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。     

MEMS-based fast scanning probe microscopes

Scanning probe microscopy is a frequently used nanometer-scale surface investigation technique. Unfortunately, its applicability is limited by the relatively low image acquisition speed, typically seconds to minutes per image. Higher imaging speeds are desirable for rapid inspection of samples and for the study of a range of dynamic surface processes, such as catalysis and crystal growth. We have designed a new high-speed scanning probe microscope (SPM) based on micro-electro mechanical systems (MEMS). MEMS are small, typically micrometer size devices that can be designed to perform the scanning motion required in an SPM system. These devices can be optimized to have high resonance frequencies (up to the MHz range) and have very low mass (10⁻¹¹ kg). Therefore, MEMS can perform fast scanning motion without exciting resonances in the mechanical loop of the SPM, and hence scan the surface without causing the image distortion from which conventional piezo scanners suffer. We have designed a MEMS z-scanner which we have integrated in commercial AFM (atomic force microscope) and STM (scanning tunneling microscope) setups. We show the first successful AFM experiments.     

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。     

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.     

Atomic and magnetic force microscopy imaging of thin-film recording heads

Investigations on the use of the scanning probe microscope (SPM) in the atomic force microscopy (AFM) mode for topography imaging and the magnetic force microscopy (MFM) mode for magnetic imaging are presented for a thin-film recording head. Results showed that the SPM is suitable for imaging the surface profile of the recording head, determining the width of the pole gap region, and mapping the magnetic field patterns of the recording head excited under current bias conditions of different polarity. For the cobalt sputter-coated tips used in MFM imaging, it was found that the magnetic field patterns obtained under different polarities of the current bias to the recording head were similar. This can be explained by the nature of the thin-film MFM tip, in which the direction of the tip magnetic moment can follow the stray magnetic field of the sample as the current bias to the recording head reverses in direction.     

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.     

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.     

Microwave atomic force microscopy imaging for nanometer-scale electrical property characterization

We introduce a new type of microscopy which is capable of investigating surface topography and electrical property of conductive and dielectric materials simultaneously on a nanometer scale. The microwave atomic force microscopy is a combination of the principles of the scanning probe microscope and the microwave-measurement technique. As a result, under the noncontact AFM working conditions, we successfully generated a microwave image of a 200-nm Au film coating on a glass wafer substrate with a spatial resolution of 120 nm and a measured voltage difference of 19.2 mV between the two materials.     

A novel atomic force microscope operating in liquid for in situ investigation of electrochemical preparation of porous alumina

A novel atomic force microscope (AFM) operating in liquid is described in this article. The specially designed AFM probe involves a tip attached to a cantilever, a tip holder, and a circular Plexiglas window. When the probe dives into the fluid, a circular meniscus is established around the Plexiglas window, preventing the tip from being affected or destroyed by surface tension of the liquid. In this setup, the whole scanning probe and the sample can completely dive into fluid. Meanwhile, the probe tip scans over the sample surface when the instrument works. These advantages enable the instrument to scan comparatively large or heavy samples with a high speed. The highest scan rate is about 30 lines/s or 14 s for a 400 x 400-pixel, 3 x 3 microm image. Using the new AFM, we carry out in-situ investigation of the formation processes of porous alumina during electrochemical anodic oxidation. A lead ring and an aluminum foil serve as cathode and anode, respectively. They are entirely immersed in the bath electrolyte, which is oxalic acid solution. During anodic oxidation, the AFM images of the sample surface are successively acquired without elevating the sample out of the solution. Experiments reveal that electrochemical reactions take place soon after the power supply is switched on, and with the progression of anodization, nanostructures of porous alumina gradually occur on the aluminum substrate, finally yielding ordered arrays of nanopores. As a typical example of applications, the results of this work show that the new AFM is an ideal and powerful tool for in-situ observation and study of materials or samples in aqueous solutions.     

Combined atomic force and scanning reflection interference contrast microscopy

A sphere attached to a cantilever is used simultaneously as an atomic force microscope (AFM) tip and as a curved reflective surface for producing scanning reflection interference contrast microscope (RICM) images of fluorescent beads dried onto a glass slide. The AFM and RICM images are acquired in direct registration which enables the identification of individually excited beads in the AFM images. The addition of a sharp, electron beam-deposited tip to the sphere gives nanometer resolution AFM images without loss of optical contrast.     

Lateral force microscope calibration using a modified atomic force microscope cantilever

A proof-of-concept study is presented for a prototype atomic force microscope (AFM) cantilever and associated calibration procedure that provide a path for quantitative friction measurement using a lateral force microscope (LFM). The calibration procedure is based on the method proposed by Feiler et al. [Rev. Sci. Instrum. 71, 2746 (2000)] but allows for calibration and friction measurements to be carried out in situ and with greater precision. The modified AFM cantilever is equipped with lateral lever arms that facilitate the application of normal and lateral forces, comparable to those acting in a typical LFM friction experiment. The technique allows the user to select acceptable precision via a potentially unlimited number of calibration measurements across the full working range of the LFM photodetector. A microfabricated version of the cantilever would be compatible with typical commercial AFM instrumentation and allow for common AFM techniques such as topography imaging and other surface force measurements to be performed.     

卧式原子力显微镜的研制

提出原子力显微镜 (AFM)的新设计 ,讨论卧式 AFM的工作原理及其性能特点 ,简要介绍 AFM的控制电路系统及其图像扫描和图像处理软件系统 ,给出 AFM扫描获得的部分样品的图像结果。     

原子力显微镜在聚合物研究中的应用

原子力显微镜以其分辨率高、样品无需特殊制备、实验可在大气环境中进行等优点而广泛应用于聚合物研究之中,弥补扫描隧道显微镜不能观测非导电样品的缺憾。近年来,其应用已由对聚合物表面几何形貌的观测发展到纳米级结构和表面性能的研究领域。在介绍原子力显微镜工作原理的基础上,简要回顾其在聚合物研究方面的若干新应用,并对其应用前景作展望。     

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。     

Application of evanescent wave optics to the determination of absolute distance in surface force measurements using the atomic force microscope

A combined scanning near field optical/atomic force microscope (AFM) is used to obtain surface force measurements between a near field sensing tip and a tapered optical fibre surface, whilst simultaneously detecting the intensity of the evanescent field emanating from the fibre. The tapered optical fibre acts as a compliant sample to demonstrate the possible use of the near field intensity measurement system in determining 'real' surface separations from normal AFM surface force measurements at sub-nanometer resolution between deformable surfaces.     

Atomic force microscopy of human hair

The atomic force microscope (AFM) was used to investigate the surface architecture of the entire lengths of cleaned human head hairs. Many features previously seen with the scanning electron microscope (SEM) were identified. However, the AFM has provided much greater detail and, in particular, the hair's cuticular surfaces appear not to be as smooth as had been previously supposed. A consistent feature was of step discontinuities or "ghosts" on the scale surfaces. These delineated the original location of each overlying scale before its edge had been chipped away. There was a change in the longitudinal angular presentation of the surfaces about each ghost. This means the distal ends of each cuticle cell have been synthesised in the follicle to be thicker than where that same cuticle cell is bounded on both sides by other cuticle cells. The undamaged outer cuticular surfaces at the root end of each hair were covered everywhere by longitudinal ridges (striations). Where the hair surface was worn, the striations terminated at a scale edge ghost. The ridges were approximately 9 nm high and were in parallel array with a lateral repeat spacing of about 350 nm. The striations are evidently formed on the outer surface of each cuticle cell following earlier contact in the hair follicle with the inner root sheath. The study of stained transverse sections of hairs in the transmission electron microscope (TEM) is suggested as a means for throwing some light on the underlying structure and chemistry of the striations. Finally, our AFM studies have revealed that the surface of the freshly emergent hair gradually changes over a distance of about 20 mm and that the surface of the hair for most of its length is quite different from that near the root. This is likely to be of import to those engaged in the hair toiletries industry.     

Comment on "Print your atomic force microscope" [Rev. Sci. Instrum. 78, 075105 (2007)

The paper of Kühner et al. [Rev. Sci. Instrum. 78, 075105 (2007)], presents a sound realization of a very nice idea. Namely, to design and prepare (via rapid prototyping) a custom head for atomic force microscope (AFM). Custom AFM heads are essential for various applications, which include the AFM force spectroscopy modes and convenient AFM coupling with other techniques. Our comment concerns the deflection data for a thermally driven AFM cantilever obtained by Kühner et al. using their AFM setup (Figure 3 therein). The results of Kühner et al. imply that a thermally excited AFM cantilever vibrates with aberrantly large amplitudes. Namely, the deflection noise amplitudes for the MLCT-D cantilever are 60-100 times larger than what is typically observed in our lab and by others. As we argue, the author's mistake is likely attributed to an improper usage of the AFM bandwidth. We explain the necessary correction and discuss the issue of bandwidth for the AFM force spectroscopy measurements.     

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。     

WiFi‐controlled portable atomic force microscope

This article proposes to develop a WiFi‐controlled portable atomic force microscope (AFM). The AFM consists of a horizontal probe, controlling circuits, digital to analog (D/A) and analog to digital (A/D) interfaces, a microcomputer (Raspberry Pi, RPi), and a laptop. The proposed AFM uses a pocket‐size power supply to drive the controlling circuits, the D/A and A/D interfaces, as well as the RPi that constructs network hotspots and generates scanning signals. With special design and integration of the whole system, both of the AFM probe and electronic controlling system are portable. At a distance of 50 m from the proposed AFM, experiments in the constant height mode and the constant force mode are conducted to evaluate its performance. The results show that this WiFi‐controlled AFM has a maximum scan range of 3.6 × 3.6 μm² with nanometer order resolution. Meanwhile, it achieves satisfactory image contrast, stability, and repeatability. Compared with conventional AFMs, the AFM proposed in this paper no longer relies on commercial AC mains supply or high‐voltage DC power supply, and realizes WiFi‐controlled AFM scanning and imaging in 50 m or farther without wire or network cable connection to a laptop or a desktop computer. Given credits to these features, WiFi‐controlled AFMs are expected to own a wider range of application, especially in isolated environments, outdoor researches, or even fieldwork investigations.