A small scanning tunnelling microscope with large scan range for biological studies

We have developed a scanning tunnelling microscope specially designed for biological applications presenting some new features: the scanner tube is mounted parallel to the surface of the sample which enables a high resolution optical microscope to be brought close to the sample when working in air or liquids. The maximum scan range is 5×20 μm with a vertical range of 20 μm and the total size of the system does not exceed 10×40 mm. The piezo-sensitivity of the scanner tube versus applied voltage was analysed by interferometry measurements and by using scanning tunnelling microscopes. We found a value for the piezoelectric constant d₁₃ of ?1·71 Å/V at low voltages (under a few volts) going up to ?2 Å/V for higher voltages. Large-scale images of a carbon grid showed a surprisingly good linearity of the scanner tube.     

A Compact 3D-nanopositioner of a scanning tunneling microscope operating at temperatures of 4.2–300.0 K

A simple compact device for three-coordinate positioning of the tip of a scanning tunneling microscope, which is intended for operation in ultrahigh vacuum and a temperature range from room to helium (4.2 K) temperature. The nanopositioner contains two independent stepping piezoelectric motors. One of them is intended for bringing the tip to a sample (the Z axis) and the other, for positioning the tip in the sample plane (X, Y). The positioning accuracies at T = 4.2 K along the Z axis and in the plane of the sample (X, Y) are up to 10 and 40 nm, respectively. The maximum amplitudes of control pulses are ±250 and 140 V for the Z piezoelectric motor and the (X, Y) positioner, respectively (at 4.2 K). The device is manufactured from nonmagnetic materials and allows heating to 150°C for operation in ultrahigh vacuum.     

An alternative flat scanner and micropositioning method for scanning probe microscope

An alternative flat scanner used for combining a scanning probe microscope with an inverted optical microscope is presented. The scanner has a novel structure basically consisting of eight identical piezoelectric tubes, metal flexure beams, and one sample mount. Because of the specially designed structure, the scanner is able to carry a sample of more than 120 g during imaging. By applying voltages of ±150 V, scanning range of more than 30 μm in three dimensions can be achieved. To improve the reliability of the stick-slip motion, a new method for sample micropositioning is proposed by applying a pulsed voltage to the piezotubes to produce a motion in the z-axis. Reliable translation of the sample has been thus accomplished with the step length from ～700 nm to 9 μm over a range of several millimeters. A homemade scanning probe microscope-inverted optical microscope system based on the scanner is described. Experimental results obtained with the system are shown.     

Experimental Results for a Heat-Sink Mechanical Seal

This work presents experimental results for a heat-sink mechanical seal installed in a 1 × 1.5 × 6 in. ANSI centrifugal water pump. The heat-sink seal is constructed of a stainless steel substrate with an electrodeposited pin fin micro-heat sink located within 3 mm of the end face. Each pin has a ten-sided polygon cross section with a flat-to-flat diameter of 675 μm, a height of 856 μm, and a 300-μm edge-to-edge spacing. The end face is coated with a WC thin film that forms the wear surface for the rotating ring. The heat-sink seal's effectiveness is demonstrated in a significant reduction of both the seal interface and seal chamber temperature when compared to a similar industry standard seal. The heat-sink seal removes 750 W of heat and reduces the stationary ring temperature by 80°C under dead-head conditions using only 1.6 W of coolant pumping power.     

A confocal laser microscope scanner for digital recording of optical serial sections

A confocal laser microscope scanner developed at our institute is described. Since an ordinary microscope is used, it is easy to view the specimen prior to scanning. Confocal imaging is obtained by laser spot illumination, and by focusing the reflected or fluorescent light from the specimen onto a pinhole aperture in front of the detector (a photomultiplier tube). Two rotating mirrors are used to scan the laser beam in a raster pattern. The scanner is controlled by a microprocessor which coordinates scanning, data display, and data transfer to a host computer equipped with an array processor. Digital images with up to 1024 × 1024 pixels and 256 grey levels can be recorded. The optical sectioning property of confocal scanning is used to record thin (～ 1 μm) sections of a specimen without the need for mechanical sectioning. By using computer-control to adjust the focus of the microscope, a stack of consecutive sections can be automatically recorded. A computer is then used to display the 3-D structure of the specimen. It is also possible to obtain quantitative information, both geometric and photometric. In addition to confocal laser scanning, it is easy to perform non-confocal laser scanning, or to use conventional microscopic illumination techniques for (non-confocal) scanning. The design has proved reliable and stable, requiring very few adjustments and realignments. Results obtained with this scanner are reported, and some limitations of the technique are discussed.     

A fully automated, ‘thimble-size’ scanning tunnelling microscope

A novel, fully automated high-stability, high-eigenfrequency scanning tunnelling microscope (STM) has been developed. Its key design feature is the application of two piezoelectric ceramic tubes, one for the x-y-z motion of the tip and one for a linear motor (‘nano-worm’) used for the coarse positioning of the tip relative to the specimen. By means of the nano-worm, the tip can be advanced in steps between 16 and 0·2 nm. The walking distance is >2 mm, with a maximum speed of 2000 steps/s. The nano-worm positioning implies that this STM is fully controlled by electronic means, and that no mechanical coupling is needed, which makes operation of the STM extremely convenient. The axial-symmetry construction is rigid, small and temperature-compensated, yielding reduced sensitivity to mechanical and acoustic vibrations and temperature variations. The sample is simply placed on a piece of invar which surrounds the scanner tube and the nano-worm and is held by gravity alone. This allows for easy sample mounting. The performance of the microscope has been tested in air by imaging a variety of surfaces, including graphite and biological samples.     

Highly controllable fabrication of fiber probe for photon scanning tunneling microscope

A selective chemical etching was used to fabricate fiber probes for the photon scanning tunneling microscope (PSTM). The cladding diameter of the fiber probe was controlled by varying the first-step etching time. The cone angle of the fiber probe tip was controlled by varying the doping ratio of the fiber and the composition of the etching solution. A cladding diameter of 8 μm and a tip diameter of about 3 nm were fabricated. The smallest cone angle was 14°.     

Highly controllable fabrication of fiber probe for photon scanning tunneling microscope

A selective chemical etching was used to fabricate fiber probes for the photon scanning tunneling microscope (PSTM). The cladding diameter of the fiber probe was controlled by varying the first-step etching time. The cone angle of the fiber probe tip was controlled by varying the doping ratio of the fiber and the composition of the etching solution. A cladding diameter of 8 μm and a tip diameter of about 3 nm were fabricated. The smallest cone angle was 14°.     

A hot stage SEM for gas-solid reaction studies

An ultra-high vacuum, field emission source, scanning electron microscope (SEM) equipped with a gas cell to permit the in situ study of high temperature gas-solid reactions is described. High resolution SEM (50 Å) and scanning Auger microscopy (300 Å resolution) can be carried out at specimen temperatures up to 1000°C. Reaction products and processes can be imaged continuously in the SEM at pressures up to ～0.2 Torr. Gas pressures up to 50 Torr are possible but with some limitations. Methods of specimen mounting, problems of temperature measurement, and the microscope performance at high specimen temperatures and gas pressures are discussed. Examples of metal surface preparation and impurity segregation under high temperature annealing and gas exposure are reported.     

Micromorphology analysis of TiO2 thin films by atomic force microscopy images: The influence of postannealing

This work describes an analysis of titanium dioxide (TiO₂) thin films prepared on silicon substrates by direct current (DC) planar magnetron sputtering system in O₂/Ar atmosphere in correlation with three‐dimensional (3D) surface characterization using atomic force microscopy (AFM). The samples were grown at temperatures 200, 300, and 400°C on silicon substrate using the same deposition time (30 min) and were distributed into four groups: Group I (as‐deposited samples), Group II (samples annealed at 200°C), Group III (samples annealed at 300°C), and Group IV (samples annealed at 400°C). AFM images with a size of 0.95 μm × 0.95 μm were recorded with a scanning resolution of 256 × 256 pixels. Stereometric analysis was carried out on the basis of AFM data, and the surface topography was described according to ISO 25178‐2:2012 and American Society of Mechanical Engineers (ASME) B46.1‐2009 standards. The maximum and minimum root mean square roughnesses were observed in surfaces of Group II (Sq = 7.96 ± 0.1 nm) and Group IV (Sq = 3.87 ± 0.1 nm), respectively.     

An ultrahigh vacuum fast-scanning and variable temperature scanning tunneling microscope for large scale imaging

We describe the design and performance of a fast-scanning, variable temperature scanning tunneling microscope (STM) operating from 80 to 700 K in ultrahigh vacuum (UHV), which routinely achieves large scale atomically resolved imaging of compact metallic surfaces. An efficient in-vacuum vibration isolation and cryogenic system allows for no external vibration isolation of the UHV chamber. The design of the sample holder and STM head permits imaging of the same nanometer-size area of the sample before and after sample preparation outside the STM base. Refractory metal samples are frequently annealed up to 2000 K and their cooldown time from room temperature to 80 K is 15 min. The vertical resolution of the instrument was found to be about 2 pm at room temperature. The coarse motor design allows both translation and rotation of the scanner tube. The total scanning area is about 8 x 8 microm(2). The sample temperature can be adjusted by a few tens of degrees while scanning over the same sample area.     

扫描式氙灯太阳模拟器十维扫描系统

为了模拟卫星在轨全年的太阳辐照情况,检验、优化整星的杂散光抑制能力,分析了光学载荷的在轨成像条件,设计了一种基于7维扫描镜+2维折反镜+1维被测样件共计10维运动机构的扫描式氙灯太阳模拟器,并建立了它们关于照明姿态和位置的控制方程,完成了被测样件的空间环境模拟照明。实验表明,对1 700mm×2 700mm的被测样件可实现方位角为-90°~+90°、俯仰角为-29°~+42.5°的模拟照明,角精度分别可达0.2°和0.1°,位置精度优于10mm。该扫描式太阳模拟器可较精确地为部分卫星提供全年太阳照明空间环境模拟实验。     

High-resolution force microscopy of in-plane magnetization

We have shown for the first time, in previous studies, that the force microscope fitted with a magnetic tip could be used to image magnetic domains in TbFe thin films. In this report we show that the information provided by the magnetic force microscope can also include a measurement of the component of magnetization in the sample which is parallel to the surface. Measurements were taken with a magnetized tip tilted at 45° with respect to the surface normal. In a first experiment, we imaged 1 μm diameter domains thermomagnetically written in a TbFe thin film. In a second measurement, we imaged a series of alternating domains in a thin film Co-alloy disc which was decorated with small magnetized particles, allowing unambiguous identification of the domain boundaries. In both cases we interpret the asymmetric portion of the images to the in-plane component of the sample magnetization.     

Low-temperature scanning tunnelling microscopy and spectroscopy on Pb and Au

We have designed and built a scanning tunnelling microscope (STM) in order to work at temperatures ranging from 1·2 to 300 K. Tunnelling spectroscopy has been performed in Au and Pb with this STM. Our results on Au show different conductance-voltage behaviours, their relation with the cleaning state of the tip being discussed. For Pb, the fitting of our I-V characteristics to a BCS density of states gives A = 1·25 meV for the superconducting energy gap at about 5 K.     

A three-axes-compensated inductive magnetometer for measurements in high pulsed magnetic fields

A high-sensititity magnetometer intended for studying the magnetic properties of materials in pulsed magnetic fields of up to 43 T is described. A distinctive feature of the magnetometer is its method for compensating pickups generated in the magnetometer sensing element by a pulsed field. The commonly used uniaxial high-order compensation is replaced by a triaxial compensation of the lowest (quadrupole) order, combined with a transverse arrangement of the main probe coils. This method has allowed us to achieve a compensation level of the signal in the working coil (with an inner diameter of 1.4 or 1.75 mm) of the magnetometer without a sample of up to 10⁻⁶ for the longitudinal and 10⁻⁴ for the transverse field components. The magnetic moment sensitivity of the magnetometer is 10⁻⁴ mA·m² in fields below 10 T and 10⁻³ mA·m² at a field pulse amplitude of 35 T. A deviation of the compensation is below 2×10⁻⁴ for a temperature increase from 77 to 300 K and below 5×10⁻⁵ after sample replacement. The sample temperature is controlled by a fast-acting temperature control system in a range of 6–300 K to an accuracy of 0.3–0.05 K.     

Note: long range and accurate measurement of deep trench microstructures by a specialized scanning tunneling microscope

A compact but practical scanning tunneling microscope (STM) with high aspect ratio and high depth capability has been specially developed. Long range scanning mechanism with tilt-adjustment stage is adopted for the purpose of adjusting the probe-sample relative angle to compensate the non-parallel effects. A periodical trench microstructure with a pitch of 10 μm has been successfully imaged with a long scanning range up to 2.0 mm. More innovatively, a deep trench with depth and step height of 23.0 μm has also been successfully measured, and slope angle of the sidewall can approximately achieve 67°. The probe can continuously climb the high step and exploring the trench bottom without tip crashing. The new STM could perform long range measurement for the deep trench and high step surfaces without image distortion. It enables accurate measurement and quality control of periodical trench microstructures.     

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。     

The preparation,examination and analysis of frozen hydrated tissue sections by scanning transmission electron microscopy and X-ray microanalysis

A method is reported for preparing, examining and analysing frozen hydrated tissue sections using transmission electron microscopy and X-ray microanalysis. Use of this method permits localization and measurement of water soluble or diffusible elements within the hydrated cell matrix. Since any change in total fresh weight of the specimen will affect the concentration of all components, great care has been taken to demonstrate that the mass neither increases nor decreases and to ensure that the tissue remains frozen-hydrated. Criteria for assessing whether or not the tissue remains frozen-hydrated are reported. After quench freezing, 1–2 μm thick sections of mouse liver were cut at 193°K and picked up on a specially designed annular specimen holder covered with an aluminium coated nylon film. Using a transfer device which prevents contamination of the tissue sections while maintaining them at a low temperature (below 143°K), the sections are transferred either to the vacuum evaporator cold stage or the scanning microscope cold stage. The tissue sections may be coated with an aluminium layer to improve electrical and thermal conductivity. The specimens are examined in the scanning transmission imaging mode and analysed using an energy dispersive X-ray analyser. Concentration of intra-nuclear and intracytoplasmic K, P, S and Cl are reported for mouse hepatocytes as ratios of the characteristic radiation to the continuum radiation used as a measure of mass. Ratios for all four elements were higher in the nucleus than the cytoplasm. Examples are given of this method as applied to plant and insect tissue.     

A new confocal scanning beam laser MACROscope using a telecentric,f-theta laser scan lens

A new confocal scanning beam system (MACROscope) that images very large-area specimens is described. The MACROscope uses a telecentric, f-theta laser scan lens as an objective lens to image specimens as large as 7·5 cm × 7·5 cm in 5 s. The lateral resolution of the MACROscope is 5 μm and the axial resolution is 200 μm. When combined with a confocal microscope, a new hybrid imaging system is produced that uses the advantages of small-area, high-speed, high-resolution microscopy (0·2 μm lateral and 0·4 μm axial resolution) with the large-area, high-speed, good-resolution imaging of the MACROscope. The advantages of the microscope/MACROscope are illustrated in applications which include reflected-light confocal images of biological specimens, DNA sequencing gels, latent fingerprints and photoluminescence imaging of porous silicon.