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Thesis Petronela Gotcu 15 ... FINAL.Pdf High temperature thermodynamic studies on the transuranium oxides and their solid solutions Proefschrift ter verkrijging van de graad van doctor aan de Technische Universiteit Delft, op gezag van de Rector Magnificus Prof.ir. K.C.A.M. Luyben, voorzitter van het College voor Promoties, in het openbaar te verdedigen op woensdag 15 juni 2011 om 10.00 uur door Petronela GOTCU-FREIS Magister in de chemie van de Faculteit Chemie van de „Alexandru Ioan Cuza” Universiteit van Iaşi, Roemenië geboren te Iaşi, Roemenië Dit proefschrift is goedgekeurd door de promotoren: Prof.dr. H.Th. Wolterbeek Prof.dr. R.J.M. Konings Samenstelling promotiecommissie: Rector Magnificus, voorzitter Prof.dr. H.Th. Wolterbeek, Technische Universiteit Delft, promotor Prof.dr. R.J.M. Konings, Technische Universiteit Delft, promotor Prof.dr.ir. A. Verkooijen, Technische Universiteit Delft Prof.dr.ir. E. Bruck, Technische Universiteit Delft Prof.dr. K. Hack, RWTH Aachen University, Duitsland Prof.dr. D. Haas, VU Brussels, België Dr. Ch. Guéneau, CEA Saclay, Frankrijk Prof.dr.ir. C. Pappas, Technische Universiteit Delft, reservelid The research described in this thesis was performed within a cooperation of the Institute of Transuranium Elements of the Joint Research Centre (JRC) of the European Commission, P.O. Box 2340, 76125 Karlsruhe, Germany and the Section of Radiation and Isotopes for Health of the Department of Radiation, Radionuclides and Reactors, Faculty of Applied Sciences, Delft University of Technology, Melkeweg 15, 2629 JB Delft, The Netherlands. © 2011 P. Gotcu-Freis and IOS Press All rights reserved. No part of this book may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, without prior permission from the publisher. ISBN 978-1-60750-779-6 Keywords: actinide oxides, americium, heat capacity, high temperature mass spectrometry, Knudsen cell, neptunium, phase diagram, plutonium, thermodynamic modelling, vapour pressure. Published and distributed by IOS Press under the imprint Delft University Press Publisher IOS Press Nieuwe Hemweg 6b 1013 BG Amsterdam The Netherlands tel: +31-20-688 3355 fax: +31-20-687 0019 email: [email protected] www.iospress.nl www.dupress.nl LEGAL NOTICE The publisher is not responsible for the use which might be made of the following information. PRINTED IN THE NETHERLANDS High temperature thermodynamic studies on the transuranium oxides and their solid solutions Contents Contents 1 Introduction ........................................................................................ 1 2 (Solid+gas) equilibrium studies for neptunium dioxide ......................... 9 2.1 Introduction .................................................................................. 10 2.2 Experimental method ................................................................... 11 2.2.1 Sample preparation ................................................................ 11 2.2.2 Mass spectrometric measurements ....................................... 12 2.3. Experimental results and discussion ........................................... 14 2.3.1 Ionisation efficiency curves .................................................... 14 2.3.2 Total and partial vapour pressure above NpO2 ...................... 18 2.3.3 Total pressure from diluted samples ...................................... 22 2.3.4 Thermodynamic evaluation .................................................... 23 2.4 Summary and Conclusions ............................................................ 25 2.5 References .................................................................................... 26 3 The high temperature heat capacity of NpO2 .......................................29 3.1 Introduction .................................................................................. 30 3.2 Experimental work ........................................................................ 31 3.3 Results ........................................................................................... 35 3.4 Discussion ..................................................................................... 38 3.5 References .................................................................................... 40 4 Mass spectrometric studies of the vapour phase in the (Pu+O) system 41 4.1 Introduction .................................................................................. 42 4.2 Samples and experimental method .............................................. 44 4.2.1 Sample preparation ................................................................ 44 4.2.2 Mass spectrometric measurements ....................................... 45 4.3 Experimental results ..................................................................... 51 4.3.1 Measurements of the PuO2-x phase field in vacuum .............. 51 4.3.2 Measurements of the (Pu2O3 - PuO2-x) two-phase field ......... 54 4.3.3 Measurements of the PuO2-x phase field in oxygen ............... 56 4.4 Discussion ..................................................................................... 57 4.4.1 Vapour speciation and vapour pressure ................................ 57 4.4.2 Ionisation and dissociation energies ...................................... 61 4.4.3 Vapour pressure as a function of the O/Pu ratio: comparison to the data by Ohse [12] .................................................................. 62 4.4.4 Comparison to the CALPHAD model for the Pu-O system ..... 64 4.4.5 The enthalpy of formation of PuO2(g) .................................... 66 V Contents 4.5 Summary and Conclusions ............................................................ 68 4.6 References .................................................................................... 69 5 The vaporisation behaviour of americium dioxide by use of mass spectrometry ...................................................................................73 5.1 Introduction .................................................................................. 74 5.2 Samples and experimental method .............................................. 75 5.3 Experimental results ..................................................................... 77 5.3.1 Ionisation efficiency curves .................................................... 77 5.3.2 Total vapour pressure ............................................................. 78 5.3.3 Partial vapour pressure over pure americium oxide sample . 79 5.4 Discussion ..................................................................................... 80 5.5 Summary and Conclusions ............................................................ 84 5.6 References .................................................................................... 85 6 A thermodynamic study of the Pu-Am-O system .................................87 6.1 Introduction .................................................................................. 88 6.2 Mass spectrometric measurements for Pu0.756Am0.244O2-x ........... 89 6.3 Thermodynamic modelling ........................................................... 92 6.3.1 Experimental data ................................................................... 93 6.3.1.1 Am-Pu system ................................................................... 93 6.3.1.2 Am-O system .................................................................... 94 6.3.1.3 Pu-Am-O system ............................................................. 100 6.3.2 Models .................................................................................. 101 6.3.2.1. Pure element and stoichiometric phases ...................... 101 6.3.2.2 Gas .................................................................................. 102 6.3.2.3 Liquid .............................................................................. 102 6.3.2.4 (Pu,Am)O2-x ..................................................................... 104 6.3.2.5 (Pu,Am)2O3 ...................................................................... 106 6.3.2.6 Metallic solid solutions ................................................... 107 6.3.3 Results ................................................................................... 107 6.3.3.1 Am-Pu system ................................................................. 107 6.3.3.2 Am-O system .................................................................. 116 6.3.3.3 Pu-Am-O system ............................................................. 121 6.4 Comparison of the mass spectrometric measurements with the ternary model ................................................................................... 123 6.5 Summary and Conclusions .......................................................... 125 6.6 References .................................................................................. 126 VI Contents 7 Vaporisation of candidate nuclear fuels and targets for transmutation of minor actinides .............................................................................. 129 7.1 Introduction ................................................................................ 130 7.2 Experimental ............................................................................... 131 7.2.1 Mass spectrometry ............................................................... 131 7.2.2 Samples ................................................................................. 132 7.3 Results ......................................................................................... 134 7.3.1 (Pu,Am)O2-x solid
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