Preparation method of graphene oxide/iron disulfide composite nano particles

A technology of composite nano-particles and iron disulfide, applied in the direction of iron sulfide, chemical instruments and methods, carbon compounds, etc., can solve high-demand problems, achieve good dispersion, good application prospects, and simple and easy-to-control production process

Inactive Publication Date: 2013-02-06
JIANGSU UNIV
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Problems solved by technology

Mainly include: electrochemical deposition method, hydrothermal method, solvothermal method and mechanical ball milling method, etc. Among these methods, the requirements of electrochemical deposition method are relatively high, and S 2- However, the mechanical ball milling method is difficult to solve the FeS 2 Therefore, hydrothermal method and solvothermal method are ideal, but their requirements are still very high. For example, Qian et al. used solvothermal synthesis technology to prepare granular FeS with toluene as solvent. 2 Powder crystal; FeS with irregular morphology was obtained by using ethylenediamine as solvent 2 Nanorods, but the above method has higher requirements for the experiment and needs to be tested in anhydrous state

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  • Preparation method of graphene oxide/iron disulfide composite nano particles
  • Preparation method of graphene oxide/iron disulfide composite nano particles
  • Preparation method of graphene oxide/iron disulfide composite nano particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In an ice bath, 0.015 g of graphite powder was dispersed into 25 mL of concentrated sulfuric acid with a mass fraction of 98%, and potassium permanganate (KMnO 4 ), the added potassium permanganate (KMnO 4 ) to graphite in a mass ratio of 3:1-4:1, stir evenly, and when the temperature rises to 30°C, add 45 mL of deionized water and 15 mL of 30% H 2 o 2 , stirred evenly, centrifuged, and washed repeatedly with 5% hydrochloric acid solution, deionized water and acetone to obtain graphene oxide nanosheets.

Embodiment 2

[0025] (1) 0.2 g ferrous chloride tetrahydrate (FeCl 2 4H 2 O) Dissolve in 20 mL deionized water, stir until dissolved to obtain solution Ⅰ;

[0026] (2) Add 10 mL of PVA solution (3% mass fraction) and 0.05 g of PVP to solution I, stir well, then add 5 mL of 0.75 mol / L sodium hydroxide dropwise to obtain solution II;

[0027] (3) Add 0.2 g of sulfur powder to solution II, stir and dissolve to obtain solution III;

[0028] (4) Add 50 mg graphene oxide to solution Ⅲ, and ultrasonically disperse until uniform to obtain a solution ;

[0029] (5) the solution Under the environment of 180°C, the hydrothermal reaction was carried out for 12 h, and iron disulfide nanoparticles were obtained after cooling and centrifuging. The microscopic morphology of the prepared samples was observed by scanning electron microscopy, and the results were as follows figure 1 As shown, the sample is a spherical structure with uniform size and good dispersion, with an average diameter of about 30...

Embodiment 3

[0031] (1) 0.3 g ferrous chloride tetrahydrate (FeCl 2 4H 2 O) Dissolve in 20 mL deionized water, stir until dissolved to obtain solution Ⅰ;

[0032] (2) Add 10 mL of PVA solution (3% mass fraction) and 0.1 g of PVP to solution I, stir well, then add 5 mL of 0.75 mol / L sodium hydroxide dropwise to obtain solution II;

[0033] (3) Add 0.2 g of sulfur powder to solution II, stir and dissolve to obtain solution III;

[0034] (4) Add 50 mg graphene oxide to solution Ⅲ, and ultrasonically disperse until uniform to obtain a solution ;

[0035] (5) Solution Under the environment of 200°C, the hydrothermal reaction was carried out for 24 h, and the graphene / iron disulfide composite nanoparticles were obtained after cooling and centrifugation. The microscopic morphology of the prepared samples was observed by scanning electron microscopy, and the results were as follows figure 2 As shown, the sample is an octahedral structure with uniform size and good dispersion, and the avera...

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Abstract

The invention relates to nano FeS2 materials, and particularly relates to a preparation method of graphene oxide / iron disulfide composite nano particles. According to the preparation method of the graphene oxide / iron disulfide composite nano particles, ferrous chloride tetrahydrate (FeCl2.4H2O) and sulfur powder are used as raw materials, are dissolved in water together with surfactant polyvinyl alcohol (PVA) and polyvinylpyrrolidone (PVP), and then mixed with graphene oxide under a certain pH (potential of hydrogen) condition; the obtained mixed solution is arranged in a reaction kettle and sealed, is held for 12 hours to 24 hours in a constant-temperature box at 180 DEG C to 200 DEG C by using a hydrothermal method, is cooled to normal temperature, stood and separated, centrifugally washed and dried, finally the graphene oxide / iron disulfide composite nano particles can be obtained.

Description

technical field [0001] The present invention relates to nanometer FeS 2 The material, specifically, is a graphene oxide / iron disulfide (GO / FeS 2 ) Preparation method of composite nanoparticles. Background technique [0002] Cubic FeS 2 It has a suitable band gap, high light absorption coefficient, abundant element reserves, good environmental compatibility, low preparation cost, and excellent photovoltaic conversion performance. In recent decades, researchers have focused on its crystal structure and photoelectric performance. , photoelectrochemical performance, film formation technology and application of photoelectric conversion devices and other aspects have carried out in-depth and meticulous research, making FeS 2 Significant progress has been made in the application of depolarized anode materials for photoelectrochemical cells, lithium-ion batteries, and hydrogen production devices. [0003] Due to nano-FeS 2 The material has its special characteristics. In recent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01G49/12B82Y30/00C01B32/198
Inventor 唐华吕绍飞李文静季晓瑞吴孔强唐国刚
Owner JIANGSU UNIV
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