功能化原子力显微镜在纳米电介质材料性能研究中的应用进展

孟菁饴; 卢红伟; 马世乐; 张嘉奇; 何富民; 苏伟涛; 赵晓东; 田婷; 王翼; 邢誉

doi:10.7498/aps.71.20221462

摘要

随着电子元件向微型化、柔性化、智能化发展, 迫切需要介电材料具有更优异的介电性能. 原子力显微镜作为一种具有纳米级高分辨率的测量仪器, 在纳米电介质的研究中表现出独特的优势, 功能化原子力显微镜的诞生更是为纳米电介质微区性质的研究做出重要贡献. 本文综述了原子力显微镜、静电力显微镜、开尔文探针力显微镜、压电响应力显微镜和原子显微镜-红外光谱在研究介电材料纳米区域的微观形貌、界面结构、电畴变化和电荷分布方面的最新研究进展, 并对现有研究中存在的问题和未来可能的发展方向进行了讨论.

关键词:

Abstract

The rapid development of the electrical and electronic industry requires components with miniaturization, flexibility, and intelligence. Dielectric materials, as important materials for the preparation of electronic components, are required to have excellent dielectric properties such as high breakdown electric field, high energy storage density and low dielectric loss. Owing to the lack of ultra-high resolution characterization tools, the research on the improvement of dielectric material properties stopped at a macroscopic level in the past. Atomic force microscopy, a measurement instrument which possesses a nanoscale high resolution, shows unique advantages in the study of nanodielectrics, and the advent of functional atomic force microscopy has made important contributions to characterization of the electrical, optical, and mechanical properties of nano-dielectric micro-regions. In this paper, we review the progress of atomic force microscopy, electrostatic force microscopy, Kelvin probe force microscopy, piezoelectric response force microscopy and atomic microscopy-infrared spectroscopy in the study of nanodielectric applications. Firstly, their structures and principles are introduced; secondly, their recent research progress of studying the microscopic morphology, interfacial structure, domain behavior and charge distribution in the nanometer region of dielectric materials is presented, and finally, the problems in the existing research and possible future research directions are discussed.

Keywords:

作者及机构信息

1.
杭州电子科技大学理学院, 杭州　310018

2.
杭州电子科技大学海宁研究院, 海宁　314408

通信作者: 卢红伟, luhongwei@hdu.edu.cn

Authors and contacts

1.
School of Sciences, Hangzhou Dianzi University, Hangzhou 310018, China

2.
Haining Institute, Hangzhou Dianzi University, Haining 314408, China

Corresponding author: Lu Hong-Wei, luhongwei@hdu.edu.cn

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施引文献

图 1 原子力显微镜的发展

Fig. 1. Development of atomic force microscopy.

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图 2 功能化原子力显微镜工作原理示意图　(a) AFM; (b) KPFM; (c) EFM; (d) PFM; (e) AFM-IR

Fig. 2. Schematic diagram of functional AFM working principle: (a) AFM; (b) KPFM; (c) EFM; (d) PFM; (e) AFM-IR.

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图 3 (a) 未经处理的PVDF薄膜的AFM三维形貌图像^[60]; (b) 拉伸的PVDF薄膜的AFM三维形貌图像^[60]

Fig. 3. Three dimensional topography images of (a) untreated PVDF film^[60] and (b) stretched PVDF film by AFM^[60].

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图 4 PVDF薄膜在不同剂量的电子辐照下的AFM三维图像^[63]　(a) 0 kGy; (b) 500 kGy; (c) 1000 kGy; (d) 1300 kGy; (e) 1700 kGy; (f) 2200 kGy

Fig. 4. Three dimensional images by AFM of PVDF films under various doses^[63]: (a) 0 kGy; (b) 500 kGy; (c) 1000 kGy; (d) 1300 kGy; (e) 1700 kGy; (f) 2200 kGy.

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图 5 PVDF样品在加热并保持在162 ℃期间结构演变过程的AFM表征, 其中图(a)—(d)是分别在162 ℃的周期退火(a) 0, (b) 2, (c) 10, (d) 24 h后拍摄^[64]; (e) PVDF样品的晶型由α相到γ相的演变过程^[64]

Fig. 5. AFM phase images show the structure evolution process of PVDF heating up to and at 162 ℃. The picture was taken after period annealing at 162 ℃ for (a) 0, (b) 2, (c) 10, and (d) 24 h^[64]. (e) Scheme showing the crystals evolution of PVDF sample^[64].

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图 6 NT07薄膜复合材料的AFM形貌图像^[71]

Fig. 6. AFM topographic image of NT07 thin film composite showing PVDF^[71].

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图 7 5% P(VDF-HFP)/GLC的(a) 表面形貌和(b) AFM-IR强度分布^[75]; (c) 图(a)和图(b)中标记区域的局部红外光谱^[75]

Fig. 7. (a) Topography signal (10 μm×10 μm) and (b) AFM-IR intensity distribution map with irradiation by a laser at 1216 cm^–1 of 5% P(VDF-HFP)/GLC^[75]; (c) local IR spectra of the sites marked in panel (a) and (b) ^[75].

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图 8 (a) f-PPTA纳米团簇的形成过程和在PVDF基体中的排列^[78]; (b) PVDF基薄膜的TEM图像^[78]; (c)具有f-PPTA的PVDF基薄膜的PFM图像^[78]

Fig. 8. (a) f-PPTA nanocluster formation process and the arrangement in PVDF matrix^[78]; (b) TEM image of PVDF-based film^[78]; (c) PFM image of the films with f-PPTA^[78].

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图 9 (a) 强制组装技术进行三组分多层薄膜共挤工艺示意图^[79]; (b) PET/PMMA/P(VDF-HFP)多层膜的AFM形貌图^[79]; (c) PET/PMMA/P(VDF-HFP)(PMMA的体积分数为8%)65层挤压薄膜(200 μm)和相应的双向拉伸薄膜(10 μm)的AFM形貌图^[79]

Fig. 9. (a) Schematics of three-component multilayer film coextrusion process via the forced assembly technique^[79]; (b) AFM phase images for PET/PMMA/P(VDF-HFP) multilayer films^[79]; (c) AFM phase images of the as-extruded PET/PMMA/P(VDF-HFP) 65-layer film (200 μm) with 8% volume fraction of PMMA and the corresponding biaxially oriented film (10 μm)^[79].

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图 10 界面模型　(a) Lewis模型^[83]; (b) Tanaka多核模型^[84]

Fig. 10. Interface model: (a) Lewis model^[83]; (b) Tanaka multi-core model^[84].

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图 11 (a) EFM局部介电性能检测结果^[87]; (b) 局部有限元模拟模型^[87]

Fig. 11. (a) Results of local dielectric property detection^[87]; (b) the local finite element models^[87].

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图 12 (a), (b) MgO/LOPE和SiO_2/LDPE的AFM高度形貌图(5 μm×5 μm)^[88]; (c), (d) MgO/LOPE和SiO₂/LDPE的EFM相位图^[88]; (e), (f) MgO/LOPE和SiO₂/LDPE的一维相位扫描曲线^[88]; (g) SiO₂在LDPE中不同嵌入形态的模型^[88]

Fig. 12. (a), (b) AFM height image of MgO/LOPE and SiO₂/LDPE material (5 μm×5 μm)^[88]; (c), (d) AFM lift mode phase image of MgO/LOPE and SiO₂/LDPE belong to the same zone^[88]; (e), (f) scanning curve in one dimension of MgO/LDPE and SiO₂/LDPE^[88]; (g) models of SiO₂ embedded in LDPE^[88].

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图 13 (a), (b) 含有质量分数为2%的F1填料的有机硅复合材料的AFM形貌图像和EFM图像^[89]; (c), (d) 含有质量分数为2%的F2填料的有机硅复合材料的AFM形貌图像和EFM图像^[89]

Fig. 13. (a), (b) AFM topography image and EFM image of the silicone composite material containing the filler F1 with mass fraction of 2% ^[89]; (c), (d) AFM topography image and EFM image of the silicone composite material containing the filler F2 with the mass fraction of 2%^[89].

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图 14 (a), (d) BTO/P(VDF-TrFE-CFE)的AFM表面高度形貌^[93]; (b), (e) 图(a)和(d)中标记位置的局部红外光谱^[93]; (c), (f) 图(a)和(d)中标记位置的归一化红外响应^[93]

Fig. 14. (a), (d) Topography (1 μm×1 μm) of BTO/P(VDF-TrFE-CFE) nanocomposites^[93]; (b), (e) local IR spectra at different sites as marked in panel (a) and (b)^[93]; (c), (f) normalized IR response at 1275 cm^–1 at different sites as marked in panel (a) and (d)^[93]

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图 15 (a) 改进KPFM工作原理示意图; (b) P(VDF-TrFE)/BT纳米复合材料界面中氢键和固有偶极子的取向示意图; (c) 不同直流偏压下P(VDF-TrFE)/BT界面附近的局部偏振特性KPFM检测结果^[96]; (d) 不同直流电压下的感应表面电位差, 以及偶极层厚度和电势的关系^[96]

Fig. 15. (a) Schematic diagram of the working principle of the modified Kelvin probe force microscope; (b) schematic diagram of hydrogen bond and intrinsic dipole orientation in P(VDF-TrFe)/BT; (c) the results of local polarization property detection near an embedded nanoparticle in P(VDF-TrFE)/BT^[96]; (d) the induced surface potential difference under different DC voltages, and the relationship between dipole layer thickness and potential^[96].

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图 16 添加摩尔浓度为(a) 0.0%, (b) 2.0%, (c) 4.0%和(d) 8.0%的AuNPs的BT陶瓷在1250 ℃下烧结2 h的PFM振幅(上图)和相位对比(下图)图像^[101]

Fig. 16. Amplitude (upper panel) and phase contrast (lower panel) PFM images of BT ceramics with (a) 0.0%, (b) 2.0%, (c) 4.0% and (d) 8.0% molar concentration of AuNPs sintered at 1250℃ for 2 h^[101].

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图 17 BF-BT-0.05 NT的垂直压电力显微镜(VPFM) (a)振幅和(b)相位图^[103]; BF-BT-0.05 NT在±20 V极化后的(c)振幅和(d)相位^[103]; BF-BT-0.12 NT的VPFM (e)振幅^[103]和(f)相位图^[103]; BF-BT-0.12 NT在±20 V极化后的(g)振幅和(h)相位图^[103]

Fig. 17. (a) Amplitude and (b) phase images of vertical piezoelectric force microscopy (VPFM) for BF-BT-0.05 NT^[103]; (c) amplitude and (d) phase images of PFM after poling with ±20 V voltage for BF-BT-0.05 NT^[103]; (e) amplitude and (f) phase images of VPFM for BF-BT-0.12 NT^[103]; (g) amplitude and (h) phase images of PFM after poling with ±20 V voltage for BF-BT-0.12 NT^[103].

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图 18 (a) 样本结构和弯曲样品的示意图(弯曲半径R); (b) 不同拉伸应变的P(VDF-TrFE)薄膜PFM相位图^[106]; (c) 不同振幅和不同持续时间的脉冲电压下, 不同拉伸应变的P(VDF-TrFE)薄膜的PFM相位图^[106]

Fig. 18. (a) Sample structure and schematic drawings of the flat and bent sample; (b) PFM phase images of a ferroelectric P(VDF-TrFE) film with different tensile strains^[106]; (c) under the condition of voltage pulses of different amplitudes and different durations, PFM phase images of a P(VDF-TrFE) film with different tensile strains^[106].

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图 19 (a) EP表面的MFM图(扫描区域5 μm×5 μm)^[113]; (b), (c) KPFM图和自由基区电势分布^[113]; (d), (e) KPFM图和非自由基区电势分布; (f) 自由基区和非自由基区的深陷参数^[113]

Fig. 19. (a) MFM map of the EP surface^[113]; (b), (c) KPFM map and value of the potential in the radical region^[113]; (d), (e) KPFM map and value of the potential in the non-radical region^[113]; (f) deep trap parameters in the radical and non-radical regions^[113].

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图 20 (a) KPFM 测试配置示意图^[115]; (b) 不同负横向电场对应的空间电荷分布^[115]

Fig. 20. (a) Schematic diagram of the KPFM testing configuration^[115]; (b) different negative lateral electric field corresponding to the space charge distribution^[115].

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图 21 KPFM 测试示意图　(a), (b) PEI/PCBM 复合材料的(a)形貌和(b)表面电位映射^[118]; (c) 沿水平轴的表面电位分布图^[118]; (d) 分子半导体捕获电子形成的内建电场示意图^[118]

Fig. 21. Schematic diagram of the KPFM testing: (a) Topography and (b) surface potential mapping of the PEI/PCBM composite^[118]; (c) surface potential profiles along the horizontal axis derived from the surface potential mappings^[118]; (d) schematic illustration of the built-in electric field formed by the molecular semiconductor captured electrons^[118].

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图 22 PP和PP-g-ITA的(a), (b)表面电位随时间变化的KPFM图^[119]; (c), (d) AFM-IR形貌图^[119]; (e), (f) 1780 cm^–1红外激光下AFM-IR化学谱图^[119]

Fig. 22. (a), (b) Time-dependent surface potential distribution on the scanned line in pristine PP and PP-g-ITA of KPFM^[119]; (c), (d) AFM-IR topography of the specimens surface for pristine PP and the PP-g-ITA^[119]; (e), (f) AFM-IR chemical map irradiated with a 1780 cm^–1 laser^[119].

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表 1 功能化原子力显微镜简介

Table 1. Introduction to functional atomic force microscopy.

分类	名称	功能	应用
表征材料电学性能	静电力显微镜^[15]	运用导电悬臂探测样品表面铁电区域, 得到纳米尺度的区域电学性能图.	样品表面电势^[21] 检测相间结构^[22] 研究电荷传播^[23] 检测电荷分布^[24] 电荷存储^[25]
	导电原子力显微镜^[26]	使用导电的偏压探针接触式扫描样品表面, 测量样品导电性.	测量局域电导率^[27] 测量电流-电压曲线^[28] 绘制能带分布^[29] 研究纳米级电阻开关^[28]
	开尔文探针力显微镜^[16]	在非接触模式下通过检测探针与样品之间的静电信号提供样品表面电势等相关信息.	测量探针尖端和样品表面电位差^[30] 测量空间电荷分布^[31] 评估缺陷状态^[32]
	压电响应力显微镜^[33]	在接触模式下基于逆压电效应原理测量样品的局域压电响应能力.	研究铁电畴^[34] 记录纳米级磁滞回线^[35] 检测电致收缩/膨胀^[36] 观察拓扑状态^[37]
	扫描电容显微镜^[38]	记录样品和金属探针之间的局部电容变化.	测量局部电容^[39] 测量载流子浓度分布^[40] 局部电荷的捕捉/释放^[41]
表征材料化学结构	原子力显微镜-红外光谱^[20]	使用AFM探针的端检测样品特定区域中由于吸收红外辐射而导致的热膨胀, 来获得样品的红外吸收光谱及化学成分分布图谱.	纳米级红外光谱^[42] 化学成分分布^[43] 材料组分逆向分析^[43] 纳米结晶度变化^[44] 纤维中的分子取向^[45]
表征材料化学结构	拉曼光谱-原子力显微镜^[46]	使用激发激光来检测样品表面光学信号, 提供局部拉曼光谱, 表征样品表面的局部化学组成.	分析化学成分^[47] 分析化学构象获取形貌信息^[48] 测量黏弹性^[49]
表征材料力学性能	力调制显微镜^[50]	计算样品表面硬度、黏弹性等力学性能.	测量存储模量和损耗模量^[51] 测量局部杨氏模量^[52] 测量表面弹性变化^[53]
表征材料力学性能	横向力显微镜^[54]	通过检测悬臂在扫描样品时的扭曲来检测样品的摩擦力、黏附力等力学性能.	测量微区摩擦性能^[55] 测量样品刚度^[56] 测量表面黏附力测量拓扑特性^[57]

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