This report was prepared as an account of Government sponsored work. Neither the United States, nor the Commission. nor any person acting on behalf of the Commission: A. Makes anywarranty orrepresentation.expressed or implied. with respect to the accu- racy, completeness. or usefulness of the information contained in this report, or that the use of any information, apparatus, method, or process disclosed in this report may not Infringe privately owned rights; or B. Assumes any liabilities with respect to the use of. or for damages resulting from the use of any information, apparatus, method, or proce88 disclosed in this report. ORNL-4350 As used in the above. “person acting on behalf of the Commission’’ includes any em- ployee or contractor of the Commission, or employee of such contractor, to the extent that such employee or contractor of the Commission, or employee of such contractor prepares, disseminates, or provides access to, any information pursuant to his employment or contract with the Commission, or hie employment with such contractor. . Contract No. W-7405-eng-26 METALS AND CERAMICS DIVISION mTELS AND MATERIALS DEVELOPMENT PROGRAM QUARTERLY PROGRESS REPORT FOR PERIOD ENDING SEPTEMBER 30, 1968 Compiled by P. Patriarca W. 0. Harms Edited by D. J. Rucker FEBRUARY 1969 OAK RIDGE NATIONAL ILBORATORY Oak Ridge, Tennessee ,” operated by UNION CARBIDE CORPORATION for the U.S. ATOMIC ENERGY COMMISSION DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency Thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. iii FOREWORD This quarterly progress report describes research and development on nuclear fuels and materials performed at the Oak Ridge National Laboratory for the U.S. Atomic Energy Commission. With several excep- tions, as noted below in the listing of specific programs, the work is sponsored by the Fuels and Materials Branch of the Division of Reactor Development and Technology. Classified aspects of the Nitride Fuels Development activity and work on fuels and materials for isotope heat sources are covered in separate ORNL progress reports. The report is presented in five parts according to AEC Activity titles provided by the Fuels and Materials Branch, RDT. Person Principal Program Title ORNL Division ( s in Charge Investigator(s ) I. Fuels and Claddings Sol-Gel Fast Reactor Metals and Ceramics P. Patriarca A. L. Lotts Fuels Chemical Technology J. L. Scott Reactor R. E. Brooksbank . .I Nitride Fuels Metals and Ceramics W. 0. Harms J. L. Scott Development Reactor H. C. McCurdy Fission-Gas Release Reactor Chemistry 0. Sisman R. M. Carroll and Physical Proper- J. G. Morgan ties of Fuel Mate- rials During Irradiation Zirconium Metallura Metals and Ceramics C. J. McHargue P. L. Rittenhouse 11. Coolants ~ Alkali-Metal Metals and Ceramics W. 0. Harms J. H. DeVan Corrosion Studies Reactor A. P. Litman R. E. MacPherson iv Person Principal Program Title ORNL Division( s) in Charge Investigator( s) 111. Radiation Damage to Structural Materials Behavior of Ref'rac- Reactor Chemistry G. M. Watson G. W. Keilholtz tory Materials Under Irradiation Fast-Neutron Irradia- Reactor Chemistry G. M. Watson G. W. Keilholtz tion Effects on Electrical Insulators* Mechanical Proper- Metals and Ceramics C. J. McHargue J. R. Weir ties Research and LMFBR Cladding and Structural Mate- rials Development** Radiation Effects Solid State D. S. Billington M. S. Wechsler in Alloys and Struc- tural Materials IV. Techniques of Fabrication and Testing ' Tungsten Metallurgy Metals and Ceramics W. 0. Harms H. Inouye .I' W. R. Martin G. M. Slaughter J. 0. Stiegler J. R. Weir Nondestructive Metals and Ceramics W. 0. Harms R. W. McClung Test Development Joining Research Metals and Ceramics G. M. Adamson G. M. Slaughter on Nuclear Materials / Fuel Element Fabri- Metals and Ceramics G. M. Adamson J. V. Cathcart cation Development W. R. Martin R. W. McClung * Sponsored by Reactor Power Systems Branch, Division of Space Nuclear Systems. ** Partially sponsored by Liquid Metals Branch, Division of Reactor Development and Technology. Person Principal Program Title OWL Division( s) in Charge Investigator( s) V. Engineering Properties of Reactor Materials Physical and Mechan- Metals and Ceramics W. 0. Harms H. Inouye ical Metallurgy of R. W. McClung Refractory AUOJGS D. L. McElroy G. M. Slaughter J. R. Weir <- a- vii CONTENTS Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Smary xiii Part I. Fuels and Claddings . . . . . . . . . . . . . . . . . 1. Sol-Gel Fast Reactor Fuels 3 . . . . . . . . . . Preparation of Sol-Gel (U,F’u)02 Fuels 3 . . . . . . . . . . Development of Fabrication Processes 4 . . . . . . . . . . . . . . . . . . . . . Sphere -Pac 4 . . . . . . . . . . . Pelletizing of Sol-Gel (U,Fu)O2 5 . . . . . . . . . . . . . . . . . Capsule Fabrication 8 . . . . . . . . . . . . . . . . Sodium Filling System 9 . . . . . . . . . . . Characterization of (TJ,Fu)02 Fuels 13 . . . . . . . . . . . . . . . . Analytical Chemistry 13 . . . . . . . Manufacture of Standard Samples of U02 14 Thermal Conducti.vi.ty. of. S.ol.-.Ge.l F.as.t . . . . . . . . . Reactor Fuels 18 . . . . . . . . . . . . . . . . . Deformation of U02 20 . . . . . Irradiation Testing of Sol-Gel (U,Pu)O2 Fuels 21 . . . . Uninstrumented Thermal Flux Irradiation Tests 22 . . . . . . . . . . . . . . . ORR Instrumented Tests 25 Transient Testing of Sol-Gel-Derived . . . . . . . . . . . . . . . . . . . (U,Pu)O2 Fuels 29 . . . . . . . . . . . . . Fast Flux Irradiation Tests 31 . . . . . . . . . . . . Irradiation Test Calculations 32 . . . . . . . . . . . . . . . . . . 2. Nitride Fuels Development 33 Synthesis, Fabricat.i.on., .an.d .C.ha.ra.c.te.ri.z.at.io.n. . . . . of Nitride Fuels 34 . . . . . . . . . . . Synthesis and Fabrication of UN 34 . . . . . . . . . . . . . . . Characterization of UN 35 Synthesis, Fabricatio.n,. a.nd. C.ha.ra.ct.er.iz.a.ti.on. . . . . of Mixed Nitrides 37 viii Studies on Synthesis. Fabrication. .an.d .Th.er.mo.dy.na.mi.c . . . . Properties of Carbonitride Fuels 39 . . . . . . Manufacture of UC. UN. and U(C. N) from UO2 39 Studies on Compatibility of Mixed-Nitride and . . . . . . Carbonitride Fuels with LMFBR Cladding Alloys 48 Compatibility of Vanadium Alloys with . . . . . . . . . . . . . . . . . . . . Nitride Fuels 48 . . . . . . . . . . . Fuel-Cladding Thermal Conductance 56 . . . . . . . . . . . Irradiation Testing of Nitride Fuels 62 . . . . . . . . . . . . Model Studies on Nitride Fuel Pins 64 . 3 Fission-Gas Release and Physical Properties of Fuel . . . . . . . . . . . . . . . . . Materials During Irradiation 67 Effect of Fission Density on Release of Fission Gas . . . . . . . . . from Enriched Single-CrystalU02 Spheres 67 Determination of Amount of Nonfission Heating Required . . . . . for In-Reactor Thermal Diffusivity Measurements 67 Effect of Temperature. Fission Density. and Burnup on the Thermal Diffusivity and Fission-Gas . . . . . . . . . . . . . . . . . . . . . . Release of UN 72 Effect of Temperature. Fission Density. and Burnup on the Fission-Gas Release from Sol-Gel . . . . . . . . . . . . . . . (U0.goPu0.20)02 Microspheres 74 Effect of Temperature. Fission Density. and Low . . . . Burnup on Fission-Gas Release from (Uo.75P~o.25)02 76 A Technique for Handling Pu02 Specimens Outside . . . . . . . . . . . . . . . . . . . . . Glove Boxes 76 Fission-Gas Release Studies on Fine-Grained High- . . . . . . . . . . . . . . . Density Spheres of (U. Pu)02 78 . . . . . . . . . . . . . . . . . . . . . . 4 Zirconium Metallurgy 79 . . . . Fabrication and Texture Control of Zirconium Tubing 79 Texture Effects. Texture Development. and Anisotropy . . . . . . . . . . . . . . . . . . . . . . ofproperties 81 Circumferential Texture Variation in Zircaloy . . . . . . . . . . . . . . . . . . . . . . . . Tubing 81 . . . Texture Gradients in Thin-Walled Zircaloy Tubing 82 ix .x Part 11. Coolants . . . . . . . . . . . . . . . . 5. Alkali-Metal Corrosion Studies 8'7 Mass Transfer of Interstitial Impurities Between . . . . . . . . . . . . . . . Vanadium Alloys and Sodium 87 Oxygen Effects on the Compatibility of . . . . . . . . . . . . . . . . . Vanadium and Sodium 8? Interstitial Mass Transport Between Type 300 Series . . . . . . . . Stainless Steels and Vanadium Alloys 91 Interstitial Effects on Mechanical Properties of . . . . . . . . . . . . . . . . . . . Vanadium Alloys 93 Compatibility of Stainless Steel and Insulation in . . . . . . . . . . . . . . . . . . . . . . LMFBR Systems 94 . Effect of Insulation on Oxidation of Stainless Steel 95 - Effect of Sodium on Oxidation of Stainless Steel . . . . . . . . . . . . . . . . . Insulation Couples 100 Corrosion of Refractory Alloys in Lithium, Potassium, . . . . . . . . . . . . . . . . . . . . . . . andsodium 102 Compatibility of Boiling Potassium with Refractory . . . . . . . . . . . . . . . . . . . . . . . Alloys 103 Effect of Oxygen on Compatibility of Refractory . . . . . . . . . . . . . . Metals and Alkali Metals 120 ,. . . . . . Corrosion of Refractory Alloys by Lithium 12'7 Part 111. Radiation Damage to Structural Materials . . . . . . 6. Behavior of Refractory Materials Under. Irradiation 139 Irradiation. D a.m a.g e. t.o .N o.n f.i s.s i.o n.a b.l e. R.e f.r a.c t.o r.y . . . . . . Materials 139 . . . . . . . . . . . . . . Refractory Metal Carbides 139 . . . . . . . . . . . . . . Refractory Metal Nitrides 143 . . . . . . . . . Effects of Irradiation on LMFBR Fuels , 145 . . . . . . . . . Irradiations of Depleted UN-UC Fuel 145 . . '7. Fast-Neutron Irradiation Effects on Electrical Insulators 146 General Survey of Fast-Neutron Effects on Electrical . . . . . . . . . . . . . . . . . . . . . . . Insulators 146 Irradiation of High-Density, Commercial A1203 Products . . . . . . . . . . Considered for Thermionic Insulators 146 . . . . . . . . . . . . . . . . . Irradiations in ETR 146 . . . . . . . . . . . . . . . . Irradiations in EBR-I1 147 . . . . . . . . Irradiations of Metal-Clad A1203 Specimens 14'7 ,