ORNL-1771 - Oak Ridge National Laboratory
ORNL-1771 - Oak Ridge National Laboratory ORNL-1771 - Oak Ridge National Laboratory
in the near future to establish solidus and liquidus re! ation sh i ps. No ternary compounds have been discovered, to date, in the NaF-ZrF,-UF, system. A tentative equilibrium diagram, which shows the general rela- tionships believed to exist in this complex system, is presented in Fig. 5.1. ‘R. J. Sheil and C. J. Barton, ANP QULN. Prog. Rep. June 10, 1954, ORNL-1729, p 42. PERIOD ENDING SEPTEMBER IO, 1954 VISUAL OBSERVATION OF MELTING TEMPERATURES IN THE NaF-UF, SYSTEM M. S. Grim Mater i al s Chem i s try Di vi si on The apparatus for visual observation of melting temperatures, described in the previous quarterly rep~rt,~ was used to observe eleven NaF-UF, mixtures in the composition range 20 to 50 mole % UF,. Liquidus temperatures obtained with this 55
ANP QUARTERLY PROGRESS REPORT apparatus, both from visual observation of crystal- lization and from thermal effects recorded during the course of the vi sua1 observations, were generally a little higher than those indicated by the published diagram for this system.' The data are shown on the partial phase diagram for the NaF-UF, system in Fig. 5.2. A solid circle indicates the tempera- ture at which the composition appeared to be com- pletely solidified. This point could not be de- termined with any degree of certainty with some compositions, uncl the disoppeorunce of the liquid phase wus not always accompanied by B noticeable thermal effect. The liquidus temperatures shown in Fiy. 5.2 seem to indicate that Na,UF, melts con- gruently at 629OC, that is, at a temperature only u few degrees higher than the eutectic temperatures on both sides of the compound. The data also support the results of petrographic studies which indicate that the compound in the 50 mole % UF, region has the approximate composition Na,U,F, rather than NaUF,. A new appnratus has been constructed that will permit some manipulations to be carried out with the fused salts in an inert utnwsphere. It consists essentially of a small dry box, with i-in.-thick 750 700 ~ 600 550 ~ 15 20 25 30 35 40 UF4 hole %) ORNL 922 Fig. 5.2. Por4ial Wase Diagram of the NaF-UF, SyeBcm. 54 Lucite side walls and top, attached to a stainless steel bottom plate which has a &in. length of 2-in.-dia stainless steel pipe welded onto it to serve CIS a furnace core. The pipe is surrounded by resistance coils and insulating tape. The box is equipped with face plates for covering the glove holes so that the box can be partly evacuated before it is filled with inert gas, PHASE REhATlONSHlPS IN UF3-5EARING SYSTEMS C. J. Barton R. J. SheiI L. M. Brntcher A. B. Wilkerson Materials Chemistry Division G. D. White, Metallurgy Division T. N. McVay, Consultant It was assuined in the previous studies* of solu- bility relationships for IJF, in various fluoride mixtures that in the presence of excess metallic uranium or zirconium the uranium present in the fused salt solution WQS trivalent, This assumption seemed justified, since, for the reaction Brewer's tabulation' of standard free energies of formation yields AF" = -16 kcal . In addition, petrographic examination of the melts obtained revealed the presence of red materials tentatively identified as complex compounds of UF,, with green compounds of UF, showing only in traces, if at all. Since these observations were those anticipated and since the petrographic ex- ominations had previously been shown to be very sensitive in detecting compounds of trivalent ura- nium in systems which had been slightly reduced, there seemed to be little reason to believe that the results of such examination might be unreliable. During the past quarter, however, considerable evi- dence ha:, been accumulated by the most accurate wet-chemicol methods yet devised for determining U3+ and U4' in fluoride mixtures which shows that the reduction of UF, by excess uranium metal is not complete at 800°C. While the reduction in *G. M. Watson and C. Ah. Blood, ANP @UT. Prog. Rep. lune IO, 1954, QHNL-1729, p 51. 'L, Brewer et ul., Thenodynarfiic Properties and Eyui- libria at High Temperalures of Uranium Halides, Oxides, Nitrides, urd Carbides, MDDC-1543 (Sept. 20, 1945, rev. Apr. 1, 11947).
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in the near future to establish solidus and liquidus<br />
re! ation sh i ps.<br />
No ternary compounds have been discovered, to<br />
date, in the NaF-ZrF,-UF, system. A tentative<br />
equilibrium diagram, which shows the general rela-<br />
tionships believed to exist in this complex system,<br />
is presented in Fig. 5.1.<br />
‘R. J. Sheil and C. J. Barton, ANP QULN. Prog. Rep.<br />
June 10, 1954, <strong>ORNL</strong>-1729, p 42.<br />
PERIOD ENDING SEPTEMBER IO, 1954<br />
VISUAL OBSERVATION OF MELTING<br />
TEMPERATURES IN THE NaF-UF, SYSTEM<br />
M. S. Grim<br />
Mater i al s Chem i s try Di vi si on<br />
The apparatus for visual observation of melting<br />
temperatures, described in the previous quarterly<br />
rep~rt,~<br />
was used to observe eleven NaF-UF,<br />
mixtures in the composition range 20 to 50 mole %<br />
UF,. Liquidus temperatures obtained with this<br />
55
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