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Small-particle-size metal phosphide nanoparticle/reduced graphene composite material and preparation method thereof

A metal phosphide and nanoparticle technology, used in phosphide, chemical instruments and methods, nanotechnology, etc., can solve the problems of large catalyst particle size, easy agglomeration, and hindering the exposure of active sites.

Active Publication Date: 2018-08-28
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particle size of transition metal phosphide catalysts currently used is relatively large, and it is very easy to agglomerate, and these disadvantages inhibit the further improvement of its catalytic activity.
Although the synthesis of metal phosphides with small particle sizes has been developed a lot, in order to prevent their agglomeration, surfactants are not lacking.
However, the presence of surfactant also hinders the exposure of its active site

Method used

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  • Small-particle-size metal phosphide nanoparticle/reduced graphene composite material and preparation method thereof
  • Small-particle-size metal phosphide nanoparticle/reduced graphene composite material and preparation method thereof
  • Small-particle-size metal phosphide nanoparticle/reduced graphene composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] (1) preparing the composite particles of silicon dioxide coated tricobalt tetroxide, specifically comprising the following steps:

[0093] (A) 348mg cobalt nitrate tetrahydrate was dissolved in 1.2ml deionized water to obtain cobalt nitrate aqueous solution;

[0094] (B) Dissolving 10g of polyoxyethylene ether in 45ml of n-hexane, heating at 50°C until clear and transparent, to obtain a n-hexane solution of polyoxyethylene ether;

[0095] (C) Add 0.2ml of cobalt nitrate aqueous solution to 50ml of polyoxyethylene ether in n-hexane solution, and stir at 50°C for 1h;

[0096] (D) Add 2ml of ammonia water to the mixed solution obtained in step (C), and continue to stir for 1h;

[0097] (E) Add 6ml of analytically pure tetraethyl silicate to the mixed solution obtained in step (D), and continue to stir for 2h;

[0098] (F) Step (E) is separated after the stirring is completed, and then the separated product is dried at 80° C. for 12 hours;

[0099] (G) calcining the produc...

Embodiment 2

[0115] (1) preparing the composite particles of silica-coated copper oxide, specifically comprising the following steps:

[0116] (A) 250mg copper sulfate pentahydrate was dissolved in 1.2ml deionized water to obtain an aqueous solution of copper sulfate;

[0117] (B) Dissolving 10g of polyoxyethylene ether in 45ml of n-hexane, heating at 55°C until clear and transparent, to obtain a n-hexane solution of polyoxyethylene ether;

[0118] (C) Add 1ml of copper sulfate aqueous solution to 50ml of polyoxyethylene ether in n-hexane solution, and stir at 55°C for 1h;

[0119] (D) Add 1ml of ammonia water to the mixed solution obtained in step (C), and continue to stir for 1h;

[0120] (E) Add 6ml of analytically pure tetraethyl silicate to the mixed solution obtained in step (D), and continue to stir for 2h;

[0121] (F) Step (E) is separated after the stirring is completed, and then the separated product is dried at 80° C. for 12 hours;

[0122] (G) calcining the product obtained...

Embodiment 3

[0130] 1) preparing composite particles of silica-coated nickel oxide, specifically comprising the following steps:

[0131] (A) 200mg nickel chloride hexahydrate is dissolved in 1.0ml deionized water to obtain an aqueous solution of nickel chloride;

[0132] (B) Dissolve 8g of polyoxyethylene ether in 45ml of n-hexane, and heat at 52°C until clear and transparent to obtain a n-hexane solution of polyoxyethylene ether;

[0133] (C) Add 0.5ml of nickel chloride aqueous solution to 50ml of polyoxyethylene ether in n-hexane solution, and stir at 52°C for 1h;

[0134] (D) Add 0.8ml of ammonia water to the mixed solution obtained in step (C), and continue to stir for 1.2h;

[0135] (E) Add 5 ml of analytically pure tetraethyl silicate to the mixed solution obtained in step (D), and continue stirring for 2 h;

[0136] (F) Step (E) is separated after the stirring is completed, and then the separated product is dried at 80° C. for 10 h;

[0137] (G) Calcining the dried product obta...

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PUM

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Abstract

The invention discloses a small-particle-size metal phosphide nanoparticle / reduced graphene composite material and a preparation method thereof. The preparation method comprises the following steps: 1) preparing silica-coated metal oxide composite particles; 2) loading the composite particles onto graphene oxide to obtain a graphene oxide-based compound; 3) removing silica of the composite particles in the graphene oxide-based compound; and 4) carrying out phosphating treatment so as to obtain the small-particle-size metal phosphide nanoparticle / reduced graphene composite material. Metal phosphide in the composite material of the invention has a small particle size, in a range of 3 nm to 5 nm; and the phosphide nanoparticles are highly dispersed in reduced graphene, which is favorable forincreasing the exposure degree of active sites. The preparation method is simple in process, low in cost, and favorable for large-scale production.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation, and relates to a small-diameter metal phosphide nanoparticle / reduced graphene composite material and a preparation method thereof, in particular to a small-diameter cobalt phosphide nanoparticle / reduced graphene composite material and its preparation method. Background technique [0002] Transition metal phosphides have been widely used in thermal catalytic hydrogenation, photo / electrocatalytic water splitting, electrocatalytic oxygen reduction, and decomposition of ammonia borane in recent years. In these applications, transition metal phosphides have shown high catalytic activity. [0003] CN 101857207 A discloses a transition metal phosphide Co 2 The preparation method and application of P. The preparation method is as follows: 1) using cobalt salt and hypophosphite as a mixed precursor, dissolving it in deionized water and stirring until completely dissolved; 2) drying the obtained ...

Claims

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Application Information

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IPC IPC(8): B01J27/14B01J27/185C01B25/08B82Y30/00
CPCB82Y30/00C01B25/08B01J27/14B01J27/1853C01P2004/04C01P2002/72C01P2004/64B01J35/394B01J35/393
Inventor 朴玲钰曹爽吴志娇司月雷张驰
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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