A versatile multipurpose scanning probe microscope

A combined scanning probe microscope has been developed that allows simultaneous operation as a non‐contact/tapping mode atomic force microscope, a scattering near‐field optical microscope, and a scanning tunnelling microscope on conductive samples. The instrument is based on a commercial optical microscope. It operates with etched tungsten tips and exploits a tuning fork detection system for tip/sample distance control. The system has been tested on a p‐doped silicon substrate with aluminium depositions, being able to discriminate the two materials by the electrical and optical images with a lateral resolution of 130 nm.     

Scanning near-field optical microscopy of a cell membrane in liquid

The applications of scanning near‐field optical microscopy to biological specimens under physiological conditions have so far been very rare since common techniques for a probe–sample distance control are not as well suited for operation in liquid as under ambient conditions. We have shown previously that our own approach for a distance control, based on a short aperture fibre probe and a tuning fork as force sensor in a tapping mode, works well even on soft material in water. By means of an electronic self‐excitation circuit, which compensates for changes of the resonance frequency due to evaporation of liquid, the stability of the force feedback has now been further improved. We present further evidence for the excellent suitability of the tapping‐mode‐like distance control to an operation in liquid, for example, by force‐imaging of double‐stranded DNA. Moreover, we demonstrate that a nuclear envelope in liquid can be imaged with a high optical resolution of ～70 nm without affecting its structural integrity. Thereby, single nuclear pores in the nuclear envelope with a nearest neighbour distance of ～120 nm have been optically resolved for the first time.     

Non-optical bimorph-based tapping-mode force sensing method for scanning near-field optical microscopy

A non‐optical bimorph‐based tapping‐mode force sensing method for tip–sample distance control in scanning near‐field optical microscopy is developed. Tapping‐mode force sensing is accomplished by use of a suitable piezoelectric bimorph cantilever, attaching an optical fibre tip to the extremity of the cantilever free end and fixing the guiding portion of the fibre to a stationary part near the tip to decouple it from the cantilever. This method is mainly characterized by the use of a bimorph, which carries out simultaneous excitation and detection of mechanical vibration at its resonance frequency owing to piezoelectric and anti‐piezoelectric effects, resulting in simplicity, compactness, ease of implementation and lack of parasitic optical background. In conjugation with a commercially available SPM controller, tapping‐mode images of various samples, such as gratings, human breast adenocarcinoma cells, red blood cells and a close‐packed layer of 220‐nm polystyrene spheres, have been obtained. Furthermore, topographic and near‐field optical images of a layer of polystyrene spheres have also been taken simultaneously. The results suggest that the tapping‐mode set‐up described here is reliable and sensitive, and shows promise for biological applications.     

Large-area topography analysis and near-field Raman spectroscopy using bent fibre probes

We present a method for combined far‐field Raman imaging, topography analysis and near‐field spectroscopy. Surface‐enhanced Raman spectra of Rhodamine 6G (R6G) deposited on silver nanoparticles were recorded using a bent fibre aperture‐type near‐field scanning optical microscope (NSOM) operated in illumination mode. Special measures were taken to enable optical normal‐force detection for control of the tip–sample distance. Comparisons between far‐field Raman images of R6G‐covered Ag particle aggregates with topographic images recorded using atomic force microscopy (AFM) indicate saturation effects due to resonance excitation.     

石英音叉扫描探针显微镜

石英音叉是一种谐振频率稳定、品质因数高的时基器件,其音叉臂的谐振参数(谐振振幅和谐振频率)对微力极其敏感。利用石英音叉对外力的敏感性,与钨探针结合,构成一种新型的表面形貌扫描测头。该测头与xyz压电工作台结合,利用测头音叉臂谐振频率对扫描微力的敏感性,研制基于相位反馈控制的扫描探针显微镜。首先介绍石英音叉测头的构成、工作原理和特性测试,以及由该测头构建的扫描探针显微镜的结构和测试、分析。通过对测头和系统的测试结果分析,系统达到1.2 nm的垂直分辨率,并通过对一维栅的测量,给出扫描获得的试样表面微观形貌图以及相位图,证明系统的有效性。另外,由于采用大长径比的钨探针,该系统具有测量大深宽比微器件表面轮廓的能力。     

Angled long tip to tuning fork probes for atomic force microscopy in various environments

We expand the range of applications of a tuning fork probe (TFP) in frequency-modulation atomic force microscopy (FM-AFM) by attaching a long metal tip at a certain angle. By the combined flexure of the metal tip and the tuning fork prong, this TFP can change the direction of the detectable force by switching the resonance frequency, which has not been realized with conventional TFPs with short tips. The oscillatory behavior of the tip apex of the TFP is predicted by computer simulations and is experimentally confirmed with scanning electron microscope. FM-AFM operations using this TFP are performed in various environments, i.e., in ultrahigh vacuum, air, and water. FM-AFM images obtained at an atomic step of highly oriented pyrolytic graphite in air show a clear difference depending on the excitation frequency. It is also revealed that the higher order flexural modes of this TFP are advantageous for FM-AFM in water due to the reduction in the degree of hydrodynamic damping.     

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.     

Calibrating a tuning fork for use as a scanning probe microscope force sensor

Quartz tuning forks mounted with sharp tips provide an alternate method to silicon microcantilevers for probing the tip-substrate interaction in scanning probe microscopy. The high quality factor and stable resonant frequency of the tuning fork allow accurate measurements of small shifts in the resonant frequency as the tip approaches the substrate. To permit an accurate measure of surface interaction forces, the electrical and piezoelectromechanical properties of a tuning fork have been characterized using a fiber optical interferometer.     

A method for manufacturing a probe for a combined scanning tunneling and atomic-force microscope on the basis of a quartz tuning fork with a supersharp metal tip

A method for manufacturing a probe for a combined scanning tunneling and atomic-force microscope on the basis of a quartz tuning fork with a metal tip, which is equipped with an independent conductor, is described. When the probe is manufactured, the billet for a tip has the form of a rather small (in order not to change the frequency and quality factor of the quartz tuning fork) metal cone, which is glued to the end of the beam of the quartz resonator-tuning fork together with a carbon fiber as a conductor. A spark is used to form a melted ball at the vertex of the cone. The thickness of the cone near the ball is reduced to a diameter of <0.5 μm by the electrochemical technique, and the ball is then mechanically detached. The main advantage of this method is that it allows manufacturing a high-quality-factor force detector with a single super sharp and clean tip, which is made of platinum (or platinum alloys) and tungsten, with a yield of ≥80%.     

Characterization and fabrication of fully metal-coated scanning near-field optical microscopy SiO2 tips

The fabrication of silicon cantilever‐based scanning near‐field optical microscope probes with fully aluminium‐coated quartz tips was optimized to increase production yield. Different cantilever designs for dynamic‐ and contact‐mode force feedback were implemented. Light transmission through the tips was investigated experimentally in terms of the metal coating and the tip cone‐angle. We found that transmittance varies with the skin depth of the metal coating and is inverse to the cone angle, meaning that slender tips showed higher transmission. Near‐field optical images of individual fluorescing molecules showed a resolution < 100 nm. Scanning electron microscopy images of tips before and after scanning near‐field optical microscope imaging, and transmission electron microscopy analysis of tips before and after illumination, together with measurements performed with a miniaturized thermocouple showed no evidence of mechanical defect or orifice formation by thermal effects.     

Fabrication of near-field optical apertures in aluminium by a highly selective corrosion process in the evanescent field

A simple, one‐step process to fabricate high‐quality apertures for scanning near‐field optical microscope probes based on aluminium‐coated silicon nitride cantilevers is presented. A thin evanescent optical field at a glass–water interface was used to heat the aluminium at the tip apex due to light absorption. The heat induced a breakdown of the passivating oxide layer and local corrosion of the metal, which selectively exposed the front‐most part of the probe tip from the aluminium. Apertures with a protruding silicon nitride tip up to 72 nm in height were fabricated. The height of the protrusion was controlled by the extent of the evanescent field, whereas the diameter depended on the geometry of the probe substrate. The corrosion process proved to be self‐terminating, yielding highly reproducible tip heights. Near‐field optical resolution in a transmission mode of 85 nm was demonstrated.     

Atomic resolution ultrafast scanning tunneling microscope with scan rate breaking the resonant frequency of a quartz tuning fork resonator

We present an ultra-fast scanning tunneling microscope with atomic resolution at 26 kHz scan rate which surpasses the resonant frequency of the quartz tuning fork resonator used as the fast scan actuator. The main improvements employed in achieving this new record are (1) fully low voltage design (2) independent scan control and data acquisition, where the tuning fork (carrying a tip) is blindly driven to scan by a function generator with the scan voltage and tunneling current (I(T)) being measured as image data (this is unlike the traditional point-by-point move and measure method where data acquisition and scan control are switched many times).     

Apertureless near-field Raman spectroscopy

We report on the tip‐enhanced Raman spectra of C60 obtained on a custom‐built apertureless scanning near‐field optical microscope. A commercial atomic force microscope tip coated with 100 nm thickness of gold was used to enhance locally the Raman signal and permit topographic and spectral information to be acquired simultaneously. We present preliminary data which demonstrate the tip enhancement effect using C60 as a test sample.     

The height regulation of a near-field scanning optical microscope probe tip

A nonoptical detection of the optical fibre tip has been developed. By detecting the output signal from a tiny piezoelectric detector attached to the vibrating fibre tip, the distance between the fibre tip and the sample has been successfully controlled. The frequency responses of the system composed of tip, the dither and the detector have been studied. The difference between the shear-force detection and the tapping-mode detection is discussed. It is found that the shear force exerted on the tip reduces the vibration amplitude with an unvaried resonance frequency. However, in the tapping mode, the resonance frequency varies with the tip–sample distance as the force is exerted on the fibre tip only within a half period. This requires better adjustments for the tapping-mode detection.     

The height regulation of a near-field scanning optical microscope probe tip

A nonoptical detection of the optical fibre tip has been developed. By detecting the output signal from a tiny piezoelectric detector attached to the vibrating fibre tip, the distance between the fibre tip and the sample has been successfully controlled. The frequency responses of the system composed of tip, the dither and the detector have been studied. The difference between the shear-force detection and the tapping-mode detection is discussed. It is found that the shear force exerted on the tip reduces the vibration amplitude with an unvaried resonance frequency. However, in the tapping mode, the resonance frequency varies with the tip-sample distance as the force is exerted on the fibre tip only within a half period. This requires better adjustments for the tapping-mode detection.     

Plasmon-coupled tip-enhanced near-field optical microscopy

Near the cut‐off radius of a guided waveguide mode of a metal‐coated glass fibre tip it is possible to couple radiation to surface plasmons propagating on the outside surface of the metal coating. These surface plasmons converge toward the apex of the tip and interfere constructively for particular polarization states of the initial waveguide mode. Calculations show that a radially polarized waveguide mode can create a strong field enhancement localized at the apex of the tip. The highly localized enhanced field forms a nanoscale optical near‐field source.     

Near-field imaging of surface plasmon on gold nano-dots fabricated by scanning probe lithography

We obtained scanning near‐field optical microscopy images to study the excitation of surface plasmons on metallic dots fabricated using scanning probe lithography. Gold nano‐dots were fabricated by applying electric voltages to conducting probes installed in an atomic force microscope using the mechanism of field‐induced diffusion and nano‐oxidation plus Au‐coating. High spatial resolution of scanning near‐field optical microscopy revealed a ‘bifold’ pattern of surface plasmon mode on fabricated Au dots in the polarization direction of incident light. We found that scanning near‐field optical microscopy imaging combined with scanning probe lithography is able to provide a systematic study of surface plasmon excitation on nano‐metallic structures.     

Fibre-top atomic force microscope probe with optical near-field detection capabilities

We present a fibre-top probe fabricated by carving a tipped cantilever on an optical fibre, with the tip machined in correspondence of the fibre core. When approached to an optical prism illuminated under total internal reflection conditions, the tip of the cantilever detects the optical tunnelling signal, while the light coupled from the opposite end of the fibre measures the deflection of the cantilever. Our results suggest that fibre-top technology can be used for the development of a new generation of hybrid probes that can combine atomic force microscopy with scanning near field optical microscopy.     

Study of the focused laser spots generated by various polarized laser beam conditions

In this work, three‐dimensional near‐field imaging of the focused laser spot was studied theoretically and experimentally. In the theoretical simulation, we use the electromagnetic equivalent of the vectorial Kirchhoff diffraction integral to calculate the intensity distribution of the focal region, and a high depolarization is found in high numerical aperture systems (NA = 0.85). The experimental set‐up is based on a near‐field scanning optical microscope (NSOM) system. A high‐NA objective lens is used to focus incident light of various polarizations, and a tapered near‐field optical fibre probe of the NSOM system is used to determine the intensity of the focal field. The results show an asymmetric distribution of the focused intensity with the linear polarized laser beam.