Thermophysical Properties of Materials: New Metrology Challenges at LNE to Reduce the Uncertainties

Within the international frameworks of the BIPM CCT-WG9 and the Euramet TC-T, and taking into account the great challenge of sustainable development, LNE as the French national metrology institute (NMI) has been developing in the recent past a unique metrological platform structured around complementary, versatile, and very accurate facilities to measure the main physical and chemical properties of materials. The objective is to address new societal issues and industrial needs. Research, development of reference measurement methods, dissemination of measurements or SI-traceable calibrations, certification of reference materials, and knowledge transfer to industry and society constitute the common cornerstones of the laboratory activities. Beyond the basic activities necessary to strengthen the different metrological scales emerging in force relative to the thermophysical properties of materials, this article aims to describe new developments in progress especially for measuring the radiative properties and the thermal transport properties. Methods and targets for associated uncertainties are also highlighted.     

Ionic liquids as diathermic fluids for solar trough collectors’ technology: A corrosion study

The AISI 304 and AISI 1018 steels (frequently used in solar collectors’ plants) in contact with four different ionic liquids (ILs) suitable as diathermic fluids, were studied. Immersion tests were performed at 220 °C (the working temperature in such plants) for 10 days. The corrosion morphologies of the steels were investigated by scanning electron microscopy coupled with energy dispersive X-ray (EDX) microanalysis and the content of metals in the solution were detected via ICP-OES. The tests showed that the most performing IL is the ethyl-dimethyl-propyl-ammonium-bis(trifluoromethylsulphonyl)imide. The corrosion properties of the two alloys in contact with such IL were investigated by means of Tafel plots and resistance polarization at room temperature in open-to-air vessels.     

Probing the cure of 13C labelled bisphenol A dicyanate ester in carbon fibre reinforced composites using solid state 13C NMR, SEM and FTIR

We report a study of the curing mechanism of ¹³C labelld bisphenol A dicyanate ester in the presence of a electrolytically surface treated XAS carbon fibre using several techniques – solid state ¹³C NMR, scanning electron microscopy (SEM) and diffuse reflectance FTIR. Comparison of the results obtained in pure matrices and solution shows that the resin undergoes the same reaction mechanism in both cases and forms the sym-triazine network structure in the composite. Received: 25 November 1996/Accepted: 23 January 1997     

Role of peripheral vision in the directional control of rapid aiming movements.

This study addresses the question of whether peripheral vision is involved in the control of hand trajectory direction during an aiming task performed at high speed. Ten adult subjects were required to aim at targets in various positions by making a punching movement with their hand. The experimental conditions were varied so that different parts of hand trajectory could be seen in the peripheral field. Two movement times were applied:     

Kinetics of oxide growth through cracks in coatings on 9%Cr steels

A model is described which accounts reasonably for the observed rate of oxide growth through cracks in silica coatings on 9%Cr steels. It is shown that diffusion through the cracks is rate limiting for narrow cracks and that even for wide cracks the metal penetration rate is far less than for an uncoated surface. The model is also extended to the situation where the protective coating is completely surrounded by oxide.     

Imputation through finite Gaussian mixture models

Imputation is a widely used method for handling missing data. It consists in the replacement of missing values with plausible ones. Parametric and nonparametric techniques are generally adopted for modelling incomplete data. Both of them have advantages and drawbacks. Parametric techniques are parsimonious but depend on the model assumed, while nonparametric techniques are more flexible but require a high amount of observations. The use of finite mixture of multivariate Gaussian distributions for handling missing data is proposed. The main reason is that it allows to control the trade-off between parsimony and flexibility. An experimental comparison with the widely used imputation nearest neighbour donor is illustrated.     

Steady-state and dynamic desorption of organic vapor from activated carbon with electrothermal swing adsorption

A new method to achieve steady-state and dynamic-tracking desorption of organic compounds from activated carbon was developed and tested with a bench-scale system. Activated carbon fiber cloth (ACFC) was used to adsorb methyl ethyl ketone (MEK) from air streams. Direct electrothermal heating was then used to desorb the vapor to generate select vapor concentrations at 500 ppmv and 5000 ppmv in air. Dynamic-tracking desorption was also achieved with carefully controlled yet variable vapor concentrations between 250 ppmv and 5000 ppmv, while also allowing the flow rate of the carrier gas to change by 100%. These results were also compared to conditions when recovering MEK as a liquid, and using microwaves as the source of energy to regenerate the adsorbent to provide MEK as a vapor or a liquid.     

Unilateral total lobectomy: is it sufficient surgical treatment for patients with AMES low-risk papillary thyroid carcinoma?

BACKGROUND: Controversy continues regarding the optimal extent of primary thyroid resection in most patients with papillary thyroid carcinoma (PTC), who are at minimal risk of cause-specific mortality (CSM). This study was designed to compare CSM and recurrence rates after either unilateral lobectomy (UL) or bilateral lobar resection (BLR) in patients with PTC considered low risk by AMES criteria. METHODS: Outcome was studied in 1685 patients initially treated during 1940 through 1991 and followed for up to 54 postoperative years (mean, 18 years). One thousand six hundred fifty-six patients (98%) had complete primary tumor resection; 634 (38%) had involvement of regional nodes. One hundred ninety-five patients (12%) had UL; BLR accounted for 1468 (near-total 60%; total thyroidectomy 18%). RESULTS: Thirty-year rates for CSM and distant metastasis were 2% and 3%, respectively. Twenty-year rates for local recurrence and nodal metastasis were 4% and 8%, respectively. There were no significant differences in CSM or distant metastasis rates between UL and BLR (P > .2). After UL, 20-year rates for local recurrence and nodal metastasis were 14% and 19%, significantly higher (P = .0001) than the 2% and 6% rates seen after BLR. CONCLUSIONS: UL was not associated with higher CSM rates, but it was associated with a significantly higher risk of locoregional recurrence. Thus BLR probably represents a preferable initial surgical approach to patients with low-risk PTC.     

Precipitation Coating of Rare-Earth Orthophosphates on Woven Ceramic Fibers—Effect of Rare-Earth Cation on Coating Morphology and Coated Fiber Strength

Monazite (La, Ce, Nd, and GdPO₄) and xenotime (Tb, Dy, and YPO₄) coatings were deposited on woven Nextel^™ 610 and 720 fibers by heterogeneous precipitation from a rare-earth citrate/phosphoric acid precursor. Coating phases and microstructure were characterized by SEM and TEM, and coated fiber strength was measured after heat treatment at 1200°C for 2 h. Coated fiber strength increased with decreasing ionic radius of the rare-earth cation in the monazite and xenotime coatings, and correlates with the high-temperature weight loss and the densification rate of the coatings. Dense coatings with trapped porosity and high weight loss at a high temperature degrade fiber strength the most. The degradation is consistent with stress corrosion driven by thermal residual stress from coating precursor decomposition products trapped in the coating at a high temperature.     

Silver electrodeposition from air and water-stable ionic liquid: An environmentally friendly alternative to cyanide baths

The influence of temperature on the kinetics and the morphology of silver deposits obtained from an air and water-stable ionic liquid (the 1-butyl-3-methyl imidazolium tetrafluoroborate) was studied by means of cyclic voltammetry and chronoamperometry. The nucleation and growth mechanisms have been investigated and the effect of temperature evaluated up to 200 °C. Dense, pure and very thin (about 0.3 μm) silver coatings, with decorative properties, have been obtained on commercial copper electrodes at different temperatures. The characterization of the deposits morphology has been performed by visual investigation and SEM microscopy. Data about thickness were acquired by Calotest® measurements. The deposits result constituted by pure silver as determined by combination of EDX microanalysis and Auger Electron Spectroscopy (AES). The deposition method promises to be a new, environmentally friendly, method for silver electrodeposition which is the reason for the absence of cyanide and volatile toxic solvents in the electroplating bath.