Use of a 4-circle goniometer for neutron and X-ray diffractometer in the study of single crystals

Objectives. This study described the 4-circle goniometer Syntex P1N and its possible applications in X-ray and neutron structure analysis of single crystals.Methods. The 4-circle goniometer Syntex P1N, due to its high-precision mechanical characteristics and individual components from domestic equipment (sets of DRON type X-ray diffractometers), formed the basis for developing an instrument complex for X-ray and neutron-structure studies.Results. The neutron diffractometer was upgraded based on the Syntex P1N goniometer. Therefore, the 10BF3-based end neutron counter, included in the diffractometer kit, was replaced by the 3He-based domestic side counter, SNM-16. Such a significant reduction in the linear dimensions of the detector allowed us to expand the range of measured angles of 2θ from 90° to 140° and increase the accuracy of the measured interplanar distances accordingly. The goniometer was adjusted relative to the primary neutron beam by placing it on a specially designed plate. Highly accurate measured parameters of the unit cell and the intensity of the reflexes were achieved by optimizing the installation geometry and the protection of the goniometer and detector. Based on the Syntex P1N goniometer, an instrument complex for X-ray diffraction studies has also been developed. Both the developed X-ray and the upgraded neutronography facilities were used to perform experiments to measure the unit cell parameters, the coordinates of atoms, and the parameters of their thermal vibrations on several crystals of domestic synthetic samples: diamond C, silicon Si, halite, or rock salt NaCl, and corundum α-Al2O3. An excellent correlation was achieved by comparing the data obtained with the corresponding chemical crystals’ parameters and reference samples recommended by the International Union of Crystallographers.Conclusions. This paper described a neutron installation and a Syntex P1N neutron diffractometer for the study of single crystals. Based on the latter, an instrument complex for X-ray diffraction studies has also been developed. Experiments on standard samples have shown a high level of accuracy in measuring the lattice parameters, the coordinates of atoms, and the parameters of their thermal vibrations on both the X-ray and neutron diffractometers.

Quantitative texture analysis using the NOMAD time-of-flight neutron diffractometer

Strategies for efficient and reliable texture measurements have been explored using the Nanoscale Ordered Materials Diffractometer (NOMAD) at the Spallation Neutron Source located at Oak Ridge National Laboratory (ORNL). To test these strategies, the texture of an Al alloy was also investigated using another neutron diffraction instrument, a constant-wavelength neutron diffractometer (NRSF2) located at the High Flux Isotope Reactor, also at ORNL. Reasonable agreement was found across the two experimental methods, but differences in overall texture strength and the symmetry of some components were noted, depending on the data reduction and analysis method selected. On the basis of these results, potential improvements are identified which would enhance the texture measurement capability on NOMAD.

Deformation Mechanisms in Ni-Based Superalloys at Room and Elevated Temperatures Studied by In Situ Neutron Diffraction and Electron Microscopy

Polycrystalline Ni-based superalloys are one of the most frequently used materials for high temperature load-bearing applications due to their superior mechanical strength and chemical resistance. In this paper, we presented an in situ diffraction study on the tensile deformation behavior of the polycrystalline Ni-based superalloy VDM® Alloy 780 at temperatures up to 500 °C performed at the STRESS-SPEC neutron diffractometer at the Heinz Maier-Leibnitz Zentrum. A detailed microstructural investigation was carried out by electron microscopy before and after testing. The results of these studies allowed us to determine the deformation mechanism in the differently orientated grains. It is shown that the deformation behavior, which is mainly dislocation motion and shearing of the γ′-precipitates, does not change at this temperature range. The deformation is strongly anisotropic and depends on the grain orientation. The macroscopic hardening can mainly be attributed to plastic deformation in grains, where the (200) lattice planes were orientated perpendicular to the loading direction. Accordingly, a remaining lattice strain and high dislocation density were detected predominantly in these grains.

Heat transfer analysis study for the design of the New Polychromatic Beam Neutron Reflectometer CANDOR (Chromatic Analysis Neutron Diffractometer Or Reflectometer)

A newly developed polychromatic beam neutron reflectometer CANDOR (Chromatic Analysis Neutron Diffractometer Or Reflectometer) on NG-1 at the NIST Center for Neutron research (NCNR) utilizes a wavelength-sensitive neutron detector consisting of 324 analyzing highly-oriented pyrolytic graphite (HOPG) crystals positioned sequentially in rows. Known for having a small thermal diffuse scattering cross section, HOPG crystals can lead to low signal-to-noise ratios in wavelength-sensitive detectors such as CANDOR. Even though it is possible to mathematically separate the desired signal from thermal diffuse scattering; by cooling the detector array of HOPG crystals in order to minimize the Debye Waller effect generates a better solution to this problem. In this heat transfer analysis study we show, within the instrument design constrains and thermodynamic considerations, technical feasibility and test results for the development of the New Polychromatic Beam Neutron Reflectometer CANDOR (Chromatic Analysis Neutron Diffractometer Or Reflectometer) at the NIST Center for Neutron Research.

WAVE – An innovative magnet devoted to spintronics

The LLB is part of a large project aiming at the development of experimental tools available for the spintronics community. This includes the design and construction of vector magnets for neutron and X-ray scattering (deployed on the Léon Brillouin-Orphée and Synchrotron SOLEIL TGIRs: neutron diffractometer 6T2 and XMRS Sextants). For neutron scattering, a very innovative design has been developed, relying solely on the use of vertical axis coils. This magnet called WAVE (for Wide Aperture VEctor) is now available at the LLB-Orphée for the user community.

High-Resolution Strain/Stress Measurements by Three-Axis Neutron Diffractometer

Resolution properties of the unconventional high-resolution neutron diffraction three-axis setup for strain/stress measurements of large bulk polycrystalline samples are presented. Contrary to the conventional two-axis setups, in this case, the strain measurement on a sample situated on the second axis is carried out by rocking the bent perfect crystal (BPC) analyzer situated on the third axis of the diffractometer. Thus, the so-called rocking curve provides the sample diffraction profile. The neutron signal coming from the analyzer is registered by a point detector. This new setup provides a considerably higher resolution (at least by a factor of 5), which however, requires a much longer measurement time. The high-resolution neutron diffraction setting can be effectively used, namely, for bulk gauge volumes up to several cubic centimeters, and for plastic deformation studies on the basis of the analysis of diffraction line profiles, thus providing average values of microstructure characteristics over the irradiated gauge volume.

Computational optimization of a 3D printed collimator

This contribution describes the computational methodology behind an optimization procedure for a scattered beam collimator. The workflow includes producing a file that can be manufactured via additive methods. A conical collimator, optimized for neutron diffraction experiments in a high pressure clamp cell, is presented as an example. In such a case the scattering from the sample is much smaller than that of the pressure cell. Monte Carlo Ray tracing in MCViNE was used to model scattering from a Si powder sample and the cell. A collimator was inserted into the simulation and the number and size of channels were optimized to maximize the rejection of the parasitic signal coming from the complex sample environment. Constraints, provided by the additive manufacturing process as well as a specific neutron diffractometer, were also included in the optimization. The source code and the tutorials are available in c3dp (Islam (2019)).