Preparation method for graphene-supported metal nanoparticle compound

A metal nanoparticle, metal-loaded technology, applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc. Mild conditions, the effect of reducing the occurrence of defects

Active Publication Date: 2012-06-20
苏州慧闻纳米科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are mainly two methods to prepare graphene-loaded metal nanoparticle composites. One is to mix the precursors of graphene oxide and metal ions uniformly, and then add a reducing agent to synthesize graphene-loaded metal nanoparticle composites in one step. One method is simple and fast, but the structure and morphology of the prepared metal nanoparticles are difficult to control, which affects the properties of the composite; the other is to reduce graphene oxide and metal ion precursors in two steps, and prepare graphene-loaded metals by adsorption. Nanoparticle composites, this method is more complicated, but it can effectively control the structure and morphology of metal nanoparticles, and give full play to the excellent performance of graphene-supported metal nanoparticle composites
[0004] Prior to the present invention, previous work mainly used hydrazine hydrate and its derivatives as reducing agents to prepare graphene-loaded metal nanoparticle composites, but hydrazine hydrate and its derivatives have strong toxicity and volatility, and cannot be used For large-scale use, and the prepared complex will be doped with a lot of nitrogen atoms, which will affect the physical and chemical properties of the complex
In the past two years, there have also been reports in the literature that ascorbic acid (VC), sodium borohydride (NaBH 4 ), polydiallyldimethylammonium chloride (PDDA), etc. as reducing agents to prepare graphene-loaded metal nanoparticle composites, but these reactions must be carried out at high temperatures, the reactions are more violent, and it is easy to increase the graphene Defects

Method used

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  • Preparation method for graphene-supported metal nanoparticle compound
  • Preparation method for graphene-supported metal nanoparticle compound

Examples

Experimental program
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Embodiment 1

[0026] (1) washing and purification

[0027] Dissolve 1 mg of graphene oxide into 10 ml of water, ultrasonically disperse and dissolve, then centrifugally wash 3 times with 3% HCl and water at 20,000 rpm, and add deionized water to obtain a uniform 1 mg / ml graphite oxide alkene aqueous solution;

[0028] (2) Synthesis of 3nm gold particles

[0029] 5ml of 0.5mM HAuCl 4 and 5ml of 0.2M cetyltrimethylammonium bromide (CTAB) into a 25ml Erlenmeyer flask, mix well, add 0.6ml of 0.01M NaBH 4 , placed at room temperature for 3 hours;

[0030] (3) Synthesis of graphene oxide-supported 3nm gold particle composite

[0031] Add 1ml of 1mg / ml graphene oxide aqueous solution to the 3nm gold particle solution, mix well, and wash with water for 6 times at 20,000 rpm to obtain the graphene oxide-loaded 3nm gold nanoparticle composite, add 5ml deionized water, and ultrasonically 5 minutes to obtain a homogeneous solution;

[0032] (4) Synthesis of graphene-loaded 3nm gold particle compo...

Embodiment 2

[0036] (1) washing and purification

[0037] Dissolve 1 mg of graphene oxide into 10 ml of water, ultrasonically disperse and dissolve, then wash with 3% HCl and water for 3 times at 20,000 rpm, and add deionized water to obtain a uniform 1 mg / ml graphene oxide aqueous solution;

[0038] (2) Synthesis of 10nm gold particles

[0039] 5ml of 0.5mM HAuCl 4 and 5ml of 0.2M cetyltrimethylammonium bromide (CTAB) into a 25ml Erlenmeyer flask, mix well, add 0.6ml of 0.01M NaBH 4 , placed at room temperature for 3 hours to obtain 3nm gold particles;

[0040] 6ml of 0.5mM HAuCl 4 and 6ml of 0.02M cetyltrimethylammonium chloride (CTAC) into a 25ml Erlenmeyer flask, mix well, then add 4.5ml of 0.1M ascorbic acid (Vc) to the flask, and finally add 0.3ml of 3nm Gold particle seeds, placed at room temperature for 3 hours to obtain 10nm gold particles;

[0041] (3) Synthesis of graphene oxide-supported 10nm gold particle composite

[0042] Add 1ml of 1mg / ml graphene oxide aqueous solu...

Embodiment 3

[0047] (1) washing and purification

[0048] Dissolve 1 mg of graphene oxide into 10 ml of water, ultrasonically disperse and dissolve, then wash with 3% HCl and water for 3 times at 20,000 rpm, and add deionized water to obtain a uniform 0.1 mg / ml graphene oxide aqueous solution;

[0049] (2) Synthesis of graphene oxide platinum nanoparticle composites

[0050] 100ul of 0.01M H2 PtCl 6 Add to 10ml of 0.1mg / ml graphene oxide aqueous solution, mix well, add 1mg of NaBH 4 , placed at room temperature for 3 hours, centrifuged and washed with water for 6 times at 20,000 rpm to obtain a graphene oxide-loaded platinum nanoparticle composite, adding 5ml of deionized water, and ultrasonicating for 5 minutes to obtain a uniform solution;

[0051] (3) Synthesis of graphene-supported platinum nanoparticle composites

[0052] Add 10mg NaBH 4 Put it into the graphene oxide-supported platinum nanoparticle aqueous solution, oscillate evenly, place at room temperature for 2 hours, centrif...

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Abstract

The invention discloses a preparation method for a graphene-supported metal nanoparticle compound. The method comprises the following steps of: preparing metal nanoparticles with uniform size through controllable synthesis; uniformly supporting the metal nanoparticles on graphene oxide through adsorption; and catalyzing NaBH4 at normal temperature to reduce the graphene oxide by taking the metal nanoparticles as a catalyst so as to obtain the graphene-supported metal nanoparticle compound. By using the method provided by the invention, the compounds with strong toxicity and volatility such as hydrazine hydrate and derivatives thereof are prevented from being used as reducing agents to prepare the graphene-supported metal nanoparticle compound; the method has the characteristics of environmental friendliness, safety and the like; meanwhile, the method can be performed under the conditions of room temperature and different acid-base (pH) conditions with mild reaction conditions. Through the method, various noble metals and transition metal nanoparticles can be supported on the graphene, and some metal oxides for catalyzing decomposition of NaBH4 can also be supported.

Description

technical field [0001] The invention relates to the technical field of nanocomposite material preparation, in particular to a method for preparing a graphene-loaded metal nanoparticle composite. Background technique [0002] Graphene-supported metal nanoparticle composites have excellent catalytic ability, outstanding electrical conductivity and optical properties, and can be widely used in many fields such as sensors, photovoltaic cells, and organic synthesis catalysts. [0003] Hummer, Brodie, Staudenmaier and other methods can prepare graphene oxide on a large scale, and then reduce it to obtain graphene by adding reducing agents such as hydrazine hydrate and benzylamine under heating conditions. At present, there are mainly two methods to prepare graphene-loaded metal nanoparticle composites. One is to mix the precursors of graphene oxide and metal ions uniformly, and then add a reducing agent to synthesize graphene-loaded metal nanoparticle composites in one step. One ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F1/00B01J37/02
Inventor 孙旭辉卓其奇马艳芸
Owner 苏州慧闻纳米科技有限公司
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