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静电力显微镜(electrostatic force microscopy, EFM)具有较高的灵敏度和空间分辨率, 在新能源材料静电性质的测量中被广泛应用. 时间分辨静电力显微镜技术主要用于材料的动态电学性质测量, 该技术中常用的泵浦探测方法存在设备装置复杂、成本昂贵、测量存在不确定性等问题. 本文采用直接时域测量方法, 减小了测量的实现复杂度, 通过应用多频激励或者激励悬臂高阶模态的方法实现了EFM多种参数同时测量和时间分辨率的提高, 达到了微秒级的时间分辨率, 并应用小波变换对测量得到的探针信号进行分析, 实现了对材料动态电学性质的提取. 通过应用该技术进行仿真实验, 实现了对模拟样品电势衰减过程中的动态电势变化和模拟电池放电过程中的离子运动特征时间等性质的测量.Electrostatic force microscopy (EFM) has high sensitivity and lateral resolution, and it is widely used to measure the electrostatic properties of new energy materials. The time-resolved electrostatic force microscope technology is used to measure the dynamic electrical properties of materials, pump detection method commonly used in this technology has problems such as complex equipment, high cost, and uncertainty in the measurement. In this work the method of directly measuring the time domain is adopted. This method reduces the complexity of measurement. By using the multi-frequency or high-frequency excitation method, the simultaneous measurement of multiple EFM parameters and the improvement of time resolution can be achieved, reaching a time resolution of microseconds, and by applying wavelet transform to the tip signal obtained by the measurement the dynamic electrical properties of the materials can be extracted. Applying this technology to simulation experiments, it is possible to measure the dynamic potential changes and the characteristic time parameter of ion movement in the microsecond-level electrical dynamic process of the simulated battery materials.
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Keywords:
- multi-frequency electrostatic force microscopy /
- time resolution /
- dynamic measurement /
- wavelet transform
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图 2 多频探针信号的小波变换分析过程 (a) 探针信号; (b) 小波时频分析结果
Fig. 2. Wavelet transform analysis process for multifrequency tip signal: (a) Tip signal; (b) the result of wavelet time-frequency analysis
图 3 整个动态过程中的探针振幅 (a) 第一模态振幅; (b) 第二模态振幅
Fig. 3. Tip amplitude during the whole dynamic process: (a) The first eigenmode amplitude; (b) the second eigenmode amplitude.
图 4 第二模态激励电压为(a) 5 V, (b) 10 V时, 分别测量第一模态振幅为5, 8, 10, 20 nm时的第二模态振幅变化; (c), (d)为(a)和(b)对应的第二模态幅值波动与第一模态振幅设定值之间的关系
Fig. 4. Changes of second eigenmode amplitude when the first mode amplitude is 5, 8, 10, 20 nm with the second eigenmode excitation of (a) 5 V, (b) 10 V; (c), (d) are the relationships between the amplitude fluctuation of the second mode and the value of the first eigenmode amplitude corresponding to (a) and (b).
图 5 (a) 参数设置恒定, 特征时间
$ \tau $ 为$2, 5, 10, 20, 30, 50~\text{μ}\mathrm{s}$ 时的整个电势衰减过程对应的探针振幅; (b) 在$t=5~\text{μ}\mathrm{s}$ 处, 不同$ \tau $ 值对应的探针振幅改变大小与样品表面电势改变大小之间的关系Fig. 5. (a) Tip amplitude of the entire potential decay processes when the other parameters are constant and the characteristic time
$ \tau $ is 2, 5, 10, 20, 30, 50 μs; (b) the relationship between the change of the tip amplitude and the change of the sample surface potential corresponding to different$ \tau $ at$t=5~\text{μ}\mathrm{s}$ .
图 6 探针振幅变化与样品电势变化大小之间的关系 (a) 激励电压为10 V, 抬升高度为50 nm; (b) 激励电压为1 V, 抬升高度为20 nm; (c) 激励电压为1 V, 抬升高度为50 nm
Fig. 6. Relationship between the change of the tip amplitude and the change of the sample surface: (a) The excitation voltage is 10 V, and the lift height is 50 nm; (b) the excitation voltage is 1 V, and the lift height is 20 nm; (c) the excitation voltage is 1 V, and the lift height is 50 nm
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[1] Binnig G, Gerber C, Stoll E, Albrecht T R, Quate C F 1987 Surf. Sci. 189–190 1
Google Scholar
[2] Li Y, Qian J Q, Li Y Z 2010 Chin. Phys. B 19 050701
Google Scholar
[3] Rugar D, Mamin H J, Guethner P, Lambert S E, Yogi T 1990 J. Appl. Phys. 68 1169
Google Scholar
[4] Kalinin S V, Eliseev E A, Morozovska A N 2006 Appl. Phys. Lett. 88 232904
Google Scholar
[5] Nonnenmacher M, Oboyle M P, Wickramasinghe H K 1991 Appl. Phys. Lett. 58 2921
Google Scholar
[6] Hansma P, Drake B, Marti O, Gould S A C, Prater C B 1989 Science 243 641
Google Scholar
[7] Girard P 2001 Nanotechnology 12 485
Google Scholar
[8] Martin Y, Abraham D W, Wickramasinghe H K 1988 Appl. Phys. Lett. 52 1103
Google Scholar
[9] Stern J E, Terris B D, Mamin H J, Rugar D 1988 Appl. Phys. Lett. 53 2717
Google Scholar
[10] Okamoto K, Yoshimoto K, Sugawara Y, Morita S 2003 Appl. Surf. Sci. 210 128
Google Scholar
[11] Lochthofen A, Mertin W, Bacher G, Hoeppel L, Bader S, Off J, Hahn B 2008 Appl. Phys. Lett. 93 022107
Google Scholar
[12] Sasahara A, Pang C L, Onishi H 2006 J. Phys. Chem. B 110 17584
Google Scholar
[13] Zhu J, Zeng K, Lu L 2012 J. Appl. Phys. 111 063723
Google Scholar
[14] Yamagishi Y, Kobayashi K, Kimura T, Noda K, Yamada H 2018 Org. Electron. 57 118
Google Scholar
[15] Araki K, Ie Y, Aso Y, Matsumoto T 2016 Jpn. J. Appl. Phys. 55 070305
Google Scholar
[16] Fukuzawa R, Takahashi T 2020 Rev. Sci. Instrum. 91 023702
Google Scholar
[17] Schumacher Z, Spielhofer A, Miyahara Y, Grutter P 2017 Appl. Phys. Lett. 110 053111
Google Scholar
[18] Murawski J, Mönch T, Milde P, Hein M P, Nicht S, Zerweck-Trogisch U, Eng L M 2015 J. Appl. Phys. 118 244502
Google Scholar
[19] Giridharagopal R, Rayermann G E, Shao G, Moore D T, Reid O G, Tillack A F, Masiello D J, Ginger D S 2012 Nano Lett. 12 893
Google Scholar
[20] Karatay D U, Harrison J S, Glaz M S, Giridharagopal R, Ginger D S 2016 Rev. Sci. Instrum. 87 053702
Google Scholar
[21] Jung W, Cho D, Kim M K, Choi H J, Lyo I W 2011 P. Natl. Acad. Sci. U. S. A. 108 13973
Google Scholar
[22] Mascaro A, Miyahara Y, Enright T, Dagdeviren O E, Grutter P 2019 Beilstein J. Nanotech. 10 617
Google Scholar
[23] Maksumov A, Vidu R, Palazoglu A, Stroeve P 2004 J. Colloid Interf. Sci. 272 365
Google Scholar
[24] Carmichael M, Vidu R, Maksumov A, Palazoglu A, Stroeve P 2004 Langmuir 20 11557
Google Scholar
[25] López-Guerra E A, Banfi F, Solares S D, Ferrini G 2018 Sci. Rep-U.K. 8 7534
Google Scholar
[26] Stark R W, Naujoks N, Stemmer A 2007 Nanotechnology 18 65502
Google Scholar
[27] Wang Z Y, Qian J Q, Li Y Z, Zhang Y X, Song Z H, Dou Z P, Lin R 2019 Micron 118 58
Google Scholar
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