Helium ion microscopy of Lepidoptera scales

In this report, helium ion microscopy (HIM) is used to study the micro and nanostructures responsible for structural color in the wings of two species of Lepidotera from the Papilionidae family: Papilio ulysses (Blue Mountain Butterfly) and Parides sesostris (Emerald-patched Cattleheart). Electronic charging of uncoated scales from the wings of these butterflies, due to the incident ion beam, is successfully neutralized, leading to images displaying a large depth-of-field and a high level of surface detail, which would normally be obscured by traditional coating methods used for scanning electron microscopy (SEM). The images are compared with those from variable pressure SEM, demonstrating the superiority of HIM at high magnifications. In addition, the large depth-of-field capabilities of HIM are exploited through the creation of stereo pairs that allows the exploration of the third dimension. Furthermore, the extraction of quantitative height information which matches well with cross-sectional transmission electron microscopy measurements from the literature is demonstrated.     

Dark field photoelectron emission microscopy of micron scale few layer graphene

We demonstrate dark field imaging in photoelectron emission microscopy (PEEM) of heterogeneous few layer graphene (FLG) furnace grown on SiC(000-1). Energy-filtered, threshold PEEM is used to locate distinct zones of FLG graphene. In each region, selected by a field aperture, the k-space information is imaged using appropriate transfer optics. By selecting the photoelectron intensity at a given wave vector and using the inverse transfer optics, dark field PEEM gives a spatial distribution of the angular photoelectron emission. In the results presented here, the wave vector coordinates of the Dirac cones characteristic of commensurate rotations of FLG on SiC(000-1) are selected providing a map of the commensurate rotations across the surface. This special type of contrast is therefore a method to map the spatial distribution of the local band structure and offers a new laboratory tool for the characterisation of technically relevant, microscopically structured matter.     

Mechanical characterization of materials at small length scales

A review on the mechanical characterization of materials at small length scale is presented. The focus is on the different micro- and nanoscale testing techniques, the variety of materials investigated by the scientific and industrial communities and the mechanical quantities identified by such methodologies.     

Broadband and low insertion loss Stark cell for microwave spectroscopy

A groove guide cell for Stark modulation spectroscopy has been constructed and tested. This structure with quasi-unique mode propagation between two isolated plates is well adapted to application of a modulation voltage. The insertion losses are low (0.6 dB for a 3-m-long cell, and R band) and the cell is free of internal reflection. A metallic casing enclosing the plates acts as a shield against electrical interference, prevents low-voltage breakdown, and reduces wall adsorption of the gas. The performance of the cell is not affected by temperature variation (-80 degrees to 25 degrees C). A high sensitivity has been obtained by converting the cell into a 3-m-long, high-Q cavity. This type of cell appears to particularly recommend itself for use in intensity measurements, broadband spectroscopy, analytical studies, and high frequency range work.     

Broadband microwave spectroscopy in Corbino geometry at 3He temperatures

A broadband microwave spectrometer has been constructed to determine the complex conductivity of thin metal films at frequencies from 45 MHz to 20 GHz working in the temperature range from 0.45 K to 2 K (in a (3)He cryostat). The setup follows the Corbino approach: a vector network analyzer measures the complex reflection coefficient of a microwave signal hitting the sample as termination of a coaxial transmission line. As the calibration of the setup limits the achievable resolution, we discuss the sources of error hampering different types of calibration. Test measurements of the complex conductivity of a heavy-fermion material demonstrate the applicability of the calibration procedures.     

微波陶瓷介质谐振器优选组合检测法

微波介质陶瓷材料的介电性能主要由3个参数表示:介电常数、介质损耗和谐振频率温度系数.本文优选组合了3种检测介质谐振器方法:短路型介质谐振器轴向的短路界面测定方便准确,用于测量微波介质陶瓷材料的相对介电常数;开路型平行板与介质谐振器无直接接触,用于测量介质损耗系数;自行研制的旋转开放腔,可同时放置多个样品,加快温度系数的测量速度.3个参数采用3种不同测试法,充分应用了不同测试法各自的优势,满足微波介质陶瓷材料介电常数跨度大、介质损耗低、温度系数快速测量的需求,可得到精确、快速的测试效果.     

Single-molecule near-field optical energy transfer microscopy with dielectric tips

The fluorescence lifetime and the fluorescence rate of single molecules are recorded as a function of the position of a Si₃N₄ atomic force microscopy tip with respect to the molecule. We observe a decrease of the excited state lifetime and the fluorescence rate when the tip apex is in close proximity to the molecule. These effects are attributed to the fact that the dielectric tip converts non‐propagating near‐fields to propagating fields within the dielectric tip effectively quenching the fluorescence. The spatial extension of the quenching area is of subwavelength dimensions. The results are discussed in terms of molecular fluorescence in a system of stratified media. The experiment provides surprising new insights into the interactions between a fluorescent molecule and a dielectric tip. The methodology holds promise for applications in ultra high‐resolution near‐field optical imaging at the level of single fluorophores.     

微波消解/ICP-AES同时测定维药材中多种微量元素

目的:准确检测出所选维药中17种微量元素的含量。方法:测定出采用微波消解样品、电感耦合等离子体原子发射光谱法(ICP-AES)同时测定维药材中:铁、锌、铜、钼、镍、钴、锰、铬、硅、锡、硒等17种微量元素的含量。结果:在最佳仪器工作条件下,所得结果较理想。结论:与常规分析方法相比,该法快速简便、准确率高、精密度好,用于标准样品、实际样品的分析,结果令人满意。     

闭式谐振腔法微波介质陶瓷介电常数测量

采用一种封闭式的圆柱形微波谐振腔,实现了微波介质陶瓷材料以及其他中低损耗材料介电常数的准确测量,通过模式匹配技术实现了介质加载条件下腔内电磁场问题的精确求解,得到了腔体谐振频率与材料介电性能之间的精确关系,对各类典型介质材料的测量结果以及多家比对数据表明,相比于传统方法,该方法的测量准确度更高,可达到0.1%;测量范围更宽,不仅能准确测量高介电常数的微波介质陶瓷,也适用于低介电常数的交联聚苯乙烯、聚四氟乙烯等材料,此外由于闭式腔不存在辐射损耗,金属表面电流损耗也较小,对低损耗材料的Q值测量更加准确,损耗角测量下限达10~(-6)以下。该方法适用于介电常数εr=1~100及以上,损耗角正切tanσ=1×10~(-3)~1×10~(-6)范围内各种材料介电性能的准确测量。     

New cavity perturbation technique for microwave measurement of dielectric constant

A new cavity perturbation technique is presented for microwave measurement of dielectric constant, which uses a modified cylindrical reentrant cavity. Though suitable for only low dielectric constants, the method has the advantages, (a) sample area does not appear in the calculations, (b) only the ratio of frequency shifts due to two samples of same area and different thickness is involved, and (c) calibration of the measuring system with known dielectric is not necessary.     

Interferometric measurement of length scales at the National Bureau of Standards

The interferometric comparator for calibrating graduated length scales at the National Bureau of Standards is described. Its origins and early development are traced, and recent modernization and automation are detailed. A measurement assurance program is used to evaluate precision, accuracy and long term performance     

Antenna-based ultrahigh vacuum microwave frequency scanning tunneling microscopy system

The instrumental synthesis of high resolution scanning tunneling microscopy (STM) with the ability to measure differential capacitance with atomic scale resolution is highly desirable for fundamental metrology and for the study of novel physical characteristics. Microwave frequency radiation directed at the tip-sample junction in an STM system allows for such high-resolution differential capacitance information. This ability is particularly critical in ultrahigh vacuum environments, where the additional parameter space afforded by including a capacitance measurement would prove powerful. Here we describe the modifications made to a commercial scanning tunneling microscope to allow for broad microwave frequency alternating current scanning tunneling microscopy (ACSTM) in ultrahigh vacuum conditions using a relatively simple loop antenna and microwave difference frequency detection. The advantages of our system are twofold. First, the use of a removable antenna on a commercial STM prevents interference with other UHV processes while providing a simple method to retrofit any commercial UHV-STM with UHV-ACSTM capability. Second, mounting the microwave antenna on a translator allows for specific tuning of the system to replicate experimental conditions between samples, which is particularly critical in sensitive systems like organic thin films or single molecules where small changes in incident power can affect the results. Our innovation therefore provides a valuable approach to give nearly any commercial STM, be it an ambient or UHV system, the capability to measure atomic-scale microwave studies such as differential capacitance or even single molecule microwave response, and it ensures that experimental ACSTM conditions can be held constant between different samples.     

Noninvasive beam-wave spectrometric instrumentation for measuring dielectric constant at microwave frequencies

From the characteristics of the reflected Gaussian beam-wave for oblique incidence, measured with a spectrometer arrangement, the dielectric properties of a selectively exposed region of a dielectric slab are ascertained at microwave frequencies. For this purpose, a focused (Gaussian) microwave beam is launched from a suitable applicator to irradiate obliquely a selected protion of the test dielectric and the complex reflection coefficient is measured and analyzed. Further, the magnitude of the angular shift involved in the direction of the reflected beam is also used to calculate the dielectric constant. Application of this method to noninvasive measurements of dielectric properties of selective partial-bodies of commercial dielectrics and biological substances is discussed.     

Quality and anti-adulteration control of vegetable oils through microwave dielectric spectroscopy

Quality control of vegetable oils is becoming more stringent, and strict laws are being enforced, especially for avoiding adulteration. The public bodies that are responsible for the prevention of the adulteration of foodstuffs necessitate methods of analysis that could facilitate large-scale in situ controls. Similarly, oil producers constantly strive to speed up internal quality control. As a direct consequence, there is an increasing demand for innovative methods of analysis that could guarantee real-time in situ monitoring and provide adequate accuracy. On such bases, the present work addresses the possibility of monitoring qualitative characteristics of vegetable oils through microwave dielectric spectroscopy. To this purpose, the Cole–Cole dielectric parameters of different vegetable oils are evaluated through an innovative automatable procedure that suitably combines traditional TDR measurements, SOL calibration, frequency domain processing, TL modelling and, finally, a minimization routine. The proposed procedure is carried out first on different “pure” oils and, secondly, on some oil mixtures. The obtained results confirm that different dielectric characteristics are associated with different oils, thus confirming the considerable potential of dielectric spectroscopy for quality and anti-adulteration control purposes, especially in view of practical applications.     

Broadband method for precise microwave spectroscopy of superconducting thin films near the critical temperature

We present a high-resolution microwave spectrometer to measure the frequency- dependent complex conductivity of a superconducting thin film near the critical temperature. The instrument is based on a broadband measurement of the complex reflection coefficient, S 11, of a coaxial transmission line, which is terminated to a thin film sample with the electrodes in a Corbino disk shape. In the vicinity of the critical temperature, the standard calibration technique using three known standards fails to extract the strong frequency dependence of the complex conductivity induced by the superconducting fluctuations. This is because a small unexpected difference between the phase parts of S 11 for a short and load standards gives rise to a large error in the detailed frequency dependence of the complex conductivity near the superconducting transition. We demonstrate that a new calibration procedure using the normal-state conductivity of a sample as a load standard resolves this difficulty. The high quality performance of this spectrometer, which covers the frequency range between 0.1 and 10 GHz, the temperature range down to 10 K, and the magnetic field range up to 1 T, is illustrated by the experimental results on several thin films of both conventional and high temperature superconductors.     

Bioluminescence microscopy using a short focal‐length imaging lens

Bioluminescence from cells is so dim that bioluminescence microscopy is performed using an ultra low‐light imaging camera. Although the image sensor of such cameras has been greatly improved over time, such improvements have not been made commercially available for microscopes until now. Here, we customized the optical system of a microscope for bioluminescence imaging. As a result, bioluminescence images of cells could be captured with a conventional objective lens and colour imaging camera. As bioluminescence microscopy requires no excitation light, it lacks the photo‐toxicity associated with fluorescence imaging and permits the long‐term, nonlethal observation of living cells. Thus, bioluminescence microscopy would be a powerful tool in cellular biology that complements fluorescence microscopy.     

Broadband nanodielectric spectroscopy by means of amplitude modulation electrostatic force microscopy (AM-EFM)

In this work we present a new AFM based approach to measure the local dielectric response of polymer films at the nanoscale by means of Amplitude Modulation Electrostatic Force Microscopy (AM-EFM). The proposed experimental method is based on the measurement of the tip-sample force via the detection of the second harmonic component of the photosensor signal by means of a lock-in amplifier. This approach allows reaching unprecedented broad frequency range (2-3×10⁴ Hz) without restrictions on the sample environment. The method was tested on different poly(vinyl acetate) (PVAc) films at several temperatures. Simple analytical models for describing the electric tip-sample interaction semi-quantitatively account for the dependence of the measured local dielectric response on samples with different thicknesses and at several tip-sample distances.     

Quantitative atom probe analysis of nanostructure containing clusters and precipitates with multiple length scales

A model Al-3Cu-(0.05 Sn) (wt%) alloy containing a bimodal distribution of relatively shear-resistant θ′ precipitates and shearable GP zones is considered in this study. It has recently been shown that the addition of the GP zones to such microstructures can lead to significant increases in strength without a decrease in the uniform elongation. In this study, atom probe tomography (APT) has been used to quantitatively characterise the evolution of the GP zones and the solute distribution in the bimodal microstructure as a function of applied plastic strain. Recent nuclear magnetic resonance (NMR) analysis has clearly shown strain-induced dissolution of the GP zones, which is supported by the current APT data with additional spatial information. There is significant repartitioning of Cu from the GP zones into the solid solution during deformation. A new approach for cluster finding in APT data has been used to quantitatively characterise the evolution of the sizes and shapes of the Cu containing features in the solid solution solute as a function of applied strain.     

介质辅助微波消解和原子荧光法测定蔬菜中的铅

利用介质辅助微波消解仪对样品进行前处理,原子荧光法测定蔬菜中铅的含量,加标回收率在87.9%～101.2%之间,RSD在2.5%～4.0%。整个方法快速、高效、安全。     

Development of a compact cylindrical reaction cavity for a microwave dielectric heating system

This paper describes a compact reaction cavity for a microwave-assisted synthesis system. The microwave dielectric heating is a key technology to improve synthesizing yield, however, the large size of the microwave generation and reaction parts in an all-in-one system is a major obstacle when applying the technique to various systems, of which the installation space is limited. For this particular problem, a compact stand-alone cylindrical reaction cavity was developed in the current study. A microwave excited from a monopole probe, which is inserted into the side of the cavity, is transferred to a reaction mixture through the upper hole of the cavity. The cavity is miniaturized by filling it with an alumina ceramic dielectric. Fine-tuning of the resonance frequency becomes available by controlling the length of the inserted screw between the probe and the upper hole. The physical properties of the cavity were simulated using high frequency structural simulator (HFSS) and the produced cavity was tested using an Agilent E8357A network analyzer. The test results show that the developed cavity is able to send enough energy to various solvents.