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Method for preparing nitrogen-doped graphene ink with assistance of sodium deoxycholate

A nitrogen-doped graphene and graphene ink technology, applied in the field of 3D printing materials, can solve the problems of small lamella size, unfavorable increase in lamella overlap rate, unfavorable lamella overlap rate, etc., and achieve stable dispersion. , Significant cost-effectiveness and environmental protection, good lap joint effect

Pending Publication Date: 2021-04-16
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The nitrogen-doped graphene prepared by it restores the integrity of the lattice, and the sheet size is uniform, but the sheet size is too small, only 200nm, which is not conducive to the improvement of the overlap rate of the sheet during the uniform droplet jet printing process.
[0005] Document 2 "Application Publication No. CN 105860677 A Chinese Invention Patent" discloses graphene oxide ink and its preparation method and application. The obtained ink has good stability and can be widely used in household inkjet printers, but it is difficult to retain it in multiple centrifuges. The method of clear liquid and microfiltration membrane filtration to remove unexfoliated graphite flakes makes the flake size too small, which is not conducive to the improvement of the overlap rate of flakes in the uniform droplet jet printing process, which greatly affects the recovery of graphene's electrical conductivity

Method used

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  • Method for preparing nitrogen-doped graphene ink with assistance of sodium deoxycholate
  • Method for preparing nitrogen-doped graphene ink with assistance of sodium deoxycholate
  • Method for preparing nitrogen-doped graphene ink with assistance of sodium deoxycholate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1: Graphene Oxide Preparation

[0035] (1) Add graphite powder into concentrated sulfuric acid, the concentration of graphite powder is 0.04g / mL, after fully mixing, mix according to the mass ratio of graphite and potassium permanganate ratio of 1:6, after gradient heating reaction, cool to room temperature , to obtain a mixture.

[0036] (2) Wash the mixture with deionized water until neutral, and pour off the supernatant. Complete this process with a centrifuge.

[0037] (3) Collect the bottom layer slurry, freeze-dry after ultrasonic treatment, and obtain graphene oxide powder.

[0038] In the above graphene oxide preparation method, in the above (1), the temperature gradient is set to 3, the temperature gradients are 5, 35, and 70°C in sequence, and the reaction time is 0.5, 1, and 0.5h in sequence.

[0039] And / or, in the above (2), the centrifugation speed is 8000rpm, and the time is 20min.

[0040] In (3), the duration of ultrasound is 0.5h, and the powe...

Embodiment 2

[0055] Step 1: Preparation of Graphene Oxide Powder Using Natural Flake Graphite Powder

[0056] (1) Add graphite powder into concentrated sulfuric acid, the concentration of graphite powder is 0.04g / mL, after fully mixing, mix according to the mass ratio of graphite and potassium permanganate ratio of 1:6, after gradient heating reaction, cool to room temperature , to obtain a mixture.

[0057] (2) Wash the mixture with deionized water until neutral, and pour off the supernatant. Complete this process with a centrifuge.

[0058] (3) Collect the bottom layer slurry, freeze-dry after ultrasonic treatment, and obtain graphene oxide powder.

[0059] In the above graphene oxide preparation method, in (1), five temperature gradients are set, the temperature gradients are 5, 15, 35, 45, and 70°C in sequence, and the reaction time is 0.5, 1, 1, 0.5, and 1h in sequence.

[0060] And / or, in the above (2), the centrifugation speed is 6000rpm, and the time is 15min.

[0061] In (3), ...

Embodiment 3

[0076] Step 1: Preparation of Graphene Oxide Powder Using Natural Flake Graphite Powder

[0077] (1) Add graphite powder into concentrated sulfuric acid, the concentration of graphite powder is 0.04g / mL, after fully mixing, mix according to the mass ratio of graphite and potassium permanganate ratio of 1:6, after gradient heating reaction, cool to room temperature , to obtain a mixture.

[0078] (2) Wash the mixture with deionized water until neutral, and pour off the supernatant. Complete this process with a centrifuge.

[0079] (3) Collect the bottom layer slurry, freeze-dry after ultrasonic treatment, and obtain graphene oxide powder.

[0080] In the above-mentioned graphene oxide preparation method, in the above (1), two temperature gradients are set, the temperature gradients are 2 and 65°C in sequence, and the reaction time is 2 and 8h in sequence.

[0081] And / or, in the above (2), the centrifugation speed is 10 000 rpm, and the time is 15 min.

[0082] In (3), the ...

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Abstract

The invention relates to a method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate. The method comprises the steps of: oxidizing natural flake graphite into graphene oxide which is high in oxygen content and most environmentally friendly in C6 element; carrying out hydrothermal nitrogen doping on the graphene oxide; and dispersing nitrogen-doped graphene in water, adding a surfactant in batches, carrying out ultrasonic treatment, alternately carrying out low-power and high-power ultrasonic treatment, dispersing, and spreading solute lamellas to finally obtain the nitrogen-doped graphene ink with a large lamellar stable dispersion, the lamellar size being 800-2000 nm and the thickness being 1-2 nm. The nitrogen-doped graphene ink can be used for a uniform micro-droplet jetting printing platform, and particularly can be used for printing a graphene metamaterial wave-absorbing microstructure through uniform micro-droplet jetting. The preparation method of the nitrogen-doped graphene ink has the advantages of stable dispersion, micron-scale lamella spreading and the like.

Description

technical field [0001] The invention belongs to the field of 3D printing materials, and relates to a method for preparing nitrogen-doped graphene ink assisted by sodium deoxycholate, in particular to a method for preparing a large thin-layer nitrogen-doped graphene water-based ink for uniform droplet injection. Background technique [0002] Graphene is a new type of nanomaterial composed of six-membered rings composed of a single layer of carbon atoms. Due to its excellent electrical, optical, mechanical, and thermal properties, it has great application potential in electronics, energy, and medical treatment. However, the zero-bandgap property of graphene limits its application in electronics. Chemical doping modification can effectively regulate the energy band structure and performance of graphene. Nitrogen-doped graphene (NG) changes the energy band structure of graphene, making it change from a conductive material to a semiconductor material. It is used in supercapacitor...

Claims

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Application Information

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IPC IPC(8): C01B32/192C01B32/194C09D11/30C09D11/52
CPCY02E60/50
Inventor 李贺军周菲菲齐乐华罗俊连洪程李艳
Owner NORTHWESTERN POLYTECHNICAL UNIV
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