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).     

双测头复合型微纳米测量仪的研制

针对当前微纳米测量中存在的大范围高精度测量及复杂微结构几何参数表征难题,基于多测头传感和精密定位平台复用技术,开发了一台具有多种测量尺度和测量模式的复合型微纳米测量仪。为使其具备大范围快速扫描测量和小范围精细测量功能,仪器集成了白光干涉和原子力显微镜两种测头,通过设计适用于两种测头集成的桥架结构及宏/微两级驱动定位平台,实现整机的开发。为保证仪器测量结果的准确性和溯源性,利用标准样板对开发完成的仪器进行了校准。仪器搭载的白光干涉测头可以达到横向500 nm,纵向1 nm的分辨力;原子力显微镜测头横向和纵向分辨力均可达到1 nm。最后,利用目标仪器对微球样品进行了测量,通过大范围成像和小范围精细扫描,获得了微球的表面特征,验证了仪器对复杂微结构的测量能力。     

The effect of deformation on the lateral resolution of atomic force microscopy

A computer model based on the elastic properties of rubber is introduced for the evaluation of the lateral resolution in atomic force microscopy of deformable specimens. The computational results show that, if the full width at half-height can be defined as the lateral resolution, it is continuously improved at greater probe forces, at the expense of a reduced molecular height. In fact, even for a probe that is bigger than the molecule, the real size of the molecule can be 'recovered' at about 25% compression. This result demonstrates that for a better lateral resolution, a greater probe force can be beneficial, provided that the molecule is not moved or damaged and the response remains elastic. Measurements on isolated low-density lipoproteins (LDL) show that with 26% vertical compression, the lateral size measured in atomic force microscopy is only about 72% of the value predicted by a simple convolution, and is only slightly larger (≈ 13%) than the known size of LDL. Therefore, the results on LDL provide a direct support for the conclusions of the computational model.     

Vacuum compatible sample positioning device for matrix assisted laser desorption∕ionization Fourier transform ion cyclotron resonance mass spectrometry imaging

The high mass accuracy and resolving power of Fourier transform ion cyclotron resonance mass spectrometers (FT-ICR MS) make them ideal mass detectors for mass spectrometry imaging (MSI), promising to provide unmatched molecular resolution capabilities. The intrinsic low tolerance of FT-ICR MS to RF interference, however, along with typically vertical positioning of the sample, and MSI acquisition speed requirements present numerous engineering challenges in creating robotics capable of achieving the spatial resolution to match. This work discusses a two-dimensional positioning stage designed to address these issues. The stage is capable of operating in ～1 × 10(-8) mbar vacuum. The range of motion is set to 100 mm × 100 mm to accommodate large samples, while the positioning accuracy is demonstrated to be less than 0.4 micron in both directions under vertical load over the entire range. This device was integrated into three different matrix assisted laser desorption∕ionization (MALDI) FT-ICR instruments and showed no detectable RF noise. The "oversampling" MALDI-MSI experiments, under which the sample is completely ablated at each position, followed by the target movement of the distance smaller than the laser beam, conducted on the custom-built 7T FT-ICR MS demonstrate the stability and positional accuracy of the stage robotics which delivers high spatial resolution mass spectral images at a fraction of the laser spot diameter.     

Ultrahigh vacuum, variable temperature, dual scanning tunneling microscope system operating under high magnetic field

We present a dual scanning tunneling microscope (DSTM) system operating between 2.2 K and room temperature, in a split-coil superconducting magnetic field up to 12 T and in ultrahigh vacuum. The DSTM consists of two compact STMs, each having x, y, and z coarse positioning piezoelectric steppers with embedded capacitive positioning sensor for navigation. Each STM can be operated independently and can achieve atomic resolution. The DSTM and the sample is configured in a way that allows the magnetic field orientation to be varied continuously from normal to parallel to the sample surface. Together with the sample, the DSTM can form a nanometer scale three terminal setup for transport measurement.     

Subject index to volume 10

The scanning transmission electron microscope with a field emission electron source operated at 100 kV allows X-ray microanalysis using electron probes as small as 1 to 2 nm. Measurements of the probe in a Vacuum Generators HB-501 STEM show that spherical aberration in the objective lens controls the probe size and shape at beam convergence half-angles of 10 mrad and greater typically used for X-ray microanalysis. A virtual objective aperture eliminates X-ray contributions from the probe-forming system, but must be aligned exactly to avoid asymmetrical broadening of the probe by spherical aberration. It is estimated that 5 nm X-ray spatial resolution can be achieved in low to medium atomic number materials. Even at this resolution however, probe broadening in the specimen controls the resolution; the main limitation is one of specimen preparation and a knowledge of the final specimen thickness. Determination of composition profiles near voids, dislocations and other individual defects in thin foils also requires a knowledge of the defect depth position and deconvolution of the probe and composition profiles.     

Development of probe-to-probe approach method for an independently controlled dual-probe scanning tunneling microscope

We developed a method of fast probe-to-probe approach for an independently controlled dual-probe scanning tunneling microscope (STM), which is essential to measure the transport property of nanostructures, without scanning electron microscopy (SEM). In the approach method, inchworm motors are used as the coarse positioning devices, which are controlled with a personal computer. The method enables an automatic approach of the probe to the other probe within a short time (typically 30 min). After the approach, a real distance between contact points of each probe tip to a sample can be measured from the overlapped part of the STM images obtained with individual probe. The approach method without SEM is also useful to measure the charge transport in the atmosphere, which will be essential for measurement of the bio molecules.     

Materials analysis with a position-sensitive atom probe

A position-sensitive detector has been combined with time-of-flight mass spectrometry in the atom probe field-ion microscope to yield a system in which both chemical identity and spatial information are obtained for individual ions field-evaporated from the specimen surface. This allows the variations in composition originally present in the sample to be reconstructed in 3-D with sub-nanometre resolution. The prototype position-sensitive atom probe is being used to study phase chemistry in a number of metallurgical alloys, including accurate composition determination of 1–2 nm Cu-rich precipitates formed in Fe–1.3% Cu–1.4%Ni aged to peak hardness. Other applications of the position-sensitive atom probe (POSAP) include the analysis of surface layers on superconductors and atom probe studies of semiconductor multiple quantum wells. These initial applications of the instrument are reported, and the limitations and intended improvements to the instrument are discussed.     

Design of a contact probe with high positioning accuracy for plasmonic lithography

Plasmonic lithography with a contact probe records nano-meter scale features and has high-throughput owing to its capability to scan in contact mode. The probe is commonly based on a micrometer-scale cantilever, which leads to the tip-positioning problem due to force-deflection that induces lateral tip displacement. We propose a geometrically modified probe to achieve high positioning accuracy. Contrary to a conventional cantilever-tip probe, we designed a "circular probe" with arc-shaped arms that hold the tip in the center. The mechanism is based on the "fixed-fixed beam" concept in material mechanics. To confirm its positioning accuracy, we used a finite element method (FEM) to calculate the tip displacement for a circular probe and compared the results with those using a conventional cantilever-tip probe. The probe was designed considering a silicon-based micro-fabrication process. The designed probe has a square outline boundary with a length of 50 μm, four arms, and a pyramidal tip with a height of 5 μm. The ratio of the lateral tip displacement to the vertical deflection was evaluated to indicate the accuracy of the probe. The probe has higher positioning accuracy by a factor of 10(3) and 10 in its approach mode and scan mode, respectively, compared with a cantilever-tip probe. We expect that the probe is suitable for the applications that require high positioning accuracy, such as nanolithography in contact mode and applications based on multiple-probe arrays.     

Dynamic adhesive force measurements under vertical and horizontal motions of interacting rough surfaces

An instrument to measure dynamic adhesive forces between interacting rough surfaces has been developed. It consists of four parts, namely, main instrument body, vertical positioning system with both micrometer and nanometer positioning accuracies, horizontal positioning system with nanometer positioning accuracy, and custom-built high-resolution, and high dynamic bandwidth capacitive force transducer. The vertical piezoelectric actuator (PZT) controls the vertical (approaching and retracting) motion of the upper specimen, while the horizontal PZT controls the horizontal (reciprocal) motion of the lower specimen. The force transducer is placed in line with the upper specimen and vertical PZT, and directly measures the adhesive forces with a root-mean-square load resolution of 1.7 microN and a dynamic bandwidth of 1.7 kHz. The newly developed instrument enables reliable measurements of near-contact and contact adhesive forces for microscale devices under different dynamic conditions. Using the developed instrument, dynamic pull-in and pull-off force measurements were performed between an aluminum-titanium-carbide sphere and a 10 nm thick carbon film disk sample. Three different levels of contact force were investigated; where for each contact force level the vertical velocity of the upper sample was varied from 0.074 to 5.922 microms, while the lower sample was stationary. It was found that slower approaching and retracting velocities result in higher pull-in and pull-off forces. The noncontact attractive force was also measured during horizontal movement of the lower sample, and it was found that the periodic movements of the lower disk sample also affect the noncontact surface interactions.     

Maximum entropy reconstruction of compositional depth profiles from electron probe microanalysis data

Electron probe microanalysis (EPMA) is a powerful method for the quantitative determination of the elemental composition of micro-regions of a sample surface. Here, we report on the development of a method of reconstructing compositional depth profiles in thin films from EPMA data measured over a range of electron beam energies, using maximum entropy data processing. The method gives quantitative information on film compositions up to approximately 1 μm in depth, with a lateral spatial resolution of approximately 1 μm. The method is tested using both simulated data and measured experimental data from well-characterized model sample structures.     

A compact CCD‐monitored atomic force microscope with optical vision and improved performances

A novel CCD‐monitored atomic force microscope (AFM) with optical vision and improved performances has been developed. Compact optical paths are specifically devised for both tip‐sample microscopic monitoring and cantilever's deflection detecting with minimized volume and optimal light‐amplifying ratio. The ingeniously designed AFM probe with such optical paths enables quick and safe tip‐sample approaching, convenient and effective tip‐sample positioning, and high quality image scanning. An image stitching method is also developed to build a wider‐range AFM image under monitoring. Experiments show that this AFM system can offer real‐time optical vision for tip‐sample monitoring with wide visual field and/or high lateral optical resolution by simply switching the objective; meanwhile, it has the elegant performances of nanometer resolution, high stability, and high scan speed. Furthermore, it is capable of conducting wider‐range image measurement while keeping nanometer resolution. Microsc. Res. Tech. 76:931–935, 2013. © 2013 Wiley Periodicals, Inc.     

Electron backscatter diffraction of grain and subgrain structures — resolution considerations

Characterization of microstructures containing small grains or low-angle grain boundaries by electron backscattered diffraction (EBSD) is limited by the spatial and angular resolution limits of the technique. It was found that the best effective spatial resolution (60 nm) for aluminium alloys in a tungsten-filament scanning electron microscope (SEM) was obtained for an intermediate probe current which provided a compromise between pattern quality and specimen interaction volume. The same specimens and EBSD equipment when used with a field-emission gun SEM showed an improvement in spatial resolution by a factor of 2–3. For characterizing low-angle boundary microstructures, the precision of determining relative orientations is a limiting factor. It was found that the orientation noise was directly related to the probe current and this was interpreted in terms of the effect of probe current on the quality of the diffraction patterns.     

A confocal beam scanning white-light microscope

We report on a confocal beam scanning microscope utilizing a continuous Xe short-arc lamp operating in the visible spectrum with unprecedented radiance. Measurements of lateral and vertical resolution will be presented and compared with those of an equivalent scanning laser microscope. Resolution of the white-light microscope is equivalent to that of the scanning laser microscope. White-light microscope images positively stand out from those of the scanning laser microscope by their lack of artefacts caused by interference.     

Modified electrical transport probe design for standard magnetometer

Making electrical transport measurements on a material is often a time consuming process that involves testing a large number of samples. It is thus inconvenient to wire up and rewire samples onto a sample probe. We therefore present a method of modifying Quantum Design's MPMS SQUID magnetometer transport probe that simplifies the process of sample mounting. One of the difficulties to overcome is the small diameter of the sample space. A small socket is designed and mounted on the probe so that various samples mounted on individual headers can be readily exchanged in the socket. We also present some test results on the topological insulator Bi(2)Te(2)Se using the modified probe.     

In situ mask designed for selective growth of InAs quantum dots in narrow regions developed for molecular beam epitaxy system

We have developed an in situ mask that enables the selective formation of molecular beam epitaxially grown layers in narrow regions. This mask can be fitted to a sample holder and removed in an ultrahigh-vacuum environment; thus, device structures can be fabricated without exposing the sample surfaces to air. Moreover, this mask enables the observation of reflection high-energy electron diffraction during growth with the mask positioned on the sample holder and provides for the formation of marker layers for ensuring alignment in the processes following the selective growth. To explore the effectiveness of the proposed in situ mask, we used it to grow quantum dot (QD) structures in narrow regions and verified the perfect selectivity of the QD growth. The grown QDs exhibited high optical quality with a photoluminescence peak at approximately 1.30 mum and a linewidth of 30 meV at room temperature. The proposed technique can be applied for the integration of microstructures into optoelectronic functional devices.     

Mass spectrometry of atmospheric aerosols--recent developments and applications. Part I: Off-line mass spectrometry techniques

Many of the significant advances in our understanding of atmospheric particles can be attributed to the application of mass spectrometry. Mass spectrometry provides high sensitivity with a fast response time to probe chemically complex particles. This review focuses on recent developments and applications in the field of mass spectrometry of atmospheric aerosols. In Part I of this two-part review, we concentrate on off-line mass spectrometry techniques, which require sample collection on filters but can provide detailed molecular speciation. In particular, off-line mass spectrometry techniques utilizing tandem mass spectrometry experiments and high resolution mass analyzers provide improved insight into secondary organic aerosol formation and heterogeneous reaction pathways through detailed structural elucidation at the molecular level.     

Calculating the effects of variations in composition on wave propagation in gases

The equations of gas dynamics in one space dimension are solved whilst considering variations in gas composition and properties. A species continuity equation is derived and coupled in a single vector equation with the three usual conservation equations; the resulting system is solved directly in conservation law form using the two-step Lax-Wendroff technique. The effects of variable gas properties and composition on wave propagation are illustrated via the shock-tube, or Riemann, problem. Significant errors are introduced, in the cases investigated, by assuming that the fluid is a perfect gas of constant composition.Flux-corrected transport (FCT) and nonupwind total variation diminishing (TVD) approaches are evaluated as a means of mitigating the spurious oscillations produced at discontinuities by the classical Lax-Wendroff scheme; these oscillations can give rise to mass fraction values from the species equation which are greater than unity or less than zero. It is found that the FCT algorithm does not suppress completely the oscillations at discontinuities and this corrupts the species transport calculations. The TVD algorithm eliminates the oscillations at shock waves and contact surfaces in the cases tested, thus maintaining the integrity of the species calculations. This is achieved at the expense of a 65% increase in computational effort over the constant gas property, constant composition case.The resolution of both the shock wave and contact surface can be improved significantly by the use of the artificial compression technique, but at an additional computational cost.     

双探针原子力显微镜视觉对准系统

传统的原子力显微镜（AFM）受针尖形状和放置方式的影响很难测量线条的宽度和两个侧壁的形状,故本文提出采用双探针对顶测量方案来消除AFM针尖形状对测量结果的影响。介绍了一种基于机器视觉的双探针原子力显微镜对准系统,该系统将两个探针接触到一起,实现了双探针在三维方向上的对准。系统采用具有亚微米级分辨率的镜头,配合高分辨率的CCD来获得探针的清晰图像,用于在水平和垂直两个方向实时监控双探针的运动情况。采用基于石英音叉式的自传感自调节的原子力探针,无需外加光学探测系统,缩小了系统体积,避免了杂散光对视觉对准系统的干扰。最后对针尖进行了亚像素边缘提取,精确地获取了探针之间的相对位置,实现了亚微米级的双探针对准（1 μm以内）。该结论由探针之间距离与幅度/相位曲线得到了验证。