A new single crystal from isotopically enriched silicon was used to determine the Avogadro constant N A by the x-ray-crystal density method. The new crystal, named Si28-23Pr11, has a higher enrichment than the former 'AVO28' crystal allowing a smaller uncertainty of the molar mass determination. Again, two 1 kg spheres were manufactured from this crystal. The crystal and the spheres were measured with improved and new methods. One sphere, Si28kg01a, was measured at NMIJ and PTB with very consistent results. The other sphere, Si28kg01b, was measured only at PTB and yielded nearly the same Avogadro constant value. The mean result for both 1 kg spheres is N A = 6.022 140 526(70) × 10 23 mol −1 with a relative standard uncertainty of 1.2 × 10 −8 . This value deviates from the Avogadro value published in 2015 for the AVO28 crystal by about 3.9(2.1) × 10 −8 . Possible reasons for this difference are discussed and additional measurements are proposed.
For the quantitative surface characterization of a monocrystalline silicon sphere, PTB has constructed and put into operation an analytical instrument, which combines x-ray fluorescence and x-ray photoelectron spectroscopy techniques. The main objective of this novel instrument is the characterization of the oxide layer and unintentional contaminations, e.g. from hydrocarbons. It is equipped with a ball manipulator allowing measurements at each point on the surface of ball-shaped samples with a diameter of about 93.7 mm. Monocrystalline silicon spheres with this diameter allow a realization of the SI base unit of mass.
The new definition of the SI kilogram requires new methods of realizing this unit. The X-ray crystal density method is a primary realization method and uses silicon spheres. The spheres get cleaned before each measurement, in order to remove surface contaminations and thus reduce their uncertainty contribution to the realization. Therefore, cleaning is an inherent part of the realization and dissemination of the kilogram. A cleaning method for silicon spheres is investigated, concerning its suitability as a part of the realization of the redefined kilogram. Six silicon spheres were used to determine the repeatability of the established cleaning method. Measurements of the spheres' mass and the quantification of their surface layer mass after cleaning were carried out in several cycles resulting in 29 mass and surface measurements. The repeatability of the cleaning method applied shows a standard deviation in the order of two micrograms for both the mass and the surface layer. The cleaning method therefore sufficiently fulfils these requirements.
<p class="Abstract">To achieve a new kilogram definition using the X-ray crystal density method, the Center for Measurement Standards, Industrial Technology Research Institute in Taiwan has established the combined XRF (X-ray fluorescence)/XPS (X-ray photoelectron spectroscopy) surface analysis system for the quantitative surface-layer analysis of Si spheres. The surface layer of a Si sphere is composed primarily of an oxide layer, carbonaceous contamination and physisorbed/chemisorbed water. This newly combined instrument has been implemented to measure the XRF for the direct determination of the mass deposition of oxygen (ng/cm<sup>2</sup>) with a calibrated silicon drift detector and the XPS for the ratio between the elements (O, Si, C) and composition identification. These two complementary methods of X-ray metrology allow an accurate determination of the surface-layer mass of the Si sphere. In this paper, the construction of a combined XRF/XPS surface-analysis system is reported, including the surface characterisation method, the assembly of parts of the load-lock chamber and ultra-high-vacuum analysis chamber, the vacuum-system design, hardware integration and the intended research on surface-layer measurement. It is anticipated that the measured surface-layer mass will be combined with the core mass of the Si sphere.</p>
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