Variety Of Sample Environments Research Articles

(Invited) Electrochemistry Combined in Situ Neutron Reflectometry: A Powerful Tool for a More Sustainable Environment

Neutrons, having extraordinary characteristics that include penetrating power, sensitivity to lighter elements (such as hydrogen and carbon), and magnetic moment, make neutron reflectometry an ideal candidate for examining surface and interfacial structures of thin films in a non-destructive and non-invasive fashion. Liquids Reflectometer (LR) at the Spallation Neutron Source at Oak Ridge National Laboratory measures specular and off specular neutron reflectivity in a horizontal sample geometry, and tracks changes of layer thickness, scattering length density, and roughness as a function of depth. The exceptional sample environment at LR offers the capability to conduct in situ electrochemistry to probe the morphological and structural changes of solid/liquid interfaces during operation as a function of chemical and electrochemical gradients over time. Furthermore, the time-resolved mode at LR can be carried out continuously over a reduced Q range and binned into 60-second intervals. The improved time resolution of the neutron reflectivity (NR) measurement can help elucidate the kinetic behavior of surface/interfaces under dynamic conditions and provide a unique perspective to the equilibrium study. In this talk, I will give a brief introduction on neutron reflectometry, the LR, and a variety of sample environments at the LR. I will focus on the electrochemical applications coupled with in situ NR measurement. In the end, I will provide a specific example of applications in electrochemically modulated separation for water remediation by using neutron reflectometry. With the rapid growth of human population, it is highly desirable to minimize energy and materials input in selective separations for a more sustainable environment. The study is critical for creating new, more selective separation systems through rationally design of the structure and operating conditions.

Radial collimator performance and future collimator updates for the high-intensity total scattering diffractometer NOVA at J-PARC

The high-intensity neutron total scattering diffractometer NOVA at the Materials and Life Science Experimental Facility in the Japan Proton Accelerator Research Complex has a variety of sample environments. For background reduction, we manufactured and installed the radial collimator NOVARC with a gauge size of ∼32 mm. We evaluated its performance and succeeded in eliminating the unwanted scattering from the sample environment equipment and reducing the background signal to less than 4%. We also confirmed that G(r) data, which is important for pair distribution function analysis, is consistent with the one obtained at the sample environment with almost no background. In the future, we plan to combine NOVARC with a radial collimator manufactured using a 3D printer for measuring even smaller specimens or for extreme environments.

Advanced Non-Destructive in Situ Characterization of Metals with the French Collaborating Research Group D2AM/BM02 Beamline at the European Synchrotron Radiation Facility

The ability to non-destructively measure the structural properties of devices, either in situ or operando, are now possible using an intense X-ray synchrotron source combined with specialized equipment. This tool attracted researchers, in particular metallurgists, to attempt more complex and ambitious experiments aimed at answering unresolved questions in formation mechanisms, phase transitions, and magnetism complex alloys for industrial applications. In this paper, we introduce the diffraction diffusion anomale multi-longueur d’onde (D2AM) beamline, a French collaborating research group (CRG) beamline at the European Synchrotron Radiation Facility (ESRF), partially dedicated to in situ X-ray scattering experiments. The design of the beamline combined with the available equipment (two-dimensional fast photon counting detectors, sophisticated high precision kappa diffractometer, a variety of sample environments, continuous scanning for X-ray imaging, and specific software for data analysis) has made the D2AM beamline a highly efficient tool for advanced, in situ synchrotron characterization in materials science, e.g., single crystal or polycrystalline materials, powders, liquids, thin films, or epitaxial nanostructures. This paper gathers the main elements and equipment available at the beamline and shows its potential and flexibility in performing a wide variety of temporally, spatially, and energetically resolved X-ray synchrotron scattering measurements in situ.

A new diffractometer for diffuse scattering studies on the ID28 beamline at the ESRF.

A new diffractometer is now available to the general user community at the ESRF. The new diffractometer is a side station of the high-resolution inelastic X-ray scattering spectrometer on beamline ID28 and is located in the same experimental hutch. Both instruments can be operated simultaneously. The new diffractometer combines a fast and low-noise hybrid pixel detector with a variable diffraction geometry. The beam spot on the sample is 50 µm × 50 µm, where focusing is achieved by a combination of Be lenses and a KB mirror. Wavelengths from 0.5 to 0.8 Å can be used for the diffraction experiments. The setup is compatible with a variety of sample environments, allowing studies under non-ambient conditions. The diffractometer is optimized to allow a rapid survey of reciprocal space and diffuse scattering for the identification of regions of interest for subsequent inelastic scattering studies, but can also be employed as a fully independent station for structural studies from both powder and single-crystal diffraction experiments. Several software packages for the transformation and visualization of diffraction data are available. An analysis of data collected with the new diffractometer shows that the ID28 side station is a state-of-the-art instrument for structural investigations using diffraction and diffuse scattering experiments.

B18: What can the new core X-ray absorption spectroscopy beamline at Diamond do?

The new Core-XAS (X-ray absorption spectroscopy) beamline (B18) at Diamond aims to provide a reliable spectrometer for a broad scientific community. With this in mind, B18 has been built as a general-purpose beamline and offers to users a variety of sample environments and detection methods. Here we will present the first commissioning results and some of the capabilities of this versatile instrument.

The D20 instrument at the ILL: a versatile high-intensity two-axis neutron diffractometer

D20 is a medium to high resolution two-axis diffractometer capable of producing a neutron flux of 108 s−1 cm−2 at the sample position. The 1536 detection cells of its curved linear position sensitive detector (PSD) cover a continuous 2θ range of 153.6° over a total solid angle of 0.27 sr. This combination of a high incident neutron flux and a large detector solid angle provides D20 with the fastest counting rate, at a given resolution, of any reactor-based neutron diffractometer. Different monochromators and take-off angles, plus optional Soller collimators and secondary slits, permit a wide choice in the Q-space range, wavelength, resolution and flux. A high-resolution configuration offers Δd/d ∼ 2 × 10−3. Fast modern counting electronics allow in situ time-resolved experiments at the timescale of a few tens of milliseconds. In addition, a variety of sample environments, including an optional radial oscillating collimator for suppressing parasitic scattering, contribute to a rich scientific programme.

The University of New Mexico/Sandia National Laboratories small-angle scattering laboratory

The University of New Mexico/Sandia National Laboratories small-angle scattering laboratory provides a wide q-range, 3×10−4 Å−1<q<0.7 Å−1, for the structural analysis of materials on length scales from a few angstrom to ∼0.1 μm. The wide q-range is accomplished by combining data from a Bonse-Hart spectrometer (3×10−4 Å−1<q<3×10−2 Å−1) and a 5 m pinhole (3×10−3 Å−1<q<0.7 Å−1) instrument. Automation of the data acquisition systems along with a variety of sample environments and sample changers yields flexible, high throughput instruments.