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高分辨显微成像技术为人们推开了探索微观世界的大门, 而飞秒激光技术又为人们提供了一把探测超快物理/化学现象的尺子. 将这两者结合, 发展既有超高空间分辨、又有超快时间分辨的新型显微成像技术, 对于人们探索极小时空尺度下新的科学现象和规律有非常重要的意义. 本文综述了目前国际上主要超高时空分辨显微成像技术的基本原理和特点, 并介绍了其在光电材料与器件表征、飞秒激光微加工监测、表面等离激元动力学表征等方面的最新应用进展. 超高时空分辨显微成像技术的发展, 不仅推动了光学显微成像领域的进步, 也为精密加工、二维材料动力学、光电器件设计与表征等领域提供了关键技术手段, 具有广阔的应用前景.High-resolution microscopy has opened the door to the exploration of the micro-world, while femtosecond laser has provided a measurement method for detecting ultrafast physical/chemical phenomena. Combination of these two techniques can produce new microscopic techniques with both ultra-high spatial resolution and ultra-fast temporal resolution, and thus has great importance in exploring new scientific phenomena and mechanisms on an extremely small spatial scale and temporal scale. This paper reviews the basic principles and properties of main microscopic techniques with ultra-high temporal resolution and spatial resolution, and introduces the latest research progress of their applications in various fields such as characterizing optoelectronic materials and devices, monitoring femtosecond laser micromachining, and detecting surface plasmon excitation dynamics. In order to conduct these researches systematically, we group these techniques based on time dimension and space dimension, including the near-field multi-pulse imaging techniques, the far-field multi-pulse imaging techniques, and the far-field single-pulse imaging techniques. In Section 2, we introduce the principles and characteristics of the ultra-high spatiotemporally resolved microscopic techniques. The near-field multi-pulse spatiotemporally microscopic techniques based on nano-probe are described in Subsection 2.1, in which is shown the combination of common near-field imaging techniques such as atomic force microscopy (AFM), near-field scanning optical microscopy (NSOM), scanning tunneling microscope (STM), and the ultra-fast temporal detection of pump-probe technique. In Subsection 2.2, we introduce the far-field multi-pulse spatiotemporal microscopic techniques. In contrast to near-field cases, the far-field spatiotemporal microscopic techniques have lower spatial resolution but possess more advantages of being non-invasive and non-contact, wider field of view, and faster imaging speed. In Subsection 2.3 we introduce the far-field single-pulse spatiotemporal microscopic techniques, in which is used a single ultrafast light pulse to capture dynamic processes at different moments in time, thereby enabling real-time imaging of ultrafast phenomena. In Section 3 , the advances in the application of the ultra-high spatiotemporal resolved microscopic techniques are introduced in many frontier areas, including the monitoring of femtosecond laser micromachining in Subsection 3.1, the detection of optoelectronic materials/devices in Subsection 3.2, and the characterization of surface plasmon dynamics in Subsection 3.3. Finally, in Section 4, we summarize the features of all above-mentioned spatiotemporal microscopic techniques in a table, including the spatial resolution and temporal resolution, advantages and disadvantages of each technique, and we also provide an outlook on future development trend in this research field. Looking forward to the future, ultra-high spatiotemporally resolved microscopy will develop rapidly toward the goal of "smaller, faster, smarter and more extensive". Its development not only promotes the research of the microscopy technology, but also provides a powerful tool for various practical applications such as precision machining, two-dimensional material dynamics, optoelectronic device design and characterization.
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图 1 (a) 飞秒近场扫描显微成像系统示意图以及延迟时间0, 500 fs和2 ps时的近场泵浦-探测信号[36]; (b) 利用tr-NSOM对WSe2进行的时间分辨纳米尺度探测实验[37]
Fig. 1. (a) Schematic representation of the femtosecond near-field scanning microscopy imaging system and the near-field pump-probe signal at the time delay of 0, 500 fs and 2 ps[36]; (b) time resolved infrared nano-imaging experiments on WSe2 by using tr-NSOM[37].
图 2 (a) tr-PiFM系统示意图[42]; 在两个不同时间延迟(–5.9和0.7 ps)下AFM所记录的(b), (c)形貌图和(d), (e)光诱导力图像[42]; (f)比较远场检测到的泵浦-探测信号(橙色实线)和光诱导力信号(黑色圆点)[42]
Fig. 2. (a) Schematic of the tr-PiFM system[42]; topography image (b), (c) and optical force image (d), (e) are simultaneously recorded at negative time delay 5.9 ps (or positive time delay 0.7 ps) [42]; (f) comparison between the far-field detected pump-probe signal (orange solid line) and the tr-PiFM signal (black circle dot)[42].
图 3 (a) 超快FMW成像系统示意图, 经过脉冲整形系统后的飞秒脉冲通过刻蚀在金针尖上的光栅激发SPP并聚焦到针尖的顶点[26]; (b) 硅-金膜表面SPP热点S1, S2, S3位置对应的FWM扫描图像[26]; (c) 每个热点对应的AFM形貌图像[26]; (d) 金膜中SPP热点动力学的飞秒FWM纳米成像, 对应热点在不同延迟时间下的相对强度变化[26]
Fig. 3. (a) Schematic of the ultrafast FMW imaging experiment, the femtosecond pulse after the pulse shaping system excited the SPP through a grating etched on the gold tip and focused to the vertex of the tip[26]; (b) near-field FWM image of a Si-Au step, showing SPP “hotspots” S1, S2 and S3[26]; (c) simultaneously acquired AFM topography[26]; (d) FWM nanoimages of the SPP “hotspots” dynamics of a Si-Au surface, corresponding to different inter-pulse delay, demonstrating evolution of the relative intensities in spots S1, S2 and S3[26].
图 4 (a) Terada等[46]所提出的时间分辨STM工作原理图; (b) 实空间上GaAs样品表面Co纳米颗粒的STM形貌图[46]; (c) 图(b)中不同位置的空穴捕获率测量结果[46]; (d) 图(b)与图(c)的图象叠加[46]; (e) 空穴捕获率与Co纳米颗粒尺寸的依赖关系[46]
Fig. 4. (a) Schematic of the time-resolved STM proposed by Yasuhiko Terada[46]; (b) STM topography of Co nanoparticles on the surface of GaAs samples in real space[46]; (c) hole capture rate measurements at different locations in Fig. (b) [46]; (d) superposition of Fig. (b) and Fig. (c) [46]; (e) size dependence of hole capture rate[46].
图 6 (a) 莫尔现象及SIM实现超分辨原理[56]; (b) 基于DMD的结构光照明泵浦-探测成像系统光路图; (c) 左侧分别为硅纳米线样品的SEM图像、SPPM成像、传统光学显微成像, 右侧为SPPM成像与传统光学显微成像分辨率对比、SPPM泵浦-探测获得样品不同位置的载流子弛豫过程[59]
Fig. 6. (a) Moire phenomenon and the SIM principle of super-resolution[56]; (b) schematic of DMD-based structured pump–probe microscope[59]; (c) the left side: SEM image, SPPM image, and image by conventional optical microscopy of silicon nanowire samples respectively; the right side: the carrier relaxation process at different positions of SPPM imaging and conventional optical microscopy imaging resolution and SPPM pump-probe[59].
图 7 (a) SPSLM系统示意图及光路图, 其中红色和紫色分别代表泵浦光和探测光[60]; (b)单个泵浦光脉冲烧蚀硅表面从0到2.5 ps采集到的原始图像及重建得到的表面形貌演化图[60]
Fig. 7. (a) Schematic of the SPSLM, where color red and color violet indicate pump light and probe light respectively[60]; (b) raw images and the reconstructed surface evolution height maps collected from 0 to 2.5 ps[60].
图 8 (a) 单个碳纳米管的PINEM时间分辨图像. 图片左上角的时间表示电子波包与飞秒脉冲到达纳米管的延迟时间, 颜色表示飞秒脉冲在纳米结构表面周围产生的场强度分布及其随时间的衰减[67]; (b) PINEM系统示意图(左)和采集的银纳米线在不同时间延迟下的电子能量损失谱(EELS)(右)[68]; (c) PINEM系统示意图及银膜表面等离激元的时间分辨能量过滤图像[69]
Fig. 8. (a) PINEM result of an individual nanotube, the time in the upper left corner of the blue figures represents the delay time of the electron wave packet reaching the nanotube, and the color reveals the field intensity distribution around the surface of the nanostructure and its decay over time[67]; (b) schematic illustration of the PINEM apparatus (left) and electron energy-loss spectroscopy (EELS) data for pulsed-electrons interacting with the plasmon near-field (right)[68]; (c) schematic diagram of the system and energy-filtered time-resolved images of the surface plasmons on the silver film[69].
图 9 (a) tr-PEEM两种泵浦-探测光路类型[74]; (b) Ag光栅上的四个局部SPP的ITR-PEEM结果. 泵浦和探测脉冲之间的延迟时间(
${\tau _{\rm{d}}}$ ) 从–0.33 fs增加到40.69 fs, 步长为0.33 fs[78]; (c)通过tr-PEEM拍摄了在光激发后, InSe/GaAs异质结构中的电子随时间的积累(红色)和耗尽(蓝色)等转移过程[79]Fig. 9. (a) Two pump-probe schematic of tr-PEEM[74]; (b) ITR-PEEM of the four localized plasmons on the silver grating framed. The delay time between the pump and probe pulses (
${\tau _{\rm{d}}}$ ) is advanced from –0.33 to 40.69 fs with an increment step of 0.33 fs[78]; (c) electron transport over time in the InSe/GaAs heterostructure showing the initial accumulation (red) and eventual recombination (blue) after photoexcitation[79].
图 10 (a) 通过飞秒LRM成像SPP波包运动的实现系统光路图[83]; (b) 延迟时间为190 fs时CMOS相机采集到的干涉图像[83]; (c) 不同时刻下(200, 230, 260 fs)实验中获得的泄露模干涉图与理论值(绿色虚线)的比较, 用于表征SPP波包运动[83]
Fig. 10. (a) Implementation of femtosecond LRM imaging SPP wave packet[83]; (b) LRM image recorded on the CMOS camera at the output of the interferometer for a time delay of 190 fs[83]; (c) SPP wave packet motion of experimental time-resolved interferograms obtained by LRM cross-cut images for the different time delays of 200, 230 and 260 fs, compared with the theoretical values (green dashed line)[83].
图 11 (a) T-CUP系统示意图. 其中黑色虚线框为条纹相机中的条纹管的详细图示[86]; (b)使用T-CUP系统得到的飞秒脉冲时间聚焦的时空演化[86]
Fig. 11. (a) Schematic of the T-CUP system, where the black dashed box is a detailed representation of the striped tube in the striped camera[86]; (b) spatiotemporal evolution of the femtosecond pulse time-focus obtained using the T-CUP system[86].
图 13 (a) 用于飞秒激光烧蚀测量的CSMUP系统[88]; (b) CSMUP在400 nm飞秒激光照射下对硅烧蚀的单脉冲不同时刻动力学成像结果[88]
Fig. 13. (a) System configuration of CSMUP for the femtosecond laser ablation measurement [88]; (b) single-shot laser ablation dynamics measurement of silicon under a 400 nm femtosecond laser exposure captured with CSMUP[88].
图 16 (a) 在1.0 J/cm2能量密度的泵浦脉冲后, 锌表面在不同延迟时间的CCD图像[96]; (b) 空气和水中的皮秒激光诱导烧蚀动力学[97]; (c) 泵浦功率为0.29 J/cm2下, 第二和第三个脉冲叠加后硅表面的超快形貌演变, 并将最终结果与原子力显微镜(AFM)进行比较[60]
Fig. 16. (a) CCD images of the Zn surface impacted by pump pulse at different delay times with energy of 1.0 J/cm2[96]; (b) picosecond laser-induced ablation in air and water[97]; (c) ultrafast topography evolution on the Si surface impacted by 2nd and 3rd pulses with energy of 0.29 J/cm2, and final results compared with AFM[60].
图 17 (a) WSe2薄片的时间分辨成像以及三个不同位点处信号强度随延迟时间变化曲线[107]; (b) 单个InAs纳米线中的热电子动力学. 在不同泵浦-探测延迟时间下拍摄的tr-PEEM图像[108]; (c) 苝四羧酸二酐分子(PTCDA)量子相干干涉的时空分辨成像[109]
Fig. 17. (a) Time-resolved imaging of WSe2 flake and Representative time traces obtained for single pixels located at three different positions[107]; (b) hot electron dynamics in a single InAs nanowire. Time-resolved PEEM images taken at different pump-probe delay time[108]; (c) space-time-resolved imaging of quantum coherent interference of PTCDA[109].
图 18 (a) 金纳米棒的瞬态近场图像中沿着棒轴的线轮廓的时间变化[112]; (b) LCP和RCP光反对称模式和对称模式的激发下的光电发射强度随时间演变图及0 fs下的PEEM扫描图像[113]; (c) tr-PEEM观测SPP携带OAM实验示意及观测结果, SPP涡旋场在约2.67 fs的单个光学周期内演化状态的快照序列图[114]; (d) ITR-PEEM对从银膜矩形沟槽发射的飞秒SPP的时空演化成像[115]; (e) 金纳米链的拓扑边态动力学过程[116]
Fig. 18. (a) Time variation of the line profiles along the rod axis in transient near-field images of nanorod[112]; (b) PEEM-measured (solid lines) and theoretically fitted (dashed lines) photoemission intensity curves against the delay time between the two pulses for LCP and RCP light, corresponding to excitation of the antisymmetric mode and symmetric mode, respectively, as indicated by the PEEM images with a delay time of 0 fs in the insets[113]; (c) schematic experimental methodology and experimental tr-PEEM snapshot sequence of the rotating field of a plasmonic vortex in the revolution stage within a single optical cycle of ~2.67 fs[114]; (d) spatial-temporal evolution imaging of the femtosecond SPP emitted from the rectangular grooves of the silver membranes by ITR-PEEM[115]; (e) topological edge state dynamic processes of gold nanocarticles[116].
图 19 超高时空分辨显微成像技术分辨率指标对比, 包括近场多脉冲显微成像技术(红色框)、远场多脉冲显微成像技术(蓝色框)以及远场单脉冲显微成像(黄色框)
Fig. 19. Resolution of the ultra-high spatiotemporal resolved imaging techniques, including the near-field multi-pulse spatiotemporal microscopic techniques (red box), the far-field multi-pulse spatiotemporal microscopic techniques (blue) and the far-field single -pulse spatiotemporal microscopic techniques (yellow box).
表 1 超高时空分辨成像技术指标及优缺点对比
Table 1. Technical indexes, advantages and disadvantages of ultra-high spatiotemporal resolution imaging.
技术手段 空间分辨率 时间分辨率 优点 缺点 近场
多脉冲超快NSOM[37] 20 nm 亚fs 可实现空间超分辨 系统复杂, 视场小, 成像速度慢 超快四波混频AFM[26] 50 nm 10 fs 可实现空间超分辨, 可以得到样品表面形貌信息 系统复杂, 视场小, 成像速度慢, 需要激发非线性效应 超快PiFM[42] 10 nm 200 fs 可实现空间超分辨, 可以得到样品表面形貌信息 系统复杂, 视场小, 成像速度慢 超快STM[46] 0.1 nm 亚fs 可实现空间超分辨, 空间分辨率最高 系统复杂, 视场小, 成像速度慢, 只适用导电样品 远场
多脉冲高NA系统[55] 接近衍射极限 fs 量级 速度快, 大视场 无法实现空间超分辨 SPPM[59] 114 nm fs量级 可实现空间超分辨 视场小, 需要多步相移, 成像速度慢 SPSLM[60] 478 nm(横向);
22 nm (纵向)256 fs 单帧成像, 大视场, 有三维成像能力 无法实现空间超分辨 PINEM[67] 小于0.7 nm 10 fs 可实现空间超分辨 电子显微镜系统复杂, 设备昂贵, 样品要求高 超快PEEM[71] 10 nm 10 fs 可实现空间超分辨 电子显微镜系统复杂, 设备昂贵, 样品要求高, 空间分辨率受材料影响 LRM[83] 接近衍射极限 10 fs 可获得SPP传播相速度和群速度信息 目前仅能对SPP成像 远场
单脉冲CUP[86] 1 μm 100 fs 帧数高, 成像速度快 压缩感知算法较复杂, 条纹相机较为昂贵 OPR[87] 11.1 μm 100 fs 重建算法简单、直接、稳定性好, 时间分辨率高 空间分辨率较低, 目前仅有微米量级 CSMUP[88] 833 nm 4 ps 较高的空间分辨率, 图像尺寸更大 时间分辨率依赖于高光谱相机光谱带, 时间分辨率较低 STAMP[89] 1 μm 227 fs 在显微和宏观成像领域都适用, 普适性强 帧数和时间分辨率存在依赖关系, 难以兼得 FINCOPA[91] 3 μm 50 fs 时空分辨率、帧数、帧间隔相互独立 空间分辨率较低 
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