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Preparation method of transition metal oxide/sulfide nano composite material

A nano-composite material, transition metal technology, applied in nickel oxide/nickel hydroxide, cobalt oxide/cobalt hydroxide, chemical instruments and methods, etc., can solve the process of difficult control reaction, difficult core-shell hollow material, complex method and other problems, to achieve the effect of uniform size, wide applicability, and simple and easy method.

Inactive Publication Date: 2017-07-21
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hard template method first prepares the core of the inner layer and then coats the hard template, and then grows the shell material to remove the middle template to obtain the hollow core-shell material. The method is relatively complicated.
The soft template method uses some self-assembled and easy-to-remove materials similar to vesicles as templates, but it is difficult to control the reaction process and it is not easy to obtain core-shell hollow materials with regular shapes.
At present, in the field of MOF materials, although there have been many reports on the preparation of MOF-based core-shell nanomaterials (see literature Huo J, Marcello M, Garai A, et al. MOF-Polymer Composite Microcapsules Derived from Pickering Emulsions. Advanced Materials, 2013 , 25(19): 2717-2722.), but generally speaking, this method is limited by two aspects. First, most of the prepared spherical hollow structures are simple, and other complex shapes and structures are rarely seen. ; Secondly, the obtained MOF material has a very wide size distribution
Therefore, it is still a challenge to use MOF materials to prepare hollow core-shell nanomaterials with regular structure and uniform size.

Method used

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  • Preparation method of transition metal oxide/sulfide nano composite material
  • Preparation method of transition metal oxide/sulfide nano composite material
  • Preparation method of transition metal oxide/sulfide nano composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Weigh 66 mg K 3 [Fe(CN) 6 ] was added to 20 ml deionized water to prepare a solution;

[0028] (2) Weigh 142 mg of NiCl 2 ·6H 2 O, 0.25 g of sodium citrate and 0.3 g of PVP (K29 model) were sequentially added to 30 mL of deionized water and mixed, and ultrasonicated for 5 min;

[0029] (3) Add the solution prepared in step (1) dropwise to solution (2), and stir vigorously for 10 min, then cover with plastic wrap and react at 30 °C for 24 h, the solution turns into an orange-yellow dispersion And there is a small amount of precipitation, put it in a centrifuge tube and centrifuge at 10,000 rpm for 5 min, and centrifuge the obtained precipitate with water and absolute ethanol for 4 times, and finally dry it in an oven at 60 °C for 12 h Obtain powder A;

[0030] (4) Weigh 30 mg of powder A obtained in step (3) and add it to a solution prepared by 5 ml of water and 20 ml of absolute ethanol, and then slowly add 0.3 g of Na 2 S·9H 2 O, after reacting for 10 min un...

Embodiment 2

[0033] (1) Weigh 99 mg K 3 [Fe(CN) 6 ] was added to 30 ml deionized water to prepare a solution;

[0034] (2) Weigh 213 mg of CoCl 2 ·6H 2 O, 0.35 g of sodium citrate and 0.65 g of PVP (K29 model) were sequentially added to 45 mL of deionized water and mixed, and ultrasonicated for 15 min;

[0035](3) Add the solution prepared in step (1) dropwise to solution (2), and stir vigorously for 15 min, then cover with plastic wrap and react at 38 °C for 16 h, the solution turns into an orange-yellow dispersion And there is a small amount of precipitation, put it in a centrifuge tube and centrifuge at 11,000 rpm for 8 min, and wash the obtained precipitate with water and absolute ethanol for 5 times, and finally dry it in an oven at 60 °C for 12 h Obtain powder A;

[0036] (4) Weigh 45 mg of powder A obtained in step (3) and add it to a solution prepared by 8 ml of water and 20 ml of absolute ethanol, and then slowly add 0.45 g of Na 2 S·9H 2 O, after reacting for 10 min under ...

Embodiment 3

[0039] (1) Weigh 132 mg K 3 [Fe(CN) 6 ] was added to 40 ml deionized water to prepare a solution;

[0040] (2) Weigh 284 mg of CoCl 2 ·6H 2 O, 0.5 g of sodium citrate and 0.6 g of PVP (K29 model) were sequentially added to 60 mL of deionized water and mixed, and ultrasonicated for 10 min;

[0041] (3) Add the solution prepared in step (1) dropwise to solution (2), and stir vigorously for 10 min, then cover with plastic wrap and react at 30 °C for 24 h, the solution turns into an orange-yellow dispersion And there is a small amount of precipitation, it is placed in a centrifuge tube and centrifuged at 10,000 rpm for 10 min, and the obtained precipitate is washed with water and absolute ethanol for 6 times, and finally dried in an oven at 60 °C for 12 h Obtain powder A;

[0042] (4) Weigh 30 mg of powder A obtained in step (3) and add it to a solution prepared by 5 ml of water and 20 ml of absolute ethanol, and then slowly add 0.6 g of Na 2 S·9H 2 O, after reacting for 10...

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Abstract

The invention discloses a preparation method of a transition metal oxide / sulfide nano composite material. The preparation method includes: adopting a room-temperature standing method to combine cobalt and nickel transition metal ions with potassium ferricyanide organic ligand to prepare a Prussian blue derivative nanocube; adding sodium sulfide into a water solution for vulcanization reaction to obtain a Prussian blue derivative nanocube with a vulcanized shell; calcining to obtain a MOF-based transition metal oxide / sulfide nanocube composite material with a core-shell structure. The transition metal oxide / sulfide nanocube composite material prepared by the method breaks through limitation that most structures of conventional MOF-based composite materials are simple spherical hollow structures, and structure of the composite material is a nanocube with the core-shell structure, so that size is uniform; the composite material has wide applicability in preparation methods of MOF-based transition metal compounds and has great application prospect in the field of supercapacitors and lithium ion batteries.

Description

technical field [0001] The invention relates to a preparation method of a transition metal oxide / sulfide nanocomposite material, belonging to the technical field of nanomaterial preparation. Background technique [0002] MOF materials have attracted people's attention due to their regular crystal structure, tunable pore structure, and open active sites. As a new type of nanomaterial, in the field of MOF materials, the core-shell hollow structure with different composition structures has shown certain advantages. Different from ordinary solid nanoparticles, hollow nanomaterials can effectively utilize the advantages of hollow volume and high specific surface area, and because the structure of this complex hollow material is stable, it can effectively improve electrochemical performance and realize energy storage and electrochemical catalysis. Wide application in the field. [0003] At present, the method of synthesizing this complex hollow core-shell structure material is m...

Claims

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Application Information

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IPC IPC(8): C01G53/04C01G53/11C01G51/04C01G51/00
CPCC01G51/04C01G51/30C01G53/04C01G53/11C01P2002/72C01P2004/03C01P2004/38C01P2004/80C01P2006/40
Inventor 詹红兵张超琦
Owner FUZHOU UNIV
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