二维材料的转移方法

廖俊懿; 吴娟霞; 党春鹤; 谢黎明

doi:10.7498/aps.70.20201425

摘要

二维材料及其异质结在电子学、光电子学等领域具有潜在应用, 是延续摩尔定律的候选电子材料. 二维材料的转移对于物性测量与器件构筑至关重要. 本文综述了一些具有代表性的转移方法, 详细介绍了各个方法的操作步骤, 并基于转移后样品表面清洁程度、转移所需时间以及操作难易等方面对各个转移方法进行了对比归纳. 经典干、湿法转移技术是进行物理堆叠制备原子级平整且界面清晰范德瓦耳斯异质结的常用手段, 结合惰性气体保护或在真空条件下操作还可以避免转移过程中二维材料破损和界面吸附. 高效、无损大面积转移方法为二维材料异质结构建和材料本征物理化学性质测量提供了强有力的技术保障. 转移技术的优化将进一步扩展二维材料在高温超导、拓扑绝缘体、低能耗器件、自旋谷极化、转角电子学和忆阻器等领域的研究.

关键词:

Abstract

The advent of two-dimensional (2D) materials, a family of materials with atomic thickness and van der Waals (vdWs) interlayer interactions, offers a new opportunity for developing electronics and optoelectronics. For example, semiconducting 2D materials are promising candidates for extending the Moore's Law. Typical 2D materials, such as graphene, hexagonal boron nitride (h-BN), black phosphorus (BP), transition metal dichalcogenides (TMDs), and their heterostrcutures present unique properties, arousing worldwide interest. In this review the current progress of the state-of-the-art transfer methods for 2D materials and their heterostructures is summarized. The reported dry and wet transfer methods, with hydrophilic or hydrophobic polymer film assistance, are commonly used for physical stacking to prepare atomically sharp vdWs heterostructure with clear interfaces. Compared with the bottom-up synthesis of 2D heterostructures using molecular beam epitaxy (MBE) or chemical vapor deposition (CVD), the construction of 2D heterostructures by transfer methods can be implemented into a curved or uneven substrate which is suitable for pressure sensing, piezoelectric conversion as well as other physical properties’ research. Moreover, the transfer of 2D materials with inert gas protected or in vacuum operation can protect moisture-sensitive and oxygen-sensitive 2D materials from degerating and also yield interfaces with no impurities. The efficient and non-destructive large-area transfer technology provides a powerful technical guarantee for constructing the 2D heterostructures and exploring the intrinsic physical and chemical characteristics of materials. Further development of transfer technology can greatly facilitate the applications of 2D materials in high-temperature superconductors, topological insulators, low-energy devices, spin-valley polarization, twistronics, memristors, and other fields.

Keywords:

作者及机构信息

1.
国家纳米科学中心, 中国科学院纳米标准与检测重点实验室, 北京　100190

2.
国家纳米科学中心, 中国科学院纳米科学卓越创新中心, 北京　 100190

3.
中国科学院大学, 北京　100049

4.
清华大学化学系, 北京　100084

通信作者: 谢黎明, xielm@nanoctr.cn

基金项目: 国家自然科学基金(批准号: 21673058, 21822502)、中国科学院前沿科学重点研究项目(批准号: QYZDB-SSW-SYS031)和中国科学院战略性先导科技专项(B类)(批准号: XDB30000000)资助的课题

Authors and contacts

1.
Key Laboratory of Standardization and Measurement for Nanotechnology, National Center for Nanoscience and Technology, Chinese Academy of Sciences, Beijing 100190, China

2.
Innovation Center for Excellence in Nanoscience, National Center for Nanoscience and Technology, Chinese Academy of Sciences, Beijing 100190, China

3.
University of Chinese Academy of Sciences, Beijing 100049, China

4.
Department of Chemistry, Tsinghua University, Beijing 100084, China

Corresponding author: Xie Li-Ming, xielm@nanoctr.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant Nos. 21673058, 21822502), the Key Research Program of Frontier Sciences, Chinese Academy of Sciences (Grant No. QYZDB-SSW-SYS031), and the Strategic Priority Research Program (B) of the Chinese Academy of Sciences (Grant No. XDB30000000)

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施引文献

图 1 二维材料的转移方法

Fig. 1. Transfer methods for two-dimensional (2D) materials

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图 2 PMMA辅助转移制备Graphene/h-BN异质结　(a) 石墨烯被剥离在水溶性高分子与PMMA表面; (b) 在去离子水的作用下高分子薄膜与基底分离; (c) 石墨烯样品与h-BN对准; (d) 将石墨烯转移至带有h-BN的SiO₂/Si基底上^[32]

Fig. 2. Preparation of graphene/h-BN heterostructure by PMMA mediated transfer: (a) Graphene is exfoliated on the surface of water-soluble layer coated with PMMA; (b) the polymer film is separated from the substrate by the interface wetting of deionized water; (c) graphene is aligned with h-BN; (d) graphene is transferred on to the h-BN on SiO₂/Si substrate^[32].

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图 3 PLLA转移纳米材料　(a) 未转移前基底上的纳米材料; (b) 在基底表面覆盖PLLA与PDMS高分子膜; (c) 在去离子水的作用下高分子薄膜与基底分离; (d) 将薄膜转移至目标基底; (e) 将PDMS从PLLA表面剥离; (f) 二氯甲烷溶液浸泡除去PLLA^[37]

Fig. 3. Transfer nanostructures onto arbitrary substrates by PLLA polymeric film: (a) Nanostructures on original substrate; (b) PLLA and PDMS are coated on the substrate; (c) the PLLA and PDMS film are separated from the substrate by the interface wetting of deionized water; (d) transfer the polymer film to the target substrate; (e) peel off the PDMS film; (f) remove PLLA by CH₂Cl₂ solution^[37].

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图 4 牺牲层转移法制备Graphene/h-BN异质结　(a) 制作牺牲层高分子薄膜/双面黏附透明胶带/透明玻璃的三层结构支撑体; (b) 在高分子薄膜表面剥离石墨烯; (c) 石墨烯样品与h-BN对准; (d) 石墨烯接触目标基底; (e)和(f)为石墨烯脱离支撑体得到Graphene/h-BN异质结^[44]

Fig. 4. Sacrificial-layer transferring graphene on to h-BN substrate: (a) A three-layer holder consists of a sacrificial film, a double-sided adhesive tape and a transparent glass; (b) graphene is exfoliated on the surface of the holder; (c) graphene is aligned with h-BN; (d) contact graphene with the target substrate; (e), (f) graphene is released from the holder and graphene/h-BN heterostructure is obtained^[44].

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图 5 小分子掺杂PS转移WS₂样品　(a) CVD生长在蓝宝石基底上的WS₂样品; (b) 将样品置于液氮中浸泡15 min; (c) 将样品置于Li⁺溶液中浸泡30 min; (d) 在样品表面旋涂小分子/高分子混合物薄膜, 并在去离子水的作用下使薄膜与蓝宝石基底分离; (e) 将样品转移至目标基底; (f) 在甲苯溶液中浸泡1.5 h去除高分子薄膜^[47]

Fig. 5. Transferring WS₂ by a thin film of PS/small molecule composite: (a) WS₂ is grown on sapphire substrate by CVD methods; (b) immerse the sample in liquid nitrogen for 15 min; (c) immerse the sample in a Li⁺ aqueous solution for 30 min; (d) a film of polymer/small molecule composite is spun-coating on the sample and then separated from the sapphire substrate by the interface wetting of deionized water; (e) transfer WS₂ to the target substrate; (f) the polymer/small molecule composite is removed by soaking in toluene solution for 1.5 h^[47].

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图 6 纤维素薄膜转移法转移图形化纳米结构　(a) 在亲水基底上的模型化纳米结构; (b) 在基底表面旋涂憎水高分子薄膜; (c) 在去离子水的作用下使薄膜与亲水基底分离; (d) 在探针的协助下使薄膜与目标基底对准; (e) 图形化纳米结构与目标基底接触; (f) 用乙酸乙酯去除高分子薄膜^[30]

Fig. 6. Transferring patterned nanostructures by a cellulose film: (a) Patterned nanostructures on hydrophilic substrate; (b) hydrophobic polymer film is spun-coating on the substrate; (c) the polymer film is separated from the hydrophilic substrate by the interface wetting of deionized water; (d) align the film with the target substrate by a mechanical probe; (e) contact the patterned nanostructures with the target substrate; (f) the polymer film is removed with ethyl acetate^[30].

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图 7 PVA吸附转移二维材料　(a) 在PVA表面剥离石墨烯样品; (b) 悬臂与石墨烯样品接触; (c) 用注射器在样品周围滴去离子水使局部的PVA溶解; (d) 将石墨烯转移至目标基底^[53]

Fig. 7. Exfoliation and transfer of 2D materials by the PVA film: (a) Graphene is exfoliated on the PVA film; (b) the cantilever is in contact with the graphene; (c) PVA is dissolved by dropping deionized water around the sample with a syringe; (d) graphene is transferred to the target substrate^[53].

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图 8 金属辅助剥离转移大面积TMDs单层　(a) 在Si基底表面沉积Au膜; (b) 在金膜表面旋涂PVP高分子膜; (c) 使用热释放胶带将PVP/金属层从Si基底上剥离; (d), (e) 利用金胶带剥离TMDs样品至目标基底; (f) 130 ℃下去除热释胶带; (g) 在去离子水中浸泡2 h去除PVP; (h) 将基底浸入KI/I₂溶液中刻蚀样品表面的金膜; (i) 在目标基底表面的单层TMDs样品^[55]

Fig. 8. Exfoliation of TMDs crystals to large-size monolayer and transferring to a target substrate: (a) Au is deposited on the Si substrate; (b) PVP polymer film is spun on the surface of the gold film; (c) the PVP/metal layer is peeled from the Si substrate by TRT; (d), (e) TMDs is exfoliated to the target substrate by TRT/PVP/Au; (f) The TRT is removed at 130 ℃; (g) PVP is removed by soaking in deionized water for 2 h; (h) the substrate is immersed in KI/I₂ solution to etch the gold film; (i) monolayer TMDs on the target substrate^[55].

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图 9 化学刻蚀转移CVD生长大面积石墨烯　(a), (b) 金属/SiO₂基底上生长或图形化的石墨烯样品; (c) 在去离子水的作用下将高分子薄膜支撑的石墨烯/金属层从SiO₂基底分离; (d) 利用FeCl3溶液刻蚀金属; (e) 将石墨烯转移至目标基底; (f) 光刻得到目标基底上的石墨烯样品^[62]

Fig. 9. Transfer of CVD synthesized graphene film: (a), (b) Graphene grown or patterned on the metal/SiO₂ substrate; (c) the graphene/metal layer supported by the polymer film is separated from the SiO₂ substrate by the interface wetting of deionized water; (d) metal is etched by FeCl₃ solution; (e) graphene is transferred to a target substrate; (f) the patterned graphene on the target substrate is obtained by lithography^[62].

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图 10 电化学剥离转移Cu箔上的石墨烯^[68]

Fig. 10. Electrochemical exfoliation and transfer of graphene from Cu foil^[68].

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图 11 PDMS干法转移设备及过程　(a) 干法转移设备由显微镜、三维操作台、样品台等装置组成; (b) 在PDMS上机械剥离二维材料; (c) 将带有样品PDMS翻转; (d) 样品与目标基底对准; (e) 使样品与目标基底接触; (f) 将PDMS从基底表面剥离; (g) 样品被成功转移至目标基底^[76]

Fig. 11. PDMS dry-transfer setup and process: (a) The dry transfer equipment consists of a optical microscope, a XYZ stamping stage and a XYZ sample stage; (b) 2D materials are exfoliated on PDMS; (c) the PDMS is turned upside down; (d) align the sample with the target substrate; (e) contact 2D materials with the target substrate; (f) the PDMS is peeled from the substrate; (g) the 2D materials are successfully transferred to target substrate^[76].

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图 12 vdWs相互作用法转移制备h-BN/Graphene/h-BN异质结　(a) 透明玻璃/PDMS/PPC担体将h-BN从SiO₂基底剥离; (b) 在110 ℃下将h-BN与石墨烯堆叠; (c) 将h-BN/Graphene从SiO₂表面剥离; (d) 在110 ℃下将h-BN/Graphene与h-BN堆叠; (e) 成功制备h-BN/Graphene/h-BN异质结^[82]

Fig. 12. The vdWs pick-up technique for preparation of h-BN/graphene/h-BN heterostructures: (a) h-BN is separated from SiO₂ substrate by transparent glass/PDMS/PPC supports; (b) h-BN is stacked on graphene at 110 ℃; (c) h-BN/graphene heterostructure is separated from SiO₂ substrate; (d) h-BN/graphene heterostructure is stacked on h-BN at 110 ℃; (e) h-BN/graphene/h-BN heterostructure is successfully fabricated^[82].

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图 13 惰性气体保护转移装置^[92]

Fig. 13. A transfer setup with inert gas protection^[92].

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图 14 真空环境转移生长样品组装堆叠形成异质结　(a) 大面积二维材料的合成; (b) 利用TRT将PMMA/二维材料从基底表面剥离; (c) 在真空中转移L₀层至L₁层表面; (d) 利用TRT将转移后的材料整体从基底表面剥离; (e) 在目标基底堆叠形成的异质结^[101]

Fig. 14. Layer-by-layer construction of wafer-scale 2D hetero-structures in vacuum: (a) Synthesis of large 2D materials; (b) PMMA/2D material is peeled from the substrate by TRT; (c) transfer L₀ layer to L₁ layer in vacuum; (d) the transferred materials are peeled from the substrate by TRT; (e) heterostructures is stacked on the target substrate^[101].

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表 1 不同转移方法的对比

Table 1. Comparison among different deterministic transfer methods.

转移类型	转移方法	载体	转移过程中使用的最高温度	能否在手套箱或真空中转移	优点	缺点	参考文献
湿法	PVA吸附转移法	PVA	室温	×	容易剥离得到大面积单层样品	需要在样品周围局部溶解高分子薄膜	[53]
	PMMA协助转移法	PMMA	110 ℃	×	容易找到单层样品, 多种方法将载体从原始基底分离	PMMA高分子薄膜需要溶液浸泡除去, 有机杂质吸附	[32]
	PLLA快速转移法	PLLA	50 ℃	×	能转移零维、一维、二维材料, 目标基底种类多	有机杂质吸附, 二氯甲烷溶液有毒性	[37]
	牺牲层转移法	MBMC	75—100 ℃	×	转移得到的样品表面更光滑	转移质量受样品与牺牲层高分子之间的结合力影响	[41]
	小分子掺杂 PS转移法	小分子掺杂PS	120 ℃	×	缩短转移时间, 降低有机残留吸附	需要降温、离子插层等技术预处理, 步骤繁琐	[47]
湿法	纤维素薄膜转移法	纤维素	室温	×	可以转移至曲面基底	操作不精细, 转移样品褶皱、裂纹密度高	[30]
	金属辅助剥离转移法	金属	130 ℃	×	转移厘米级单层样品, 可控实现AA堆积结构	要求金属表面原子级平整, 刻蚀金属难以回收利用	[55]
	化学刻蚀转移法	PDMS, PMMA	室温	×	可以转移金属和SiO₂/Si基底上连续生长的样品	刻蚀液污染环境, 刻蚀基底难以回收利用	[62]
	电化学剥离转移法	PMMA	室温	×	金属基底可以重复循环利用	H₂会使样品卷曲、褶皱	[68]
干法	PDMS剥离转移法	PDMS	室温	√	无溶液接触, 转移迅速	样品质量受基底表面平整度与接触按压压力大小影响	[76]
干法	vdWs相互作用转移法	h-BN	110 ℃	√	无高分子接触	转移过程相对复杂	[82]

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