamine is 1:2.2), transfer to a 100mL volumetric flask, and dilute to 100mL 0.8mol with deionized water / L[Cu(en) 2 ] 2+ solution.

[0041] (2) Mix 1.69mL of alkylphenol polyoxyethylene (10) ether (OP-10), 2.19mL of n-octanol and 39mL of n-octane with 2mL of 0.8mol / L [Cu(en) 2 ] 2+ The solutions are mixed (ω=40, P=5.0), and the volume of n-octane is 10 times of the sum of volumes of alkylphenol polyoxyethylene (10) ether and n-octanol. Heating to 45°C, and stirring vigorously for 30 minutes, a uniform [Cu(en)-containing 2 ] 2+ inverse microemulsion. Then, add 0.34mL CS to the inverse microemulsion 2 (CS 2 The amount of the substance is 1.6 times that of ethylenediamine), and stirred evenly to obtain a mixed solution. The mixed solution was injected into a Teflon-lined reactor, and reacted at 110° C. for 1...

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Abstract

The invention provides a preparation method for a chestnut-shaped copper sulphide hollow micron spheres composed of nanosheets. The method comprises the steps of dissolving soluble cuprate through deionized water, adding ethaidene diamine (en), obtaining a [Cu(en)2]2+ solution, mixing a surface active agent, cosurfactant and an oil phase with the [Cu(en)2]2+ solution, heating and stirring the mixed solution, obtaining reversed-phase microemulsion containing the [Cu(en)2]2+, adding CS2 into the reversed-phase microemulsion containing the [Cu(en)2]2+, after stirring and hydro-thermal treatment, cooling and centrifugally separating the microemulsion, obtaining black precipitation, washing and drying the precipitation, and obtaining the hexagonal-phase chestnut-shaped copper sulphide hollow micron spheres with the diameter of 0.5 to 0.9 micron. Each chestnut-shaped copper sulphide hollow micron sphere is composed of single crystal nanosheets with the length of 50 to 190nm, the width of 10 to 20nm and the thickness of 2 to 4nm. Products manufactured by the method are controllable in particle size and shape, good in dispersity and free of agglomeration. The method has the advantages that production technology is simple, reaction parameters are easy to control, implementation cost is low, and large-scale industrial production is prone to achievement. The method can be widely used for preparation of metal sulfide nanostructure materials with special shapes.

Description

technical field [0001] The invention relates to a method for preparing an inorganic functional nanostructure material, in particular to a method for preparing chestnut-shaped copper sulfide hollow microspheres composed of nanosheets by using a hydrothermal-inverted microemulsion-interface reaction method. Background technique [0002] As an important P-type semiconductor material, copper sulfide has excellent optical, electrical, magnetic and other physical and chemical properties, and is widely used in solar cell devices, thermoelectric cooling materials, photocatalysis, high-capacity lithium-ion battery cathode materials, Microwave protective coatings and nonlinear optical materials and other fields. In recent years, nanomaterials, especially nanostructures with special morphology constructed of one-dimensional and two-dimensional nanomaterials, have attracted scientific and technological workers due to their excellent optical, electrical, catalytic and other properties an...

Claims

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Application Information

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IPC IPC(8): C01G3/12
Inventor 朱启安吴尧谭志刚郭讯枝谭香占凯
Owner XIANGTAN UNIV
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