Design Of Sample Holder Research Articles

Characterization of Ultrathin Conductive Films Using a Simplified Approach for Terahertz Time-Domain Spectroscopic Ellipsometry

We present two ideas to simplify the measurement and analysis of terahertz time-domain spectroscopic ellipsometry data of ultrathin films. The measurement is simplified by using a specially designed sample holder with mirrors, which can be mounted on a cryostat. It allows us to perform spectroscopic ellipsometry by simply inserting the holder into a conventional terahertz spectroscopy system for measurements in transmission geometry. The analysis of the obtained data is simplified by considering a single interface with a certain sheet conductivity σs\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${\\sigma }_{s}$$\\end{document} (since the film thickness is significantly smaller than the wavelength of the terahertz light). We demonstrate the application of these ideas by evaluating the sheet conductivities of two perovskite rare-earth nickelate thin films in the temperature range 78–478 K. The use of this particular analytical method and the sample holder design will help to establish terahertz time-domain spectroscopic ellipsometry as a characterization technique for ultrathin films.

High Current Measurement of Commercial REBCO Tapes in Liquid Helium: Experimental Challenges and Solutions

Recent advances in high-temperature superconductors (HTS) have made them extremely attractive for low-temperature, high-magnetic-field-power applications such as in fusion technology, where the advantages over traditional low-temperature superconductors (LTS) allow for the design of fusion reactors operating in different and more convenient regimes. However, the performance enhancement exhibited by novel conductors poses several challenges for the measurement of their superconducting properties. The high critical currents coupled with the relatively low thermal stability of the conductors and their mechanical fragility render this task a challenge, as the angular anisotropies complicate the experimental setup. In this work, we describe the development of our novel high-current measurement facility, focusing on the solutions introduced regarding critical aspects such as the superconducting leads and the sample holder design. We show how simple but effectively designed solutions can be adopted to combat the complexity of the measurement. The results reported in this work guide the development of a measurement system able to withstand high critical currents (I > 1500 A) at high magnetic fields (µ0H > 12 T) by evaluating the angular response of 4 mm wide short samples (L ~ 7.5 cm) in a robust and reproducible manner.

Correlative Light and Electron Microscopy (CLEM): A Multifaceted Tool for the Study of Geological Specimens

Correlative light and electron microscopy (CLEM) is an advanced imaging approach that faces critical challenges in the analysis of both materials and biological specimens. CLEM integrates the strengths of both light and electron microscopy, in a hardware and software correlative environment, to produce a composite image that combines the high resolution of the electron microscope with the large field of view of the light microscope. It enables a more comprehensive understanding of a sample’s microstructure, texture, morphology, and elemental distribution, thereby facilitating the interpretation of its properties and characteristics. CLEM has diverse applications in the geoscience field, including mineralogy, petrography, and geochemistry. Despite its many advantages, CLEM has some limitations that need to be considered. One of its major limitations is the complexity of the imaging process. CLEM requires specialized equipment and expertise, and it can be challenging to obtain high-quality images that are suitable for analysis. In this study, we present a CLEM workflow based on an innovative sample holder design specially dedicated to the examination of thin sections and three-dimensional samples, with a particular emphasis on geosciences.

A precision dimple grinder-polisher produced by 3D printing

A precision dimple grinder-polisher has been designed and constructed using 3D printing. The purpose of the device is to produce a thin central area in 3 mm round samples for transmission electron microscopy before ion milling to electron transparency. The device can be self-made by any laboratory with a 3D printer for scientific research or teaching, and when combined with recycling and use of biodegradable filaments it can help labs reach their sustainable development goals. A novel sample holder design allows sample alignment without a monocular and thickness detection by light transmission. Novel solutions are developed for aligning the grinding disc and sample rotation motors and for fixing the polishing cloth to the polishing disc. The diameter-depth relationship is investigated for steel and plastic grinding discs. Design principles and materials are discussed, and the tool is evaluated by preparing samples from copper, silicon and tungsten, which are then examined in the transmission electron microscope to evaluate their quality.

A new methodology to efficiently test pitting corrosion: design of a 3D-printed sample holder to avoid the occurrence of crevice corrosion in chemically aggressive media

A new methodology to efficiently test pitting corrosion: design of a 3D-printed sample holder to avoid the occurrence of crevice corrosion in chemically aggressive media

Improved quantitation of SIMS depth profile measurements of niobium via sample holder design improvements and characterization of grain orientation effects

The importance of SIMS analyses for “N-doped” impurity alloyed niobium and other surface-alloyed materials continues to increase. A major hurdle is the uncertainty of instrument calibration due to changes in sample height either from sample surface topography or from the sample holder itself. The CAMECA sample holder design allows for many types of samples to be analyzed. However, a drawback is that the holder faceplate can bend, contributing an uncertainty in the relative sensitivity factor (RSF) used to quantify the SIMS results. Here, we describe an improved sample holder having a reinforced faceplate, which prevents deflection and reduces uncertainty. Simulations show that the new design significantly reduces deflection from 10 μm to 5 nm. Sample measurements show a reduction of RSF uncertainty from this source from 4.1% to 0.95%. Grain orientation has long been suspected to affect RSF measurement as well. A bicrystal implant standard, consisting of randomly oriented and [001] grains, was successively rotated 15° between analyses. It was observed that 20% of the analyses performed on the randomly oriented grain exhibited anomalously high RSF values as well as slow sputter rates. These features were associated with the changing grain normal orientation with respect to the primary Cs+ beam. The grain orientation associated with the rise in RSF was simulated and determined to be the [101] crystallographic plane, thus indicating that ion channeling was responsible for the significantly increased RSF. Focused ion beam analysis confirmed slower sputter rates for the cardinal crystallographic orientations, indicating that ion channeling occurred for each.

Sample Holders for Sub-THz Electron Spin Resonance Spectroscopy

Electron spin resonance (ESR) is a powerful spectroscopic technique used to investigate samples with unpaired electrons in a broad range of scientific fields. High-frequency ESR (HF-ESR) spectrometers operating at sub-THz frequencies are mostly custom-made with non-standard solutions. This article presents a set of six different exchangeable sample holders with a fast-loading flange for a sub-THz ESR spectrometer operating at high magnetic fields up to 16 T and temperature ranges of 4–400 K. Here, we report on the concept, design, and illustrative measurements of non-resonant ESR sample holders for the measurements of samples in a liquid solution, polycrystalline-compressed powders, oriented single crystals, electrical devices under sub-THz irradiation, as well as for samples transferred from the ultrahigh vacuum (UHV) systems without air contamination. Our solution expands the usage possibilities for HF-ESR spectroscopy, showing that one spectrometer with the presented concept of sample holders enables a wide range of applications.

A compact, dual-zone vertical tube furnace for the determination of tritium and carbon-14 in decommissioning wastes

A compact dual zone, two work-tube, vertical tube furnace system (Raddec Pyrolyser-Mini) has been designed for the determination of H-3 and C-14 in decommissioning wastes. An optimised methodology was developed following improvements to sample holder and bubbler trap design, sample loading and loading temperature, as well as length and style of heating programmes. A significant efficiency enhancement was obtained through ‘hot-loading’ of the sample into the furnace at 600 °C before finally ramping to 900 °C. Direct trapping of H-3 and C-14 in a scintillation vial located in a special anti-suck-back bubbler further improved operations, leading to a reduction in analysis time and measurement sensitivity. Co-trapping of the analytes and dual-label liquid scintillation counting also proved effective. Overall, the developed methodology led to a reduced analyte extraction/trapping time of 150 min whilst achieving limits of detection of <1 Bq/g. Validation of the procedure was assessed using a range of spiked matrices relevant to nuclear site decommissioning, reference materials and operationally-exposed materials. The compact size of this thermal extraction system is such that it allows for deployment in fume cupboards, gloveboxes and a mobile laboratory.

Oxygen K-edge X-ray absorption spectra of liquids with minimization of window contamination.

Oxygen K-edge X-ray absorption spectroscopy is used routinely to study a range of solid materials. However, liquid samples are studied less frequently at the oxygen K-edge due to the combined challenges of high-vacuum conditions and oxygen contamination of window materials. A modular sample holder design with a twist-seal sample containment system that provides a simple method to encapsulate liquid samples under high-vacuum conditions is presented. This work shows that pure silicon nitride windows have lower oxygen contamination than both diamond- and silicon-rich nitride windows, that the levels of oxygen contamination are related to the age of the windows, and provides a protocol for minimizing the background oxygen contamination. Acid-washed 100 nm-thick silicon nitride windows were found to give good quality oxygen K-edge data on dilute liquid samples.

Transmission Kikuchi diffraction: The impact of the signal-to-noise ratio

Signal optimization for transmission Kikuchi diffraction (TKD) measurements in the scanning electron microscope is investigated by a comparison of different sample holder designs. An optimized design is presented, which uses a metal shield to efficiently trap the electron beam after transmission through the sample. For comparison, a second holder configuration allows a significant number of the transmitted electrons to scatter back from the surface of the sample holder onto the diffraction camera screen. It is shown that the secondary interaction with the sample holder leads to a significant increase in the background level, as well as to additional noise in the final Kikuchi diffraction signal. The clean TKD signal of the optimized holder design with reduced background scattering makes it possible to use small signal changes in the range of 2% of the camera full dynamic range. As is shown by an analysis of the power spectrum, the signal-to-noise ratio in the processed Kikuchi diffraction patterns is improved by an order of magnitude. As a result, the optimized design allows an increase in pattern signal to noise ratio which may lead to increase in measurement speed and indexing reliability.

New method of transport measurements on van der Waals heterostructures under pressure

The interlayer coupling, which has a strong influence on the properties of van der Waals heterostructures, strongly depends on the interlayer distance. Although considerable theoretical interest has been demonstrated, experiments exploiting a variable interlayer coupling on nanocircuits are scarce due to the experimental difficulties. Here, we demonstrate a novel method to tune the interlayer coupling using hydrostatic pressure by incorporating van der Waals heterostructure based nanocircuits in piston-cylinder hydrostatic pressure cells with a dedicated sample holder design. This technique opens the way to conduct transport measurements on nanodevices under pressure using up to 12 contacts without constraints on the sample at the fabrication level. Using transport measurements, we demonstrate that a hexagonal boron nitride capping layer provides a good protection of van der Waals heterostructures from the influence of the pressure medium, and we show experimental evidence of the influence of pressure on the interlayer coupling using weak localization measurements on a transitional metal dichalcogenide/graphene heterostructure.

Automated system for surface photovoltage spectroscopy.

This paper details the development of a lab-made experimental setup for surface photovoltage spectroscopy (SPS) measurements using an open-source and Arduino® microcontroller to control a monochromator and some off-the-shelf electronic components. The experimental setup is interfaced to a computer, where LabVIEW® based software manages system control and data acquisition. We also report the design of a compact sample holder, simple and easy to manufacture and handle. Results of the application of SPS to the characterization of MoO3 thin films and semiconductor laser structures are presented to validate the performance of the setup, highlighting the effectiveness of SPS for the characterization of semiconductor materials and devices.

Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution

Synchrotron x-ray imaging techniques, like x-ray computed tomography (CT) and radiography have proven instrumental in expanding the communities knowledge of complex transport and reaction kinetics in electrochemical devices such as fuel cells and electrolyzers. This work presents the development of novel x-ray CT imaging techniques for operando visualization of water within low temperature fuel cells at spatial resolutions spanning the micro and nano scales. The design of operando sample holders, for both micro x-ray CT and nano CT experiments is described in depth, and prototypes of these sample holders were evaluated across a set of requirements, the most important of which are x-ray transmissibility, electrical conductivity and mechanical stability. Water segmentation from micro x-ray CT data was enabled by an image subtraction method, where the image without water is subtracted from the one with water. Through iterative experimentations, the operando nano CT cell was developed to optimize mechanical compression, electric conductivity and gas flow. While three-dimensional fuel cell reconstructions were shown possible, there remain challenges to overcome at typical lower energies (8 keV) due to beam damage, whereas it is not as significant for higher energies (>17.5 keV).

Combinatorial laser molecular beam epitaxy system integrated with specialized low-temperature scanning tunneling microscopy.

We present a newly developed facility comprising a combinatorial laser molecular beam epitaxy system and an in situ scanning tunneling microscope (STM). This facility aims at accelerating the materials research in a highly efficient way by advanced high-throughput film synthesis techniques and subsequent fast characterization of surface morphology and electronic states. Compared with uniform films deposited by conventional methods, the so-called combinatorial thin films will be beneficial in determining the accurate phase diagrams of different materials due to the improved control of parameters such as chemical substitution and sample thickness resulting from a rotary-mask method. A specially designed STM working under low-temperature and ultrahigh vacuum conditions is optimized for the characterization of combinatorial thin films in an XY coarse motion range of 15 mm × 15 mm with submicrometer location precision. The overall configuration and some key aspects such as the sample holder design, scanner head, and sample/tip/target transfer mechanism are described in detail. The performance of the device is demonstrated by synthesizing high-quality superconducting FeSe thin films with gradient thickness and imaging surfaces of highly oriented pyrolytic graphite, Au (111), Bi2Sr2CaCu2O8+δ (BSCCO), and FeSe. In addition, we also have obtained clean noise spectra of tunneling junctions and the superconducting energy gap of BSCCO. The successful manufacturing of such a facility opens a new window for the next generation equipment designed for experimental materials research.

Measuring electrical properties of mortar and concrete samples using the spectral induced polarization method: laboratory set-up

Abstract Electrical impedance spectroscopy (EIS), also known as Spectral Induced Polarization (SIP) has proven to be a successful non-destructive technique able to characterize the chemical and physical properties of a complex structure (concrete, rocks, and soil) under various environmental conditions. Because this technique aims to measure small amplitude signals, it can easily be influenced by parasitic effects which are not representative of the intrinsic properties of the investigated material. The purpose of this paper is to validate the resolution of our experimental methodology as a preliminary step to ensure an accurate measurement of the bulk complex resistivity response of concrete samples within a wide frequency range (1.43 mHz–20 kHz). A cement mortar sample is first used as a homogeneous (isotropic) material to improve the sample holder design for reducing the errors and controlling the external parameters (such as coupling effect, geometric factor, contact impedance, electrode polarization) during the laboratory measurements. Also, the performance and installation of the measuring components such as the electrodes (current and potential) and the sample holder design are assessed. The specimen dimensions and designs are selected based on a sample standard size that will be used to determine the physico-mechanical properties of concrete (compressive strength, modulus of elasticity, ultrasonic pulse velocity, length variation). The examinations are performed in parallel with the SIP measurement on the same sample. The accuracy of our measurement setup is then validated using aluminum-bronze plates bonded to the sample using a conductive gel to transmit electric current with a density less than 10 - 3 A m−2. The results showed that by controlling the sponge moisture in the Ag/AgCl non-polarizable voltage electrodes, our SIP measurement system is able to measure the phase lag with an error smaller than 1 mrad over a frequency range from 1.43 mHz to 20 kHz.

Challenges and Solutions for Handling and Characterizing Alkali-Tc-Oxide Salts

ABSTRACTThough not often discussed explicitly in literature, sample handling and preparation for advanced characterization techniques is a significant challenge for radiological materials. In this contribution, a detailed description is given of method development associated with characterization of highly radioactive and, in some cases, hygroscopic oxides of technetium. Details are given on developed protocols, fixtures, and tooling designed for x-ray and neutron diffraction, x-ray absorption, Raman spectroscopy, magic angle spinning nuclear magnetic resonance, and electron paramagnetic resonance. In some cases, multiple iterations of improved sample holder design are described. Lessons learned in handling Tc compounds for these and similar characterization methods are discussed.

A Newly Designed Infrared Reflection Absorption Spectroscopy System for In Situ Characterization from Ultrahigh Vacuum to Ambient Pressure.

We present a novel ultrahigh vacuum (UHV) compatible polarization modulation infrared reflection absorption spectroscopy (PM-IRRAS) system that is designed for in situ surface spectroscopic characterization on a transferable single crystalline sample. The innovative design of manipulator rod and high-pressure cell (HPC) ensures free movement of the sample between the preparation chamber and the HPC, and perfect separation of them during high pressure experiments. The pressure in the HPC can be varied from UHV (10-9 mbar) to ambient pressure (1000 mbar) while keeping the preparation chamber under UHV conditions. The design of the transferable sample holder and receiving stage allows precise temperature measurement and allows convenient sample changing. In situ IRRAS measurements under variable pressure and temperature can be conducted either in the conventional mode or with polarization modulation. Other surface characterization methods can also use the preparation chamber; thus, the system is endowed with the capability for systematic investigations of surface catalytic reactions. A case study of CO adsorption and oxidation on Pt(111) demonstrates the performance of the system.

Towards a compact and precise sample holder for macromolecular crystallography.

Most of the sample holders currently used in macromolecular crystallography offer limited storage density and poor initial crystal-positioning precision upon mounting on a goniometer. This has now become a limiting factor at high-throughput beamlines, where data collection can be performed in a matter of seconds. Furthermore, this lack of precision limits the potential benefits emerging from automated harvesting systems that could provide crystal-position information which would further enhance alignment at beamlines. This situation provided the motivation for the development of a compact and precise sample holder with corresponding pucks, handling tools and robotic transfer protocols. The development process included four main phases: design, prototype manufacture, testing with a robotic sample changer and validation under real conditions on a beamline. Two sample-holder designs are proposed: NewPin and miniSPINE. They share the same robot gripper and allow the storage of 36 sample holders in uni-puck footprint-style pucks, which represents 252 samples in a dry-shipping dewar commonly used in the field. The pucks are identified with human- and machine-readable codes, as well as with radio-frequency identification (RFID) tags. NewPin offers a crystal-repositioning precision of up to 10 µm but requires a specific goniometer socket. The storage density could reach 64 samples using a special puck designed for fully robotic handling. miniSPINE is less precise but uses a goniometer mount compatible with the current SPINE standard. miniSPINE is proposed for the first implementation of the new standard, since it is easier to integrate at beamlines. An upgraded version of the SPINE sample holder with a corresponding puck named SPINEplus is also proposed in order to offer a homogenous and interoperable system. The project involved several European synchrotrons and industrial companies in the fields of consumables and sample-changer robotics. Manual handling of miniSPINE was tested at different institutes using evaluation kits, and pilot beamlines are being equipped with compatible robotics for large-scale evaluation. A companion paper describes a new sample changer FlexED8 (Papp et al., 2017, Acta Cryst., D73, 841-851).

Sample holder design for effective thermal conductivity measurement of pebble-bed using laser flash method

Since the stress due to the thermal load on breeding blanket structure is one of the main design driver, the thermal conductivity is necessary input data for thermal-structural and thermo-hydraulic analyses performed in order to understand the heat transfer phenomena and estimate the thermal stress. Since for the functional materials of solid type breeding blanket a pebble-bed form is mainly adopted instead of a bulk form such as a block or a disk, it should be needed to measure the thermal conductivity of pebble-bed. In this study, the effective thermal conductivity of pebble-bed is measured by laser flash method, which is one of the various thermal conductivity measurement methods, because this method has several advantages such as a wide thermal conductivity range of the measurement and a small amount of pebbles. A sample holder considering the heat transfer mechanism from the laser source to pebble-bed has been specially designed in order to apply the laser flash technique to the pebble-bed sample and it has been validated by the experiments. This paper introduces preliminary results of the effective thermal conductivity on the pebble-bed using this sample holder.

Automated instrumentation for high-temperature Seebeck coefficient measurements

ABSTRACTThe fabrication of automated instrumentation for high-temperature Seebeck coefficient measurements is presented. K-type thermocouples were used to measure the average temperature of the sample and the Seebeck voltage. The temperature dependence of the Seebeck coefficients of the thermocouple and its negative leg were obtained by the integration method. A steady-state-based differential technique was used for Seebeck coefficient measurement. The use of limited components and a thin heater simplified the sample holder design and minimized heat loss. The power supplied to the heater determined the temperature difference across the sample and the measurement was carried out by achieving a steady state. A LabVIEW-based program was constructed to automate the measurements. The complete setup was fabricated using commonly available materials. This instrument is standardized for materials with a wide range of Seebeck coefficients and temperature differences. High temperature measurements for iron, constantan, bismuth, and Bi0.36Sb1.45Te3 were carried out and the results were in good agreement with standard values.