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Nitrogen-doped graphene-metal nanoparticle film and preparation method thereof

A metal nanoparticle, nitrogen-doped graphene technology, applied in graphene, metal processing equipment, nano-carbon and other directions, can solve the limitations of large-scale, continuous preparation of graphene films, difficult to disperse, coordinate and solidify, impossible Solidification molding and other problems, to achieve the effect of good strength and toughness, simple operation, excellent thermal conductivity

Pending Publication Date: 2022-04-15
杭州嘉悦智能设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]Macroscopically assembled graphene film is a main form of macroscopic nano-scale graphene sheets. Commonly used methods include suction filtration, scraping film, and spin coating and spraying methods, etc., but these methods limit the large-scale and continuous preparation of graphene films
The patent literature with the publication number CN104229784A discloses two methods for preparing graphene membranes: one, by wet spinning, depositing a membrane in a coagulation solution such as an inorganic metal salt solution, drying it, and then reducing it with a reducing agent The two-step method prepares ion-enhanced graphene membranes. Although this method provides a method for continuously preparing graphene membranes by wet spinning, the preparation process is cumbersome, and two-step methods are required to achieve graphene membranes. The defect that the precipitant remains in the film and cannot be removed by heat treatment; second, the graphene solution is used as a raw material, and the film is solidified in a coagulation solution containing coordination ions, and dried to obtain an ion-enhanced graphene film. , although the preparation method is simple, due to the characteristics of graphene itself without special functional groups, it is difficult to disperse in organic solvents or water and coordinate solidification with coordination ions, and the concentration of the solution is also difficult to meet the requirements of solidification and forming. Concentration, so it is basically impossible to solidify and form graphene solution as a raw material in the coagulation solution of coordination ions

Method used

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  • Nitrogen-doped graphene-metal nanoparticle film and preparation method thereof
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Examples

Experimental program
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Effect test

Embodiment 1

[0042] The preparation method of graphene oxide solution:

[0043]10g of graphite, 150ml of 98% sulfuric acid, 30ml of 69% nitric acid were added to a 500ml Erlenmeyer flask and stirred at room temperature for 24 hours, slowly poured into 1L of water to collect the solid, washed 3 times, and dried at 80°C for 4 hours to obtain pre-oxidized graphite. Repeat the pre-oxidation process twice. Put the dried pre-oxidized graphite into a box furnace to thermally expand at 950°C for 20s to obtain thermally expanded graphite oxide. Mix 5g of heat-expandable graphite oxide with 300ml of sulfuric acid (concentration 98%), 5g of potassium persulfate, and 7g of phosphorus pentoxide in a 500ml wide-mouth conical flask, heat at 80°C for 4 hours, dilute with 2L of water, filter and wash, and air Dry for 3 days to obtain pre-oxidized heat-expandable graphite. Mix dry pre-oxidized heat-expandable graphite with 200ml sulfuric acid (concentration 98%) at a low temperature of 0-5°C, add 20g pota...

Embodiment 2

[0046] The preparation method of graphene oxide solution is as embodiment 1.

[0047] Mix the graphene oxide solution, platinum nanoparticles with a particle size of 20-50nm, and ethylenediamine to obtain a mixture (slurry), wherein the content of graphene oxide is 1mg / mL mixture, graphene oxide and platinum nanoparticles The mass ratio of ethylenediamine is 1:0.1, and the mass fraction of ethylenediamine relative to the mixture is 20%. The mixture is coated into a film, dried at 85°C for 4h to obtain an amine-based cross-linked graphene oxide-metal nanoparticle film, and then heat-treated to obtain a nitrogen-doped graphene-metal nanoparticle film (heat treatment temperature is 2000°C, time is 3h) , and finally the nitrogen-doped graphene-metal nanoparticle film is calendered to obtain a nitrogen-doped graphene-metal nanoparticle film with high thermal conductivity. The thickness and thermal conductivity of the resulting highly thermally conductive nitrogen-doped graphene-me...

Embodiment 3

[0049] The preparation method of graphene oxide solution is as embodiment 1.

[0050] A mixture of graphene oxide solution, silver nanoparticles and lead nanoparticles with a particle size of 100-200nm (the mass ratio of silver nanoparticles and lead nanoparticles is 1:1), ammonia and triethylenetetramine is uniformly mixed to obtain a mixture (slurry), wherein, the content of graphene oxide is 80mg / mL mixture, the mass ratio of graphene oxide and metal nanoparticles total amount is 1:1, and the mass fraction of ammonia relative to the mixture is 30%, triethylenetetramine The mass fraction relative to the mixture is 5%. The mixture is coated into a film, dried at 75°C for 8 hours to obtain an amine-based cross-linked graphene oxide-metal nanoparticle film, and then heat-treated to obtain a nitrogen-doped graphene-metal nanoparticle film (heat treatment temperature is 1500°C, time is 4h) , and finally the nitrogen-doped graphene-metal nanoparticle film is calendered to obtain ...

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Abstract

The invention discloses a nitrogen-doped graphene-metal nanoparticle film and a preparation method thereof, and the preparation method comprises the following steps: (1) uniformly mixing a graphene oxide solution, metal nanoparticles and a water-soluble amine cross-linking agent to obtain a mixture; wherein the mass ratio of the graphene oxide to the metal nanoparticles is (1: 0.01)-(1: 5); (2) coating the mixture obtained in the step (1) to form a film, and drying at 20-95 DEG C to obtain an amino cross-linked graphene oxide-metal nanoparticle film; and (3) carrying out heat treatment on the amino cross-linked graphene oxide-metal nanoparticle film obtained in the step (2) under the protection of inert gas to obtain the nitrogen-doped graphene-metal nanoparticle film. In the graphene oxide solution, the metal nanoparticles and the water-soluble amine cross-linking agent, a graphene oxide solution coating method is adopted, solidification and self-assembly of the amino cross-linked graphene oxide-metal nanoparticle film can be achieved at the same time in one step, and the method is low in reaction temperature, easy to operate, environmentally friendly, capable of achieving large-scale preparation, simple, controllable and suitable for industrial production. The single condition is easy to operate.

Description

technical field [0001] The invention relates to the field of graphene films, in particular to a nitrogen-doped graphene-metal nanoparticle film and a preparation method thereof. Background technique [0002] As the most basic structural unit of all carbon materials, graphene has a true single atomic layer thickness and strict two-dimensional structure, and has high mechanical strength, elasticity, thermal conductivity, electrical conductivity, and quantum Hall effect. Since British scientists (Andre Geim) Andre Geim and (Konstantin Novoselov) Kostyanovosenov won the Nobel Prize for discovering graphene in 2010, the research on graphene has reached an unprecedented climax, and more and more researches It is found that it has great application prospects in special fields such as energy storage, electrical devices, catalysis and biomedicine. [0003] The macroscopically assembled graphene film is a main form of macroscopic nanoscale graphene sheets. The commonly used methods i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/192C01B32/194B22F1/054B82Y30/00
CPCC01B32/192C01B32/194B82Y30/00C01B2204/32C01B2204/24
Inventor 安学会张鹏李迎春程进辉
Owner 杭州嘉悦智能设备有限公司
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