A two-channel measuring acoustic microscope

A continuous-wave acoustic Doppler microscope designed for measuring the angular dependence of the ultrasonic reflectance from sample surfaces is described. The acoustic and electronic units of the microscope are equipped with an additional reference channel for the precise measurement of the scanning coordinate. This simplifies the instrument design and increases its robustness relative to mechanical vibrations and alterations of the immersion liquid properties. The design of a device with a 40 to 90 MHz operation frequency and algorithms for digital signal processing are considered. The results of the investigation of the acoustic reflectance function for titanium nitride films deposited on a steel surface are presented as an example.     

A pulse ultrasonic gauge for measuring velocities of surface acoustic waves

A pulse broadband gauge designed for measurements of the velocities of surface acoustic waves is described. The gauge’s output signal is formed during mechanical translation of focused ultrasonic transducers relative to a specimen under study placed in an immersion liquid. A design of the device with line-focused lensless ultrasonic transducers for the frequency range 2–25 MHz is considered. The results of measurements of test samples are presented, and the algorithms for processing the output spatial-temporal signals for determining the frequency dependences of phase velocities of acoustic waves are described. Using a carbon steel sample as an example, it is shown that the random error component in acoustic-wave velocity measurements can be estimated as ±(2–8) and ±(1–3) m/s for longitudinal and lateral scanning modes, respectively.     

A flexible microrobotic platform for handling microscale specimens of fibrous materials for microscopic studies

One of the most challenging issues faced in handling specimens for microscopy, is avoiding artefacts and structural changes in the samples caused by human errors. In addition, specimen handling is a laborious and time‐consuming task and requires skilful and experienced personnel. This paper introduces a flexible microrobotic platform for the handling of microscale specimens of fibrous materials for various microscopic studies such as scanning electron microscopy and nanotomography. The platform is capable of handling various fibres with diameters ranging from 10 to 1000 μm and lengths of 100 μm–15 mm, and mounting them on different types of specimen holders without damaging them. This tele‐operated microrobotic platform minimizes human interaction with the samples, which is one of the main sources contributory to introducing artefacts into the specimens. The platform also grants a higher throughput and an improved success rate of specimen handling, when compared to the manual processes. The operator does not need extensive experience of microscale manipulation and only a short training period is sufficient to operate the platform. The requirement of easy configurability for various samples and sample holders is typical in the research and development of materials in this field. Therefore, one of the main criteria for the design of the microrobotic platform was the ability to adapt the platform to different specimen handling methods required for microscopic studies. To demonstrate this, three experiments are carried out using the microrobotic platform. In the first experiment, individual paper fibres are mounted successfully on scanning electron microscopy specimen holders for the in situ scanning electron microscopy diagonal compression test of paper fibres. The performance of the microrobotic platform is compared with a skilled laboratory worker performing the same experiment. In the second experiment, a strand of human hair and an individual paper fibre bond are mounted on a specimen holder for nanotomography studies. In the third experiment, individual paper fibre bonds with controlled crossing and vertical angles are made using the microrobotic platform. If an industrial application requires less flexibility but a higher speed when handling one type of sample to a specific holder, then the platform can be automated in the future.     

Disposable sample holder for high temperature measurements in MPMS superconducting quantum interference device magnetometers

A sample holder for high temperature (300 K相似文献   

Stencil mask methodology for the parallelized production of microscale mechanical test samples

A new methodology to parallelize the production of micromechanical test samples from bulk materials is reported. This methodology has been developed to produce samples with typical gage dimensions on the order of 20-200 μm, and also to minimize the reliance on conventional focused ion beam fabrication methods. The fabrication technique uses standard microelectronic process methods such as photolithography and deep-reactive ion etching to create high aspect ratio patterned templates-stencil masks-from a silicon wafer. In the present work, the stencil mask pattern consists of a linear row of tensile samples, where one grip of each sample is integrally attached to the bulk substrate. Once fabricated, the stencil mask is placed on top of a pre-thinned substrate, and the pattern and substrate are co-sputtered using a broad ion beam milling system, which ultimately results in the transfer of the mask pattern into the substrate. The methodology is demonstrated using a Si stencil mask and a polycrystalline Ni foil to manufacture an array of metallic micro-tensile samples.     

RB-SiC亚表面损伤检测及其旋转超声磨削亚表面损伤特征

分别采用截面抛光法(包括以硅片作陪衬与以聚酯作陪衬两种形式)和界面黏接法检测了反应烧结碳化硅(Reaction Bonded SiC,RB-SiC)旋转超声磨削加工的亚表面损伤。为确定其中的最佳检测形式,采用表面破碎层深度、最大破碎层深度、平均裂纹深度、最大裂纹深度4个亚表面损伤评价指标对两种方法分别检测到的RB-SiC旋转超声磨削亚表面损伤进行对比分析。结果显示:截面抛光法(硅片作陪衬)检测到的4个指标值依次为3.30μm、6.59μm、8.64μm、17.44μm;截面抛光法(聚酯作陪衬)检测到的4个指标值依次为5.71μm、14.33μm、15.36μm、54.82μm;而界面黏接法检测到的4个指标值依次为9.19μm、19.45μm、13.04μm、32.20μm。试验结果表明,截面抛光法(硅片作陪衬)检测的精度更高,检测的亚表面损伤更符合实际情况。最后,基于此方法,对旋转超声磨削RB-SiC材料的亚表面损伤特征进行了总结。     

Cryofixation of plant tissues without pretreatment

Root tips from Sorghum and Dahlia were frozen without cryoprotection by dipping into nitrogen slush, rapid immersion in liquid propane and by the high-pressure method. Structural preservation of the samples was studied using freeze-fracture (FF) and freeze-substitution (FS) techniques for electron microscopy. It was found that most of the organelles were disrupted by freezing in nitrogen slush and that only the boundary beween the cytoplasm and the vacuole remained visible. If the samples were frozen by rapid immersion in liquid propane, small membraneous organelles, such as dictyosomes, were preserved in peripheral regions of the rhizodermal cells up to 10 μm below the surface of the tissue. Specimens frozen by the high-pressure freezing technique showed good ultrastructural preservation throughout the tissues up to a depth of more than 100 μm.     

The NanoBeamBalance: a passive, tensile-test device for the atomic force microscope

An add-on device is presented, which significantly expands the force measurement capabilities of the atomic force microscope (AFM). The device consists of a completely passive mechanism, which translates the vertical motion of the AFM tip in force measurements into a horizontal motion of two sample support pads. The advantage is that it is much easier to deposit microscopic samples from suspension onto flat surfaces than to attach them reliably between tip and a surface. The working-principle and the design of the device is comprehensively described and demonstrated on the example of collagen fibres with a diameter of a few μm. Well-defined tensile measurements in longitudinal direction were performed, showing that the tensile stiffness of collagen fibres from rat tail tendon decreases by a factor of 5 when rehydrated from a dried sample and slowly increases upon cross-linking with glutaraldehyde.     

Preparation of cross-sectional transmission electron microscopy samples by electron beam lithography and reactive ion etching

A cross-sectional sample preparation technique is described that relies on lithographic and dry-etching processing, thus avoiding metallographic polishing and ion milling. The method is capable of producing cross-sectional transmission electron microscopy samples with a large amount of transparent area (1 μm × 2.5 mm) which allows the examination of many patterned test sites on the same sample from the same chip of a silicon wafer. An example of the application of the technique is given for localized oxidation through a mask.     

Transmission scanning electron microscopical investigation of a gas microjet

Expansion flows from different kinds of nozzles (pipe, orifice) into the specimen chamber of a scanning electron microscope (JSM 50A, JEOL, Tokyo) were imaged by means of a transmitted electron detection device using its dark field mode of operation. The experimental videosignal distribution has been numerically transformed in order to get particle number density distributions. Absolute quantification using a thin known foil target yields reasonable particle number densities. The experimental investigation of a nonstationary gaseous microjet ejected from a circular orifice (20 μm in diameter) in the wall of a closed vessel (6 cm³ volume) provides for another estimation of the particle number density at an arbitrarily selected point on the microjet axis.     

Cryofixation of monolayer cell cultures for freeze-fracturing without chemical pre-treatments

A cryofixation method is presented which gives excellent ultrastructural preservation of monolayer cell cultures without any chemical pretreatments. Rat hepatocytes in primary culture were used in this study. The equipment needed is inexpensive and easy to manufacture. Cells are grown on a usual tissue culture support material (Thermanox plastic sheets). For cryofixation, samples are prepared essentially by a combined sandwich-cryogen-jet technique. 3 mm large discs are punched out and sandwiched with Cu- or Au-object holders of little mass; a 15 μm spacer is put in between. The viability of the cells is not impaired by the manipulations before freezing. The sandwich sample is quickly frozen by shooting a propane jet from a simple pressure chamber on to the metal object holder. The relevant parameters were optimized by parallel freeze-fracture analyses of 5% glycerol as a model system and by thermocouple measurements. Sandwich samples are then mounted in an appropriate double replication specimen table for further analysis by freeze-fracturing. It is possible to obtain a certain selectivity of the fracture plane with regard to apical, lateral or basal aspects of the cell layer. Alternatively, disc samples can be processed by chemical fixation methods (including freeze substitution to determine the freeze-fracture plane), since the support material Thermanox is insensitive to organic solvents and easy to cut. In each case the cells remain attached to their substratum throughout the whole procedure. Thus, the ultrastructural data can be directly correlated with parallel functional analyses obtained from the same cell cultures.     

A wall-free climate unit for acoustic levitators

Acoustic levitation represents the physical background of trapping a sample in a standing acoustic wave with no contact to the wave generating device. For the last three decades, sample holders based on this effect have been commonly used for contact free handling of samples coupled with a number of analytical techniques. In this study, a wall-free climate unit is presented, which allows the control of the environmental conditions of suspended samples. The insulation is based on a continuous cold/hot gas flow around the sample and thus does not require any additional isolation material. This provides a direct access to the levitated sample and circumvents any influence of the climate unit material to the running analyses.     

Anatomical analysis of turgescent and semi‐dry resurrection plants: The effect of sample preparation on the sample,resolution, and image quality of X‐ray micro‐computed tomography (μCT)

Computer tomography has been used frequently for the 3‐D visualization of plant anatomical traits but sample preparation has been widely neglected. Without any preparation smaller (i.e., up to 1 × 1 cm²) turgescent or semi‐dry plant samples (especially leaf samples) diminish the image quality of a scan due to gradual water loss and therefore constant movement. A suitable preparation for scans of turgescent and semi‐dry plant samples with a high resolution μCT (<1–5 μm) has to be very thin, heat‐resistant (up to 35°C), have a low attenuation coefficient, and should not alter the water content and structure of the sample. Several agents have been tested, but only a coating with vaseline conserved the water content of a plant sample efficiently. However, water molecules and vaseline both attenuate the X‐ray beam, which decreases the image quality of scans of turgescent or semi‐dry plant samples. Therefore, trade‐offs between the spatial resolution, sample water content, sample size, and image quality have to be considered: larger samples have to be placed further away from the X‐ray tube, which leads to a lower spatial resolution; water and preparation agents attenuate the X‐ray beam, causing low‐quality images which may be accompanied by motion artifacts compared to a scan of a dry sample, where no preparation is necessary. Microsc. Res. Tech., 2011. © 2010 Wiley‐Liss, Inc.     

Water-Jet Cavitation Shock Bulging as Novel Microforming Technique

With the continuous expansion of the application range of microelectromechanical systems,microdevice forming technology has achieved remarkable results.However,it is challenging to develop new microforming processes that are low cost,environmentally friendly,and highly flexible;the high-energy shock wave in a cavitation bubble's collapse process is used as the loading force.Herein,a new process for the microbulging of the water-jet cavitation is proposed.A series of experiments involving the water-jet cavitation shock microbulging process for TA2 titanium foil is performed on an experimental system.The microforming feasibility of the water-jet cavitation is investigated by characterizing the shape of the formed part.Subsequently,the effects of the main parameters of the water-jet cavitation on the bulging profile,forming depth,surface roughness,and bulging thickness distribution of TA2 titanium foil are revealed.The results show that the plastic deformation increases nonlinearly with the incident pressure.When the incident pressure is 20 MPa,the maximum deformation exceeds 240 μm,and the thickness thinning ratio changes within 10%.The microbulging feasibility of water-jet cavitation is verified by this phenomenon.     

Fully automated measurement setup for non-destructive characterization of thermoelectric materials near room temperature

A measurement setup is presented that allows for a complete and non-destructive material characterization of electrochemically deposited thermoelectric material. All electrical (Seebeck coefficient α, electrical conductivity σ), thermal (thermal conductivity λ), and thermoelectric (figure of merit ZT) material parameters are determined within a single measurement run. The setup is capable of characterizing individual electrochemically deposited Bi(2+x)Te(3-x) pillars of various size and thickness down to a few 10 μm, embedded in a polymer matrix with a maximum measurement area of 1 × 1 cm(2). The temperature range is limited to an application specific window near room temperature of 10?°C to 70?°C. A maximum thermal flux of 1 W∕cm(2) can be applied to the device under test (DUT) by the Peltier element driven heat source and sink. The setup has a highly symmetric design and DUTs can be mounted and dismounted within few seconds. A novel in situ recalibration method for a simple, quick and more accurate calibration of all sensors has been developed. Thermal losses within the setup are analysed and are mathematically considered for each measurement. All random and systematic errors are encountered for by a MATLAB routine, calculating all the target parameters and their uncertainties. The setup provides a measurement accuracy of ±2.34 μV∕K for α, ±810.16 S∕m for σ, ±0.13 W∕mK for λ, and ±0.0075 for ZT at a mean temperature of 42.5?°C for the specifically designed test samples with a pillar diameter of 696 μm and thickness of 134 μm, embedded in a polyethylene terephthalate polymer matrix.     

Off-normal solar optical property measurements using an integrating sphere

Shading devices attached to windows can be used to control solar gain and hence reduce building peak load and annual energy consumption. The performance of a shading device in this regard is strongly dependent on its solar optical properties. The current study discusses a unique measurement technique that was used to obtain off-normal solar optical properties of flat shading materials. The off-normal properties were needed in order to develop solar optical property models both for shading materials and shading devices. These models provide useful input to building peak load calculation and annual energy simulation tools. Special sample holders were designed and fabricated to facilitate measurements using a commercial spectrophotometer with integrating sphere attachment. A combination of theory and companion tests were used to confirm the validity of the approach.     

光学相干层析技术在光学表面间距测量中的应用

搭建了适于镜头中光学表面间距测量的实验装置,用于非接触高精度测量镜面间距.该装置以光纤型时域光学相干层析系统为基础,通过光学表面的层析成像精确测量其相对位置.对样品扫描装置进行了改进,利用高精度导轨移动光纤准直器来移动成像范围,实现对不同深度光学表面的层析成像.利用实验测量系统完成了对空气间隙样品及已装调好镜头的光学表面间距的测量,其中空气间隙样品的测量值为6.026mm,用游标卡尺得到的对比测量值为6.02mm;对镜头关键参数空气间隙的测量值为10.750mm,其设计值为(10.7±0.03)mm.实验系统误差为3.871μm,测量灵敏度为10.5μm.结果显示该方法具有非接触、高精度、高灵敏度的特点.     

Aberrations in confocal fluorescence microscopy induced by mismatches in refractive index

The effect of refractive-index mismatch, as encountered in the observation of biological specimens, on the image acquisition process in confocal fluorescence microscopy is investigated theoretically. The analysis takes the vectorial properties of light into account and is valid for high numerical apertures. Quantitative predictions on the decrease of resolution, intensity drop and shift of focus are given for practical situations. When observing with a numerical aperture of 1·3 (oil immersion) and an excitation wavelength of 514 nm the centre of the focus shifts 1·7 μm per 10 μm of axial displacement in an aqueous medium, thus yielding an image that is scaled by a factor of 1·2 in the axial direction. Furthermore, it can be expected that for a fluorescent plane 20 μm deep inside an aqueous medium the peak intensity is 40% less than for a plane which is 10 μm deep. In addition, the axial resolution is decreased by a factor of 1·4. The theory was experimentally verified for test samples with different refractive indices.     

新型石墨消解仪控制系统

样品的湿法消解是大多数有机、无机分析过程中样品处理的重要环节。传统的方法使用平板或者浴式加热消解设备,前者存在温度精度不高、温度不均匀,后者则有样品间、样品和消解设备间相互干扰等问题。本项目创造性使用预制石墨块作为导热媒质,把浴式加热和平板加热二者的优点结合在一起,解决了上述问题。同时,在仪器的研发中引入蓝牙通讯技术,实现远程及点对多的控制模式。特别适合在中大型分析实验室中应用。     

New photoacoustic cell design for studying aqueous solutions and gels

A new photoacoustic (PA) cell design, which is particularly suitable for investigations of liquids, gels, and outgassing samples is presented. The setup is based on a PA cell of only 78.5 mm(3) volume, which is sealed on the sample side with either a 163 μm thick chemical vapor deposition diamond window or a 3.91 μm thin diamond membrane. This design offers great advantages compared to traditionally used open-ended PA cells especially when investigating volatile compounds. The new PA cell design is particularly interesting in the studies of biological samples characterized by a high water content. The performance was demonstrated with mid-infrared PA measurements of glucose in aqueous solutions using a tunable quantum-cascade laser as a light source. A detection limit of 100?mg/dl (SNR = 3) has been achieved. Furthermore, the spectral changes of glucose dissolved in water caused by mutorotation have been monitored time-resolved.