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We present a system for the growth of molecular films in vacuum that exhibits high versatility with respect to the choice of molecular species. These can be either evaporated from powders or injected from solutions using an electrospray system, making it possible to handle particularly large and/or fragile molecules in a controlled environment. The apparatus is equipped with a reflectance anisotropy spectroscopy system for the in situ characterization of the optical response of the films and can be directly connected to a photoelectron spectrometer without breaking the vacuum. The system is conceived for the study and characterization of porphyrin films. Here, to showcase the range of possible analyses allowed by the experimental setup and test the operation of the system, novel results are provided on electrospray deposition on highly oriented pyrolytic graphite of Zn tetraphenyl porphyrins and Zn proto porphyrins, the latter featuring fragile side groups that make deposition from solution more attractive. In situ characterization is complemented by ex situ atomic force microscopy. Thanks to this multi-technique approach, changes in the film morphology and spectroscopic response are detected and directly related to the choice of the molecular moiety and growth method. [ABSTRACT FROM AUTHOR]

A high-fidelity synthetic diagnostic has been developed for the ITER core x-ray crystal spectrometer diagnostic based on x-ray ray tracing. This synthetic diagnostic has been used to model expected performance of the diagnostic, to aid in diagnostic design, and to develop engineering tolerances. The synthetic model is based on x-ray ray tracing using the recently developed xicsrt ray tracing code and includes a fully three-dimensional representation of the diagnostic based on the computer aided design. The modeled components are: plasma geometry and emission profiles, highly oriented pyrolytic graphite pre-reflectors, spherically bent crystals, and pixelated x-ray detectors. Plasma emission profiles have been calculated for Xe44+, Xe47+, and Xe51+, based on an ITER operational scenario available through the Integrated Modelling & Analysis Suite database, and modeled within the ray tracing code as a volumetric x-ray source; the shape of the plasma source is determined by equilibrium geometry and an appropriate wavelength distribution to match the expected ion temperature profile. All individual components of the x-ray optical system have been modeled with high-fidelity producing a synthetic detector image that is expected to closely match what will be seen in the final as-built system. Particular care is taken to maintain preservation of photon statistics throughout the ray tracing allowing for quantitative estimates of diagnostic performance. [ABSTRACT FROM AUTHOR]

We have built and commissioned a novel standalone multi-crystal x-ray spectrometer (MOSARIX) in the von Hamos configuration based on highly annealed pyrolytic graphite crystals. The spectrometer is optimized for the energy range of 2–5 keV, but this range can be extended up to 20 keV by using higher reflection orders. With its nine crystals and a Pilatus detector, MOSARIX achieves exceptional detection efficiency with good resolving power (better than 4000), opening the door to study small cross section phenomena and perform fast in situ measurements. The spectrometer operates under a He atmosphere, which provides a flexible sample environment for measurements in gas, liquid, and solid phases. [ABSTRACT FROM AUTHOR]

Low-temperature scanning tunneling microscopy and spectroscopy (STM/S) help to better understand the fundamental physics of condensed matter. We present an ultracompact STM within a Φ 10 piezo tube in a 20 T superconducting magnet. The carefully cut piezo tube contains the STM's coarse-positioning assembly. Loading an STM tip–sample mechanical loop into the piezo tube with special cut openings enables an ultracompact pencil-size dimension down to Φ 10 mm, in which fine-machined nonmagnetic parts are assembled to enable slide–stick motion and xyz-scanning procedures. The small size leads to a higher resonant frequency, a typical feature of a rigid STM instrument, increasing its vibration immunity. Scanning by moving the sample while keeping the tip stationary improves the stability of the tip–sample junction compared to moving the tip. Taking advantage of its high-field compatibility and rigid design, our STM captures the atomically resolved topography of highly oriented pyrolytic graphite (HOPG) at 1.5 K and in magnetic fields up to 17 T. The topography of graphene lattice and graphite is simultaneously recorded on an atomic terrace of HOPG, unveiling a modified local charge density at a surface defect. The superconducting energy gaps of layered type-II superconductors NbSe2 and PdBi2 are well resolved through dI/dV tunneling spectra at sub-2 K. Our unique STM is highly suitable for potential STM/S applications in world-class high-field facilities where the strong magnetic field can exceed 30 T. [ABSTRACT FROM AUTHOR]

A methodology for measuring x-ray continuum spectra of inertial confinement fusion (ICF) implosions is described. The method relies on the use of ConSpec, a high-throughput spectrometer using a highly annealed pyrolytic graphite crystal [MacDonald et al., J. Instrum. 14, P12009 (2019)], which measures the spectra in the ≃20–30 keV range. Due to its conical shape, the crystal is sagittally focusing a Bragg-reflected x-ray spectrum into a line, which enhances the recorded x-ray emission signal above the high neutron-induced background accompanying ICF implosions at the National Ignition Facility. To improve the overall measurement accuracy, the sensitivity of the spectrometer measured in an off-line x-ray laboratory setting was revised. The error analysis was expanded to include the accuracy of the off-line measurements, the effect of the neutron-induced background, as well as the influence of possible errors in alignment of the instrument to the ICF target. We demonstrate how the improved methodology is applied in the analysis of ConSpec data with examples of a relatively low-neutron-yield implosion using a tritium–hydrogen–deuterium mix as a fuel and a high-yield deuterium–tritium (DT) implosion producing high level of the background. In both cases, the shape of the measured spectrum agrees with the exponentially decaying spectral shape of bremsstrahlung emission to within ±10%. In the case of the high-yield DT experiment, non-monotonic deviations slightly exceeding the measurement uncertainties are observed and discussed. [ABSTRACT FROM AUTHOR]

In this study, we present the absolute calibration of the conical crystal for the zinc spectrometer (ZSPEC), an x-ray spectrometer at the OMEGA laser facility at the Laboratory for Laser Energetics. The ZSPEC was originally designed to measure x-ray Thomson scattering using flat or cylindrically curved highly oriented pyrolytic graphite crystals centered around Zn He-alpha emission at 9 keV. To improve the useful spectral range and collection efficiency of the ZSPEC, a conical highly annealed pyrolytic graphite crystal was fabricated for the ZSPEC. The conically bent crystal in the Hall geometry produces a line focus perpendicular to the spectrometer axis, corresponding to the detector plane of electronic detectors at large scale laser facilities such as OMEGA, extending the useful range of the spectrometer to 7–11 keV. Using data collected using a microfocus Mo x-ray source, we determine important characteristics of ZSPEC such as the dispersion, spatial resolution, and absolute sensitivity of the instrument. A ray-trace model of ZSPEC provides another point of agreement in calculations of the ZSPEC dispersion and crystal response. [ABSTRACT FROM AUTHOR]

A novel dual-reflection configuration is introduced for the International Tokamak Experimental Reactor (ITER) core x-ray spectrometer to fit the allocated space where it will be placed accompanied by moving the detectors backward to reduce the incident radiation dose. The highly oriented pyrolytic graphite, which has a mosaic structure of microscopic crystallites, is chosen for the front reflector motivated by higher x-ray throughput and stronger misalignment tolerance compared to the perfect crystal reflector. In the ITER core x-ray spectrometer, a combination of several reflector-deflected Lines of Sight (LOSs) and a direct LOS is proposed for the first time named X-Ray Crystal Spectroscopy Core (XRCS-Core). The system is optimized to observe lines from externally seeded xenon and the intrinsic tungsten impurity, meeting both port integration needs and measurement requirements. Its spectral performance is simulated using an analytical-raytracing mixed code——XRSA, showing good imaging quality with a spectral resolution higher than 8000. The XRCS-Core system is thought to be applicable in various ITER scenarios through the assessment taking into account the spectrometers' specifications and the chosen lines' emissivity in different plasma parameters. [ABSTRACT FROM AUTHOR]

A novel double full-cylinder crystal x-ray spectrometer for x-ray emission spectroscopy (XES) has been realized based on a modified von Hamos geometry. The spectrometer is characterized by its compact dimensions, its versatility with respect to the number of crystals used in series in the detection path, and the option to perform calibrated XES measurements. The full-cylinder crystals used are based on highly annealed pyrolytic graphite with a thickness of 40 μm, which was bent to a radius of curvature of 50 mm. The flexible design of the spectrometer allows for an easy change—within the same setup—between measurements with one crystal for maximized efficiency or two crystals for increased spectral resolving power. The spectrometer realized can be used at different end-stations of synchrotron radiation beamlines or can be laboratory-based. The main application focus of the spectrometer is the determination of x-ray fundamental atomic parameters in the photon energy range from 2.4 to 18 keV. The evaluation of chemical speciation is also an area of application, as demonstrated in the example of battery electrodes using resonant inelastic x-ray scattering. [ABSTRACT FROM AUTHOR]

We have built an x-ray spectrometer in a von Hamos configuration based on a highly annealed pyrolytic graphite crystal. The spectrometer is designed to measure x-ray emission in the range of 2–5 keV. A spectral resolution E/ΔE of 4000 was achieved by recording the elastic peak of photons issued from the GALAXIES beamline at the SOLEIL synchrotron radiation facility. [ABSTRACT FROM AUTHOR]

A compact, ultrahigh vacuum, radiative heater based on pyrolytic boron nitride that efficiently directs nearly all of its radiation to the sample was designed and constructed. It is shown that the heater reaches temperatures of 1300 K experimentally at 60% of its maximum power. A COMSOL Multiphysics® simulation and an analytical model predict an ultimate temperature of up to 1500 K. Furthermore, the heater does not introduce any contamination to the sample. This is accomplished by a custom-made Nb radiation shield, which was manufactured by selective laser melting and holds a flag-style sample holder. Before manufacturing, the whole assembly was simulated with COMSOL Multiphysics to validate the design of the radiation shield. [ABSTRACT FROM AUTHOR]

Determining real-time changes in the local atomistic order is important for a mechanistic understanding of shock wave induced structural and chemical changes. However, the single event and short duration (nanosecond times) nature of shock experiments pose challenges in obtaining Extended X-ray Absorption Fine Structure (EXAFS) measurements—typically used for monitoring local order changes. Here, we report on a new single pulse (∼100 ps duration) transmission geometry EXAFS capability for use in laser shock-compression experiments at the Dynamic Compression Sector (DCS), Advanced Photon Source. We used a flat plate of highly oriented pyrolytic graphite (HOPG) as the spectrometer element to energy disperse x rays transmitted through the sample. It provided high efficiency with ∼15% of the x rays incident on the HOPG reaching an x-ray area detector with high quantum efficiency. This combination resulted in a good signal-to-noise ratio (∼103), an energy resolution of ∼10 eV at 10 keV, EXAFS spectra covering 100 s of eV, and a good pulse to pulse reproducibility of our single pulse measurements. Ambient EXAFS spectra for Cu and Au are compared to the reference spectra, validating our measurement system. Comparison of single pulse EXAFS results for ambient and laser shocked Ge(100) shows large changes in the local structure of the short lived state of shocked Ge. The current DCS EXAFS capability can be used to perform single pulse measurements in laser shocked materials from ∼9 keV to 13 keV. These EXAFS developments will be available to all users of the DCS. [ABSTRACT FROM AUTHOR]

Measuring anisotropic thermal conductivity has always been a challenging task in thermal metrology. Although recent developments of pump–probe thermoreflectance techniques such as variable spot sizes, offset pump–probe beams, and elliptical beams have enabled the measurement of anisotropic thermal conductivity, a metal film transducer enabled for the absorption of the modulated pump laser beam and the detection of the thermoreflectance signal. However, the existence of the transducer would cause in-plane heat spreading, suppressing the measurement sensitivity to the in-plane thermal conductivity. In addition, the transducer film also adds complexity to data processing, since it requires careful calibration or fitting to determine extra parameters such as the film thickness and conductivity, and interface conductance between the transducer and the sample. In this work, we discussed the methodology for measuring in-plane thermal conductivity of layered semiconductors and semimetals without any transducer layer. We show that the removal of transducer results in the dominantly large sensitivity to in-plane thermal conductivity compared with other parameters, such as cross-plane thermal conductivity and the absorption depth of the laser beams. Transducerless frequency-domain thermoreflectance (FDTR) measurements are performed on three reference layered-materials, highly ordered pyrolytic graphite, molybdenum disulfide (MoS2), and bismuth selenide (Bi2Se3) and demonstrated using the analytical thermal model that the measured in-plane thermal conductivity showed much-improved accuracy compared with conventional FDTR measurement with a transducer. [ABSTRACT FROM AUTHOR]

Sandia's Z Pulsed Power Facility is able to dynamically compress matter to extreme states with exceptional uniformity, duration, and size, which are ideal for investigating fundamental material properties of high energy density conditions. X-ray diffraction (XRD) is a key atomic scale probe since it provides direct observation of the compression and strain of the crystal lattice and is used to detect, identify, and quantify phase transitions. Because of the destructive nature of Z-Dynamic Material Property (DMP) experiments and low signal vs background emission levels of XRD, it is very challenging to detect a diffraction signal close to the Z-DMP load and to recover the data. We have developed a new Spherical Crystal Diffraction Imager (SCDI) diagnostic to relay and image the diffracted x-ray pattern away from the load debris field. The SCDI diagnostic utilizes the Z-Beamlet laser to generate 6.2-keV Mn–Heα x rays to probe a shock-compressed material on the Z-DMP load. A spherically bent crystal composed of highly oriented pyrolytic graphite is used to collect and focus the diffracted x rays into a 1-in. thick tungsten housing, where an image plate is used to record the data. [ABSTRACT FROM AUTHOR]

We report the fabrication, characterization, and use of rubidium vapor dispensers based on highly oriented pyrolytic graphite (HOPG) intercalated with metallic rubidium. Compared to commercial chromate salt dispensers, these intercalated HOPG (IHOPG) dispensers hold an order of magnitude more rubidium in a similar volume, require less than one-fourth the heating power, and emit less than one-half as many impurities. Appropriate processing permits exposure of the IHOPG to atmosphere for over ninety minutes without any adverse effects. Intercalation of cesium, potassium, and lithium into HOPG has also been demonstrated in the literature, which suggests that IHOPG dispensers may also be made for those metals. [ABSTRACT FROM AUTHOR]

A method is presented to characterize the anisotropic thermal properties of materials based on nanosecond transient thermoreflectance (TTR). An analytical heat transfer model is derived for the TTR signal, showing that the signal is sensitive to out-of-plane and in-plane heat conductions at distinct time scales. This sensitivity feature can be exploited to simultaneously determine the out-of-plane and in-plane thermal conductivities. Examples are given for molybdenum disulphide, hexagonal boron nitride, and highly oriented pyrolytic graphite to assess the validity of this method. [ABSTRACT FROM AUTHOR]

A new type of high intensity and high resolution time-of-flight near backscattering neutron spectrometer is presented which is capable of an energy resolution of 4.0 μeV with a data collection rate an order of magnitude larger than current near backscattering spectrometers capable of this resolution. This design challenges two accepted norms of high resolution indirect neutron spectrometers: it uses large mosaic pyrolytic graphite (002) crystals instead of nearly perfect silicon (111) crystals to select the final neutron energy, and it operates well away from the normal backscattering condition 2φ ≈ 180° instead using 2φ = 160°. This paper describes the methodology behind this spectrometer along with ray-tracing simulations of the instrument using the McStas program. [ABSTRACT FROM AUTHOR]

Limited Z-axis bandwidth of piezotube scanners employed in conventional Scanning Tunneling Microscopes (STMs) has been a major limiting factor in achieving high scan speeds in STM applications. Slow Z-axis dynamics of typical piezotube scanners combined with the weight of the STM tip/tip holder assembly, that the scanner has to carry, substantially limit the achievable Z-axis bandwidth in both imaging and lithography modes. To tackle this issue, we propose a high bandwidth microelectromechanical-system-based nanopositioner to be integrated into an existing STM scanner. The device is designed to replace the STM tip and fine Z-positioning mechanisms in the conventional STM setup, while providing an order of magnitude higher bandwidth in Z axis. The device is microfabricated using double silicon-on-isolator technology, and standard cleanroom processes. Experiments show that tunneling current between the device tip and a highly ordered pyrolytic graphite sample can be successfully established and maintained in air using the proposed device in a feedback loop. Results indicate that the proposed device uniquely combines a very high resolution and a large stroke with a substantially larger Z-axis bandwidth compared to that of conventional STM piezotube scanners, enabling higher scanning speeds in STM operations. [ABSTRACT FROM AUTHOR]

We have built a laboratory spectrometer for X-ray emission spectroscopy. The instrument is employed in catalysis research. The key component is a von Hamos full cylinder optic with Highly Annealed Pyrolytic Graphite (HAPG) as a dispersive element. With this very efficient optic, the spectrometer subtends an effective solid angle of detection of around 1 msr, allowing for the analysis of dilute samples. The resolving power of the spectrometer is approximately E/ΔE = 4000, with an energy range of ∼2.3 keV–10 keV. The instrument and its characteristics are described herein. Further, a comparison with a prototype spectrometer, based on the same principle, shows the substantial improvement in the spectral resolution and energy range for the present setup. The paper concludes with a discussion of sample handling. A compilation of HAPG fundamentals and related publications are given in a brief Appendix. [ABSTRACT FROM AUTHOR]

We propose and demonstrate the implementation of an alternative work function tip calibration procedure for Kelvin probe force microscopy under ultrahigh vacuum, using monocrystalline metallic materials with known crystallographic orientation as reference samples, instead of the often used highly oriented pyrolytic graphite calibration sample. The implementation of this protocol allows the acquisition of absolute and reproducible work function values, with an improved uncertainty with respect to unprepared highly oriented pyrolytic graphite-based protocols. The developed protocol allows the local investigation of absolute work function values over nanostructured samples and can be implemented in electronic structures and devices characterization as demonstrated over a nanostructured semiconductor sample presenting Al0.7Ga0.3As and GaAs layers with variable thickness. Additionally, using our protocol we find that the work function of annealed highly oriented pyrolytic graphite is equal to 4.6 ± 0.03 eV. [ABSTRACT FROM AUTHOR]

We present the design and performance of a cryogenic scanning tunneling microscope (STM) which operates inside a water-cooled Bitter magnet, which can attain a magnetic field of up to 38 T. Due to the high vibration environment generated by the magnet cooling water, a uniquely designed STM and a vibration damping system are required. The STM scan head is designed to be as compact and rigid as possible, to minimize the effect of vibrational noise as well as fit the size constraints of the Bitter magnet. The STM uses a differential screw mechanism for coarse tip—sample approach, and operates in helium exchange gas at cryogenic temperatures. The reliability and performance of the STM are demonstrated through topographic imaging and scanning tunneling spectroscopy on highly oriented pyrolytic graphite at T = 4.2 K and in magnetic fields up to 34 T. [ABSTRACT FROM AUTHOR]

This paper presents a preliminary study of an elementary device consisting of a small plate made from pyrolytic carbon levitated above a magnet array which is sensitive to any irradiating laser power. This device might provide an interesting alternative to power meters based on thermal measurement techniques via the Stefan-Boltzmann law or the photon-electron interaction. We show that the photoresponse of a pyrolytic carbon plate in terms of levitation height versus irradiation power in the range of 20 mW to 1 W is sufficiently linear, sensitive, and reproducible to be used as a laser power sensor. The elevation height change as a function of irradiance time appears to be a suitable measurement parameter for establishing a relation with the irradiating laser power. The influence of some quantities affecting the measurement results has been highlighted. The study demonstrates that such a device should prove useful for applications in metrology, industry, or emerging technologies. [ABSTRACT FROM AUTHOR]

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) × 15 mm (H) × 1mm(D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement. [ABSTRACT FROM AUTHOR]

We have built an absolutely calibrated, highly efficient, Bragg crystal spectrometer in von Hamos geometry. This zinc von Hamos spectrometer uses a crystal made from highly oriented pyrolytic graphite that is cylindrically bent along the non-dispersive axis. It is tuned to measure x-ray spectra in the 7-10 keV range and has been designed to be used on a Ten Inch Manipulator for the Omega and OmegaEP target chambers at the Laboratory for Laser Energetics in Rochester, USA. Significant shielding strategies and fluorescence mitigation have been implemented in addition to an imaging plate detector making it well suited for experiments in high-intensity environments. Here we present the design and absolute calibration as well as mosaicity and integrated reflectivity measurements. [ABSTRACT FROM AUTHOR]

VESPA, Vibrational Excitation Spectrometer with Pyrolytic-graphite Analysers, aims to probe molecular excitations via inelastic neutron scattering. It is a thermal high resolution inverted geometry time-of-flight instrument designed to maximise the use of the long pulse of the European Spallation Source. The wavelength frame multiplication technique was applied to provide simultaneously a broad dynamic range (about 0-500 meV) while a system of optical blind choppers allows to trade flux for energy resolution. Thanks to its high flux, VESPA will allow the investigation of dynamical and in situ experiments in physical chemistry. Here we describe the design parameters and the corresponding McStas simulations. [ABSTRACT FROM AUTHOR]

We demonstrate the construction of a novel low-noise continuous flow humidity controller and its integration with a commercial variable-temperature atomic force microscope fluid cell, allowing precise control of humidity and temperature at the sample during nanoscale measurements. Based on wet and dry gas mixing, the design allows a high mechanical stability to be achieved by means of an ultrasonic atomiser for the generation of water-saturated gas, improving upon previous bubbler-based architectures. Water content in the flow is measured both at the inflow and outflow of the fluid cell, enabling the monitoring of water condensation and icing, and allowing controlled variation of the sample temperature independently of the humidity. To benchmark the performance of the controller, the results of detailed noise studies and time-based imaging of the formation of ice layers on highly oriented pyrolytic graphite are shown. [ABSTRACT FROM AUTHOR]