the Molten Salt Energy Technologies Web Site

ANP PROJECT QUARTERLY PROGRESS REPORT
-
0- 4
B- 5
TABLE 10.5. ANALYSIS OF LOW- APNIUM ZrF, FOR PRODUCTION OPERATION
RATCH
~. COMPO SI TI ON ( %)
.. .. . .
HAFNIUM
NO. Zr F Cl C
43. a 0.01
44. I 0.01
P rep ar at i o n o f My d 1-0 f 1 u o r i PI a& e d
Fuel samples (F. P. Boody, Materials
Chemistry Division). Ten small
samples containing enriched UF, have
been treated in the program for
preparing fuels for the cold critical
test and for radiation-damage tests
in the MTR. The base material was a
mixture of NaF and ZrF, that had been
hydrofluorinated before the cnriched
UF, was added. Samples containing
10.8, 16.5, and 35.0 w t % UF, have
been prepared for the radiation-damage
experiments.
The batches of NaF-ZrF, -IJF, (45 -50 -4
mole %) for the cold critical test
were treated in the same manner as
bat,ches containingnormal UF,. However,
the batches required for radiationdamage
tests were small (10 to 20 g),
and the procedure was modified so
that the HF, H,, and He gases were not
bubbled through the melt but were
applied as an atmosphere.
The melt was contained in either
a nickel or platinum crucible inside
the nickel reactor. The reactor wzs
opened and the sample transfer'red to
a gas-tight glass shipping cont,ainer
in a dry box that had an inert atmoswhere
that wits produced by evacuating
and flushirig with dry helium three
times. A small amount of NaK was
included in the sealed glass shipping
container to ensure the quality of the
inert atmosphere.
The formation of a black crust on
the surface of several of the samples
124
1 0.07
...~ .... I ...... ~
BO RON
1 1 0. 14 50 0.5
0.5
50
I
I
has caused considerable concern.
This crust has been examined petrogr
a p hi c a l l y , s p e c t r o s c o p i c a l l y ,
chemically, and by x-ray diffraction.
The spectroscopic and x-ray diffraction
analyses showed only NaUF5 and NaZrFs
to be present in appreciable quantity;
however, the petrographic microscope
indicat,ed s m a l l amounts of carbon
and UO,. Chemical analyses indicated
0.06 to 0.20% carbon and approximately
0 .2% [JQ,.
Hydroflusrination of ZrO,-N*aF
k!lxtvres (C. M. Blood, R. E. Thoma,
Materials Chemistry Division). Efforts
to determine the optimum conditions
for the smooth and complete hydrofluorination
of NaF-ZrQ, mixtur~ to
NaZrF5 have continued. The successful
results obtained during the previous
quarter' 2, with the hydrofluorination
of small samples (300 to 400 g)
encouraged attempts to treat 1 arger
batches (2 to 3 kg) without the aid
of a mechanical stirrer. Because of
the high temperatures (700 to 900°C)
involved and the pronounced inconvenience
of mechanical stirring
in the presence of HF at this temperaature,
a technique was sought that
required no more agitation than that
provided by gas bubbling through 6 in.
of melt 4 in. in diameter.
Completion of the reaction by
passing HF through a nickel reactor at
(12)F. F. Blankenship, R. E. Thomn, Jr., F. P.
Boody, and C. M. Blood, ANP Quar. Prog. Rep.
Sept. 10, 1952. OWL-1375, p. 91.