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ORNL-1965.txt
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AR
3 4456 0360719 4
- M e R 8 Y i
CENTRAL RESEARCH LIBRARY
DOCUMENT COLLECTION
i
i
F LIBRARY LOAN COPY
'f
DO NOT TRANSFER TO ANOTHER PERSON
If you wish someone else to see this document, ."
send in name with document and the library will
arrange a loan.
ORNL-1965
This document consists of 56 pages.
Copy}/f of 232 copies. Series A,
Contract No. W-7405-eng«26
SOLID STATE DIVISION
A FLUORIDE FUEL IN-PILE LOOP EXPERIMENT
O. Sisman, W. E. Brundage, and W. W. Parkinson
Work Done by
C. D. Baumann W. W. Parkinson
W. E. Brundage O. Sisman
R. M. Carroll F. M. Blacksher
J. G. Morgan C. Ellis
M. T. Morgan J. R. Duckworth
A. S. Olson
DATE ISSUED
JAN 151357
OAK RIDGE NATIONAL LABORATORY
Operated by
UNION CARBIDE NUCLEAR COMPANY
A Division of Union Corbide and Carbon Cerporation
Post Office Box X
Qck Ridge, Tennessee
MARTIN MAR STEMS LIBRARIE
AR
3 4456 0360719 Y
VNG ARWN~
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OUEPIMPMEOAOMPMME="TNY
AU E I AOVIEMIO—ATIMOPXRXIOPZIIC®D
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MMEONEE-PPIMEME-POrEMOrE-MAVODE-ODOIPNEZOEOMMOZIOD
INTERNAL DISTRIBUTION
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ORNL-1965
C-84 — Reactors-Special Features of Aircraft Reoctors
CAMEOPOECOPMAIPIZPIICPRAIECPOELMACIPPOMECMENDDD L
D= mMmTTnNIx=x
Si
TEODCrrITENEMET<ADPOONZOD >
omI» O T V-
. ane
. Lindaver
Livingston
. Lyon
. Maienschein
. Manly
. Mann
. Mann
. McDonald
. McQuilkin
. Meghreblian
. Milford
Miller
. Moore
. Morgan
. Morgan
Murphy
. Murray (Y-12)
. Nelson
Nessle
. Oliver
. Overholser
. Parkinson
atriarca
. Peelle
. Perry
. Pigg
. Poppendiek
. Reyling
. Richt
. Robinson
. Savage
. Savolainen
. Schultheiss
. Shipley
. Simon
. Si
sman
tes
Skinner
. Smith
. Snell
. Susano
. Swartout
. Taylor
. Thoma
. Trauger
CONTENTS
A B ST R A C T ettt es v e st st asbe s et aan e e este st e st hsbassbs St ees en et en e S a st enn e b s A s e e b e R e e e e e ra e e 1
INTRODUGCTION e ettt et oo e eeee e et estestestsetessesabessansseese saseseaeaeseeeeeasassubasoRessa e s e s b e sa e s Ren e b e ab e s s s eneabasbes bt sbean et ne 1
SUMMARY oottt ettt e e e e et ebetaees s e st ebeeas et e s araas e st aseee e seemteateatbebesas e b b e SR e on s Sensae eRe L Ra et et e st st 2
DESIGN ottt te ettt ee et e st eeesebesa b e ssesae e basseseaestessesnaese s s e beb bbb e s b e R Ee e S AR SRR e ST e Ae RS e Re e Rt e nA e E e e 3
GOVEIMING FACTOFS ittt bbb s b e et bbb b 3
Experience with the First Loop ..o e 5
The Basic LOOp APPAratus ......coieiivieiiieenineiscieresiie it ieeai bt sa e bbb e sb e 6
Safety ............................................................................................................................................................ 6
The AUXilIAry Sy StEMS .oueiiirireeiieee ettt bbbt e e bbb 8
CONSTRUGCTION oottt it oottt ee s e e e e ae e e s e ase e ssaat e st e beassos st s e s e e s e s e e b 4 obs e b ab e s s s beer e s b st e et sa b 8
T @ U QU coeeeeeeeeee et ettt ettt cettesssabeseseeaebesbees s se e s bessse e s ee b e s oate s s it e s e s en s e e it abe s ba s s abn e see s e be s st bt s e as 8
The PUMP SYSTEM .viviivieieeeeeirieceststeeaeseieie s eratbe s ers st s s h s s s b s et h bbbt bbb 11
The Off-Gas SySTEm ..ottt eb bbb b e s 12
The Assembly Procedure..... ..ottt 15
Instrumentation ANd CONTIOl ..ottt se et b s b s bbb s 18
Radiation Shielding .....civvereiereiet it e 22
P E R ATION oottt e ete st e et e e e e s teseesbe et easaas s e s aatesheeseemtsaber e s se e oRE e s e ek b e b s e b e AR e AR e e R e st st e b e 26
Leak Testing and Cleaning......cccoriiiiiiniieie sttt s 26
FS Al I QEION 1M REGCEOT caenveeee e et tee et ee e et esteate s etaebesasesee e st sonaesassan e e be s sheaas e e ba s s s onres s s meend s b b s s an s a e s 27
F LT ING eevetiteeeee et b et enee st e e s e st bbb e b b e b e e e AR SEAELehERES LSRR S e 27
Reactor Startup and Operation of the Loop ..o 27
ShutdOWN Of the LOOP .vevee ettt e st 30
Removal and Disassembly of the L.oop ..o 31
DISCUSSION OF RESULTS oot ceeeteesbessesneseesbasre s eesasas esbaesessasasaabesassssaasess e sabe bt easn e suasr b s s nrn e e 32
Measurement of Fission Power Generation ...t 32
Chemical Analysis of FUl .ttt e 33
FisSiON-Product RUMENTUM c.oeeeee et eette e et e e st e bar e e ee s ns s as s s n s e s b e aaa s s e s b s as s s bbb 34
Metallographic EXGMiNGtion ..o es ettt st 34
CONC USTOMS 1ot eeeeeeeee e esetee e e ee e eeeaeeeaate s asbeaeates s essaeeseaaee e s aee s saesenbbe e abn e s s b e e e s n s e bm st e et e e s e ne s n b e bt v s 45
APPENDIX A —~ DISASSEMBLY PROCEDURE AND EQUIPMENT ..o 45
APPENDIX B — ANALYSIS OF INCONEL TUBING ... vttt a e et aas 50
A FLLUORIDE FUEL IN-PILE LOOP EXPERIMENT
0. Sisman W. E. Brundage W. W. Parkinson
ABSTRACT
An Inconel loop circulating fluoride fuel (62]/2 mole % NaF, ]2]/2 mole % ZrF4, 25 mole % UF4,
93% enriched) was operated at 1485°F with a temperature difference of about 35°F in the Low-
Intensity Test Reactor for 645 hr. For 475 hr of this time the reactor was at full power, and
fission power generation in the loop was 2.7 kw, with a maximum power density of 0.4 kw/cc.
The tatal volume of fuel was 1290 cc (5.0 kg), and the flow through the irradiated section was
8.6 fps (Reynolds number 5500).
chemical and metallographic analyses.
The loop has been disassembled and has been examined by
No acceleration of corrosion or decomposition of fuel by
irradiation was noted, although deposition of fission-product ruthenium was observed. No mass
transfer of Inconel was found, and the corrosive attack was general and relatively light, The
average corrosive penetration, in the usual form of subsurface voids, was 0.5 mil; the maximum
penetration was 2 to 3 mils.
INTRODUCTION
High power densities and effective heat transfer
are paramount requirements in the development of
mobile power reactors. In order to provide a system
meeting these requirements for the Aircraft Nuclear
Propulsion Project, circulating molten-salt fuels
have been investigated extensively, This experi-
ment, as the first of its kind, was designed and
operated primarily to demonstrate feasibility as
well as to study the effect of reactor radiation on
a dynamic-corrosion system of high-melting liquid
fuel. It was anticipated that the fluoride fuels
would be used at 1500°F in Inconel.
At the time of the conception of this experiment,
1 for several
there were available corrosion data
alloys in a number of compositions of fluoride
salts at temperatures up to about 1800°F. There
were also available data for very small Inconel
capsules containing the fluoride mixtures which
had been irradiated in the MTR at about 1500°F.
Very little, if any, corrosion of Inconel was de-
tected for either the irradiated or the nonirradiated
capsules of the more recent tests.2:3 Thermal-
1. S. Richardson, D. C. Vreeland, and W, D. Manly,
Corrosion
17, 1953).
2y, J. Sturm, R. J. Jones, and M. J. Feldman, The
Stability of Several Inconel-UF4 Fused Salt Fuel Sys-
tems Under Proton Bombardment, ORNL-1530 (June
19, 1953).
by Molten Fluorides, ORNL-1491 (March
convection loops of very low flows but large
differences in (AT)
transfer to be a serious problem.4 No high-velocity
temperature showed mass
experiments had been run either in the reactor or
out of the reactor. It was anticipated that the
Aircraft Reactor Experiment would be the first
high-velocity system, either with or without radi-
ation. Here, the flow rate and the AT would have
values expected for a full-scale reactor, but the
power density would be too low for an accurate
measurement of any effect of radiation. A loop
experiment is different from the ARE in that a
part of the system can be in a high-radiation field.
Loop experiments are therefore designed to
produce a very high power density in some part
of the system and to maintain, as nearly as
possible, many of the other conditions expected in
the reactor. ldeally, it would be desirable to have
a high power density and a low dilution factor
(ratio of total volume to irradiated volume), high
flow rate with high AT, and precisely the same
fuel composition as that anticipated for the full-
scale reactor.
3W’. E. Browning, Solid State Semiann. Prog. Rep.
Aug. 30, 1954, ORNL-1762, p 39.
4(3. M. Adamson, ANP Quar. Prog. Rep. June 10,
1954, ORNL-1729, p 72.
The radiation facility available for the experi-
ment was a horizontal beam hole (HB-2) in the
LITR. In order to obtain the highest possible
power in this reactor a special fuel was blended
which contained about 50 wt % U235, This mixture
of NaF, ZrF,, and UF, was somewhat harder to
work with than the standard mixture because it
had a higher melting point (1170°F vs about 950°F
for the ARE fuel) and a considerably higher
viscosity,
The intention was that the fuel loop be as short
as possible in order to keep the dilution factor
down and the fuel inventory low, The first design
had the entire loop located in the innermost 4 ft of
the beam hole, and this had the additional obvious
advantage of permitting the use of equipment
which was relatively small and, being completely
inside the reactor, was easy to shield. However,
this design required the development of a pump
small enough to fit inside the beam hole of the
reactor, Unfortunately, the urgency of the experi-
ment would not allow for the development of a
special pump. The only readily available one
was a sump pump, which had to be located outside
the reactor. As will be discussed later, this
changed the entire conception of the experiment,
The loop now became 15 ft long, contained a large
inventory of fuel and, consequently, a large
dilution factor, and required a tremendous amount
of radiation shielding outside the reactor,
With such a large dilution factor, the experiment
can no longer be considered a test of fuel stability,
but the effect of radiation on corrosion can still
be seen at the *‘in-pile’’ end of the loop, where the
radiation intensity is high, To simulate reactor
conditions it was desired that, in addition to
maintaining the maximum temperature of 1500°F,
a large temperature drop be maintained between the
hot and cold ends of the loop. Although the
attainment of a high AT was somewhat |imited by
the high melting point of the fuel, it turned out
that, because of the geometry imposed on the
experiment (see the section entitled ‘‘Design’’),
there was a choice between a high AT with fow
flow rate or a very low AT with high flow rate,
Since it was necessary and desirable to have a
relatively high flow rate, the loop was operated
practically isothermally, The temperature was
maintained at a maximum of 1500°F at the in-pile
end of the loop, and the flow was selected so
that turbulence was maintained in the hot end of
the loop (Reynolds number, ~5000).
SUMMARY
The experiment ran very smoothly throughout the
month that it was in the reactor. An early plugging
in one of the off-gas lines was easily corrected,
and the only adjustments required were heater
power reguiation for reactor shutdown and startup.
Temperatures, fuel flow rate, and reactor power are
plotted in Fig. 24 for the entire period of operation;
the conditions of operation are summarized in
Table 1. Termination of the experiment was
caused by flow stoppage due to failure of the pump
drive belt, The flow stoppage caused an overshoot
in temperature which scrammed the reactor by
means of the safety circuit built into the equipment,
The temperature overshoot was 70°F and lasted
for about 1 sec, after which time the reactor was
shut down (see Fig. 25).
Metallographic examination showed that cor-
rosion in the loop was relatively light and es-
sentially uniform, Maximum penetration was
2.5 mils, and such penetration was confined to a
limited region outside the radiation field, In the
remainder of the loop, maximum penetration was
about 1 mil, and average penetration was 0.5 mil,
No enhancement of corrosion by irradiation was
observed, and no mass transfer of metal was noted
anywhere in the loop.
Chemical analysis indicated that the fuel was
diluted by the preliminary flushing salt (nonuranium)
to 43.7 wt % (~25 mole %). The other changes
observed in the composition were in the traces of
nickel and chromium, constituents of Inconel,
The nickel content decreased slightly, while the
chromium content increased from 44 ppm in the
original charging material to about 150 ppm. These
changes confirmed the moderate degree of cor-
rosion,
The generation of power in the loop by fission
was estimated by electrical heating measurements
during operation to be 2.8 kw. Activation of the
Inconel of the loop corresponded to a flux which
Table 1. Summary of Operating Conditions
Totol operating time, hr
Time at full reactor power, hr
Location of experiment
Reactor po wer, Mw
645
475
LITR hole HB-2
3
Fission power in loop, kw 2.7
Maximum power density, kw/cc 0.4
Temperature, average, °F
Inlet to high-flux region 1475 + 10
Outlet from high-flux region 1485 + 10
Maximum in loop 1485 + 10
Minimum in loop 1450 + 15
AT in loop, °F 35 x15
Flow, averoge
Mass flow, g/ sec 250
Volume flow, gpm 11
Velocity in high-flux region, fps 8.6
R in high-flux region 5500
Velocity in most of loap, fps 2.7
Pressure (at pump reservoir) Atmospheric
Cycle time, sec
Complete circuit 19.6
Time in pump 8.5
Time in high-velocity section 0.4
Time in rest of loop 10.7
Fuel (as received)
Table 1 (continued)
Density ot 1500°F, g/cc 3.93
Viscosity at 1500°F, centipoises 10.0
Uranium enrichment, % 93
Container material Inconel .
Fuel inventory, kg 5.0
Volume of system ot 1500°F, cc 1290
Dilution factor 180
would have produced 2.8 kw. The maximum power
density in Table 1 was determined by this method,
The activity of zirconium fission product in the
fuel indicated that the power was about 2.4 kw,
Radiation instruments
activity of effluent gas from several locations
were included in the instrumentation as safety
devices, These instruments were affected by the
general background radiation but showed the only
other activity to be that from fission products in
the pump purge gas. The activity of this gas
after passage through the charcoal adsorber can
be estimated roughly by means of the stack-gas
monitor of the Reactor Operations Department,
About (.001 curie/sec was discharged to the
off-gas stack,
Radiochemical examination of the fuel showed
indicating only relative
Composition, mole % UF ¢ ZrF ¢NoF that less than 20% of the ruthenium fission product
(25-12'/2-62]/2) was retained in the fuel; the rest was found to be
Melting point, °F 1170 deposited on the inconel walls of the loop system,
DESIGN
Governing Factors
As mentioned in the Introduction, time would
not permit the development of a pump small enough
to be located inside the beam hole and equal to
the severe temperature and corrosion conditions of
the loop. The only suitable existing pump was a
centrifugal sump pump developed by the Experi-
mental Engineering Section of the Aircraft Reactor
Engineering Division., The capacity of the pump
was 600 cc, the output at 3000 rpm was about
1.3 gpm of fuel at 45 psi discharge pressure, and
the over-all dimensions were 23 in, in height and
10 in. The characteristics of the
pump dictated many of the features of the loop.
in diameter,
The beam hole in the LITR available for the
experiment extended about 12 ft through the reactor
shield and moderator structure and into the active
lattice. Since the diameter of the hole required
that the pump be located outside the reactor shield
at a distance sufficient to permit utilities con-
nections and shielding, the loop had to be about
15 ft long. A schematic drawing of the loop
apparatus in its final form is shown in Fig. 1.
The need to attain maximum fission-power
density in the fuel and the practical limitation
on the removal of heat, while an assembly was
retained which could be kept hot in the absence of
fission heat, required that the volume of fuel in
the neutron flux be small, The low thermal
conductivity® of the fuel made it mandatory to have
3S. |. Cohen et al., Physical Property Charts [or
Some Reactor Fuels, Coolants, and Miscellaneous
Materials, ORNL CF-54-6-188 (June 21, 1954),
- ~JACKET ASSEMBLY
NOSE PIECE
JLN HEATER
L
Al
®
FUEL TUBING
- NOSE COVER
ALSIMAG 202
HEATER CORE
NICHROME V
CORE HEATER
SECTION A-A
CADMIUM SHIELD
HELIUM PURGE LINE
OIL IN THROUGH SHAFT ORNL- LR - DWG 5969
HELIUM EXHAUST !
\
OlL OVERFLOW
OlL INLET FOR | }
RING COOLING
SPARK PLUG PROBE
CENTRIFUGAL PUMP MODEL LFA
- CONTROL GAS
KOVAR SEAL
FITTINGS — PUMP ENCLOSURE
DRAIN TUBE SEAL
FREEZE TUBE
EXPANSION BELLOWS
HELIUM ATMOSPHERE
WATER OQUTLET
EXPANSION BELLOWS .
1 NOSE PIECE - A-J
BORON SHIELD
NOSE COVER
20 in. REF : —
JACKET ASSEMBLY HEAT EXCHANGER LINER SEAL
Y5-in. DIA SUPPORT ROD AND FLANGE
F TURBI CALRODS .
S JE- TUBING FUEL. TUBING \ - 0" RING
a-in. OIA SUPPORT ROD- Ut 7y
*: '":-j”—"——:i"”:—:—:———*a:::"::f;—l'fifii’f AIR INLET
= R ) o
fhkL i T *M/ 4J!
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G ! wd -
A e ,JV
e P e e aenagd /
" - : e O Al |
ANNULUS FOR g i | /
"KOWLR SEAL
WATER FLOW TRANSITION . Y DIA FUEL TUBING (IN} - J
PLATE SUPPORT ROD FUEL LEADS \PRESSURE FITTINGS
T¢ DIAPHRAGM™ TRANSMITTER CELLS WATER INLET
“HELIUM LEADS TO
DIAPHRAGM
'
- {21t 5in REF W - . e -
Fig. 1. Fluoride Fuel Loop.
turbulent flow in the irradiated section in order to
remove the fission heat from the fuel adjacent to
the tube walls (where the velocity is low in laminar
flow). Tubing having an inside diameter of
0.225 in, was selected for the section in the
neutron flux. In a tube of this size, the fuel mixture
(density, 3.9 g/cc; viscosity, 10 centipoises)3:6
cannot be maintained at turbulent flow (R~ 5000)
through a length much greater than 4 ft without
exceeding the output characteristics of the pump
described above. Accordingly, the irradiated
section was made up of about 3]/2 ft of 0.225 in.-ID
Inconel tubing bent into a U-shape 2 in. across,
and, to keep the pressure-drop low, the connecting
tubing used between the pump and the irradiated
section was 0.40 in. 1D and 0.50 in. OD.
Safety considerations strongly influenced the
design of control equipment and instrumentation
as well as the loop structure, A major consider-
ation was the problem of dissipating fission heat if
fuel should become stagnant in the neutron flux
region. As a precaution, temperatures at many
points were recorded, with provision for shutting
down the reactor in case of excessive values,
A further safeguard was in the fabrication of the
irradiated U-bend from thick-walled tubing for
added heat capacity as well as protection against
corrosion, The thermal capacity thus incorporated
into the irradiated section served to retard the
temperature rise in case of flow stoppage and to
allow time for the temperature monitors and reactor
controls to operate, Inconel fins brazed to the
U-bend assembly and the omission of insulation
from this part of the loop were additional means
of controlling a possible runaway condition,
Personnel safety required shielding around the
pump and the fuel tubing outside the reactor shield.
It was necessary, therefore, to keep the radioactive
parts as compact as possible,
Experience with the First Loop
The first loop experiment was assembled and
was inserted in the reactor after being tested as
thoroughly as possible without actually being
operated with molten salt, The appearance of a
leak in this loop as it was being filled with fuel
demonstrated the need for an operating test prior
6S. 1. Cohen and T. N. Jones, Preliminary Measure-
ments of the Densily and Viscosity of NaF-ZrF4-UF;
(62.5-12,5-25,0 Mole %), ORNL CF-53-12-179 (Dec.
22, 1953).
to the rather lengthy reactor installation, The
performance of a preliminary operating test re-
quired that the addition of a drain and fill
connection be made in the final loop design, since
it was not feasible to remelt the fuel after the
test because of the danger of bursting the tubing
from thermal expansion of the fuel (~20% from the
mp to 1500°F). The drain and fill connection is
described below,
The leak occurred in a thin section of a flange-
weld joint after the joint had been satisfactorily
Although this type
of weld had proved satisfactory on other loops,
the combination of stress concentrations at the
weld and of incomplete weld penetration caused
failure in this instance, To provide butt joints of
greater strength, fillet-weld joints were employed
in the assembling of the final loop (Fig.2). Tech-
niques were developed by the Metallurgy Division
for making sound welds of this type on small
tubing without obstructing the bore.
vacuum-tested at temperature,
UNCLASSIFIED
ORNL-LR-DWG t4444
~ %
_______
- -
”
3 5
”
& .
&
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o
i
P
CROSS SECTION OF FLANGE-WELD BUTT JOINT BEFORE WELDING
b
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= 5