The METAPHIX programme is a collaboration between the Central Research Institute of Electric Power Industry (CRIEPI, Japan) and the Joint Research Centre - Institute for Transuranium Elements (JRC-ITU) of the European Commission dedicated to investigate the safety and effectiveness of a closed nuclear fuel cycle based on Minor Actinides (MA: Np, Am, Cm) separation from spent fuel, incorporation in metal alloy fuel and transmutation in fast reactor.
Progress in Nuclear Energy 94 (2017) 194e201 Contents lists available at ScienceDirect Progress in Nuclear Energy journal homepage: www.elsevier.com/locate/pnucene Characterization of metallic fuel for minor actinides transmutation in fast reactor mier a, K Inagaki b, P Po €ml a, D Papaioannou a, H Ohta b, T Ogata b, L Capriotti a, *, S Bre V.V Rondinella a a b European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O Box 2340, 76125 Karlsruhe, Germany Central Research Institute of Electric Power Industry, 2-11-1 Iwado-kita, Komae, Tokyo 201-8511, Japan a r t i c l e i n f o a b s t r a c t Article history: Received September 2015 Received in revised form March 2016 Accepted April 2016 Available online May 2016 The METAPHIX programme is a collaboration between the Central Research Institute of Electric Power Industry (CRIEPI, Japan) and the Joint Research Centre - Institute for Transuranium Elements (JRC-ITU) of the European Commission dedicated to investigate the safety and effectiveness of a closed nuclear fuel cycle based on Minor Actinides (MA: Np, Am, Cm) separation from spent fuel, incorporation in metal alloy fuel and transmutation in fast reactor Nine Na-bonded experimental pins of metal alloy fuel were prepared at ITU and irradiated at the Phenix reactor (CEA, France) achieving 2.5 at.%, at.% and 10 at.% burn-up Four metal alloy compositions were irradiated: U-Pu-Zr used as fuel reference, U-Pu-Zr ỵ wt.% MA, U-Pu-Zr ỵ wt.% MA ỵ wt.% Rare Earths (RE: Nd, Y, Ce, Gd), and ỵ5 wt.% MA ỵ wt.% RE, respectively RE reproduce the expected output of a pyrometallurgical reprocessing facility Post Irradiation Examination is performed using several techniques, covering properties ranging from the macroscopic morphology of the fuel matrix to the microanalysis of phases and elemental redistribution/segregation The irradiated fuel is characterized by many phases occurring along the fuel radius The fuel underwent large redistribution of the fuel constituents (U, Pu, Zr) and many secondary phases are present with a variety of compositions The distribution of phases in the irradiated fuel containing minor actinides and rare earths is essentially similar to that observed in the basic ternary alloy fuel © 2016 The Authors Published by Elsevier Ltd This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/) Keywords: Metallic fuel Minor actinides Electron probe micro analysis Irradiation experiment Post irradiation examination Introduction Advanced nuclear reactors and closed nuclear fuel cycles are important options to achieve sustainable nuclear energy supplies to satisfy future demands while reducing the long-term radiotoxicity of high level waste (GIF, 2002; GNEP, 2007; Funasaka and Itho, 2007; Haas et al., 2009; JRC-EASAC, 2014) Spent fuel reprocessing and the subsequent recycling of U and Pu as fuel and transmutation of Minor Actinides (MA) Np, Am, Cm in fast reactors are necessary steps to achieve this goal (Yokoo et al., 1996; Inoue et al., 1991; Ohta et al., 2005) Fast reactors brings different advantages compare to thermal reactors in term of transmutation of actinides Hereafter the main reasons are reported from OECD/NEA, (2012): * Corresponding author E-mail address: luca.capriotti1987@gmail.com (L Capriotti) A favourable neutron balance, which allows to introduce MA of any type and in significant amounts, without perturbing the reference performances of the corresponding core without MA A neutron spectrum which allows fissions to dominate captures for all TRUs This feature allows limiting with respect to thermal reactors the build-up of higher mass nuclei, e.g the build-up of 252 Cf during TRU multi-recycle The flexibility to burn or breed fuel, or to be iso-generator (a system that has a zero net production of TRU constituents in the fuel) The possibility to benefit from the favourable characteristics indicated above, whatever the Pu vector, the type of fuel (oxide, metal, nitride, carbide) and the type of coolant (sodium, heavy liquid metal, gas) The METAPHIX programme is a collaboration between the Central Research Institute of Electric Power Industry (CRIEPI, Japan) and the Joint Research Centre-Institute for Transuranium Elements http://dx.doi.org/10.1016/j.pnucene.2016.04.004 0149-1970/© 2016 The Authors Published by Elsevier Ltd This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/) L Capriotti et al / Progress in Nuclear Energy 94 (2017) 194e201 Table Average composition (wt.%) of the fuel alloys as fabricated (impurities content < 0.3 wt.%) El U-Pu-Zr U-Pu-Zr 2MA-2RE U-Pu-Zr 5MA U-Pu-Zr 5MA-5RE U Pu Zr MA Np Am Cm RE Y Ce Nd Gd 71.00 18.93 10.19 0.03 0.03 66.85 19.80 9.46 2.08 1.23 0.67 0.18 1.73 0.12 0.20 1.25 0.16 66.30 19.35 8.97 4.74 2.97 1.45 0.32 e 63.50 19.75 8.19 4.78 3.04 1.52 0.31 3.40 0.31 0.45 2.30 0.32 e 195 (JRC-ITU) of the European Commission with the support of the Commissariat a l'Energie Atomique et aux Energies Alternatives (CEA, France) It is dedicated to the study of the safety and effectiveness of a closed nuclear fuel cycle based on MA separation and irradiation in metallic fuel using fast reactor In this context, three assemblies containing nine Na-bonded experimental pins of metal alloy fuel prepared at ITU (Kurata et al., 1999) were loaded in the nix reactor in 2003 and irradiated at three different burnups, Phe 2.5 at.% (METAPHIX-1), ~7 at.% (METAPHIX-2) and ~10 at.% (METAPHIX-3) Extensive metal fuel irradiation tests were conducted in the USA in the Integral Fast Reactor (IFR) program (Carmack et al., 2009; Chang, 1989; Till and Chang, 1991) both on U-10 wt.%Zr binary alloy fuel and on U-Pu-10 wt.%Zr ternary fuel Of these test pins, the highest burnup achieved for the U-19 wt.%Pu-10 wt.%Zr fuel without pin breach was more than 19 at.% (Crawford et al., 2007) The first irradiation of MA-bearing metal fuel was conducted in the X501 test assembly in EBR-II up to 7.6 at.% burnup (Meyer et al., 2009; Kim et al., 2009) Preliminary post irradiation examinations revealed that the macroscopic behavior in pile of MA-bearing metallic fuel is similar to the basic alloy metallic fuel The main objective of the PIE studies on the irradiated METAPHIX fuel is to study the safety of this concept during irradiation The presence, distribution and behavior of the various phases in the fuel is a key aspect of these investigations The possible effects investigated include abnormal behavior of secondary phases (e.g in terms of thermal stability, fuel-cladding chemical interaction, etc.) The present paper describes some of the recent findings in this campaign of studies In particular, it focuses onto the distribution of phases as evidenced by the PIE This examination is part of a broader effort aimed at confirming the safety of the fuel during irradiation and the achievement of effective transmutation rates Materials and methods Fig Schematic view of the different fuel pins irradiated in PHENIX reactor The top of the fuel pin is approximately at the middle of the PHENIX core Post Irradiation Examination (PIE) is performed at JRC-ITU Nondestructive examinations and fission gas analysis showed that MA-bearing fuel pin behavior during irradiation was in line with that of the base alloy (Papaioannou et al., 2012; Ohta et al., 2011, Rondinella et al., 2010) Destructive examinations, including optical microscopy, scanning electron microscopy (SEM) and electron probe micro analysis (EPMA) are ongoing for METAPHIX-1 and Fig Temperature axial distribution in the metallic fuel alloys at the beginning of irradiation and end of irradiation for the different burn-ups and for fuel centre and periphery (Ohta et al., 2015a,b) 196 L Capriotti et al / Progress in Nuclear Energy 94 (2017) 194e201 Fig Optical microscopy image of the periphery region of the sample, precipitates are visible in dark grey color (pointed by arrows) Fig Optical microscopy macrograph showing a cross-section of a METAPHIX-1 specimen of U-19Pu-10Zr-5MA-5RE, with burnup 2.4 at.% METAPHIX-2 This paper highlights some recent results concerning microstructure, morphology and phase distribution for METAPHIX1 and METAPHIX-2 2.1 Fuel preparation and irradiation experiment characteristics Table describes the average compositions of four different metallic alloys ingots prepared using arc melting process (Kurata et al., 1999): U-19Pu-10Zr used as reference, U-19Pu-10Zr-2MA2RE, U-19Pu-10Zr-5MA-5RE and U-19Pu-10Zr-5MA RE were added to reproduce the output of a pyrometallurgical reprocessing facility Alloy samples of U-Pu-Zr, U-Pu-Zr-MA, and U-Pu-Zr-MA-RE were prepared by arc melting in argon atmosphere The homogenization of the U, U-Pu, or U-Pu-MA alloys was obtained by melting and mixing with molten Zr For U-Pu-Zr-MA-RE alloy samples, metal powders of U-Zr or U-Pu-Zr-MA and RE were blended mechanically before melting (Kurata et al., 1999) The metallic alloys ingots were cast using yttria molds, which are compatible with the molten fuel alloys, and cut into rodlets 20e50 mm long The metallic fuel present a U-Pu-Zr fuel matrix with homogenous dispersion of RE-MA precipitates (Kurata et al., 1999) More detailed information and properties on the as fabricated metallic alloy are reported in Kurata et al., 1999 and Ohta et al., 2011 The metallic fuel alloy ingots were loaded into fuel pins in different configurations, as illustrated in Fig 1, with a total active fuel length of 485 mm The cladding utilized was the alloy 15-15Ti (Seran et al., 1992; Millard et al., 1994; Fissolo et al., 1994) The fuel pins were bonded with Na to optimize the thermal conductivity The irradiation took place in an irradiation capsule placed in the core of the PHENIX reactor up to the different burnup levels Fig Optical microscopy images showing the structure along the radius of a METAPHIX-1 specimen of U-19Pu-10Zr-5MA-5RE, burnup 2.4 at.% Fig Central region of the cross-section shown in Fig 3a) BSE image highlighting the large fission gas bubbles; b) optical microscopy image of precipitates (pointed by arrows) and gas bubbles L Capriotti et al / Progress in Nuclear Energy 94 (2017) 194e201 Fig Optical microscopy images showing the structure along the radius of a METAPHIX-2 specimen of U-19Pu-10Zr-5MA-5RE, with burnup 6.8 at.% Fig Optical microscopy of a METAPHIX-2 specimen showing a macrograph and the radius of U-19Pu-10Zr basic alloy, burnup 6.9 at.% Fig Redistribution of the main fuel components (Pu, Zr, U) in a METAPHIX-2 sample obtained by EPMA (qualitative analysis), (Bremier et al., 2013) 197 198 L Capriotti et al / Progress in Nuclear Energy 94 (2017) 194e201 Irradiation conditions were evaluated in order to predict the temperature conditions at the beginning and end of irradiation by means of the ALFUS code (Ohta et al., 2015a, 2015b) Fig presents the axial temperature calculated for the different burnups and for fuel centre and periphery According to predictions, at the end of the irradiation a high temperature phase, g-phase (Ogata, 2012), should be present in the upper part of METAPHIX-1 fuel pins This phase is observed for temperature above 650 C 2.2 Experimental techniques Standard metallographic procedure was employed Fine grinding of the sample was carried out using diamond paper and alcohol as a lubricant Grinding was followed by polishing with a series of diamond powder suspensions of increasing fineness 45 40 Zr Conc, Wt.% 35 Outer: U,Pu,Zr fuel Outer U,Pu,Zr (Zr rich) Crust Core Fuel I Core Fuel II U-rich Core I Pu-rich Core II 30 25 20 Results and discussion 3.1 Microstructure investigation of U-19Pu-10Zr-5MA-5RE 15 10 100 90 80 U, wt.% 70 60 50 Outer: U,Pu,Zr fuel 40 Outer: U,Pu,Zr (Zr rich) Crust 30 Core Fuel I Core Fuel II U-rich Core I 20 Pu-rich Core II 10 40 30 Pu, wt.% Grinding and polishing were performed using a polishing device specially adapted for operation in a hot cell The fuel samples were examined using a Leica Telatom-3 optical microscope connected to the sample preparation cell by a shielded tunnel, and the sample is transported using a motorized cart The shielded SEM used for analysis of highly radioactive specimens at ITU is a JEOL JSM-6400 The EDX device combined to this SEM equipment used for the characterization described here was SAMx Numerix DXD-X10P; the detector was equipped with a lead collimator The background radiation from the different fuel samples was not negligible; therefore, quantitative evaluation of the results of EDX measurements is considered as not sufficiently accurate; semiquantitative analysis was achieved EPMA was carried out using a state of the art shielded Cameca SX 100 specially shielded and modified to permit the analysis of irradiated nuclear fuels (Walker, 1999) The analysis was performed on a specimen coated with a conducting film of aluminium approximately 20 nm thick to avoid charging effects The standards were also coated at the same time; this removed the necessity for correction for the film 20 10 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 r/r0 Fig 10 Concentration and redistribution profiles of the main fuel constituents along the radius of a METAPHIX-2 sample: (a) Zr, (b) U (c) Pu (Bremier et al., 2013) Figs and present optical microscopy macrographs of a pin cross section and a detailed radius overview of a METAPHIX-1 specimen of U-19Pu-10Zr-5MA-5RE The sample was cut at an axial position of 370 mm from the bottom of the fuel stack, corresponding to a burnup of 2.4 at.% different regions exhibiting various degrees of porosity are visible The central part appears to be separated from the rest of the fuel by a circular crack (or fuel-fuel gap) In this region, large fission gas bubbles, characteristic of the high temperature phase (g-phase) that forms above 650 C (Ogata, 2012; Hofman and Walters, 1994), are present A back scattered electron (BSE) high magnification image of the gas bubbles is shown in Fig 5(a) Second phase precipitates are also visible in this region (Fig 5(b)) and are inferred to be agglomerates of MA and fission products (Ohta et al., 2015a) The intermediate radius region is characterized by a dense phase, considered to be z-phase (Ogata, 2012), together with relatively large voids (Fig 4) In the periphery a highly porous phase and a second phase are present This second phase occurs preferentially around pores and is rich in fission products and rare earths (Ohta et al., 2015a), as shown in Fig Thermochemical and thermal gradients (Hofman and Walters, 1994; Carmack et al., 2009) lead to an increase (compare to nominal value) of the Zr content in the high temperature region The SEM/EDX radial scanning confirmed this redistribution of Zr (and of the others main elements Pu and U) as shown in Ohta et al., 2015a The fuel-cladding gap is already closed at 2.5 at.% burnup and remains closed at higher burnup The fuel alloy is in contact with the cladding owing to fuel swelling and to an increase in the overall volume of fission gas bubbles (Ohta et al., 2015a) In the medium burn-up sample (Fig 7), the high temperature phase is not present and the central region appears as a dense phase where no MA precipitates are visible The central region appears denser compared to the other regions of the fuel exhibiting both intragranular and intergranular fine porosity In the METAPHIX-2 specimen, the fuel-fuel gap is clearly delineated and thicker compare to the METAPHIX-1 sample L Capriotti et al / Progress in Nuclear Energy 94 (2017) 194e201 199 Fig 11 Zr-rich precipitates alloyed with Ru in the fuel central region of a METAPHIX-2 sample Fig 12 Zr-rich quasi-square precipitates at the mid-radius of a METAPHIX-2 sample Fig 13 RE-rich phases in different fuel locations of a METAPHIX-2 sample: a) centre of fuel; b) fuel periphery 3.2 Redistribution of main elements and secondary phases in U19Pu-10Zr basic alloy EPMA was performed on a sample of U-19Pu-10Zr basic alloy from METAPHIX-2, Fig (Bremier et al., 2013) The sample was cut 480 mm from the bottom of fuel stack; this location corresponds to the highest burnup, 6.9 at.% The calculated temperatures are 600 C in the centre of the fuel and 500 C at the fuel-cladding interface The ternary phase diagrams U-Pu-Zr experimentally measured by O'Boyle and Dwight (1970) and calculated by Kurata (2010) were selected in order to identify the different phases of the fuel matrix using the quantitative point analysis performed For the phase identification of the other intermetallic 200 L Capriotti et al / Progress in Nuclear Energy 94 (2017) 194e201 compounds containing RE and noble metals, the binary phase diagrams of Okamoto (1993) were used The distribution of the fuel constituents (U, Pu, Zr) and selected fission products (e.g Nd, Mo, La, Ru, Xe, Cs) was assessed by X-ray mapping Fig shows the qualitative (re)distribution of U, Pu, Zr in the irradiated fuel In Fig 10(a)e(c) the results of the quantitative concentration analysis for the three main fuel constituents are plotted In the centre of the fuel an almost complete depletion of Zr is observed (Fig 10 (b)); moreover, Pu and U (Fig 10(a) and (c)) formed two heterogeneously distributed phases (core phase I and II, respectively) with different U/Pu ratio The almost complete depletion of Zr in this region is the main reason why it was assumed that the temperature at the end of the irradiation was around 600 C; this assumption is not in contradiction with the temperature profile calculated by ALFUS because it is within the 15% uncertainty affecting the irradiation parameters (Ohta et al., 2009) Taking in consideration this aspect, the ternary phase diagram at 595 C from Kurata (2010) identifies as b-U and z phases the distinct phases, core phase I and II No molten phases were visible in the centre of the fuel and according to the U-Pu phase diagram (Okamoto H., 1993), for this range of compositions, the melting temperature is significantly higher than 600 C In the “dense phase” or “crust” stripe at mid-radius (Fig 8), the Zr content is still very low; this region consists of one single phase, which results in z phase, considering the ternary diagram at 550 C From the mid-radius to the periphery of the fuel, the microstructure is very porous U and Pu exhibit symmetric radial profiles; the Pu concentration is decreasing close to the periphery (Fig 10 (c)) and the Zr content in the fuel matrix is close to its nominal, as-prepared value Zr-rich phase is present also in the outer radial region, as shown in Fig 10 (a) (“outer Zr-rich”) Taking in consideration the U-Pu-Zr phase diagrams at 550 C (close to mid-radius) and 500 C (radial periphery of fuel) from O'Boyle and Dwight (1970), the matrix fuel phases are estimated to be a mixture of z, d and a-U; the appearance of the fuel in this region is quite heterogeneous Zr-rich phases or Zr segregations are found throughout the fuel radius Fig 11 shows Zr-rich precipitates found in the central region with a concentration of Zr up to 25 wt.% alloyed with noble metals (Ru, Pd, Rh) Fig 12 shows at mid-radius precipitates appearing in quasi-squares shapes with Zr concentration up to 40 wt.% combined with Ru, U, Rh, Mo, Pd, Pu in different quantities Zr-rich precipitates are found also in other studies such as in D.D Keiser, 2012 RE-rich phases, incorporating also noble metals, are observed at different radial locations; in Fig 13 lanthanum precipitate are shown at different locations, in the centre region (Fig 13 (a)) and at the fuel periphery (Fig 13 (b)) From the ratio between RE and noble metals these precipitates are inferred to be of two kinds: RE7(Pd,Rh)3, found throughout the fuel, and RE3(Pd,Rh)2 found only at the radial periphery These RE-rich precipitates are well studied in literature and of concern for the integrity of the cladding (Kim et al., 2009; Carmack et al., 2009) Conclusion Destructive post irradiation examinations were performed on low and medium burn up METAPHIX fuel pins The morphology, composition and distribution of fuel matrix and secondary phases were characterized by optical and scanning electron microscopy and by electron probe micro-analysis The irradiated fuel is characterized by many phases occurring along the fuel radius The distribution of phases in the irradiated fuel containing minor actinides and rare earths is essentially similar to that observed in the basic ternary alloy fuel (Ogata, 2012; Hofman and Walters, 1994) In the sample exhibiting a g-phase zone (i.e achieving higher irradiation temperature) some large precipitates, estimated to be inclusions of MA and RE, are observed Second phases are present also in the lower temperature region at the radial periphery of the fuel EPMA analysis was performed on U-Pu-Zr fuel irradiated to at.% burnup, providing more detailed insight in the complex configuration of irradiated ternary alloy fuel The redistribution behavior of the fuel constituents (U, Pu, Zr) is in line with findings reported in the literature, and many secondary phases are present with a variety of compositions PIE performed so far confirms a substantially positive irradiation behavior of MA-containing alloy fuel, in line with what is known about U-Pu-Zr irradiation behavior Ongoing and planned investigation campaigns will extend the range of compositions and burnup levels analyzed with the aim of obtaining a complete picture to assess the irradiation behavior of ternary alloy fuel containing minor actinides The outcome of the post-irradiation examination studies will be integrated with the ongoing experimental and modeling activities carried out in the METAPHIX project to assess the overall safety and performance of this closed fuel cycle concept Acknowledgments Important contributions to the PIE were provided by R Nasyrow, R Hasnaoui, R Gretter, G Paperini, (JRC-ITU); many other colleagues in JRC-ITU 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Ogata, T., 2013 Electron microprobe examination of metallic fuel for minor actinides transmutation in fast reactor In: Proc ANS Winter Conf Nov 10e14, Washington, DC, USA Carmack, W.J., Porter,... Rondinella, V.V., Glatz, J.P., 2009 Postirradation examination of fast reactor metal fuels containing minor actinides - fission gas release and metallography of 2.5 at.% burnup fuels In: Proceedings... effectiveness of a closed nuclear fuel cycle based on MA separation and irradiation in metallic fuel using fast reactor In this context, three assemblies containing nine Na-bonded experimental pins of metal