METALS Aid CERAMICS DIVISION
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-s-- r . Z Ls> > ORNL-4870 METALS aid CERAMICS DIVISION Annual Progress Report Period Ending June 30, 1973 "1 BLANK PAGE t Printed in the Untied States c* Amtfitt. Available from Nation*) Technical information Service U.S. Department of Commerce 5285 Port Royal Road. Springfield, Virginia 22151 Price: °rtnwd Copy $5.45; Micro!*!* S0.9S • ~ • Thit report was prepared as an account of work sponsored by the United Statas Government. Neither the United Statas nor the United States Atomic Energy Commission, nor any of tfc*ir employees, nor any of their contractors, subcontractors, or their employees, rnakat afty 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 m use would not infringe privately owned rights. ORNL-4870 UC 25 - Materials Contract No. W-74C5-«ng-26 METALS ANO CER'«MICS DIVISION ANNUAL PROGRESS REPORT for Period Endtnf June 30.1973 j. H Frye, Jr., Director* J. E. Cunninohem. Associate Director G. M. Adamson. Jr. C. J. McHar«uc P Patriarca i. R. Weir. Jr.* Compiled and Edited by Sigfred Petef too 'Rtwid June 30.1973. preawtt Uwwerutv o* fN©w Owieon Director. -NOTlCI OCTOBER 1973 OAK RlOGE NATIONAL LABORATORY O* R«ie*. Ttmnw 37830 optr»t«dbv UNION CARBIDE CORPORATION for th« U S ATOMIC ENERGY COMMISSI 0\ amim Reports prtviously issued in this series are as follows: ORNL 28 Period Ending March 1, 1948 ORNL 69 Period Ending May 31. 1948 ORNL407 Period Ending July 31. 1949 ORNL 511 Period Ending October 31, 1949 ORNL 583 Period Ending January 31, 1950 ORNL 754 Period Ending April 30. 1950 ORNL 827 Period Ending July 31. 1950 ORNL QiQ Period Ending October 31. 1350 ORNLC87 Period Ending January 31. 1951 ORNL 1033 Period Ending April 30, 1951 ORNL 1108 Period Ending July 31. 1951 ORNL -1161 Period Ending October 31. 1951 OANL-1367 Period Ending January 31. 1952 ORNL 1302 Period Ending April 30. 1952 ORNL 1366 Period Ending July 31. 1952 ORNL 1437 Period Ending October 31. 1952 ORNL 1503 Period Ending January 31. 1953 ORNL-1551 Period Ending April 10.1953 ORNL 1625 Period Ending October 10. 1953 ORNL 1727 Period Ending April 10. 1954 ORNL 1675 Period Ending October 10. 1954 ORNL 1911 Period Ending April 10.1955 ORNL 1938 Period Ending October ;0.1955 ORNL 2080 Period Ending April 10. 1956 ORNL 2217 Period Ending October 10. 1956 ORNL-24>* Period Ending October 10, 1957 ORNL 2632 Period Ending October 10. 1956 ORNL 2839 Period Ending September 1,1959 ORNL 2988 Period Ending July 1.1960 ORNL31A0 Period Ending May 31. 1961 ORNL 3313 Period Ending May 31. 1962 ORNL 3470 Period Ending May 31.1963 ORNL 3670 Per 3d Ending June 30. 1964 ORNL 3870 Period Ending June 30. 1965 ORNL 3970 Period Ending June 30. 1966 ORNL 4170 Period Ending June 30. 1967 ORNL 4370 Period Ending June 30. 1968 ORNL 4470 Period Ending June 30. 1969 ORNL 4570 Period Ending June 30. 1970 ORNL 4770 Period Ending June 30. 1971 ORNL 4820 Period Ending June 30. 1972 Contents FOREWORD ix SUMMARY xi PARTI. FUNDAMENTAL PROGRAMS 1. CRYSTAL PHYSICS 1 Metal Oxide-Metal Binary and Ternary Eutectics 1 Growth of Ternary Metal-Metai Oxide Eutectics 2 Eutectk Solidification in Binary and Ternary Metal-Metal Oxide Systems 2 Crystal Growth of Oxides by CzochraJski and Edge-Defined Film-Fed Methods 2 Bridgman-Stockbarger Growth of Single-Crystal BaF2 and BaF3 Doped with 1 at. % La 2 SrClj Crystal Containing " * Es 2 2 Electron Paramagnetic Resonance of **Bk** in Th03 Single Crystals 3 Zero-Field Splittings of Gd* andCm* inCeO, artdTh02 3 HydrothermaJ Studies of Quart/ 3 2. DEFORMATION OF CRYSTALLINE SOLIDS 4 The Nature of the Limitations or'Second-Law Determinations of Solution Thermodynamics 4 A Computer Program for the Reduction of Diffuse X-Ray Data from Solid Solutions 4 Fracture Mechanism in Precipitation-Hardened BCC Alloys 4 3. DIFFUSION IN SOUDS 7 Rele -ance of Tracer Diffusion Experiments to Problems in Nuclear Systems 7 Cation Self-Diffusion in Rutile 7 Effect of Dislocations on Self-Diffusion of Uranium in UO} Single Crystals , 7 Diffusion Under High Pressures 8 Tracer Self-Diffusion in Fe 17 wt %Cr 12 wt % Ni Austenitic Alloy 8 The Volume Diffusion of Carbon in F< 17 wt % Cr- 12 wt % Ni Austeniiic Alloy 8 Thermotransporf of Cadmium and Thallium in Sodium and Potassium Chlorides 9 Binary Intrinsic Diffusk** and Interdtffusion in Vanadium-Titanium Solid Solutions 9 4. ELECTRON MICROSCOPY , 10 Radiation-Induced Strengthening and Embrittlemem in Aluminum 10 iii IV Reply to "Comments on "On the Question of Void Formation in Neutron Irradiated Zirconium' " 10 Ei'ft :t of Silicon on Void Formation in Aluminum 11 Eff< cts of Solute Interstitial Elements on Swelling of Si^inkrss Steel 11 A High-Voltage Electron Microscope Study of the Effects of Preinjected Helium on Electron Damage in Aluminum 11 Electron Irradiation Damage in Titanium 12 Effect of Purity on Loop Formation in Aluminum and Nickel 12 Detect Structure of Neutron-irradiated Boron Carbide 12 Nucleation of Voids in Solids Containing Excess Vacancies, lnterstitials, and Helium Atoms 12 Reply to Comment on Some Calculations of Vacancy Characteristics in Substitutional Alloys 13 Nearest Neighbor Pair Models for Solution 13 Reply to Comments on *The Energy Stored in Porycrystalline Copper Deformed at Room Temperature" - More Details of the Single-Step Isoperibot Deformation Calorimeter 13 The Efficiency of Energy Storage During Plastic Deformation of he>;als 13 Creep Properties ot'CVD Tungsten 14 5. FUNDAMENTAL CERAMICS RESEARCH 15 Observation of Lattice and Giatn Boundary Dislocations in U02 Deformed at High Temperatures 15 Optical Absorption i.i Deformed CaF2 15 Redox Equilibria in Molten Uranium Dioxide 15 Synthesis. Structure, and Properties of Titaniumdi) Tetracrdoroaluminate 16 Electronic Absorption Spectra of P!atinum(II) Centers in Liquid Alkali Metal Chlorides 16 6. FUNDAMENTAL PHYSICAL METALLURGY 17 Phase Transformations in U-Nb-Zr and U-Tt Alloys 17 Texture Inhomogeneities in Cold-Rolled Niobium 17 Dispersion Hardening of Aluminum 17 Structural Effects on Radiation Damage 18 7. PHYSICAL PROPERTY RESEARCH 19 Apparatus Development 19 improved Linear Heat Flow Apparatus 19 Electrical Resistivity Measurements 19 Computerized Data Acquisition 19 Heat Flow Analysts 20 Transport in Metals 20 Aluminum 20 Platinum aid Lead 21 Chromium ? I Lattice Heat Transport in Alkali Halides 21 Coefficient of Thermal Expansion of Nickel 21 Applied Research 21 8. SUPERCONDUCTING MATERIALS 23 Measurement of Critical Bulk and Surface Current Densities in Type II Superconductor* in the Mixed State 23 V Effects of Interstitial Ox.'gen on the Superconductivity of Niobium 23 Annealing. Long-k*nge Order, and Supcrconducnnc Transition Temperature in the V,Ga A-i5 Compound 24 A Low-Temperature X-Ray lnvestv - ion of Technetium and the Tc-Mo A-15 Compound 24 Critical Current Densities in Sputter-Deposited Nb-Al-Ge 24 Thermodynamic Properties of Zirconium-Cadmium and Certain Other Solid Solutions 24 Superconducting Materials Technology for Power Transmission 25 9. SURFACE PHENOMENA 26 Oxidation of Uranium-Base Alloys 26 The Mechanical Properties of T^o Uranium Alleys sr.d Their Role in :hc Oxidation of the Alloys 26 The Oxidation of U-14 at. % Zx Between 700 and 900CC 26 Oxidation of Refractory Metal Alloys 26 Diffusion Studies 27 >0. TriEORETKTAL RESEARCH 28 KKR Band Structure Calculations for Complex Crystals 28 Density of States Expressed as Continued Fraction of Matrices: Application to Disordered Systems 28 Self-Consistent Cluster Theories of Disordered Alloys 2fc Problems in Strong Scattering Binary Alloy* 28 Charged Impurity Drift and Dispersion in Di*crete Media 29 Auger Catalog Calculated Transition Energies Listed by Energy and Element 29 Diffusion of Vacancies Near Faulted Dislocation Loops in Aluminum 29 Electronic States o( Multilayer Graphite 29 Observation of High-Energy Excited States in Graphite 29 A Combined Korrinfa-Kohn-Rostoker- Discrete Variational Method for the Electronic Structure of Crystals and Molecules with General Potentials 30 A Combined Multiple-Scattering-Discrete-Variationa! Method for the Molecular Ouster Problem 50 Effects of Thermcelastic Properties on Void Formation in Hexagonal Metals 30 Equilibrium Shape of a Prismatic Dislocation Loop 31 II. X-RAY DIP FRACTION 32 Routine Analyses 32 Lattice Expansions of Boron Carbides 32 Crystal Structure of a Hypostoichiometric Boron Carbide 33 Models of the 7* St ucture in Uranium-Base BCC Alloys 33 The Short-Range Structure of Titanium and Zirconium BCC Solid Solutions 34 Thermally Excited Fc-bidden Reflections 34 Structural and Dynamical Properties of Neutron-Irradiated Quartz and Noncrystalltne SiOj 34 Optimization of the Kratky Small-Angle X-Ray Scattering Collimation System Parameters , 35 Inelastic Resonance Emission o( X Rays: Anomalous Scattering Associated with Anomalous Dispersion 35 VI Strengthening and Fracture of Ta. Nb. Mo. and W Binary Solid Solutions with Short-Range Order 35 Development of High-Sensitivity X-Ray Fluorescence for Analysis of Trace Elements 36 Short-Range Order with Large Atomic Displacements in Niobium-Vanadium Alloys 36 PART II. SPACE POWER TECHNOLOGY 12. HIGH-TEMPERATURE ALLOYS FOR ISOTOPiC HEAT SOURCES 37 Development of »ndium-Base Alloys 37 Development of Platinum-Base Alloys 37 Iridium Purification and Scrap Recycle 38 Special Problems and Consulting 38 13. CURIUM-244 COMPATIBILITY TESTING 39 14. IRIDIUM FABRICATION 41 Iridium Sheet Development 41 Preparation of Compacts for Melting 41 Electron-Beam Melting and Casting 41 Sheet Roiling 42 Iridium Purification 43 15. PHYSICAL METALLURGY OF HEAT-SOURCE CONTAINMENT MATERIALS 45 Structure and Medianical Properties of Internally Oxidized Ta-8% W-2% Hf (T-l 11) Alloy 45 Low-Pressure Oxidation and Tensile Pr->perties of Oxygen-Contaminated T-l 11 *5 Mechanical Properties and Interstitial Contamination in a Molybdenum-Base Alloy, TZM 46 Effects of Exposure to Oxygen and Graphite on the Physical and Mechanical Properties of Iridium and Iridium Afloys 46 Special Problems and Consulting 46 16.