| Copyright note | This is an author-created, un-copyedited version of an article accepted for publication in Metrologia. IOP Publishing Ltd is not responsible for any errors or omissions in this version of the manuscript or any version derived from it. The definitive publisher-authenticated version is available online at 10.1088/0026-1394/48/2/S10 |
|---|---|
| Title | Surface layer determination for the Si spheres of the Avogadro project  |
| Author(s) | , , , , , , , , and |
| Journal | Metrologia |
| Year, Month | 2011, March |
| Volume | 48 |
| Issue | 2 |
| DOI | 10.1088/0026-1394/48/2/S10 |
| Language | English |
| Keywords | surface layer, XPS measurements, XRF measurements. |
| Abstract | For the accurate determination of the Avogadro constant, two 28Si spheres were produced, whose macroscopic density, in addition to other values, must be determined. To make a contribution to the new definition of the kilogram, a relative standard uncertainty of less than 2 × 10-8 has to be achieved. Each silicon surface is covered by a surface layer (SL). Consequently, correction parameters for the SL are determined to be applied to the mass and volume determination of the enriched spheres. With the use of a large set of surface analysing techniques, the structure of the SL is investigated. An unexpected metallic contamination existing on the sphere surface enlarges the uncertainty contribution of the correction parameters above the originally targeted value of 1 × 10-8. In the framework of this investigation this new obstacle is resolved in two ways. A new combination of analytical methods is applied to measure the SL mass mSL and the thickness dSL, including this new contamination, with an uncertainty of u(mSL) = 14.5 µg and 14.4 µg, respectively, and u(dSL) = 0.33 nm and 0.32 nm for the 28Si spheres AVO28-S5 and AVO28-S8, respectively. In the second part of the work, the chemical composition of these metallic contaminations is found to be Cu, Ni and Zn silicide compounds. For the removal of this contamination, a special procedure is developed, tested and applied to the spheres to produce the originally expected surface structure on the spheres. After the application of this new procedure the use of x-ray reflectometry directly at the spheres will be possible. It is expected to reduce the uncertainty contribution due to the SL down to 1 × 10-8. |
| Project title (JRP) | T1.J1.2: NAH: Avogadro and molar Planck constants for the redefinition of the kilogram |
| Funding programme | iMERA-Plus: Call 2007 SI and Fundamental Metrology |