CN108609615B - A kind of transfer method of uniform graphene film - Google Patents

A kind of transfer method of uniform graphene film Download PDF

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CN108609615B
CN108609615B CN201810851362.XA CN201810851362A CN108609615B CN 108609615 B CN108609615 B CN 108609615B CN 201810851362 A CN201810851362 A CN 201810851362A CN 108609615 B CN108609615 B CN 108609615B
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graphene
pmma
copper foil
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sio
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CN108609615A (en
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王敏
杨金华
徐志勇
贾良鹏
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Hefei University of Technology
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/186Preparation by chemical vapour deposition [CVD]
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/194After-treatment
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
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Abstract

本发明公开了一种均匀石墨烯薄膜的转移方法,用带氧化层的硅片作为中介转移基底,转移得到的石墨烯薄膜平整度更好。同时,在将石墨烯制作成透明电极时,将石墨烯/PMMA一起转移到目标基底后,使石墨烯处于PMMA/基底的上方,无须去除PMMA,从而完全避免石墨烯中缝隙的产生,石墨烯薄膜连续性更好,制作成透明电极具有更好的均匀性和高电导率。本发明提供这种新的石墨烯薄膜高电导率均匀透明电极转移方法工艺简单,成本低廉。The invention discloses a method for transferring a uniform graphene film. A silicon wafer with an oxide layer is used as an intermediate transfer substrate, and the obtained graphene film has better flatness. At the same time, when graphene is made into a transparent electrode, after the graphene/PMMA is transferred to the target substrate together, the graphene is placed on the top of the PMMA/substrate without removing the PMMA, thereby completely avoiding the generation of gaps in the graphene. The film continuity is better, and the transparent electrode has better uniformity and high conductivity. The invention provides the novel high-conductivity, uniform and transparent electrode transfer method of the graphene film with simple process and low cost.

Description

Transfer method of uniform graphene film
Technical Field
The invention belongs to the technical field of conductive materials, and particularly relates to a transfer method of a uniform graphene film.
Background
Transparent electrodes with high optical transparency, electrical conductivity and uniformity are an important component of devices including touch screens, displays, solar cells and light emitting diodes. Graphene is a new carbonaceous material with a two-dimensional cellular structure formed by tightly packing single-layer or multiple-layer carbon atoms, wherein the carbon atoms are mutually subjected to SP (SP) passage2The carbon atoms are hybridized into bonds, each carbon atom and three adjacent carbon atoms form a strong sigma bond, the connection is very firm, a stable hexagonal shape is formed, and the light transmittance and the electrical conductivity are excellent. These characteristics make graphene an ideal substitute material for Indium Tin Oxide (ITO) which is a traditional transparent electrode material, and particularly, a high-quality single-layer or multi-layer graphene film is successfully grown on some metals by a Chemical Vapor Deposition (CVD) method, which greatly promotes the development of a graphene thin film transparent electrode. It has some inherent disadvantages including the increased cost of indium thin and brittleness due to its ceramic nature.
It is known that transparent electrodes having high conductivity and uniformity are essential for application devices. Typically, after PMMA/graphene is transferred to a target substrate with a polymer as a carrier (usually PMMA), the PMMA needs to be removed to expose the graphene surface to act as an electrode. However, in the process of removing PMMA, gaps are inevitably generated in graphene, and the generated gaps reduce charge transfer channels, thereby making the graphene sheet resistance uneven. Meanwhile, according to the experimental result, the size of the surface resistance is proportional to the size of the graphene gap, that is, the larger the gap area is, the larger the graphene surface resistance is, the smaller the conductivity is, and thus the requirement of the transparent electrode on high conductivity cannot be met. Similarly, the graphene film grown on some metals by the chemical vapor deposition method replicates the morphology of the metal substrate, and the PMMA is used to transfer the graphene from the metal substrate, so the unevenness of the microstructure of the metal substrate also causes poor flatness of the graphene, which also has a great influence on the uniformity and conductivity of the graphene transparent electrode. Therefore, it is very important to develop a method capable of improving the flatness of graphene, reducing the sheet resistance of graphene and improving the uniformity of the sheet resistance of graphene.
Disclosure of Invention
The invention aims to make up for the defects of the prior art and provides a uniform graphene film transfer method.
The invention is realized by the following technical scheme:
a uniform graphene film transfer method comprises the following steps:
(1) growing on the surface of copper foil with the thickness of 24-25um by a chemical vapor deposition method to obtain continuous graphene, spin-coating PMMA with the concentration of 100mg/ml on the surface of the graphene by a spin coater, and baking for 5-6min on a constant temperature table at the temperature of 168-172 ℃;
(2) after baking, putting the surface which is not coated with PMMA into a plasma cleaning machine for treatment for 1-2min, removing graphene on the copper foil on the back surface, and then putting PMMA/graphene/copper foil into FeCl with the concentration of 5mol/L3Etching copper foil in the solution for 25-35min, transferring to deionized water, soaking for 8-12min, and transferring to new 5mol/L FeCl3Etching the residual copper foil in the solution for 2-2.5 h to remove floccules on the copper foil, transferring the completely etched copper foil to deionized water to clean the residual FeCl3Etching solution, transferring to dilute hydrochloric acid to further clean the surface residueRemaining FeCl3Etching liquid and other impurities, finally transferring the graphene film into deionized water to clean residual hydrochloric acid on the surface of the graphene film, and after cleaning is finished, beating the graphene film for 14-16min by using a plasma cleaning machine to obtain SiO2Obtaining a sample PMMA/graphene/SiO by taking PMMA/graphene with Si2/Si;
(3) Mixing PMMA/graphene/SiO2Drying the Si sample for 2.5-3h, completely baking the sample on a constant temperature table, and then putting the sample into a tubular furnace for low-pressure annealing to remove PMMA glue;
(4) annealing and then carrying out graphene/SiO2Taking out the Si sample, spin-coating PMMA glue again, placing the sample on a constant temperature table at 165-175 ℃, baking for 5-6min, and scraping the sample to enable the SiO to be in a side-scraping mode2Exposing the/Si substrate, then putting the exposed/Si substrate into 1 mol/L HF acid for etching, transferring the substrate into deionized water after etching, and cleaning up residual HF to obtain PMMA/graphene;
(5) and (3) putting the two pieces of cleaned PET into a plasma cleaning machine for treatment for 15-16min, making the surfaces of the PET hydrophilic, and then reversely buckling PMMA/graphene to obtain graphene/PMMA, and finally transferring the graphene/PMMA/PET onto a target substrate PET to obtain the graphene/PMMA/PET with good flatness.
The PMMA model is Sigma Aldrich, #182265, and the molecular weight is 996K.
In the step 3, the temperature is controlled to be 55-65 ℃ firstly, the temperature is kept for 25-30min, then the temperature is raised to be 95-105 ℃, the temperature is kept for 25-30min, then the temperature is raised to be 165-175 ℃, and the temperature is kept for 25-30 min.
The low-pressure annealing condition in the step 3 is controlled to be 580-620 ℃ and 20 sccm Ar for 2-2.5 hours.
The invention has the advantages that:
(1) the novel graphene film transfer method does not remove PMMA carriers, does not affect the application of the graphene film as a transparent electrode, avoids the generation of graphene gaps in the PMMA removing process, and is good in continuity and uniform in conductivity.
(2) In the process of transferring graphene, the silicon wafer with the oxide layer is used as an intermediary transfer substrate, and the transferred graphene film has better flatnessThe conductivity is higher, the surface resistance value is smaller, and the conductivity is mainly distributed at 210 omega sq-1About, the minimum energy is 109 Ω sq-11/5 for graphene sheet resistance transferred directly from copper foil to remove PMMA carrier.
(3) The change coefficient of the resistance of the graphene transparent electrode film prepared by the novel graphene film transfer method can reach 3.37%, and the graphene transparent electrode film has good uniformity.
(4) The novel graphene film uniform transparent electrode transfer method is simple in process and low in cost.
Detailed Description
The technical scheme of the invention is further explained by combining the specific examples as follows:
a uniform graphene film transfer method comprises the following steps:
(1) growing on the surface of copper foil with the thickness of 25um by a chemical vapor deposition method to obtain continuous graphene, spin-coating PMMA with the concentration of 100mg/ml on the surface of the graphene by a spin coater, and baking for 5min at 170 ℃ on a constant temperature table after the spin coating;
(2) after baking, the side which is not coated with PMMA is placed into a plasma cleaning machine for treatment for 1min, graphene on the copper foil on the back side is removed, and then PMMA/graphene/copper foil is placed into FeCl with the concentration of 5mol/L3Etching copper foil in the solution for 30min, transferring to deionized water, soaking for 10min, and transferring to new 5mol/L FeCl3Etching the residual copper foil in the solution for 2 h to remove floccules on the copper foil, transferring the completely etched copper foil to deionized water to clean the residual FeCl3Etching solution, transferring to dilute hydrochloric acid to further clean FeCl remained on the surface of the etching solution3Etching liquid and other impurities, finally transferring the graphene film into deionized water to clean residual hydrochloric acid on the surface of the graphene film, and after cleaning is finished, beating the graphene film for 15min by using a plasma cleaning machine to obtain SiO2Obtaining a sample PMMA/graphene/SiO by taking PMMA/graphene with Si2/Si;
(3) Mixing PMMA/graphene/SiO2Drying the Si sample for 2.5h, completely baking the sample on a constant temperature table, wherein the baking process is carried outFirstly controlling the temperature to be 60 ℃, keeping the temperature for 30min, then heating to 100 ℃, keeping the temperature for 30min, then heating to 170 ℃, keeping the temperature for 30min, then placing the material into a tubular furnace for low-pressure annealing, controlling the condition to be 20 sccm Ar at 600 ℃, keeping the annealing for 2 hours, and removing PMMA glue;
(4) annealing and then carrying out graphene/SiO2Taking out the Si sample, spin-coating PMMA glue again, placing the sample on a constant temperature table at 170 ℃, baking for 5min, and scraping the sample to enable the SiO to be in a side-scraping mode2Exposing the/Si substrate, then putting the exposed/Si substrate into 1 mol/L HF acid for etching, transferring the substrate into deionized water after etching, and cleaning up residual HF to obtain PMMA/graphene;
(5) and (3) putting the two pieces of cleaned PET into a plasma cleaning machine for treatment for 15min, making the surfaces of the PET hydrophilic, and then reversely buckling PMMA/graphene to obtain graphene/PMMA, and finally transferring the graphene/PMMA/PET onto a target substrate PET to obtain the graphene/PMMA/PET with good flatness.

Claims (4)

1.一种均匀石墨烯薄膜的转移方法,其特征在于,包括以下步骤:1. a transfer method of uniform graphene film, is characterized in that, comprises the following steps: (1) 在24-25um厚的铜箔表面通过化学气相沉积法生长得到连续石墨烯,用匀胶机在石墨烯表面旋涂浓度为100mg/ml PMMA,旋涂完之后,放在恒温台上于168-172℃下烘烤5-6min;(1) Continuous graphene is obtained by chemical vapor deposition on the surface of 24-25um thick copper foil, and spin-coating concentration of 100mg/ml PMMA on the surface of graphene with a glue dispenser. After spin-coating, place it on a constant temperature table Bake at 168-172℃ for 5-6min; (2) 烤干后,将未旋涂PMMA那面放入等离子体清洗机中处理1-2min,去除背面铜箔上的石墨烯,然后将PMMA/石墨烯/铜箔放入浓度为5mol/L的FeCl3溶液中刻蚀铜箔,刻蚀25-35min后,再转移至去离子水中浸泡8-12min,接着再转移至新的5mol/L的FeCl3溶液中刻蚀残余的铜箔,刻蚀2-2.5 h,去除铜箔上的絮状物,铜箔完全刻蚀之后转移至去离子水中清洗残留的FeCl3刻蚀液,之后再转移至稀盐酸中进一步清洗其表面残留的FeCl3刻蚀液及其他杂质,最后将石墨烯薄膜转移至去离子水中清洗其表面的残留盐酸,清洗完毕后,用等离子体清洗机打过14-16min的SiO2/Si捞PMMA/石墨烯,得到样品PMMA/石墨烯/SiO2/Si;(2) After drying, put the non-spin-coated PMMA side into the plasma cleaning machine for 1-2min, remove the graphene on the copper foil on the back, and then put the PMMA/graphene/copper foil into a concentration of 5mol/ The copper foil was etched in L of FeCl3 solution, after etching for 25-35min, then transferred to deionized water for 8-12min, and then transferred to a new 5mol/ L FeCl3 solution to etch the remaining copper foil, Etch for 2-2.5 h to remove flocs on the copper foil. After the copper foil is completely etched, transfer it to deionized water to clean the remaining FeCl 3 etching solution, and then transfer it to dilute hydrochloric acid to further clean the remaining FeCl on the surface. 3. Etching liquid and other impurities, and finally transfer the graphene film to deionized water to clean the residual hydrochloric acid on its surface. After cleaning, use a plasma cleaning machine to scour SiO 2 /Si for 14-16min to remove PMMA/graphene, Obtain the sample PMMA/graphene/SiO 2 /Si; (3) 将PMMA/石墨烯/ SiO2/Si样品风干2.5-3h后,放恒温台上将样品完全烤干,之后放进管式炉中进行低压退火,去除PMMA胶;(3) After air-drying the PMMA/graphene/SiO 2 /Si sample for 2.5-3 hours, put it on a constant temperature table to completely dry the sample, and then put it into a tube furnace for low-pressure annealing to remove the PMMA glue; (4) 退火后将石墨烯/ SiO2/Si样品取出来再次旋涂PMMA胶,放置在165-175℃的恒温台上烤5-6 min,然后对样品进行刮边使SiO2/Si基底暴露出来,再放进1 mol/L的HF酸中刻蚀,刻蚀完转移至去离子水中清洗干净残留HF,最后得到PMMA/石墨烯;(4) After annealing, the graphene/SiO 2 /Si sample was taken out and spin-coated with PMMA glue again, placed on a constant temperature table at 165-175 °C for 5-6 min, and then the sample was scraped to make the SiO 2 /Si substrate exposed, and then etched in 1 mol/L HF acid. After etching, it was transferred to deionized water to clean the residual HF, and finally PMMA/graphene was obtained; (5) 用俩片清洗过的PET放进等离子体清洗机中处理15-16min,使其表面亲水后反扣PMMA/石墨烯,得到石墨烯/PMMA,最后再转移至目标基底PET上,得到平整度很好的石墨烯/PMMA/PET。(5) Put the cleaned PET into the plasma cleaning machine for 15-16min, make the surface hydrophilic and reverse the PMMA/graphene to obtain the graphene/PMMA, and finally transfer to the target base PET, Graphene/PMMA/PET with good flatness is obtained. 2.根据权利要求1所述的均匀石墨烯薄膜的转移方法,其特征在于,所述PMMA 型号为Sigma Aldrich,#182265,分子量为996K。2. the transfer method of uniform graphene film according to claim 1, is characterized in that, described PMMA model is Sigma Aldrich, #182265, and molecular weight is 996K. 3.根据权利要求1所述的均匀石墨烯薄膜的转移方法,其特征在于,所述步骤3中样品在恒温台上烤干过程中先控制温度为55-65℃,保持25-30min,再升温至95-105℃,保持25-30min,再升温至165-175℃,保持25-30min。3. the transfer method of homogeneous graphene film according to claim 1, is characterized in that, in described step 3, in described step 3, the control temperature is 55-65 ℃ first in the drying process on constant temperature table, keep 25-30min, then The temperature was raised to 95-105°C and kept for 25-30min, and then raised to 165-175°C and kept for 25-30min. 4.根据权利要求1所述的均匀石墨烯薄膜的转移方法,其特征在于,所述步骤3中低压退火条件控制为580-620℃下20 sccm Ar,持续2-2.5小时。4 . The method for transferring uniform graphene films according to claim 1 , wherein the low-pressure annealing conditions in the step 3 are controlled to be 20 sccm Ar at 580-620° C. for 2-2.5 hours. 5 .
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CN110156001B (en) * 2019-07-11 2023-01-03 电子科技大学 Method for transferring graphene film
CN112265985B (en) * 2020-10-30 2022-03-08 中国科学院重庆绿色智能技术研究院 Clean transfer method of wafer-level two-dimensional material
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