石墨烯谐振式力学量传感器研究进展

万震; 李成; 刘宇健; 宋学锋; 樊尚春

doi:10.7498/aps.71.20220215

摘要

传统谐振式传感器的谐振敏感元件大多采用金属、石英晶体、硅等材料制成, 但随着谐振式传感器朝着小型化、微型化、实用化的趋势发展, 不但要求新型谐振子材料可进行微纳加工, 还对其灵敏度和精度提出了更高的要求. 石墨烯这种新型二维纳米材料, 因具有出色的力学、电学、光学、热学特性, 在谐振传感领域有着巨大的应用潜力和研究价值, 因此基于石墨烯材料的力学量传感器有望在小型化、高性能和环境适应性等多方面超越硅基力学量传感器. 本文针对石墨烯谐振式力学量传感器, 介绍了石墨烯材料的基本性质、制备与转移方法, 阐述了谐振式传感器的工作原理与应用特点, 进而分析了关于石墨烯谐振特性优化与谐振器制备的理论与实验研究; 在此基础上, 重点总结了石墨烯谐振器在压力、加速度、质量等传感器领域的研究进展, 梳理了石墨烯谐振式力学量传感器在薄膜转移、结构制备与激振/拾振等方面的技术问题, 同时也明确了石墨烯在谐振传感领域的研究价值和发展潜力.

关键词:

Abstract

The resonant sensor is a kind of high-sensitivity and high-stability sensor that directly outputs digital signals. The resonance sensitive elements of traditional resonant sensors are mostly made of metal, quartz crystal, silicon and other materials. However, with the development of resonant sensor toward the miniaturization and intellectualization, the sensitive materials of new resonator are micro-nano machined and highly sensitive. As a new type of two-dimensional nanomaterial, graphene has the great potentials in the field of resonance sensing because of its excellent mechanical, electrical, optical and thermal properties. Therefore, the mechanical quantity sensor based on graphene material is expected to surpass the silicon material mechanical quantity sensor in many aspects such as micro-nano size, high performance, and environmental adaptability. This review focuses on the graphene resonant mechanical quantity sensor. In the first part, we summarize the basic properties, preparation methods, and transfer methods of graphene materials. The preparation and transmission methods of graphene are key to high-performance graphene resonator, but there are still different problems in the preparation and transfer of graphene, which also greatly restricts the development of graphene resonator. In the second part, the basic theory of resonant sensors is given, and the common methods of transferring graphene films are introduced in detail. Then the theoretical and experimental studies of graphene resonator are discussed. For example, the theoretical studies of graphene resonator are investigated by using the classical elastic theory, non-local elastic theory, molecular structure mechanics and molecular dynamics. Then the effects of graphene preparation method, graphene layer number and shape, excitation and detection methods on the resonance performance are estimated in the resonant experiments of graphene resonators. After that, the research progress of graphene resonator is summarized in the fields of pressure, acceleration and mass sensors. Compared with traditional silicon resonators, graphene resonators have a small dimension and demonstrate preferable resonant performance under low-temperature and low-pressure conditions. In this case, the technical issues of graphene resonant sensor are introduced to emphasize the importance of suspended graphene film transfer, structure fabrication of harmonic oscillator and vibration excitation/detection of resonators, which contributes to the potential applications in the fields of aerospace, intelligent detection and biomedical sensing for graphene resonant sensors.

Keywords:

作者及机构信息

1.
北京航空航天大学仪器科学与光电工程学院, 北京　100191

2.
深圳北航新兴产业技术研究院, 深圳　518057

3.
南方科技大学量子科学与工程研究院, 深圳　518055

通信作者: 李成, licheng@buaa.edu.cn ; 宋学锋, songxf@sustc.edu.cn ;

基金项目: 国家自然科学基金(批准号: 62173021)、北京市自然科学基金(批准号: 4212039)、航空科学基金 (批准号: 2020Z073051002)和深圳市科技创新委员会(批准号: JCYJ20180504165721952)资助的课题.

Authors and contacts

1.
School of Instrumentation and Optoelectronic Engineering, Beihang University, Beijing 100191, China

2.
Emerging Industry Technology Research Institute of Beihang University in Shenzhen, Shenzhen 518057, China

3.
Institute of Quantum Science and Engineering, Southern University of Science and Technology, Shenzhen 518055, China

Corresponding author: Li Cheng, licheng@buaa.edu.cn ; Song Xue-Feng, songxf@sustc.edu.cn ;

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 62173021), the Beijing Natural Science Foundation, China (Grant No. 4212039), the Aviation Science Foundation of China (Grant No. 2020Z073051002), and the Science Technology and Innovation Commission of Shenzhen Municipality, China (Grant No. JCYJ20180504165721952).

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施引文献

图 1 不同大学制作的石墨烯谐振器结构示意图　(a) 康奈尔大学^[53]; (b) 巴塞罗那自治大学^[54]; (c) 哥伦比亚大学^[57]; (d) 康奈尔大学(阵列式)^[58]; (e) 石溪大学^[59]; (f) 康奈尔大学(圆形)^[60]; (g) 东京大学^[61]; (h) 哥伦比亚大学^[62]

Fig. 1. Schematic diagrams of the structure of graphene resonators made by different universities: (a) Cornell University^[53]; (b) Autonomous University of Barcelona^[54]; (c) Columbia University^[57]; (d) Cornell University (array)^[58]; (e) Shixi University^[59]; (f) Cornell University (circular)^[60]; (g) University of Tokyo^[61]; (h) Columbia University^[62].

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图 2 石墨烯谐振式压力传感器结构示意图　(a) 康奈尔大学制作的石墨烯谐振器的光学图像^[65]; (b) 香港理工大学使用的陶瓷插芯^[66]; (c) 香港理工大学使用的石墨烯纳米带^[66]; (d) 代尔夫特大学制造的哑铃形挤压膜石墨烯压力传感器^[67]; (e) 原子力显微镜下的悬浮石墨烯束, 其中氧化物为黑色, 石墨烯束为橙色^[68]; (f) 封闭腔式 F-P 谐振传感器^[69]; (g) 开放腔式 F-P 谐振传感器^[69]; (h) 单模光纤与石英毛细管熔接制成的石墨烯谐振探头^[70]; (i) 经丙酮蚀刻处理后的插芯上石墨烯膜显微图像^[71]; (j) 350 ℃退火处理的插芯上石墨烯膜显微图像^[71]; (k) 经丙酮蚀刻和退火处理的插芯上石墨烯膜显微图像^[71]

Fig. 2. Schematic diagram of the structure of graphene resonant pressure sensor: (a) Optical image of graphene resonator made by Cornell University^[65]; (b) ceramic ferrules used by the Hong Kong Polytechnic University^[66]; (c) graphene nanoribbons used by the Hong Kong Polytechnic University^[66]; (d) dumbbell shaped squeeze-film graphene pressure sensor made by Delft University^[67]; (e) suspended graphene beam under atomic force microscope, in which the oxide is black and the graphene beam is orange^[68]; (f) closed cavity F-P resonant sensor^[69]; (g) open cavity F-P resonant sensor^[69]; (h) graphene resonant probe made by fusion of single-mode optical fiber and quartz capillary^[70]; (i) microscopy image of graphene on the ferrule treated by acetone etching^[71]; (j) microscopy image of graphene on the ferrule treated by 350 ℃ annealing^[71]; (k) microscopy image of graphene on the ferrule treated by acetone etching and annealing^[71].

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图 3 石墨烯谐振式加速度计结构及其性能测试　(a) 韩国国立交通大学设计的石墨烯谐振式加速度计^[73]; (b) 在石墨烯谐振式加速度计上附着微小质量^[74]; (c) 不同附着质量的频率-加速度关系曲线^[74]; (d) 美国哥伦比亚大学设计的鼓式石墨烯谐振式加速度计^[62]; (e) 中国国防科技大学设计的石墨烯谐振加速度计^[76]

Fig. 3. Structure and performance test of graphene resonant accelerometer: (a) Graphene resonant accelerometer designed by Korea National Jiaotong University^[73]; (b) small mass attached to graphene resonant accelerometer^[74]; (c) accelerations against frequency for different attached masses^[74]; (d) drum graphene resonant accelerometer designed by Columbia University, USA^[62]; (e) graphene resonant accelerometer designed by National University of Defense Technology, China^[76].

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图 4 石墨烯谐振式质量传感器及其性能表征　(a) 查尔姆斯理工大学设计的石墨烯谐振式质量传感器^[78]; (b) 韩国世明大学设计的石墨烯谐振式质量传感器^[83]; (c) 石墨烯谐振式质量传感器在不同边界条件下的灵敏度^[84]; (d) 单层和多层石墨烯的谐振频率-质量变化曲线^[85]; (e) 单层和多层石墨烯的谐振频移-质量变化曲线^[85]; (f) 谐振频率和频移与质量的关系曲线, 蓝色曲线表示谐振频率随石墨烯层数的变化, 红色曲线表示频移随石墨烯层数的变化^[86]

Fig. 4. Graphene resonant mass sensor and its performance characterization: (a) Graphene resonant mass sensor designed by Chalmers University of Technology^[78]; (b) graphene resonant mass sensor designed by Semyung University^[83]; (c) sensitivity of graphene resonant mass sensor under different boundary conditions^[84]; (d) resonant frequency mass variation curve of monolayer/multilayer graphene films^[85]; (e) frequency shift mass curve of monolayer/multilayer graphene films^[85]; (f) relation curve of resonant frequency and frequency shift with mass, the blue curve represents the change of resonant frequency with the number of graphene layers, and the red curve is the change of frequency shift^[86].

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图 5 日本北陆先端科学技术大学制作的石墨烯谐振式质量传感器^[88]　(a)—(h) 在285 nm厚的SiO₂衬底上使用CVD法得到的石墨烯来制作石墨烯谐振器的工艺流程; (i) 制作的石墨烯谐振器光学图像

Fig. 5. Process of graphene resonant mass sensor produced by Japan Advanced Institute of Science and Technology^[88]: (a)—(h) Schematic diagrams of top gated graphene resonator fabrication processes with CVD graphene on Si substrate with 285 nm SiO₂; (i) optical image of the fabricated top-gated graphene resonator.

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表 1 石墨烯谐振器性能指标对比

Table 1. Comparison of performance indicators of graphene resonant pressure sensors.

制备方法	层数	固支方式	谐振频率f/MHz	品质因数Q	激励方式	检测方式	实验环境 (温度, 压强P/Pa)	文献
机械剥离法	1—224	双端固支	1—170	20—850	电学/ 空间光	空间光	室温, P < 1.3×10^–4	[53]
	1	双端固支	30—120 30—120	125 14000	电学	电学	室温, P < 1.3×10^–3; 5 K, P < 1.3×10^–3	[57]
	<5	双端固支	108—122	—	电学	电学	室温, P < 6.7	[59]
	～31	圆形固支	1—30	2400±300	空间光	空间光	室温, P < 0.79	[60]
	2—5	双端固支	8—23	7000	热噪声	电学	室温, P < 10^–3	[61]
	1	圆形固支	15.7	120	空间光	空间光	室温, P = 1.013×10⁵	[64]
	1	周边固支	30—90	25	空间光	空间光	室温, P = 27—3×10⁴	[65]
	～30	圆形固支	12—16	1—100	空间光	空间光	室温, P = 8×10²—10⁵	[67]
CVD法	1	双端固支	5—75	25 9000	电学/ 空间光	电学/ 空间光	室温, P < 6.7×10^–3; 10 K, P < 6.7×10^–3	[58]
	30—60	双端固支	0.060—0.204	81—103	光纤光	光纤光	室温, P = 10^–2—10⁵	[66]
	～13	圆形固支	0.509—0.542	13.3—16.6	光纤光	光纤光	室温, P = 10⁵—2.99×10⁵	[69]

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表 2 石墨烯谐振式压力传感器性能指标对比

Table 2. Comparison of performance indicators of graphene resonant pressure sensors.

层数/层	形状	长度或直径/μm	激励方式	检测方式	测压范围/Pa	谐振频率f	品质因数Q (室温)	压力灵敏度 (kHz·kPa^–1)	文献
1—75	正方形	4.75	空间光	空间光	10^–4—10⁵	30— 90 MHz	～25	—	[65]
多层	圆形	125	光纤光	光纤光	10^–2—10⁵	60—204 kHz	81—103	/	[66]
少层	圆形	5	空间光	空间光	8×10²—10⁵	12— 16 MHz	1—100	10—90	[67]
多层	正方形	4	空间光	空间光	10²—10⁵	15.5— 25.5 MHz	50—80	1.65—3.10	[68]
13	圆形	125	光纤光	光纤光	(1—2.99)×10⁵	509— 542 kHz	13.3—16.6	0.135	[69]
10	圆形	125	光纤光	光纤光	0—6.895×10⁴	1.43— 1.64 MHz	10.2—13.9	2.93	[70]
10	圆形	125	光纤光	光纤光	2—10⁵	481— 760 kHz	110—1034	1—110.4	[71]

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表 3 石墨烯谐振式加速度计性能指标对比

Table 3. Comparison of performance indicators of graphene resonant accelerations.

分析方法	薄膜形状	长度或直径	激励方式	检测方式	谐振频率 f	文献
分子动力学仿真	长方形	10.8 nm×0.7 nm	电学		0—250 GHz	[73]
		12.0 nm×0.7 nm		电学	0—225 GHz	[74]
		$1.2\;{\mu }\mathrm{m}\times 1.0\;{\mu }\mathrm{m}$			0—10 MHz	[76]
实验	圆形	$3—10\;{\mu }\mathrm{m}$	电学	电学	1—10 MHz	[62]

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表 4 石墨烯谐振式质量传感器仿真性能指标对比

Table 4. Comparison of simulation performance indicators of graphene resonant mass sensors.

实验/仿真	分析方法	薄膜形状	检测目标	谐振频率f	可检测到的最小质量/(10^–21 g)	品质因数Q	文献
仿真	分子结构力学仿真	长方形	质点/原子尘埃	0—104 GHz	1	—	[77]
	分子动力学仿真	正方形	惰性气体原子	—	1	—	[81]
	有限元模拟	圆形	质点	～0—200 GHz	1	—	[86]
	连续弹性介质模型和瑞利能量法	圆形	质点	0—105 GHz	10^–3	—	[82]
	分子动力学仿真	长方形	纳米粒子	0—230 GHz	10^–3	—	[83]
	连续弹性介质模型	正方形	纳米粒子	0—105 GHz	10	—	[85]
	薄膜理论和有限元模拟	长方形	烟草花叶病毒	～200—1500 MHz	—	—	[87]
实验	—	长方形	氩氢混合气	95.5 MHz	886	45	[88]

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