(54b) Assessment of the Homogeneity of an Alumina Powders Mixture Using Rheological Parameters | AIChE

(54b) Assessment of the Homogeneity of an Alumina Powders Mixture Using Rheological Parameters

Authors 

Berthiaux, H., Université de Toulouse
Giraud, M., CEA-Marcoule
This study has been carried out in order to improve the comprehension of powder mixing in the nuclear fuel manufacturing process. Thus, a binary mixture of two Alumina (Al2O3) powders, GE15 and CR6, was used to simulate the oxides powders actually involved in the process. Different mixing technics and parameters were tried and compared in terms of homogeneity of the mixtures produced. The concept of intensity of segregation [1] was used for assessing mixture homogeneity through a sampling protocol and classical statistical analysis tools [2]. One of the difficulties of working with these compounds is that, due to the similarities between CR6 and GE15 powders (same chemical composition, same colour, etc.), the direct measure of the composition of a given sample is not possible. Since homogeneity of a mixture is assessed from the variation of the composition between samples, it is important to find an indirect way to measure the composition of an Alumina powders mixture. Therefore, different correlations between measurable parameters (specific surface area, Sauter diameter, cohesion and flow function coefficient) and the composition of the mixtures were found empirically allowing indirect measurement of the composition of a given sample.

The four studied parameters: specific surface area (, measured by nitrogen adsorption using BET method), Sauter diameter (, measured by laser granulometry, dry transportation with air at 0.1 bar), cohesion and flow function coefficient ( and , measured by FT4 shear test at 9 kPa on a 10 mL cell), were compared in terms of precision, relevance and feasibility.

It appears that the homogeneity assessment methods involving rheological parameters (cohesion and flow function coefficient) show many advantages compared to the other methods. Not only are they the most accurate correlations found but both parameters are measured simultaneously, meaning that it is possible to apply both methods on the same samples while all the tests (N2 adsorption, laser granulometry and FT4) are destructive. Those two methods also allow the estimation of the homogeneity at a more interesting scale (around 7 g of powder), indeed, specific surface area and Sauter diameter methods give a homogeneity at a scale of less than one gram which is not relevant for the end-use properties of the final product.

[1] P. Danckwerts, The definition, measurement and some characteristics of mixtures, Applied scientific research. Section A, 3 (1952) 279-296

[2] S. Massol-Chaudeur, H. Berthiaux, S. Muerza, et J. Dodds, A numerical model to identify the structure of a high-dilution powder mixture, Powder Technol., 128 (2002) 131-138