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Preparation method of high-quality wafer-level graphene single crystal

A graphene and wafer-level technology, which is applied in the field of high-quality wafer-level graphene single crystal preparation, can solve the problems of time-consuming and consumable materials, complex process, harsh conditions, etc., and achieve short time-consuming, simple processing method and repeatability high effect

Active Publication Date: 2019-11-15
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods are dangerous, complex process, harsh conditions, time-consuming consumables and other deficiencies [1],[5],[6]

Method used

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  • Preparation method of high-quality wafer-level graphene single crystal
  • Preparation method of high-quality wafer-level graphene single crystal
  • Preparation method of high-quality wafer-level graphene single crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The difference between this Example 1 and Comparative Example 1 is that the electrochemically polished copper foil is subjected to plasma treatment, the plasma equipment is used, the air valve is opened, the power is adjusted to 100W, the pressure is stabilized between 400-500Pa, and the treatment time for 30 minutes. Other implementation methods are the same as Comparative Example 1. The resulting graphene single crystal SEM morphology is as follows figure 1 As shown in (b), it can be seen from the figure that the nucleation density of the graphene single crystal is effectively reduced, and there are only two graphene single crystals in the area in the figure. Experimental comparison shows that the number of graphene single crystal nucleation drops sharply after copper foil is treated by plasma. This method proves that plasma treatment can effectively control the nucleation density of graphene single crystal.

Embodiment 2

[0053] The copper foil is electrochemically polished, the electrolyte solution is pure phosphoric acid, the constant voltage is 3V, and the polishing time is 30 minutes. Then wash with deionized water and ethanol, and blow dry with nitrogen. The polished and cleaned copper foil is treated with plasma, the plasma equipment is used, the air valve is opened, the power is adjusted to 100W, the pressure is stabilized between 400-500Pa, and the treatment time is 30 minutes. Then put it into a chemical vapor deposition reaction furnace, feed 500 sccm argon gas, heat up to 1000°C, then feed 10 sccm hydrogen gas, anneal at constant temperature for 30 minutes, and introduce 10 sccm methane to react for 60 minutes. Turn off methane after reaction finishes, cool down to room temperature rapidly (cooling time is 20 minutes). The photo of the obtained graphene single crystal is shown in the figure figure 2 As shown in (a), and its graphene single crystal domain area is 1-2mm, the monolay...

Embodiment 3

[0055] The difference between the present embodiment 3 and the embodiment 2 is that the graphene single crystal is grown by temperature programming, and after the constant temperature annealing treatment, the graphene single crystal growth temperature is raised from 1000°C to 1080°C (the heating rate is about 1.3°C / min ) process imports carbon source, and the continuation reaction time is 60 minutes. Other implementation methods are the same as in Example 2. The photo of the obtained graphene single crystal is shown in the figure figure 2 As shown in (b), and its graphene single crystal domain area is about 5mm, the monolayer graphene coverage rate is 96%, and the mobility is 12000cm -2 v -1 the s -1 . Depend on figure 2 It can be seen that the temperature-programmed growth method can effectively accelerate the growth rate of graphene single crystal. Combined with Ranman ( image 3 ) and TEM ( Figure 4 ) shows that the prepared graphene single crystal has good cryst...

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Abstract

The invention provides a preparation method of a high-quality wafer-level graphene single crystal. The method comprises the following steps: placing plasma-treated metal foil into a reaction furnace,introducing an inert atmosphere, performing heating to an annealing temperature, introducing hydrogen gas, and performing annealing treatment, wherein the metal foil is one selected from the group consisting of copper foil, nickel foil, molybdenum foil and cobalt foil, the plasma treatment atmosphere is at least one selected from the group consisting of air, hydrogen gas, argon gas, oxygen gas, and nitrogen gas, the power is 100-150 W, the pressure is 400-500 Pa, and the time is 1-30 min; and introducing a carbon source into the reaction furnace, adjusting the annealing temperature to a growthtemperature of the graphene single crystal, starting growth of the graphene single crystal, and after growth is completed, performing cooling to a room temperature.

Description

technical field [0001] The invention relates to a method for preparing high-quality wafer-level graphene single crystals, belonging to the field of graphene single crystals. Background technique [0002] Since the discovery of graphene by two scientists from the University of Manchester in 2004, and its research and application so far, graphene has shown immeasurable application prospects due to its excellent performance. The unique crystal structure of graphene endows it with novel properties, such as high thermal conductivity, high mechanical strength, high mobility, high light transmission, etc. [0003] Although graphene has great potential applications in many fields, there is still a long way to go to study how to prepare high-quality and large-scale graphene single crystals. Among the existing preparation methods, the vapor phase deposition method is generally adopted. This method mainly uses metal as a catalyst, which is simple to operate and prepares graphene sing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B25/18C30B29/02
CPCC30B25/186C30B29/02
Inventor 黄富强程园毕辉
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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