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Structure factors describe how incident radiation is scattered from materials such as silicon and germanium and characterize the physical interaction between the material and scattered particles. We use neutron pendell\"{o}sung interferometry to make precision measurements of the (220) and (400) neutron-silicon structure factors, and achieve a factor of four improvement in the (111) structure factor uncertainty. These data provide measurements of the silicon Debye-Waller factor at room temperature and the mean square neutron charge radius $\langle r_n^2 \rangle = -0.1101 \pm 0.0089 \, \mathrm{fm}^2$. Combined with existing measurements of the Debye-Waller factor and charge radius, the measured structure factors also improve constraints on the strength of a Yukawa-modification to gravity by an order of magnitude over the 20 pm to 10 nm length scale range.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to be used to evaluate specific aspects of the instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 640f, the seventh generation of this powder diffraction SRM, which is designed to be used primarily for calibrating powder diffractometers with respect to line position; it also can be used for the determination of the instrument profile function. It is certified with respect to the lattice parameter and consists of approximately 7.5 g of silicon powder prepared to minimize line broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the Si powder. Both statistical and systematic uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.5431144 ± 0.000008 nm.

The NIST Vacuum Double-Crystal Spectrometer (VDCS) has been modernized and is now capable of recording reference-free wavelength-dispersive spectra in the 2 keV to 12 keV x-ray energy range. The VDCS employs crystals in which the lattice spacings are traceable to the definition of the meter through x-ray optical interferometry with a relative uncertainty

This rather long-standing project has resulted in a National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) for the analysis of crystallite size from a consideration of powder diffraction line profile broadening. It consists of two zinc oxide powders, one with a crystallite size distribution centered at approximately 15 nm, and a second centered at about 60 nm. These materials display the effects of stacking faults that broaden specific hkl reflections and a slight amount of microstrain broadening. Certification data were collected on the high-resolution powder diffractometer located at beamline 11-BM of the Advanced Photon Source, and on a NIST-built laboratory diffractometer equipped with a Johansson incident beam monochromator and position sensitive detector. Fourier transforms were extracted from the raw data using a modified, two-step profile fitting procedure that addressed the issue of accurate background determination. The mean column lengths, (L)area and (L)vol, were then computed from the Fourier transforms of the specimen contribution for each reflection. Data were also analyzed with fundamental parameters approach refinements using broadening models to yield (L)area and (L)vol values. These values were consistent with the model-independent Fourier transform results; however, small discrepancies were noted for the (L)area values from both machines and both crystallite size ranges. The fundamental parameters approach fits to the laboratory data yielded the certified lattice parameters.

We report recent advances in absolute x-ray wavelength metrology in the context of producing modern standard reference data. Primary x-ray wavelength standards are produced today using diffraction spectrometers using crystal optics arranged to be operated in dispersive and non-dispersive geometries, giving natural-line-width limited profiles with high resolution and accuracy. With current developments, measurement results can be made traceable to the Systeme internationale definition of the meter by using diffraction crystals that have absolute lattice-spacing provenance through x-ray-optical interferometry. Recent advances in goniometry, innovation of electronic x-ray area detectors, and new in situ alignment and measurement methods now permit robust measurement and quantification of previously-elusive systematic uncertainties. This capability supports infrastructures like the NIST Standard Reference Data programs and the International Initiative on X-ray Fundamental Parameters and their contributions to science and industry. Such data projects are further served by employing complementary wavelength- and energy-dispersive spectroscopic techniques. This combination can provide, among other things, new tabulations of less-intense x-ray lines that need to be identified in x-ray fluorescence investigation of uncharacterized analytes. After delineating the traceability chain for primary x-ray wavelength standards, and NIST efforts to produce standard reference data and materials in particular, this paper posits the new opportunities for x-ray reference data tabulation that modern methods now afford.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to evaluate specific aspects of instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 660c, the fourth generation of this powder diffraction SRM, which is used primarily for calibrating powder diffractometers with respect to line position and line shape for the determination of the instrument profile function (IPF). It is certified with respect to lattice parameter and consists of approximately 6 g of lanthanum hexaboride (LaB6) powder. So that this SRM would be applicable for the neutron diffraction community, the powder was prepared from an isotopically enriched 11B precursor material. The microstructure of the LaB6 powder was engineered specifically to yield a crystallite size above that where size broadening is typically observed and to minimize the crystallographic defects that lead to strain broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the LaB6 powder. Both Type A, statistical, and Type B, systematic, uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.415 682 6 ± 0.000 008 nm (95% confidence).

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to address specific aspects of the performance of X-ray powder diffraction instruments. This report describes SRM 1879b, the third generation of this powder diffraction SRM. SRM 1879b is intended for use in the preparation of calibration standards for the quantitative analyses of cristobalite by X-ray powder diffraction in accordance with National Institute for Occupational Safety and Health (NIOSH) Analytical Method 7500, or equivalent. A unit of SRM 1879b consists of approximately 5 g of cristobalite powder bottled in an argon atmosphere. It is certified with respect to crystalline phase purity, or amorphous phase content, and lattice parameter. Neutron powder diffraction, both time-of-flight and constant wavelength, was used to certify the phase purity using SRM 676a as an internal standard. A NIST-built diffractometer, incorporating many advanced design features was used for certification measurements for lattice parameters.

The densities of 22 large highly perfect silicon single crystals have been measured by hydrostatic weighing in water, yielding an average value of dSi(25 ∘C)=2.329002±(7×10-6) g/cm3. An experimental precision has been achieved which exceeds the accuracy with which the absolute density of water is known. The effect of variations of the water surface tension force on the suspension wire has been mimized by using a 0.001 in. suspension wire coated with platinum black, and by doing a large number of repeated weighings of each crystal.

A Cauchois-type spectrometer utilizing the (203) lattice planes at an oblique angle of 11.53° to the normal to the surface of a quartz transmission crystal recorded the Kα and Kβ spectral lines of six elements from Fe to Ag in the 6–22 keV energy range from a laboratory x-ray source. After deconvolving the natural lifetime widths and the image plate detector broadening from the observed spectral linewidths, the intrinsic crystal resolving power was determined to be 4000 at the lower energies and decreasing to 1000 at the higher energies. Previously, a Si wafer crystal exhibited twice this resolving power when the (331) planes had been used in asymmetric geometry. The investigation of diffraction with this quartz crystal, with a very similar lattice spacing and therefore spectral coverage, was motivated by the larger integrated reflectivity of quartz due to its well-known quasimosaicity upon elastic bending. The measured spectral linewidths were in good agreement with the widths calculated by accounting for various broadening mechanisms, including source size, crystal thickness, crystal height, crystal rocking curve width, geometrical aberrations, and possible spectrometer configuration errors. This is the first, to the best of our knowledge, demonstration of high resolving power achieved by asymmetric diffraction over a wide energy range (6–22 keV) and with detailed comparisons with theoretical broadenings. Based on these results, Cauchois spectrometers employing asymmetric planes of perfect quartz and silicon crystals can be reliably designed and optimized for high-resolution spectroscopy in the >6 keV energy range.

We present newly measured spectra of the X-ray emission of a molybdenum metal anode subject to electron bombardment, using a very high dispersion silicon double-crystal spectrometer. The measurement includes the dipole-allowed KL, KM, and KN emission lines, based on an energy scale traceable to the Système International (SI) definition of the meter with a systematic uncertainty below ΔE/E = 10(−6). The data are presented as parametrized multi-Lorentzian fits to the results, and as supplementary data with the complete spectrum of each line group, corrected for instrumental effects. The MoKL(3) (Kα(1)) line energy was in complete statistical agreement with published measurements, and it showed no asymmetry. Other lines showed varying discrepancies with the literature which lie outside the bounds of probable experimental errors.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to address specific aspects of the performance of X-ray powder diffraction instruments. This report describes SRM 1878b, the third generation of this powder diffraction SRM. SRM 1878b is intended for use in the preparation of calibration standards for the quantitative analyses of α-quartz by X-ray powder diffraction in accordance to National Institute for Occupational Safety and Health Analytical Method 7500, or equivalent. A unit of SRM 1878b consists of approximately 5 g of α-quartz powder bottled in an argon atmosphere. It is certified with respect to crystalline phase purity, or amorphous phase content, and lattice parameter. Neutron powder diffraction, both time of flight and constant wavelength, was used to certify the phase purity using SRM 676a as an internal standard. A NIST-built diffractometer, incorporating many advanced design features was used for certification measurements for lattice parameters.

We present details on the alignment and calibration of a goniometer assembly consisting two stacked, optically encoded, vertical axis rotation stages. A technique for its calibration is presented that utilizes a stable, uncalibrated, third stage to position a mirror in conjunction with a nulling autocollimator. Such a system provides a self-calibrating set of angular stages with absolute accuracy of ±0.1 second of plane angle (k=2 expanded uncertainty) around the full circle, suitable for laboratory application. This calibration technique permits in situ, absolute angular calibration of an operational goniometer assembly that is requisite for fully traceable angle measurement, as the installation of the encoder is known to change its performance from the angular calibration data provided by the manufacturer.