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Method of printing and in situ reduction of graphene

A technology of graphene and graphene ink, which is applied in the field of materials, can solve the problems of etching transfer, inability to tile and disperse, and high production cost, and achieve the effect of sufficient reduction process, novel preparation path, and simple reduction process

Inactive Publication Date: 2021-02-26
南通第六元素材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Among these three methods, (1) graphene prepared by vapor deposition method has the most complete conjugated structure of its six-membered carbon ring, which can be used to prepare high-quality graphene films, but the shrinkage of the film is poor, and the preparation process It needs to be carried out on metal substrates such as copper, and it needs to be etched and transferred after completion, which will cause problems such as defect introduction and pattern destruction, and the preparation cost is extremely high
The patterning operations of graphene mainly include maskless direct laser writing, masked plasma etching, and vapor deposition growth on pre-patterned metal substrates. Although these techniques provide relatively high-resolution graphene patterns, but The method of using laser, mask and vacuum will increase the process cost, and the above-mentioned technologies are mostly used in small-area manufacturing in the actual production process
(2) Using the method of graphene powder slurry printing, graphene itself has a large surface energy and curls and agglomerates, which requires the use of high-boiling polar solvents, and it cannot be spread flat and dispersed in solvents, and in most cases However, additional surfactants or dispersants are required, so the graphene sheets cannot be effectively overlapped to form a conductive network after printing, which is affected by additives such as surfactants and dispersants, and the prepared patterns have poor conductivity.
(3) The graphene oxide powder slurry printing method is adopted. Due to the presence of polar functional groups, graphene oxide can be flattened and dispersed in water. After printing into a pattern, as the water volatilizes, the graphene oxide sheets can be densely stacked face to face to form It is better to build a plane, but it needs to further reduce the graphene oxide film. Thermal reduction can be used, but it requires a higher temperature (usually above 800 ° C), which will damage the substrate. Chemical reduction can also be used, but it needs Soak the pattern in chemical agents, soaking will cause the film to fluff up and dissolve again, and the restoration effect is not good

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0040] A normal temperature reaction in-situ reduction graphene circuit pattern, the preparation process of which comprises the following steps:

[0041] (1) Use graphene oxide and deionized water as raw materials, 30KHz ultrasonic in a water bath for 1 hour, prepare graphene oxide ink, the mass fraction of graphene oxide is 0.5% (the consumption ratio of graphene oxide and water is 5.0 mg: 1.0mL), the viscosity is 10cp, and the surface tension is 30mN / m.

[0042] figure 1 It is a picture of the graphene oxide ink prepared in Example 1 of the present invention. The graphene oxide ink is stable and can be stored for a long time.

[0043] (2) Clean the PET flexible substrate by immersing it in ethanol solution, take it out, wipe it dry with dust-free paper, and place it in an oven at 60°C for 30 minutes to dry.

[0044](3) Wash the liquid storage tank of the inkjet printer (MicroFab Jetlab 4) for 3 times with deionized water, and observe whether the liquid at the nozzle (80 μm...

Embodiment 2

[0049] A kind of thick graphene circuit pattern of normal temperature reaction in-situ reduction, its preparation process comprises the following steps:

[0050] (1) Use graphene oxide and deionized water as raw materials, use an emulsifier, rotate at 5000rpm, stir for 30min, prepare graphene oxide ink, the mass fraction of graphene oxide is 1% (that is, the consumption ratio of graphene oxide and water 10.0mg: 1.0mL), the viscosity is 30cp, and the surface tension is 70mN / m.

[0051] (2) Soak the PET flexible substrate in pure water for cleaning, take it out and dry it with a dust-free paper.

[0052] (3) Wash the liquid storage tank of the inkjet printer (MicroFab Jetlab 4) for 3 times with deionized water, and observe whether the liquid at the nozzle (80 μm) is a uniform and elongated fluid. When it is observed that the nozzle has no fibers or ink stains, the prepared graphene oxide solution can be injected into the No. 1 liquid storage tank, and the printing parameters of...

Embodiment 3

[0059] A graphene pattern reduced in situ by normal temperature reaction, the preparation process of which comprises the following steps:

[0060] (1) Use graphene oxide and a solvent as raw materials, wherein the solvent is a mixed solvent of water and ethanol, and the volume ratio of water and ethanol is 9:1. Ultrasound at 30KHz in a water bath for 1 hour at 30°C to prepare a graphene oxide ink with a mass fraction of graphene oxide of 1% (that is, the ratio of graphene oxide to water is 10.0mg: 1.0mL) and a viscosity of 30cp. The tension is 70mN / m.

[0061] (2) Wash the liquid storage tank of the inkjet printer (model MicroFab Jetlab 4) with deionized water for 3 times, and observe whether the liquid at the nozzle (80 μm) is a uniform and slender fluid. When it is observed that the nozzle has no fibers or ink stains, the prepared graphene oxide solution can be injected into the No. 1 liquid storage tank, and the printing parameters of the inkjet printer can be adjusted. Th...

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Abstract

The invention discloses a method for printing and in-situ reduction of graphene. On the basis of a printing technology, graphene oxide slurry is used for patterning printing on a substrate, a chemicalreducing agent is further used, normal-temperature chemical reduction is carried out on the pattern in situ, and then the reduced high-conductivity graphene pattern is obtained. According to the method, the graphene oxide pattern does not need to be transferred, and the reducing agent is directly printed on the pattern in situ, so that rapid chemical reduction is carried out, compact stacking ofgraphene sheet layers and original precise patterns can be kept in the process, the reduction process is simple, and the reduction effect is good.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to a method for printing and in-situ reducing graphene. Background technique [0002] Graphene has gradually become a potential substitute for existing conductors and semiconductors due to its excellent optical and electrical properties. Graphene's intrinsic optoelectronic properties can be used in electronic components, such as sensors, diodes, photodetectors, radio frequency antennas, terahertz antennas, etc. Its preparation method has three kinds usually: (1) adopt chemical vapor deposition method, prepare transparent, patterned graphene monolayer material [quote patent, CN104023993B forms patterned graphene layer; CN108545725A a kind of graphene preparation device and application The device patterned method for growing graphene], (2) disperse the graphene powder to form a slurry, and prepare a patterned graphene assembly by coating, printing and other methods [citing patent CN1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184
CPCC01B32/184C01B2204/22C01B2204/24
Inventor 唐润理吕松伟吴艳红瞿研
Owner 南通第六元素材料科技有限公司
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