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A pilot study for the thickness measurement of HfO2 films was performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The aim of this pilot study was to ensure the equivalency in the measurement capability of national metrology institutes for the thickness measurement of HfO2 films. In this pilot study, the thicknesses of six HfO2 films with nominal thickness from 1 nm to 4 nm were measured by X-ray Photoelectron Spectroscopy (XPS), X-ray Reflectometry(XRR), X-ray Fluorescence Analysis (XRF), Transmission Electron Spectroscopy (TEM), Spectroscopic Ellipsometry (SE) and Rutherford Backscattering Spectrometry (RBS). The reference thicknesses were determined by mutual calibration of a zero-offset method (Medium Energy Ion Scattering Spectroscopy (MEIS) of KRISS) and a method traceable to the length unit (the average thicknesses of three XRR data except the thinnest film). These reference thicknesses are traceable to the length unit because they are based on the traceability of XRR. For the thickness measurement by XPS, the effective attenuation length of Hf 4f electrons was determined. In the cases of XRR and TEM, the offset values were determined from a linear fitting between the reference thicknesses and the individual data by XRR and TEM. The amount of substance of HfO2, expressed as thickness of HfO2 films (in both linear and areal density units), was found to be a good subject for a CCQM key comparison.
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The final report has been peer-reviewed and approved for publication by the CCQM.
The lead authors failed to name two collaborators as co-authors. The authors listed should include:
Miss Claudia L. Compean-Gonzalez (ORCID:
0000-0002-2367-8450) and Dr. Giacomo Ceccone (ORCID:
0000-0003-4637-0771).
These co-authors participated in VAMAS project A27, provided data that were analyzed and presented in this publication (and supporting information), and reviewed the manuscript before submission.
We report the results of a Versailles Project on Advanced Materials and Standards interlaboratory study on the intensity scale calibration of x-ray photoelectron spectrometers using low-density polyethylene (LDPE) as an alternative material to gold, silver, and copper. An improved set of LDPE reference spectra, corrected for different instrument geometries using a quartz-monochromated Al Kα x-ray source, was developed using data provided by participants in this study. Using
these new reference spectra, a transmission function was calculated for each dataset that participants provided. When compared to a similar calibration procedure using the NPL reference spectra for gold, the LDPE intensity calibration method achieves an absolute offset of ∼3.0% and a systematic deviation of ±6.5% on average across all participants. For spectra recorded at high pass energies (≥90 eV), values of absolute offset and systematic deviation are ∼5.8% and ±5.7%, respectively, whereas for spectra collected at lower pass energies (<90 eV), values of absolute offset and systematic deviation are ∼4.9% and ±8.8%, respectively; low pass energy spectra perform worse than the global average, in terms of systematic deviations, due to diminished count rates and signal-to-noise ratio. Differences in absolute offset are attributed to the surface roughness of the LDPE induced by sample preparation. We further assess the usability of LDPE as a secondary reference material and comment on its performance in the presence of issues such as variable dark noise, x-ray warm up times, inaccuracy at low count rates, and underlying spectrometer problems. In response to participant feedback and the results of the study, we provide an updated LDPE intensity calibration protocol to address the issues highlighted in the interlaboratory study. We also comment on the lack of implementation of a consistent and traceable intensity calibration method across the community of x-ray photoelectron spectroscopy (XPS) users and, therefore, propose a route to achieving this with the assistance of instrument manufacturers, metrology laboratories, and experts leading to an international standard for XPS intensity scale calibration.
Three high-strength Nb-,.Ti- and Ti+ V-bearing S690QL steels were welded to investigate and compare the effects of microalloy addition on heat-affected zone (HAZ) toughness. Charpy V notch impact tests from three microalloyed welds under different cooling rates have been performed. Fractographic examination shows that several factors, including large-sized grain, upper bainite or hard second phase, interact to determine brittle fracture and impaired toughness in Nb-bearing weld with high heat input. In contrast to this reduced toughness, Ti-bearing welds exhibits satisfied toughness regardless of at fast or slow cooling. This is attributed to its limited austenite grain and refines favorable intragranular acicular ferrite structure. Moreover, in the case of such refined structure as matrix, TiN particles are found to be irrelevant to the facture process. The crystallographic results also confirm that high-angle boundaries between fine ferrites plates provide effective barriers for crack propagation and contribute to improved toughness.
The numerical simulations of high power laser keyhole welding at different welding positions are performed by using Volume-Of-Fluid (VOF) method. The main material is SS400. The multi-physics phenomenon is considered using several models, such as the heat flux of Gaussian heat source, the recoil pressure with Clausisus-Clapeyron equation, the Marangoni flow considering temperature gradient, the buoyancy force with Boussinesq approximation, the additional shear stress and heat source due to metallic vapor ejected through keyhole entrance, the bubble formation assumed as adiabatic bubble, and the multiple-reflection by solving proper discriminant, are used. To analyze the fluid flow pattern, the concept of streamline formed by reconstructing the value of the velocity vector is applied.
Partial and full penetration cases at different welding positions are considered. The welding position seems to have only a minor influence on bead formation characteristics in both cases. This is probably due to the fact that the recoil pressure has a major influence when compared to other driving forces. The flow characteristics and fluid velocity in weld pool are analyzed to compare the gravity direction effect at different welding positions. It is observed that the clockwise flow pattern is mainly formed by the recoil pressure on the keyhole surface in the case of partial penetration. The laser energy can't maintain the whole weld pool when the weld pool size becomes too large. And then the solidification starts from the middle part of weld pool and a necked weld pool shape is formed. In the full penetration welding, the weld pool flow patterns are affected by the leakage of laser power through the full penetration keyhole and also by surface tension. Furthermore, the numerical simulation of full penetration welding with AISI316L is also performed to analyze the effect of material properties. The weld bead shapes obtained by simulations were compared with the corresponding experimental results to confirm the validity of the process models adopted and the CFD simulation tool.