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Continuous super-light regularly-oriented pure graphene aerogel film and preparation method thereof

A graphene airgel, graphene technology, applied in the direction of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of unnoticed airgel film performance, unguaranteed graphene airgel film, size limitation Structural design and other issues to achieve the effect of reducing edge defects, enhancing performance, and reducing the internal resistance of electrical and thermal conduction

Active Publication Date: 2016-07-06
ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the size limitation of graphene and the lack of structural design, graphene airgel does not inherit the superior properties of graphene.
[0005] At present, the method used to prepare continuous graphene airgel films is mainly solution spinning, but it does not pay attention to the influence of graphene size on the performance of airgel films, and the rough high-temperature reduction process does not guarantee that graphite Graphene airgel film can successfully inherit the perfect properties of graphene itself

Method used

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  • Continuous super-light regularly-oriented pure graphene aerogel film and preparation method thereof
  • Continuous super-light regularly-oriented pure graphene aerogel film and preparation method thereof
  • Continuous super-light regularly-oriented pure graphene aerogel film and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1: Preparation of Graphene Oxide without Fragmentary Super Large Sheets

[0033] Example 1-1

[0034] (1) Slowly add potassium permanganate into the rapidly stirring concentrated sulfuric acid at -10°C. After fully dissolving, add graphite, stir slowly at 60 rpm for 2 hours, then stop stirring. Reaction 6h, obtain the graphite oxide crystal of wide distribution respectively; As figure 1 As shown, there are more fragments in the graphite oxide wafers obtained under the two temperatures, which makes its corresponding graphene oxide also have a lot of fragments ( figure 2 ).

[0035](2) The reaction solution obtained in step 1 is diluted with concentrated sulfuric acid (the dilution factor can be any multiple, and the present embodiment is diluted about 10 times), and the graphite oxide crystals are filtered out with a titanium alloy mesh sieve with a 150um aperture (140 mesh) (Reaction solution recovery), and slowly pour into rapidly stirred ice water relative...

Embodiment 2

[0043] Embodiment 2: Using the non-fragmented super large sheet of graphene oxide prepared in embodiment 1 to prepare a continuous ultra-light and regularly oriented pure graphene airgel film.

[0044] (1) After continuously extruding the graphene oxide aqueous solution with a concentration of 10 mg / mL and an average size of 110 um from a preparation device with an inline outlet at a constant speed (between 10 m / min), stay in liquid nitrogen for 20 seconds, and solidify To form a graphene oxide gel film, freeze the graphene oxide gel film in a refrigerator at -4°C for 5 hours.

[0045] (2) Send the graphene oxide airgel film after the freezing treatment in step 1 into a high-temperature furnace for high-temperature heat treatment. The treatment method is: first raise the temperature to 400°C at 2°C / min in an inert gas atmosphere, keep it warm for 1h, and then In an inert gas atmosphere, heat up to 1300°C at 3°C / min, hold for 2h, then raise the temperature to 3000°C at 4°C / min,...

Embodiment 3

[0049] Embodiment 3: Using the non-fragmented super large sheet of graphene oxide prepared in embodiment 1 to prepare a continuous ultra-light and regularly oriented pure graphene airgel film.

[0050] Continuously extrude an aqueous solution of a certain concentration of ultra-large pieces of non-fragmented graphene oxide (average size of 150um) from a preparation device with a straight-shaped outlet (the device is a cuboid structure with a gradually narrowing straight-shaped die opening in the middle) After exiting, enter the coagulation solution for a period of time, solidify into a graphene oxide gel film, and put it into the refrigerator for slow freezing or quick freezing in liquid nitrogen. The concentration of the ultra-large flake-free graphene oxide solution is between 100 mg / mL. The speed of the continuous uniform extrusion into the coagulation liquid is between 10m / min and the temperature is 30°C. The coagulation liquid is liquid nitrogen. The residence time in t...

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Abstract

The invention relates to a continuous super-light regularly-oriented pure grapheme aerogel film and a preparation method thereof. The preparation method comprises: after oversized fragment-free graphene oxide with a certain concentration is extruded out by virtue of a linear die orifice, solidifying the graphene oxide into a graphene oxide gel film, and putting the graphene oxide gel film into a refrigerator for slow freezing or into liquid nitrogen for quick freezing; and performing freeze-drying or supercritical drying to obtain a graphene oxide aerogel film, and performing high-temperature heat treatment on the graphene oxide aerogel film in a high-temperature furnace to obtain a high-thermal-conductivity and high-electric-conductivity super-light oriented graphene aerogel film. The electric conductivity of the graphene aerogel film is 100-10000S / m, the thermal conductivity of the graphene aerogel film is 50-800W / mK, and the shielding effectiveness of the graphene aerogel film at 500MHz-40GHz reaches 100-150dB. The preparation method provided by the invention is simple in process, low in energy consumption, green and environment-friendly, capable of realizing continuous operation, capable of being applied to efficient electromagnetic shielding, flexible thermal conduction and electric conductive materials and the like.

Description

technical field [0001] The invention relates to the field of high-performance carbon film materials, in particular to a continuous ultra-light regularly oriented pure graphene airgel film and a preparation method thereof. Background technique [0002] With the rapid development of the electronic industry, the integration of electronic devices is getting higher and higher, the electromagnetic wave emission power of electronic devices is getting higher and higher, and the size of electronic devices is getting smaller and smaller. In addition, nuclear power and aerospace materials have higher and higher requirements for low-density thermal and conductive shielding, and light-weight high-performance carbon materials have attracted more and more attention. [0003] Graphene is a two-dimensional monolayer crystal with the highest strength (Young's modulus, 1100GPa; breaking strength, 125GPa) of known materials, extraordinary specific surface area of ​​2630M2 / g) and excellent elect...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01B2204/22C01B2204/24C01B2204/32C01P2002/72C01P2004/03
Inventor 高超彭蠡孙海燕杨清
Owner ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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