Cleaning AFM colloidal probes by mechanically scrubbing with supersharp “brushes”

Contamination control of atomic force microscope (AFM) tips (including standard but supersharp imaging tips and particle/colloidal probes) is very important for reliable AFM imaging and surface/interface force measurements. Traditional cleaning methods such as plasma, UV–ozone and solvent treatments have their shortcomings. Here, we demonstrate that calibration gratings with supersharp spikes can be employed to scrub away contaminants accumulated on a colloidal sphere probe by scanning the probe against the spikes at high load at constant-force mode. The present method is superior to traditional cleaning methods in several aspects. First, accumulated lump-like organic/inorganic material can be removed; second, removal is non-destructive and highly efficient based on a “targeted removal” strategy; third, removal and probe shape/morphology study can be completed in a single step (we report, to our best knowledge, the first evidence of the wear of the colloidal sphere during force measurements); and fourth, both colloidal/particle probes and standard but supersharp AFM imaging tips can be treated.     

An integrated approach to piezoactuator positioning in high-speed atomic force microscope imaging

In this paper, an integrated approach to achieve high-speed atomic force microscope (AFM) imaging of large-size samples is proposed, which combines the enhanced inversion-based iterative control technique to drive the piezotube actuator control for lateral x-y axis positioning with the use of a dual-stage piezoactuator for vertical z-axis positioning. High-speed, large-size AFM imaging is challenging because in high-speed lateral scanning of the AFM imaging at large size, large positioning error of the AFM probe relative to the sample can be generated due to the adverse effects--the nonlinear hysteresis and the vibrational dynamics of the piezotube actuator. In addition, vertical precision positioning of the AFM probe is even more challenging (than the lateral scanning) because the desired trajectory (i.e., the sample topography profile) is unknown in general, and the probe positioning is also effected by and sensitive to the probe-sample interaction. The main contribution of this article is the development of an integrated approach that combines advanced control algorithm with an advanced hardware platform. The proposed approach is demonstrated in experiments by imaging a large-size (50 microm) calibration sample at high-speed (50 Hz scan rate).     

Non-optical tip–sample distance control method for scanning near-field optical microscopy using a piezoresistive micro cantilever

A piezoresistive micro cantilever is applied to monitor the displacement of an optical fibre probe and to control tip–sample distance. The piezoresistive cantilever was originally made for a self-sensitive atomic force microscopy (AFM) probe and has dimensions of 400 µm length, 50 µm width and 5 µm thickness with a resistive strain sensor at the bottom of the cantilever. We attach the piezoresistive cantilever tip to the upper side of a vibrating bent optical fibre probe and monitor the resistance change amplitude of the strain sensor caused by the optical fibre displacement. By using this resistance change to control the tip–sample distance, the two-cantilever system successfully provides topographic and near-field optical images of standard samples in a scanning near-field optical microscopy (SNOM)/AFM system. A resonant characteristic of the two-cantilever system is also simulated using a mechanical model, and the results of simulation correspond to the experimental results of resonance characteristics.     

基于 LSTM 的矩形纳米光栅 AFM 图像复原方法

原子力显微镜(AFM)利用探针与待测物之间的交互作用力进行成像,通过获取矩形纳米光栅计量标准器具的高分辨率成像得到相关的几何量参数并进行标定,实现从标准计量器具到工作计量器具的量值传递。在AFM扫描过程中,由于针尖的影响作用,使得扫描所获图像是探针和样品共同作用的结果,而不是样品形貌的真实描述。针对这一现象,本文提出了一种基于长短期记忆网络(LSTM)的AFM图像复原方法,该方法对通过膨胀法获得的仿真图像各扫描行进行训练,进而获得适用于矩形纳米光栅AFM图像复原模型。实验结果表明,针对线宽20 nm,高40 nm的矩形纳米光栅,经过该方法复原后光栅线宽的相对误差为7.40%,相较于传统的复原方法进一步提高了测量准确度。     

快速大面积测量用原子力显微镜扫描速度对测量结果的影响

构建了一种可快速大面积测量光栅表面微结构的原子力显微镜(AFM)系统,研究了不同扫描模式下扫描速度对测量结果的影响。分别测量了微悬臂探针在恒高模式与恒力模式下的频谱,获得了这两种模式下微悬臂探针的有效带宽。基于恒高模式与恒力模式,在不同扫描速度下分别测量了光栅微结构表面上的一条直线与一个圆周,进而分析了扫描速度对测量结果的影响。基于该AFM系统,采用恒高模式下不失真扫描速度对光栅微结构表面进行了快速、大面积三维形貌测量实验。实验结果表明:测量光栅微结构表面上直径为4.0mm的圆形区域所用时间仅为40s。当扫描速度不超过微悬臂探针有效带宽所对应的速度时,所构建的AFM系统可无失真地实现微结构表面的快速、大面积测量。     

Resonant control of an atomic force microscope micro-cantilever for active Q control

Active Q control may be used to modify the effective quality (Q) factor of an atomic force microscope (AFM) micro-cantilever when operating in tapping mode. The control system uses velocity feedback to obtain an effective cantilever Q factor to achieve optimal scan speed and image resolution for the imaging environment and sample type. Time delay of the cantilever displacement signal is the most common method of cantilever velocity estimation. Spill-over effects from unmodeled dynamics may degrade the closed loop system performance, possibly resulting in system instability, when time delay velocity estimation is used. A resonant controller is proposed in this work as an alternate method of velocity estimation. This new controller has guaranteed closed loop stability, is easy to tune, and may be fitted into existing commercial AFMs with minimal modification. Images of a calibration grating are obtained using this controller to demonstrate its effectiveness.     

原子力显微镜管式扫描器运动学建模与误差分析

针对样本扫描模式原子力显微镜,对其管式扫描器-样本-探针系统进行了运动学分析,建立了该系统的运动学模型,该模型表明:对于给定原子力显微镜扫描器,样本上与探针接触点的横向和纵向位移取决于探针尖端相对于扫描管轴心的偏置量、所加电压(或名义扫描范围)及样本厚度。据此模型,对由于弯曲运动模式所产生的两种重要误差—交叉耦合误差及扫描范围误差进行了定量分析,分析表明:扫描范围误差主要受样本厚度及名义扫描范围影响,而Z向交叉耦合误差主要受探针偏置量及名义扫描范围影响,实验验证了所建立的运动学模型和误差计算公式的正确性;另外,还提出了相应的减小误差的方法。     

Simulation-aided design and fabrication of nanoprobes for scanning probe microscopy

We proposed and demonstrated a flexible and effective method to design and fabricate scanning probes for atomic force microscopy applications. Computer simulations were adopted to evaluate design specifications and desired performance of atomic force microscope (AFM) probes; the fabrication processes were guided by feedback from simulation results. Through design-simulation-fabrication iterations, tipless cantilevers and tapping mode probes were successfully made with errors as low as 2% in designed resonant frequencies. For tapping mode probes, the probe tip apex achieved a 10 nm radius of curvature without additional sharpening steps; tilt-compensated probes were also fabricated for better scanning performance. This method provides AFM users improved probe quality and practical guidelines for customized probes, which can support the development of novel scanning probe microscopy (SPM) applications.     

Wear characteristics of diamond-coated atomic force microscope probe

In atomic force microscope (AFM) applications, the wear of the probe is undoubtedly a serious concern since it affects the integrity of the measurements. In this work, wear tests were performed using an AFM with lateral force monitoring capability with the aim to better understand the wear characteristics of diamond-coated probes. For the assessment of the probe wear, a transmission electron microscope (TEM) as well as a scanning electron microscope were utilized. The degree of the probe wear was quantified using the Archard's wear equation. The structure of the diamond-coated probe was analyzed by using the TEM and Raman spectroscopy. From the experimental results, two different wear characteristics, the gradual wear and the abrupt fracture of the diamond coating, were observed. In the case of gradual wear, the wear coefficient of the diamond-coated probe slid against a silicon nitride specimen was about 10(-5)-10(-6). It was also found that the wear rate significantly decreased with increase in the sliding distance. Raman spectroscopy analysis showed that the difference in the chemical structure of the diamond coating may induce the different wear phenomena. These results may be effectively utilized for fundamental understanding of nano-wear characteristics of AFM probes.     

Nanotribology: tip–sample wear under adhesive contact

In this report, the irreversible variation of mass of the probe tip of an atomic force microscope (AFM) is considered from theoretical and numerical points of view through statistical methods. The tip–sample interaction due to the intermittent-contact operating mode of an AFM is modelled as a double-well potential where the wear mechanism, which reveals itself as mass sticking to the probe tip, is described as a transition between the two potential wells. We evaluate the interaction of a silicon nitride AFM/FFM tip with gold in order to compare the results with those obtained from previous experimental and numerical studies.     

气/液两用型原子力显微镜及其应用研究

发展了一种气/液两用型原子力显微镜(AFM)系统,讨论了其工作原理,给出了优化的气/液两用型探头及扫描与反馈控制电路。利用该型AFM系统分别对大气环境下的硅片以及液体环境下的刀片和多孔氧化铝样品进行了扫描检测。实验结果表明,该型AFM系统在大气和液体环境中均可扫描获得理想的AFM图像,分辨力达到纳米量级,扫描范围可达4000nm×4000nm,可满足各种微纳米扫描测量的要求。     

A silanized mica substrate suitable for high-resolution fiber FISH analysis by scanning near-field optical/atomic force microscopy

We applied a novel silanized mica substrate with an extremely flat surface constructed according to Sasou et al. (Langmuir 19, 9845-9849 (2003)) to high-resolution detection of a specific gene on a DNA fiber by scanning near-field optical/atomic force microscopy (SNOM/AFM). The interaction between the substrate and fluorescence-dye conjugated peptide nucleic acid (PNA) probes, which causes fluorescence noise signal, was minimal. By using the substrate, we successfully obtained a fluorescence in situ hybridization signal from the ea47 gene on a λphage DNA labeled with an Alexa 532-conjugated 15-base PNA probe. As the results, no fluorescence noises were observed, indicating that the surface adsorbed almost none of the PNA probe. The combination of the substrate and SNOM/AFM is an effective tool for visualizing DNA sequences at nanometer-scale resolution.     

Computational models of a nano probe tip for static behaviors

It is difficult to predict the measurement bias arising from the compliance of the atomic force microscope (AFM) probe. The issue becomes particularly important in this situation where nanometer uncertainties are sought for measurements with dimensional probes composed of flexible carbon nanotubes mounted on AFM cantilevers. We have developed a finite element model for simulating the mechanical behavior of AFM cantilevers with carbon nanotubes attached. Spring constants of both the nanotube and cantilever in two directions are calculated using the finite element method with known Young's moduli of both silicon and multiwall nanotube as input data. Compliance of the nanotube-attached AFM probe tip may be calculated from the set of spring constants. This paper presents static models that together provide a basis to estimate uncertainties in linewidth measurement using nanotubes. In particular, the interaction between a multiwall nanotube tip and a silicon sample is modeled using the Lennard-Jones theory. Snap-in and snap-out of the probe tip in a scanning mode are calculated by integrating the compliance of the probe and the sample-tip interacting force model. Cantilever and probe tip deflections and points of contact are derived for both horizontal scanning of a plateau and vertically scanning of a wall. The finite element method and the Lennard-Jones model provide a means to analyze the interaction of the probe and sample and measurement uncertainty, including actual deflection and the gap between the probe tip and the measured sample surface.     

Frequency shifts and analytical solutions of an AFM curved beam

The squeeze damping coefficient between the cantilever of a straight AFM probe and the surface of a biological sample in liquids is inversely proportional to their distance to the third power. Due to the small cantilever-sample distance, the quality factor of AFM in liquid is too small and results in a low signal–noise ratio. In this study, an AFM curved beam is proposed to solve this problem. Results show that the squeeze damping is significantly decreased and thus the quality factor of an AFM curved beam is greatly increased. An effective mass-spring-damper model is presented and its analytical solution is derived. Moreover, the formulas of the resonant quality factor and frequency shift are discovered. In addition to the requirement of the low squeeze damping, high frequency shifts or sensitivities is necessary for accurate measurement. Results indicate that the effects of the arc angle and several parameters on the quality factor and the frequency shifts are significant. The optimum parameters for high quality and frequency shift are also investigated.     

Developments of scanning probe microscopy with stress/strain fields

An innovative stress/strain fields scanning probe microscopy in ultra high vacuum (UHV) environments is developed for the first time. This system includes scanning tunneling microscope (STM) and noncontact atomic force microscope (NC-AFM). Two piezo-resistive AFM cantilever probes and STM probes used in this system can move freely in XYZ directions. The nonoptical frequency shift detection of the AFM probe makes the system compact enough to be set in the UHV chambers. The samples can be bent by an anvil driven by a step motor to induce stress and strain on their surface. With a direct current (dc) power source, the sample can be observed at room and high temperatures. A long focus microscope and a monitor are used to observe the samples and the operation of STM and AFM. Silicon(111) surface in room temperature and silicon(001) surface in high temperature with stress were investigated to check the performance of the scanning probe microscope.     

A new method of Q factor optimization by introducing two nodal wedges in a tuning-fork/fiber probe distance sensor

We report on a new method of achieving and optimizing a high Q factor in a near-field scanning optical microscope (NSOM) by introducing two nodal wedges to a tuning-fork/fiber probe distance sensor and by selecting a vibrational mode of the dithering sensor. The effect of the nodal wedges on the dynamical properties of the sensor is theoretically analyzed and experimentally confirmed. The optimization achieved by the proposed method is understood from the vibration isolation and the subsequent formation of a local vibration cavity. The optimal condition is found to be less susceptible to the variation of the fiber tip length. This method allows effective NSOM measurement of samples placed even in aqueous solution.     

新型电化学原子力显微镜的研制

电化学原子力显微镜将电化学分析技术与原子力显微镜结合起来,能对生物传感器,新型电池和电腐蚀进行原位电化学扫描探针显微测量分析。为了实现电化学与扫描探针功能的系统集成,在控制电路设计中采用现场可编程门阵列,提高了系统的可靠性。电化学控制箱与原子力显微镜的头部紧密集成,保证微弱信号不受干扰,并具有多种电化学工作模式。系统具有稳定性好,重复性高,抗干扰能力强等优点。     

X轴分离式高速原子力显微镜系统设计

为了提高原子力显微镜(Atomic Force Microscope,AFM)的成像速度,本文提出了一种新的AFM结构设计方案并搭建了相应的实验系统。在该方案中,Y、Z扫描器集成于测头内驱动探针进行慢轴扫描和形貌反馈;X扫描器与测头分离,驱动样品做快轴扫描。X扫描器采用高刚性的独立一维纳米位移台,能够承载尺寸和质量较大的样品高速往复运动而不易发生共振;同时Z扫描器的载荷实现最小化,固有频率得以显著提高。为了避免测头的扫描运动引起检测光束与探针相对位置的偏差,设计了一种随动式光杠杆光路;为了便于装卸探针以及精确调整激光在探针上的反射位置,设计了基于磁力的探针固定装置和相应的光路调节方案。对所搭建的AFM系统的初步测试结果表明,该系统在采用三角波驱动和简单PID控制算法的情况下,可搭载尺寸达数厘米且质量超过10g的较大样品实现13μm×13μm范围50Hz行频的高速成像。     

猪笼草蜡质滑移区表面反粘附特性的研究

利用环境扫描电子显微镜(ESEM)和原子力显微镜(AFM)表征红瓶猪笼草蜡质滑移区表面微观形貌,并提取粗糙度的相关参数。利用AFM分别在低载荷和高载荷下对蜡质区表面同一区域进行扫描,在不同条件下的扫描形貌一致,且扫描后的探针针尖上未发现附着污染物。利用胶体探针技术在无针尖的探针悬臂上粘附15 μm SiO2小球,模拟单根刚毛与猪笼草蜡质区表面的接触,并测试蜡质区表面的粘附力和摩擦力,并与不同粗糙度的抛光纸表面做对照。考虑到表面物理化学性质对其粘附特性的重要影响,利用接触角测量仪测量蜡质区表面和同粗糙度范围抛光纸表面对水和二碘甲烷的表观接触角并利用二滴法计算其表面能。研究结果表明：蜡质滑移区表面单个蜡质晶体具有力学稳定性,不会因脱落而污染昆虫的粘附器官,污染学说不成立;表面微粗糙度能有效地减小界面间的接触面积,降低了蜡质滑移区表面的粘附力和摩擦力;蜡质滑移区超疏水特性和低表面能是降低表面粘附力和摩擦力的另一个重要因素,两者共同作用形成了猪笼草蜡质滑移区的反粘附特性。     

Modeling scanning probe microscope lateral dynamics using the probe-surface interaction signal

In this paper, a novel scanning probe microscope (SPM) modeling technique is presented. The novelty of this technique is that it exploits the SPM's probe-surface interaction measurement capabilities [e.g., the topography signal in atomic force microscopy (AFM)] to determine the SPM's lateral positioning dynamics. SPM operation speed is limited due to mechanical vibrations induced by movement of the SPM nanopositioner. In order to facilitate high-speed SPM operation, the dynamics of the SPM can be modeled and used to design feedforward and feedback controllers that reduce nanopositioner vibrations. The proposed technique seeks to develop a transfer function model of the SPM dynamics using only the SPM probe-surface interaction signal obtained while scanning a calibration sample. The technique is presented in the context of an AFM example, errors associated with the method are analyzed, and the method is experimentally verified using a commercial AFM. Experimental modeling results show that the method is capable of modeling the dynamics of SPM systems.