New progress and prospects of mechanical exfoliation technology of two-dimensional materials

Huang Xin-Yu; Han Xu; Chen Hui; Wu Xu; Liu Li-Wei; Ji Wei; Wang Ye-Liang; Huang Yuan

doi:10.7498/aps.71.20220030

Abstract

Since the monolayer graphene was first obtained in the year of 2004, mechanical exfoliation technique has been widely used to prepare various two-dimensional materials such as transition metal dichalcogenides and black phosphorus. Among a variety of preparation techniques of two-dimensional materials, mechanical exfoliation technique shows advantages in its simplicity and universality. More importantly, the exfoliated two-dimensional samples are the ideal ones for many novel phenomena. This paper introduces the background of mechanical exfoliation technique and summarizes the problems of conventional mechanical exfoliation technique in the development of two-dimensional materials. In order to solve the problems of low efficiency and small sample size of conventional mechanical exfoliation technique, some modified mechanical exfoliation techniques have been developed, such as oxygen-plasma-assisted exfoliation method and gold-film-assisted exfoliation method. As a commonly used “top-down” preparation method, the new exfoliation technology is still full of vitality in basic research and application of two-dimensional materials. In the future, larger size and higher quality will be the development direction of exfoliation technology.

Keywords:

Authors and contacts

1.
Advanced Research Institute of Multidisciplinary Sciences, Beijing Institute of Technology, Beijing 100081, China
2.
MIIT Key Laboratory for Low-Dimensional Quantum Structure and Devices, School of Integrated Circuits and Electronics, Beijing Institute of Technology, Beijing 100081, China
3.
School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China
4.
Department of Physics, Renmin University of China, Beijing 100872, China

Corresponding author: Wang Ye-Liang, yeliang.wang@bit.edu.cn ; Huang Yuan, yhuang@bit.edu.cn

Funds: Project supported by the National Key Research and Development Program of China (Grant Nos. 2019YFA0308000, 2018YFA0704201), the National Natural Science Foundation of China (Grant Nos. 62022089, 92163206, 61725107, 11874405) and the Chongqing Science Fund for Distinguished Young Scholars (Grant No. 2021ZX0400005).

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References

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Cited By

图 1 (a)(b)美国华盛顿大学的Ruoff等利用AFM针尖在石墨烯柱上将石墨烯推开^[3]; (c)英国曼切斯特大学Geim课题组利用胶带解理的薄层石墨烯^[5]; (d)利用STM针尖实现了对石墨烯的折叠和展开^[4] .

Figure 1. (a)(b) Ruoff et al. from the University of Washington in the United States used AFM tip to push graphene away on a graphene column^[3]; (c) The thin layers of graphene was exfoliated from tape, which reported from Geim's group at the University of Manchester in the UK^[5]; (d) folding and unfolding graphene using STM tips^[4].

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图 2 (a)第1个单层MoS₂材料中观察到的荧光光谱^[16]; (b)单层MoS₂的场效应晶体管中观察到高开关比电流响应^[14]; (c)薄层黑磷器件在电场调控下的输运特性^[18]

Figure 2. (a) Fluorescence spectra was observed in the first monolayer MoS₂ material^[16]; (b) high switching ratio current response was observed in monolayer MoS₂ FET^[14]; (c) transport characteristics of thin layer black phosphorus devices under electric field regulation^[18] .

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图 3 转角石墨烯中的能带结构及超导特性^[19,20]

Figure 3. Band structure and superconductivity in magic-angle graphene superlattices^[19,20] .

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图 4 (a)氧气等离子体辅助的方法制备的单层石墨烯和Bi2212样品^[23]; (b)大面积的单层Bi2212晶体中的超导特性^[24]

Figure 4. (a) Monolayer graphene and Bi2212 samples prepared by an oxygen plasma-assisted exfoliation method^[23]; (b) superconductivity in a large-area of monolayer Bi2212 crystal^[24].

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图 5 普适性解理技术制备的多种二维材料及表征 (a) 新型机械解理的步骤; (b)—(e)不同基底上解理得到的大面积MoS₂; (f)(g)解理得到的多种大面积二维材料; (h)—(j)异质结及悬空二维材料的拉曼光谱及荧光光谱^[26]

Figure 5. Mechanical exfoliation of different monolayer materials with macroscopic size: (a) Illustration of the modified exfoliation process; (b)–(e) optical images of large-area MoS₂ exfoliated on different substrates; (f)(g) a variety of large-area two-dimensional materials obtained by exfoliation; (h)–(j) Raman and photoluminescence (PL) spectra of heterostructure and suspended 2D material^[26].

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图 6 (a)(b)解理在金膜上的单层WSe₂和MoTe₂的STM图像; (c)单层MoTe₂的低能电子衍射斑点; (d)利用ARPES测得的单层WSe₂能带结构; (e)金属膜导电性测试, 以及在薄层金属膜上观察到的MoTe₂超导电性^[26]

Figure 6. (a)(b) STM images of monolayer WSe₂ and MoTe₂ exfoliated onto Au layer; (c) LEED pattern of monolayer MoTe₂; (d) ARPES band structure of monolayer WSe₂; (e) electrical measurements of metal films and superconductivity of MoTe₂ observed on thin metal films^[26].

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图 7 块状TMDs单晶的逐层解理过程示意图(a)方法(1)在超平整的硅晶圆上沉积金膜; (2)在表面悬涂一层PVP; (3)使用热敏胶带(TRT)提取PVP和金膜; (4)将超平整的金膜压在块状vdW晶体的表面上; (5)解理单层并转移到衬底上; (6)加热去除TRT; (7)将PVP溶解在水中; (8)将金溶解在I₂/I^–蚀刻剂溶液中; (9)获得具有宏观尺寸的单晶单层. (b)从AB堆垛的TMDs晶体产生偶数层和奇数层的逐层解理技术示意图. (c)从左上角所示的厘米大小的WSe₂单晶中依次解理的6个单层样品(在SiO₂/Si衬底上)的光学图像^[32]

Figure 7. Schematic illustration of the layer-by-layer exfoliation procedure of bulk TMDs single crystals. (a) Method: (1) Depositing gold on ultraflat silicon wafer; (2) spin-coating the surface with a layer of PVP; (3) using thermal release tape (TRT) to pick up the PVP and gold; (4) pressing the ultraflat gold onto the surface of a bulk vdW crystal; (5) peeling off a monolayer and transferring onto a substrate; (6) removing the TRT with heat; (7) dissolving PVP in water; (8) dissolving gold in an I₂/I^– etchant solution; and (9) obtaining the single-crystal monolayer with macroscopic dimensions. (b) Schematic of the layer-by-layer exfoliation technique to yield even and odd layers from an AB stacked TMDs crystals. (c) Optical images of six monolayer samples (on SiO₂/Si substrate) sequentially exfoliated from a centimeter-size WSe₂ single crystal shown at the upper left corner^[32].

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图 8 二维材料悬浮结构的制备路线图(a)及解理后的二维材料(b)—(d); 解理后的悬浮WSe₂展现出良好的荧光特性(e); (f)是将衬底图案化(十二生肖图案)加工后, 通过优化解理工艺制备的悬浮WSe₂荧光成像图片, 比例尺为4 μm^[33]

Figure 8. Fabrication process and characterization of suspended 2D materials. (a) Schematic images for preparing suspended samples. (b)–(d) Optical images of exfoliated graphene, MoS₂ and WSe₂ on different patterned substrates, including rectangle, Hall bar and circular hole structures. (e) PL mapping image of suspended monolayer WSe₂. (f) PL mapping images of Chinese zodiac signs, which were collected on suspended WSe₂ flakes. Some details are added artificially, such as eyes and mouths. The scale bar is 4 μm^[33]

DownLoad: Full-Size Img PowerPoint

map

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[2]	Iijima S 1991 Nature 354 56 Google Scholar
[3]	Lu X K, Yu M F, Huang H, Ruoff R S 1999 Nanotechnology 10 269 Google Scholar
[4]	Chen H, Zhang X L, Zhang Y Y, Wang D F, Bao D L, Que Y D, Xiao W D, Du S X, Ouyang M, Pantelides S T, Gao H J 2019 Science 365 1036 Google Scholar
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Vol. 71, Issue 10 - 2022-05-20

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