二维原子晶体的转移堆叠方法及其高质量电子器件的研究进展

王浩林; 宗其军; 黄焱; 陈以威; 朱雨剑; 魏凌楠; 王雷

doi:10.7498/aps.70.20210929

摘要

可剥离至原子层厚度的层状材料被称为二维原子晶体, 是凝聚态物理研究的前沿材料体系之一. 与体材料相比, 二维原子晶体的原子完全暴露, 对外界环境极为敏感, 因此剥离、转移、旋转、堆叠、封装和器件加工技术对于其电子器件质量和电学输运性质研究尤为关键. 本文介绍了二维原子晶体转移工艺的重要发展, 尤其是对其二维电子气的输运性质有突破性提升的进展. 针对基于二维原子晶体的电子器件, 从二维电子气的无序、接触电阻、载流子迁移率、可观测的量子霍尔态等角度衡量器件质量, 并详细介绍了与之相对应的转移技术、器件结构与加工工艺.

关键词:

Abstract

Two-dimensional atomic crystals (2DACs) are the layered materials that can be exfoliated into the thickness of one unit cell, and attract extensive attention in current condensed matter physics. The atoms contained in a 2DAC are completely exposed, thus rendering them extremely sensitive to the external environment. Therefore, the exfoliation, transfer, rotation, stacking, encapsulation and device fabrication processes are particularly important for the electronic device quality and electrical transport properties of 2DACs. We review the recent progress of the transfer methods for 2DACs, especially the milestones in the improving of the transport properties of these two-dimensional electron gases (2DEGs). For electronic devices based on 2DACs, the quality of the devices is evaluated in terms of the disorder of 2DEG, contact resistance, carrier mobility, and observed quantum Hall states, and their corresponding transfer technology, device structure and fabrication processes are also discussed in detail.

Keywords:

作者及机构信息

1.
南京大学物理学院, 固体微结构物理国家重点实验室, 人工微结构科学与技术协同创新中心, 南京　210093

2.
西安电子科技大学先进材料与纳米科技学院, 西安　710126

通信作者: 王雷, Leiwang@nju.edu.cn

基金项目: 国家自然科学基金(批准号: 12074173, 61804117)、陕西省自然科学基础研究计划(批准号: 2018JQ5162)和南京大学技术创新基金资助的课题

Authors and contacts

1.
Collaborative Innovation Center of Advanced Microstructures, National Laboratory of Solid-State Microstructures, School of Physics, Nanjing University, Nanjing 210093, China

2.
School of Advanced Materials and Nanotechnology, Xidian University, Xi’an 710126, China

Corresponding author: Wang Lei, Leiwang@nju.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant Nos. 12074173, 61804117) and the Natural Science Foundation for Basic Research of Shaanxi Province, China (Grant No. 2018JQ5162)

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施引文献

图 1 二维原子晶体的机械剥离及层数的快速识别　(a)石墨烯的机械剥离过程示意图, 以及具体步骤的照片((1)—(4))和样品的光学照片((5)), 其中可以看到不同层数的样品^[55]; (b)石墨烯^[57]和(c)h-BN^[49,58]在不同厚度SiO₂上(即Si/SiO₂衬底), 不同波长的入射光下的光学对比度变化规律, 以及相应光学照片和原子力显微镜图片; (d) SiO₂上MoS₂的光学照片, 也可以看出对比度随着SiO₂的厚度变化显著^[59]

Fig. 1. Mechanical exfoliation and rapid identification of layer number for two-dimensional atomic crystal (2DACs): (a) Schematic diagram of the mechanical exfoliation process of graphene, photos of the individual exfoliation steps ((1)–(4)) and optical images of the sample ((5)), in which flakes with different layers can be observed^[55]. Optical contrast of graphene^[57] (b) and h-BN^[49,58] (c) on Si/SiO₂ substrate with different thickness of SiO₂ for the incident light with different wavelengths, and corresponding optical images and atomic force microscope (AFM) images. (d) Optical images of MoS₂ on SiO₂, exhibiting that optical contrast varies notably with the thickness of SiO₂^[59].

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图 2 大尺寸二维原子晶体的剥离技术　(a)金辅助的超大面积剥离法的示意图以及利用该法制备的毫米级黑磷和三氯化钌(RuCl₃)的光学照片^[63]; (b)金辅助剥离后的湿法去除金薄膜的过程和大面积样品的照片^[64]; (c) Al₂O₃辅助剥离法及器件制备过程示意图, 以及制备的Fe₃GeTe₂样品的光学照片和原子显微镜图片^[65]

Fig. 2. Exfoliation technique of large-sized 2DACs: (a) Schematic illustration of the ultra-large area Au-assisted exfoliation and optical images of millimeter-sized black phosphorus and ruthenium trichloride (RuCl₃) obtained by this method^[63]; (b) wet chemical removal of gold films after Au-assisted exfoliation and optical images of large-area flakes^[64]; (c) schematic of Al₂O₃-assisted exfoliation and device fabrication process, optical images and AFM images of Fe₃GeTe₂ flakes^[65].

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图 3 转移堆叠过程示意图和常用转移台的照片^[55]

Fig. 3. Schematic of the transfer and stacking process and photos of commonly used probe station^[55].

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图 4 (a)PMMA转移过程的具体步骤示意图以及(b)对应的光学照片^[49]; (c)石墨烯在SiO₂和h-BN衬底表面的形貌图和电荷密度图^[71]; (d)石墨烯分别在SiO₂和h-BN衬底上的转移特性曲线^[49]

Fig. 4. (a) Schematic of individual steps of the PMMA transfer process and (b) the corresponding optical images of the flakes taken for each step^[49]; (c) topography and charge density maps of graphene on SiO₂ and h-BN^[71]; (d) transfer curves of graphene on SiO₂ and h-BN substrates^[49].

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图 5 (a)聚合物基转移法导致的界面杂质及气泡的AFM图^[37]; (b)利用含有气泡的叠层制备的器件光学照片, 其中将顶栅电极设计为复杂形状是为避开气泡^[77]

Fig. 5. (a) AFM images of interfacial impurities and bubbles resulting from polymer-based transfer process^[37]; (b) optical images of the devices fabricated with stacks containing bubbles, in which the complex top gate shape was designed to avoid the bubbles^[77].

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图 6 (a) pick-up转移法的过程示意图; 所制备的叠层结构的(b)光学照片、(c) AFM图像和(d)截面TEM图像; (e)器件的转移特性曲线. 插图分别为器件的光学照片和低温电学输运测量结果^[36]

Fig. 6. (a) Schematic of the pick-up transfer process; (b) optical images, (c) AFM images and (d) cross-sectional TEM images of the obtained h-BN/graphene/h-BN stacks; (e) transfer curves of the device. The left and right insets are optical images of the device and low-temperature electrical transport measurements, respectively^[36].

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图 7 (a)石墨烯/h-BN莫尔超晶格的波长(黑色)和超晶格旋转角(红色)与层间转角的关系曲线, 插图为波长11.5 nm的莫尔超晶格的STM图像^[79]; (b)单层石墨烯晶体边缘对应特定的晶向, 插图为石墨烯晶格模型中标示出的对应晶向^[7]; (c)退火前后, h-BN/石墨烯/h-BN叠层的光学照片^[81]

Fig. 7. (a) Plot of the wavelength of the graphene/h-BN moiré superlattice (black) and the rotation angle of the superlattice (red) as function of the rotation angle between layers^[79]. The inset represents STM image of the moiré superlattice with a wavelength of 11.5 nm. (b) edges of the monolayer graphene crystal correspond to specific crystal orientation^[7]. The inset shows the corresponding crystal orientation denoted with dashed line in the lattice model. (c) optical images of h-BN/graphene/h-BN stacks before (upper penal) and after (lower penal) annealing^[81].

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图 8 (a)“撕裂+堆叠”法制备石墨烯莫尔超晶格的过程示意图以及相应的光学照片^[82]; (b)转移台的旋转过程示意图^[83]; (c)“切割+堆叠”法制备石墨烯莫尔超晶格叠层的光学照片; (d)制备的莫尔超晶格的STM图像^[82]

Fig. 8. (a) Schematic diagram of the preparation process of graphene moiré superlattice by “tearing + stack” method and the corresponding optical images^[82]; (b) schematic of the rotating the stage (supporting the underlying graphene) during “tearing + stack” process^[83]; (c) optical images of the graphene moiré superlattice prepared by “tearing + stack” method; (d) STM image of the obtained graphene/h-BN moiré superlattice^[82].

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图 9 石墨烯器件的无序降低以及由此带来的器件质量提升, 以可观测到的量子霍尔态为评价标准

Fig. 9. Progress of reducing the disorder in graphene-based devices and the resulting improvement of device quality, evaluated by the observable quantum Hall state.

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图 10 (a)基于STM测量结果推导出的SiO₂/Si衬底上MoS₂的能带结构变化^[102]; (b) SiO₂/Si衬底上MoS₂的迁移率随温度的变化, 插图为器件结构示意图^[104]; 通过(c) h-BN封装技术^[109]和(d) HfO₂钝化技术^[107]屏蔽外部无序后, MoS₂的迁移率随温度的变化

Fig. 10. (a) Variation of energy band structure of MoS₂ on SiO₂/Si substrate, deduced from STM measurements^[102]; (b) Plots of MoS₂ mobility as function of temperature on SiO₂/Si substrates^[104]. The inset illustrates the device structure. The mobility of MoS₂ vs. temperature after screening the external disorder by (c) encapsulation with h-BN^[109] and (d) passivation with HfO₂^[107].

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图 11 h-BN封装结构用于空气敏感型二维原子晶体的电学输运、磁学及铁电极化特性的研究　(a)—(c)半导体: BP^[113]; (d), (e)铁电体: WTe₂^[31]; (f), (g)超导体: NbSe₂^[114]; (h), (i)铁磁体: CrI₃^[32]

Fig. 11. Study on the electrical transport, magnetic and ferroelectric polarization characteristics of unstable 2DACs with h-BN encapsulation: (a)−(c) semiconductor: black phosphorous^[113]; (d), (e) ferroelectric: WTe₂^[31]; (f), (g) superconductor: NbSe₂^[114]; (h), (i) ferromagnet: CrI₃^[32].

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图 12 (a)石墨烯的一维边缘接触结构的工艺示意图; (b)截面TEM图像及相应的EDS图像; (c)接触界面的原子结构示意图; (d)接触电阻与沟道长度的关系曲线^[36]

Fig. 12. (a) Schematic of the one-dimensional edge contact process for graphene devices; (b) cross-sectional TEM image and corresponding EDS mapping; (c) atomic structure diagram of contact interface; (d) Plot of the contact resistance as function of the channel length^[36].

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图 13 “混合型”边缘接触结构及电学输运测量结果　(a)—(c) MoS₂^[109]; (d)—(f) InSe^[116]; (g), (h) NbSe₂^[117]

Fig. 13. Mixed edge contact configuration and the corresponding electrical transport measurements: (a)−(c) MoS₂^[109]; (d)−(f) InSe^[116]; (g), (h) NbSe₂^[117].

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图 14 顶电极范德瓦耳斯接触工艺. 在MoS₂表面直接沉积(a)—(c)金属电极和(d)—(f)转移金属电极形成的界面原子结构示意图、相应的界面TEM图像和转移特性曲线, 其中图(f)中的插图为不同栅压下的输出特性曲线^[132]; (g)兼容h-BN封装结构的顶电极范德瓦耳斯接触结构的工艺流程示意图; (h)基于顶电极范德瓦耳斯接触的WSe₂器件的输出特性曲线^[114]

Fig. 14. van der Waals contact between the top electrodes and TDACs. The schematic of atomic structure at the interface, the TEM images of the interface and the corresponding transfer curves of the contacts formed by (a)−(c) the direct deposition of metal electrode and (d)−(f) transferring metal electrode on the MoS₂, respectively^[132]. The inset in panel (f) is the output curves. (g) Schematic of the fabrication process for top electrode with van der Waals contact structure, compatible with h-BN encapsulation. (h) Output curves of WSe₂ device with top electrodes^[114].

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图 15 底电极范德瓦耳斯接触　(a)结构和(b)工艺示意图.(c), (d)表征欧姆接触特性的I-V特性曲线^[133]. 基于底电极范德瓦耳斯接触的WSe₂((e), (f))^[134], MoS₂((g)−(i)), MoSe₂((j), (k))和WTe₂((l)−(n))的电学输运测量结果^[135-138]

Fig. 15. (a) Schematic and (b) fabrication process of van der Waals contact between bottom electrodes and WSe₂^[133]. (c), (d) I-V curves indicating ohmic contact. Electrical transport measurements of WSe₂ (e), (f)) ^[134], MoS₂ ((g)−(i)), MoSe₂ ((j), (k)) and WTe₂ ((l)−(n)) using bottom electrode contacts^[135-138].

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图 16 叠层器件的量子电容测试法　(a)双层石墨烯的量子电容测量示意图; (b) N = 1和N = 0朗道能级的不同填充数对应的量子电容^[95]; WSe₂的(c)量子电容测量结构示意图, (d)光学照片以及(e)不同填充数对应的量子电容随磁场的变化关系^[146]

Fig. 16. Quantum capacitance measurement of devices based on stacks: (a) Schematic of quantum capacitance measurement of bilayer graphene; (b) quantum capacitance of different filling factors of N = 1 and N = 0 Landau levels ^[95]; (c) schematic of quantum capacitance measurement, (d) optical image and (e) the relationship between quantum capacitance and magnetic field for various filling factors of WSe₂ ^[146].

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图 17 Corbino结构的石墨烯器件的电学输运特性　(a)金属栅极的Corbino器件的光学照片和结构示意图; (b)器件电阻随位移场的变化曲线^[150]; (c)基于石墨栅极的Corbino器件的微加工过程示意图^[152]; (d)双电层结构的Corbino器件的测量装置示意图; (e)纵向电导率随填充数的变化, 其中涌现出一系列符合复合费米子模型的新的分数量子霍尔态^[153]

Fig. 17. Electrical transport properties of Corbino devices based on graphene: (a) Schematic and optical image of the Corbino device with metal gate; (b) relationship between the resistance and displacement field^[150]; (c) schematic of the fabrication process of Corbino device with top and bottom gate^[152]; (d) Corbino device with the electric double layer (EDL) structure; (e) variation of the longitudinal conductivity with filling factor, in which a series of emergent fractional quantum hall states corresponding to the composite fermion model appear^[153].

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图 18 基于局域定义的石墨栅极研究石墨烯器件的电学输运特性　(a)局域定义的石墨顶栅器件结构示意图; (b)器件纵向电导率与局域石墨栅压关系曲线, 在N = 0和N = 1朗道能级中可以观测到大量的分数量子霍尔态^[157]; (c)基于局域石墨栅极的Corbino器件的结构示意图; (d)器件的纵向电导率与局域石墨栅压的关系曲线^[159]

Fig. 18. Electrical transport properties of graphene devices with locally defined graphite gates^[157]: (a) Locally defined graphite top gate structures and optical images; (b) Relationship between the longitudinal conductivity and the local gate voltage, and a large number of fractional quantum Hall states can be observed within the N = 0 and N = 1 Landau levels; (c) schematic of Corbino device with local graphite gates; (d) Relationship between the longitudinal conductivity and the local gate voltage^[159].

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图 19 零磁场下石墨烯双电层(EDL)结构的库仑拖曳效应研究利用聚合物基转移法制备的石墨烯EDL器件的　(a)示意图, (b)光学照片, (c)测量结构示意图, (d)拖拽电阻率的相图^[165]; 利用pick-up转移法制备的(e)器件结构示意图以及(f)叠层结构和(g) EDL器件的光学照片; (h)拖拽电阻与两层石墨烯的朗道能级填充数的关系曲线^[168]

Fig. 19. Coulomb drag effect of graphene electric double layer (EDL) in zero magnetic field: (a) Schematic, (b) optical image, (c) measurement setup and phase diagram of drag resistivity of graphene EDL device prepared by polymer-based transfer method (d) ^[165]; (e) structure diagram, (f) optical image of the stack and (g) final EDL device fabricated by the pick-up transfer method; (h) curves of drag resistance as function of total Landau level filling factors of two layers of graphene^[168].

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图 20 利用介电环境及近邻效应调控石墨烯中电子基态　(a)以二维周期性介质为栅极的石墨烯叠层结构的制备工艺示意图; 周期性外部电场作用下的石墨烯的(b)STM图和(c)朗道能级扇形图^[177]; (d)基于一维周期性栅介质的石墨烯叠层结构示意图; (e)石墨烯的纵向电阻率与载流子浓度和底栅电压的关系^[178]; R_xx(f)和R_yy(g)的朗道能级扇形图; (h)基于高介电常数栅介质的叠层器件结构示意图; (i)主要狄拉克点的电阻与温度和磁场的变化关系^[182]; WSe₂/h-BN/WSe₂叠层的(i)电容测量结构示意图和(k)器件光学照片; (l)石墨烯主要狄拉克点的量子电容与位移场和载流子浓度的关系图^[194]

Fig. 20. Tuning the ground state of electrons in graphene by changing the dielectric environment and proximity effects: (a) Schematic of the fabrication process of graphene stack based on two-dimensional periodic gate dielectric pattern; (b) STM image and (c) Landau fan diagrams of graphene under the applied periodic electric field^[177]; (d) schematic of graphene stack with one-dimensional periodic gate dielectric; (e) relationship between longitudinal resistivity and carrier concentration with periodic gate voltage in the graphene device^[178]; (f), (g) the Landau fans of R_xx and R_yy, respectively; (h) schematic of the device based on a high-κ gate dielectric; (i) relationship between the resistance of main Dirac point with the temperature and magnetic field^[182]; (j) schematic of capacitance measurement for WSe₂/h-BN/WSe₂ stack and (k) optical images of the device; (l) relationship between the quantum capacitance of the main Dirac point with the displacement field and carrier concentration^[194].

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图 21 石墨烯/h-BN莫尔超晶格的电学输运特性　(a) Geim课题组^[77]和(b)Kim课题组^[198]报道的Hofstadter蝴蝶分形能谱; (c)室温附近观测到的SdH振荡^[201]; (d)实验观测到的对称破缺整数量子霍尔态(红色虚线框标识)和(e)对应的Wannier图(彩色实线标识了态密度极小值)^[200]; (f), (g) t为整数和s非零的量子霍尔态^[80]; (h)电容测量中观察到的t为分数和s为零的量子霍尔态^[202]

Fig. 21. Electrical transport properties of graphene/h-BN moiré superlattice: (a) Hofstadter butterfly fractal spectrum reported by Geim’s group^[77] and (b) Kim’s group^[198]; (c) SdH oscillations observed near room temperature^[201]; (d) observed quantum Hall ferromagnetic states and (e) theoretically predicted Landau fan diagram^[200]; (f), (g) quantum Hall state with integer t and non-zero s^[80]; (h) quantum Hall state where t is a fraction and s is zero observed in the capacitance measurement^[202].

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图 22 石墨烯莫尔平带系统　单层-单层石墨烯莫尔超晶格(魔角双层石墨烯)器件的　(a)示意图, (b)电子相图和(c)能带结构^[209]; (d), (e)魔角双层石墨烯中的轨道铁磁性^[222]; 双层-双层石墨烯莫尔超晶格的(f)器件结构和晶格结构示意图以及(g)电阻率随位移场的变化关系图^[215]; ABC三层石墨烯/h-BN莫尔超晶格器件的(h)结构示意图和(i)纵向电阻率随位移场的变化关系图, 其中插图为器件的光学照片^[212]; 转角三层石墨烯莫尔超晶格的(j)器件结构示意图和(k)纵向电阻率随位移场和莫尔单胞填充数的变化关系图^[219]

Fig. 22. Graphene moiré flat band system: (a) Schematic, (b) electronic phase diagram and (c) energy band structure of a monolayer-monolayer graphene moiré superlattice (magic-angle twisted bilayer graphene, MATBG) device^[209]; (d), (e) orbital ferromagnetism in MATBG^[222]; (f) schematic of device geometry and (g) relationship between the resistivity and the displacement field of the twisted bilayer-bilayer graphene (twisted double bilayer graphene, TDBG) moiré superlattice^[215]; (h) schematic and (i) relationship between the longitudinal resistivity and the displacement field of the ABC trilayer graphene/h-BN moiré superlattice device. The inset in panel (i) is the corresponding optical image^[212]. (j) Schematic of device structure and (k) relationship of the longitudinal resistivity with the displacement field and the filling factors of the moiré unit cell of the twisted trilayer graphene moiré superlattice^[219].

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图 23 转角WSe₂器件中的电子关联态^[241]底电极接触的器件　(a)结构示意图和(b)光学照片; (c)零磁场时, 不同转角的器件的纵向电阻随载流子浓度的变化关系图, 重点标示了其中的半填充电子态的电阻; (d)转角WSe₂器件的电子相图

Fig. 23. Correlated electronic states in a twisted WSe₂ device^[241]: (a) Schematic and (b) optical image of the device with bottom electrode; (c) curves of the longitudinal resistance vs. the carrier concentration for devices with different twisted angles under zero magnetic field. The resistance of the half-filling state is marked. (d) The phase diagram of the twisted WSe₂ device.

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图 24 (a)利用AFM针尖原位调控石墨烯/h-BN莫尔超晶格的装置示意图; (b)—(d)不同转动时, 叠层结构的AFM图像^[246]; (e)石墨烯的次级狄拉克点随原位转角的变化关系;石墨烯/h-BN莫尔超晶格的静压力测试(f)装置和原理示意图及(g)装置照片^[248]; (h)主要狄拉克点和次级狄拉克点的带隙随压力的变化; (i)魔角石墨烯器件的结构示意图; (j)莫尔原胞半填充处的关联绝缘态随压力的变化; (k)有(蓝色曲线)/无(灰色曲线)静压的情况下, 器件的纵向电导率随载流子浓度及相应莫尔单胞填充数的变化曲线^[249]

Fig. 24. (a)Schematic of the graphene/h-BN moiré superlattice in situ controlled by AFM tip; (b)−(d) AFM images of the stack with different twisted angels^[246]; (e) relationship between the secondary Dirac point of graphene and the in situ controllable twisted angles^[248]; (f) top, cartoon of the piston-cylinder pressure cell. Bottom, schematic of the graphene stack under ambient and high pressure. (g) optical images of the device; (h) bandgaps as a function of pressure; (i) schematic of the magic angle graphene device^[249]; (j) plots of the conductance (left penal) and resistance (right penal) of the half-filling states as function the pressure; (k) dependence of longitudinal conductivity on the carrier concentration and the corresponding filling factors of the moiré unit cell with (blue curve) and without (grey curve) high pressure.

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图 25 转角石墨烯器件中关联电子态的外部调控　(a)通过调控叠层结构中魔角石墨烯和石墨栅极之间的h-BN的厚度调控系统中电子相互作用; (b)随着库仑屏蔽作用的增强, 关联绝缘体逐渐淬灭^[250]. (c)利用Bernal双层石墨烯调控魔角石墨烯的器件结构示意图; (d)在不同的双层石墨烯载流子浓度下, ν = 2填充对应的电导随温度变化曲线及(e)能隙随双层石墨烯载流子浓度的变化曲线^[251]; (f)魔角石墨烯/单层WSe₂叠层结构示意图; (g)—(i)三个非魔角的转角石墨烯器件中的超导转变; (j)利用单层WSe₂的近邻效应调控魔角石墨烯的器件结构示意图^[252]; (k)器件的横向电阻和纵向电阻随载流子浓度及相应朗道能级填充数的变化曲线; (l) ν = 1和(m) ν = 2填充对应的电子态的轨道磁性测量结果^[253]

Fig. 25. Tuning of interaction between electrons in twisted graphene devices: (a) Interaction between electrons can be tuned by adjusting the thickness of the h-BN between the MATBG and the graphite gate in the stack; (b) with enhancing the Coulomb screening effect, the correlated insulator phase is quenched^[250]. (c) Schematic of the device utilizing Bernal bilayer graphene to tune MATBG; (d) under different carrier concentration in Bernal bilayer graphene, plots of the conductance corresponding to ν = 2 filling vs. temperature and (e) energy gap vs. carrier concentration in bilayer graphene^[251]; (f) schematic of MATBG/monolayer WSe₂ stack; (g)−(i) superconducting transition observed in the three twisted devices with non-magic angles^[252]; (j) schematic of the device to tune the MATBG using the proximity effect of monolayer WSe₂; (k) curves of the transverse (upper curve) and longitudinal (lower curve) resistance vs. the carrier concentration (the filling factor of the Landau level). Orbital magnetic measurement of the electron states corresponding to (l) ν = 1 and (m) ν = 2 filling^[253].

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二维原子晶体的转移堆叠方法及其高质量电子器件的研究进展