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.     

The FAST module: an add-on unit for driving commercial scanning probe microscopes at video rate and beyond

We present the design and the performance of the FAST (Fast Acquisition of SPM Timeseries) module, an add-on instrument that can drive commercial scanning probe microscopes (SPM) at and beyond video rate image frequencies. In the design of this module, we adopted and integrated several technical solutions previously proposed by different groups in order to overcome the problems encountered when driving SPMs at high scanning frequencies. The fast probe motion control and signal acquisition are implemented in a way that is totally transparent to the existing control electronics, allowing the user to switch immediately and seamlessly to the fast scanning mode when imaging in the conventional slow mode. The unit provides a completely non-invasive, fast scanning upgrade to common SPM instruments that are not specifically designed for high speed scanning. To test its performance, we used this module to drive a commercial scanning tunneling microscope (STM) system in a quasi-constant height mode to frame rates of 100 Hz and above, demonstrating extremely stable and high resolution imaging capabilities. The module is extremely versatile and its application is not limited to STM setups but can, in principle, be generalized to any scanning probe instrument.     

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.     

Design of a scanning probe microscope with advanced sample treatment capabilities: An atomic force microscope combined with a miniaturized inductively coupled plasma source

We describe the design and performance of an atomic force microscope (AFM) combined with a miniaturized inductively coupled plasma source working at a radio frequency of 27.12 MHz. State-of-the-art scanning probe microscopes (SPMs) have limited in situ sample treatment capabilities. Aggressive treatments such as plasma etching or harsh treatments such as etching in aggressive liquids typically require the removal of the sample from the microscope. Consequently, time consuming procedures are required if the same sample spot has to be imaged after successive processing steps. We have developed a first prototype of a SPM which features a quasi in situ sample treatment using a modified commercial atomic force microscope. A sample holder is positioned in a special reactor chamber; the AFM tip can be retracted by several millimeters so that the chamber can be closed for a treatment procedure. Most importantly, after the treatment, the tip is moved back to the sample with a lateral drift per process step in the 20 nm regime. The performance of the prototype is characterized by consecutive plasma etching of a nanostructured polymer film.     

大气状态下SPM纳米加工系统的开发

对现有的商业化SPM进行了一些必要的改造，使其适合于扫描探针加工的要求。讨论了在DI公司多功能SPM基础上开发纳米加工系统的可能性，并提供了一套完整的信号施加，过程监测和环境控制的方法，实现了矢量式的纳米氧化加工，得取了30nm宽的氧化结构，为下一步进行纳米电子器件的构建奠定了基础。     

General three-dimensional image simulation and surface reconstruction in scanning probe microscopy using a dexel representation

The ability to image complex general three-dimensional (3D) structures, including reentrant surfaces and undercut features using scanning probe microscopy, is becoming increasing important in many small length-scale applications. This paper presents a dexel data representation and its algorithm implementation for scanning probe microscope (SPM) image simulation (morphological dilation) and surface reconstruction (erosion) on such general 3D structures. Validation using simulations, some of which are modeled upon actual atomic force microscope data, demonstrates that the dexel representation can efficiently simulate SPM imaging and reconstruct the sample surface from measured images, including those with reentrant surfaces and undercut features.     

Atomic force microscope imaging and force measurements at electrified and actively corroding interfaces: challenges and novel cell design

We report the design of an improved electrochemical cell for atomic force microscope measurements in corrosive electrochemical environments. Our design improvements are guided by experimental requirements for studying corrosive reactions such as selective dissolution, dealloying, pitting corrosion, and∕or surface and interface forces at electrified interfaces. Our aim is to examine some of the limitations of typical electrochemical scanning probe microscopy (SPM) experiments and in particular to outline precautions and cell-design elements, which must necessarily be taken into account in order to obtain reliable experimental results. In particular, we discuss electrochemical requirements for typical electrochemical SPM experiments and introduce novel design features to avoid common issues such as crevice formations; we discuss the choice of electrodes and contaminations from ions of reference electrodes. We optimize the cell geometry and introduce standard samples for electrochemical AFM experiments. We have tested the novel design by performing force-distance spectroscopy as a function of the applied electrochemical potential between a bare gold electrode surface and a SAM-coated AFM tip. Topography imaging was tested by studying the well-known dealloying process of a Cu(3)Au(111) surface up to the critical potential. Our design improvements should be equally applicable to in situ electrochemical scanning tunneling microscope cells.     

基于SPM的纳米加工技术研究进展

扫描探针显微镜(SPM)使人们不仅可以观察到物质表面的微观形貌,还可以在微纳米尺度上对样品表面进行加工,这种方法有可能成为未来微纳米器件的主要制作方法,成为推动人类科学和技术发展的新动力。主要介绍基于SPM的三种纳米加工方法:单原子操纵法、阳极氧化法和机械刻蚀法。详细阐述了各自的原理、特点及发展状况,并指出阳极氧化法是目前最有可能应用在实际生产制造中的加工方法,而机械刻蚀法则不仅可以作为纳米加工的手段,还可以应用于纳米加工机理方面的研究。     

Compact ultra-fast vertical nanopositioner for improving scanning probe microscope scan speed

The mechanical design of a high-bandwidth, short-range vertical positioning stage is described for integration with a commercial scanning probe microscope (SPM) for dual-stage actuation to significantly improve scanning performance. The vertical motion of the sample platform is driven by a stiff and compact piezo-stack actuator and guided by a novel circular flexure to minimize undesirable mechanical resonances that can limit the performance of the vertical feedback control loop. Finite element analysis is performed to study the key issues that affect performance. To relax the need for properly securing the stage to a working surface, such as a laboratory workbench, an inertial cancellation scheme is utilized. The measured dominant unloaded mechanical resonance of a prototype stage is above 150 kHz and the travel range is approximately 1.56 μm. The high-bandwidth stage is experimentally evaluated with a basic commercial SPM, and results show over 25-times improvement in the scanning performance.     

模块化扫描探针显微镜的研究

介绍一种多功能、模块化扫描探针显微镜,它综合了ＳＴＭ、ＡＦＭ、ＭＦＭ、ＦＦＭ等的功能,不仅能检测物质表面微观形貌,还能检测微小静电力、磁力、原子力和摩擦力,具有较好的灵活性和较宽的应用范围。     

Atomic force microscope (AFM) combined with the ultramicrotome: a novel device for the serial section tomography and AFM/TEM complementary structural analysis of biological and polymer samples

A new device (NTEGRA Tomo) that is based on the integration of the scanning probe microscope (SPM) (NT‐MDT NTEGRA SPM) and the Ultramicrotome (Leica UC6NT) is presented. This integration enables the direct monitoring of a block face surface immediately following each sectioning cycle of ultramicrotome sectioning procedure. Consequently, this device can be applied for a serial section tomography of the wide range of biological and polymer materials. The automation of the sectioning/scanning cycle allows one to acquire up to 10 consecutive sectioned layer images per hour. It also permits to build a 3‐D nanotomography image reconstructed from several tens of layer images within one measurement session. The thickness of the layers can be varied from 20 to 2000 nm, and can be controlled directly by its interference colour in water. Additionally, the NTEGRA Tomo with its nanometer resolution is a valid instrument narrowing and highlighting an area of special interest within volume of the sample. For embedded biological objects the ultimate resolution of SPM mostly depends on the quality of macromolecular preservation of the biomaterial during sample preparation procedure. For most polymer materials it is comparable to transmission electron microscopy (TEM). The NTEGRA Tomo can routinely collect complementary AFM and TEM images. The block face of biological or polymer sample is investigated by AFM, whereas the last ultrathin section is analyzed with TEM after a staining procedure. Using the combination of both of these ultrastructural methods for the analysis of the same particular organelle or polymer constituent leads to a breakthrough in AFM/TEM image interpretation. Finally, new complementary aspects of the object's ultrastructure can be revealed.     

开放式多功能扫描探针显微镜系统

开放式多功能扫描探针显微镜、集成扫描隧道显微镜、原子力显微镜、横向力显微镜和静电力显微镜．具有接触、半接触和非接触工作模式，可进行作用力、电流、电位、光能量等参数的高度局域综合测量,具有极高的开放性和可扩展性，支持用户进行二次开发。     

扫描探针显微镜的进展

扫描探针显微镜（SPMs）经过近30年的发展，已经应用到科学研究的各个方面。为适应不同研究的需要，扫描探针显微镜本身的发展也非常迅速。如其中原子力显微镜（AFM）从发明初期的单一的接触工作模式发展到包括可以测量粘弹性的相位模式在内的多种工作模式，同时通用型方面也高度发展，已经形成了一个庞大的高度自动化的扫描探针显微镜的家族。在这个家族中，严格环境控制的扫描探针显微镜的出现，很好的解决了各种务件下对样品的原位观察，环控化扫描探针显微镜的发展已经引起了人们的足够重视，必将成为扫描探针显微镜发展的一个重要方向。新近出现的各种显微镜集成的扫描探针显微镜系列是这个家族中的新成员，这个成员可以同时完成大范围、高分辨和精确定位等各种研究，必将在半导体制造厂的异物检查、金属和绝缘体等表面测定以及生物大分子研究等领域发挥重要作用。扫描探针显微镜的发明和发展促进了一门新兴的高科技——一纳米科学技术的诞生，宣告一个科枝新纪元，纳米科技时代已经来临。     

High-resolution scanning near-field EBIC microscopy: application to the characterisation of a shallow ion implanted p+-n silicon junction

High-resolution electron beam induced current (EBIC) analyses were carried out on a shallow ion implanted p⁺–n silicon junction in a scanning electron microscope (SEM) and a scanning probe microscope (SPM) hybrid system. With this scanning near-field EBIC microscope, a sample can be conventionally imaged by SEM, its local topography investigated by SPM and high-resolution EBIC image simultaneously obtained. It is shown that the EBIC imaging capabilities of this combined instrument allows the study of p–n junctions with a resolution of about 20 nm.     

Effect of microstructures of PVDF on surface adhesive forces

This research studies the effects of microstructures of poly vinylidene fluoride (PVDF) on its adhesion force with the probe of an atomic force microscope (AFM). The adhesion problem is currently a bottleneck for the development of micro-electro-mechanical systems (MEMS). Understanding the surface adhesion mechanisms is an important step to advance MEMS technology. In the present work, we fabricated PVDF thinfilms using spin casting and in situ corona poling methods. The microstructure was thus changed from α to the mixture of β and γ phases. Surface forces were then evaluated using an AFM. It was found that the adhesion forces between the AFM probe and the polymer surfaces were affected by microstructures. This article discusses details of our findings.     

散射式太赫兹扫描近场光学显微技术研究

基于散射式近场探测原理,设计并搭建了散射式太赫兹扫描近场光学显微系统(THz s-SNOM),实现了纳米量级空间分辨率的太赫兹近场显微成像测量。该系统以输出频率范围为0.1~0.3THz的太赫兹倍频模块为发射源,通过纳米探针的针尖产生纳米光源与样品相互作用,并将样品表面的倏逝波转化为可在远场测量的辐射波。通过探针逐点扫描样品表面,同时获得了样品表面的形貌图和太赫兹近场显微图。该系统的显微分辨率取决于探针针尖的曲率半径,而与太赫兹波的波长无关。使用该系统测量了金薄膜/硅衬底样品和石墨烯样品的近场显微图,结果表明,近场显微的空间分辨率优于60nm,波长与空间分辨率之比高达λ/26000。     

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.     

Scanning probe microscopy installed with nanotube probes and nanotube tweezers

We have developed well-controlled processes for the growth and manipulation of carbon nanotubes. The relatively thin multiwalled nanotubes were prepared with high purity by arc discharge with a high gas temperature. In the manipulation of nanotubes, the first crucial process is to prepare a nanotube array, so-called nanotube cartridge. We have found the alternated current electrophoresis of nanotubes by which nanotubes are aligned at the knife-edge of a disposal razor. The second important process is to transfer a nanotube from the nanotube cartridge onto a substrate in a scanning electron microscope. Using this method, we have developed nanotube probes and nanotube tweezers that operate in a scanning probe microscope (SPM). The nanotube probes have been applied for observation of biological samples and industrial samples to clarify their advantages. The nanotube tweezers have been demonstrated for their motion in scanning electron microscope and operated to carry a nanomaterial in a SPM.     

Design and performance of a combined secondary ion mass spectrometry-scanning probe microscopy instrument for high sensitivity and high-resolution elemental three-dimensional analysis

State-of-the-art secondary ion mass spectrometry (SIMS) instruments allow producing 3D chemical mappings with excellent sensitivity and spatial resolution. Several important artifacts however arise from the fact that SIMS 3D mapping does not take into account the surface topography of the sample. In order to correct these artifacts, we have integrated a specially developed scanning probe microscopy (SPM) system into a commercial Cameca NanoSIMS 50 instrument. This new SPM module, which was designed as a DN200CF flange-mounted bolt-on accessory, includes a new high-precision sample stage, a scanner with a range of 100 μm in x and y direction, and a dedicated SPM head which can be operated in the atomic force microscopy (AFM) and Kelvin probe force microscopy modes. Topographical information gained from AFM measurements taken before, during, and after SIMS analysis as well as the SIMS data are automatically compiled into an accurate 3D reconstruction using the software program "SARINA," which was developed for this first combined SIMS-SPM instrument. The achievable lateral resolutions are 6 nm in the SPM mode and 45 nm in the SIMS mode. Elemental 3D images obtained with our integrated SIMS-SPM instrument on Al/Cu and polystyrene/poly(methyl methacrylate) samples demonstrate the advantages of the combined SIMS-SPM approach.     

原子力显微镜发展近况及其应用

扫描隧道显微镜(简称STM)和原子力显微镜(简称AFM),它们也可统称为扫描探针显微镜(简称SPM)。原子力显微镜(AFM) 是近十几年来表面成像技术中最重要的进展之一。与扫描电子显微镜相比,它具有较高的分辨率。本文将讨论原子力显微镜的工作原理、原子力显微镜的发展概况和应用。