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A kind of preparation method of nanometer fluorinated graphene with high fluorine content

A technology of fluorinated graphene and fluorine content, applied in graphene, chemical instruments and methods, nano-carbon, etc., can solve problems such as impossible to reach nano-level, no practical significance, etc., to increase the reaction contact area, reduce The effect of small particle size

Active Publication Date: 2022-06-14
厦门中科希弗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has no practical significance. The traditional so-called nano-graphite is prepared by mechanical grinding, and it is impossible to reach the nanometer level. The micron level is already the limit that grinding can achieve.

Method used

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  • A kind of preparation method of nanometer fluorinated graphene with high fluorine content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Step 1: Put 50g of graphene into the fluorination equipment, pass fluorine gas, keep the pressure at 95KPa, and react at 450-500℃ for 12h.

[0020] Step 2: Weigh 100 g of the low-fluorine fluorinated graphene prepared in step 1, add 500 mL of N-methylpyrrolidone, transfer it to a ball milling jar of a planetary ball mill, and perform ball milling for 5 hours at a rotational speed of 600 r / min to obtain fluorinated graphene slurry.

[0021] Step 3: Transfer the fluorinated graphene slurry prepared in step 2 into a plastic bottle, add 200 mL of N-methylpyrrolidone, and carry out ultrasonic separation under the condition of 50 kHz for 24 hours to obtain a fluorinated graphene dispersion, which is spray-dried, A low fluorine content nano-fluorinated graphene powder is obtained.

[0022] Step 4: Put 50g of the low fluorine content nano-fluorinated graphene powder prepared in step 3 into the fluorination equipment, pass in the mixed gas containing 20% ​​fluorine gas, keep th...

Embodiment 2

[0030] Step 1: Put 50g graphene into the fluorination equipment, pass fluorine gas, keep the pressure at 80KPa, and react at 450°C for 8h.

[0031] Step 2: Weigh 100 g of nano-fluorinated graphene with low fluorine content obtained in step 1, mix the nano-fluorinated graphene with low fluorine content with 500 mL of liquid-phase solvent, and transfer to a planetary ball mill for ball milling after mixing evenly. In the tank, the fluorinated graphene slurry was obtained at a rotational speed of 300 r / min and a ball milling time of 2 h.

[0032] Step 3. Transfer the fluorinated graphene slurry obtained in step 2 into a plastic bottle, add a liquid-phase solvent to mix, and after mixing evenly, transfer it to an ultrasonic separator, and perform ultrasonic treatment at an ultrasonic frequency of 20 kHz for 1 h to obtain For the fluorinated graphene dispersion liquid, the fluorinated graphene dispersion liquid is spray-dried to obtain nano-fluorinated graphene powder with low fluo...

Embodiment 3

[0036] Step 1: Put 50g of graphene into the fluorination equipment, pass fluorine gas, keep the pressure at 90KPa, and react at 485°C for 12h.

[0037] Step 2: Weigh 100 g of nano-fluorinated graphene with low fluorine content obtained in step 1, mix the nano-fluorinated graphene with low fluorine content with 2000 mL of liquid-phase solvent, and transfer it to a planetary ball mill for ball milling after mixing evenly. In the tank, the fluorinated graphene slurry was obtained at a rotational speed of 500 r / min and a ball milling time of 12 h.

[0038] Step 3: Transfer the fluorinated graphene slurry obtained in step 2 into a plastic bottle, add a liquid-phase solvent to mix, and after mixing evenly, transfer to an ultrasonic separator, and ultrasonically treat it for 12 hours at an ultrasonic frequency of 60 kHz to obtain For the fluorinated graphene dispersion liquid, the fluorinated graphene dispersion liquid is spray-dried to obtain nano-fluorinated graphene powder with lo...

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Abstract

The invention relates to the technical field of nanomaterials, and discloses a method for preparing nano-fluorinated graphene with high fluorine content. Firstly, fluorine gas is used as a fluorine source through step 1. The fluorine gas has strong reactivity and can carry out graphene Etching, so as to realize chemical fragmentation, reduce the particle size of graphene, and effectively prepare nano-fluorinated graphene with low fluorine content in nanometer size. Secondly, through ultrasonic dispersion and high-energy ball milling in steps 2 and 3, further reduce fluorine The particle size of fluorinated graphene, and finally through the high-temperature fluorination reaction of fluorine-containing gas in step 4, the fluorine content in the nano-fluorinated graphene powder with high fluorine content is finally guaranteed; after rationally designed reaction steps, finally obtained The nano-fluorinated graphene powder with high fluorine content and nano-scale particle size has a structural size below 100nm.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a preparation method of nanometer fluorinated graphene with high fluorine content. Background technique [0002] As a new derivative of graphene, fluorinated graphene not only maintains the high strength of graphene, but also brings novel interface and physicochemical properties such as surface energy reduction, hydrophobicity enhancement and band gap broadening due to the introduction of fluorine atoms. . At the same time, fluorinated graphene has high temperature resistance, stable chemical properties, and exhibits properties similar to PTFE, which is called "two-dimensional Teflon". Fluorinated graphene has reduced surface energy, enhanced hydrophobicity, high temperature resistance, and stable chemical properties. It can be used as a tunnel barrier or as a high-quality insulator or barrier material, and can also be used in light-emitting diodes and displays. New nanoe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/194B82Y40/00
CPCB82Y40/00C01B32/194C01B2204/32
Inventor 叶荣森
Owner 厦门中科希弗科技有限公司