‘ IR A sy
3 445L 00LODOOS2 5 ._

AEG RESEARCH AND DEVELOPMENT REPORT < oi™veccron- .. 5 4

Special Features of Aircraft lgaactors

 

EFFECT OF RADIATION ON CORROSION
OF STRUCTURAL MATERIALS BY
MOLTEN FLUORIDES
4 G. W. Keilholtz

J. G. Morgan
W. E. Browning

E

  
  
  
   

| o IS SR
o A-JL-&.‘L
B (LT e T
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B

OAK RIDGE NATIONAL LABORATORY

OPERATED BY
UNION CARBIDE NUCLEAR COMPANY

A Division of Union Carbide and Carbon Corporation

POST OFFICE BOX X * OAK RIDGE, TENNESSEE

 
 

 

 

LEGAL NOTICE

 

This report was prepared os an occount of Government sponsored work. Neithsr the United States,

nor the Commission, nor any parson acting on behalf of the Commission:

A. Mokss any warranty or representation, express or Implied, with respect to the accurocy,
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or distributes, or provides occess fo, any information pursuant to his employment or contract
with the Commission.

 

 

 

 
 

— ORNL—EfiS R

  

This document consists of 2

ages. Copy /1P of 246 copi
Contract No. W-Th05-eng-26 gefies A.py P

SOLID STATE DIVISION

EFFECT OF RADIATION ON CORROSION OF STRUCTURAL MATERIALS BY

MOLTEN FLUORIDES

G. W. Kellholtz
J. G. Morgan
W. E. Browning

DATE ISSUED

AUG 131957

OAK RIDGE NATIONAL LABORATORY
Operated by
UNION CARBIDE NUCLEAR COMPANY
A Division of Union Carbide and Carbon Corporation
Post Office Box X
Oak Ridge, Tennessee

‘l Hiflflm’m MA|R1|E‘T|'I"|\’ ENERGY SYSTEMS LIBRARIES —

J 4456 00LOOSE 5

 

 
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29,
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Borkowski
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Boyd
Bredig
Breeding
Browvning

E.
A.
Je.
E.

. R. Bruce
. Do

Callihan

W. Cardwell
Center (K-25)
A. Charpie
Clark

E. Clifford

H. Coobs

. B. Cottrell

Cromer
Crouse
L. Culler

. R. Cuneo

DeVan
M. Doney

. A. Douglas

Dytko
Eister
Emlet (K-25)
Ferguson
Fraas

H. Frye, Jr.
Furgerson
Gray
Gresky

Grindell

Guth
S. Harrill

S. Householder

gT. Howe

 

=11~

INTERNAL DISTRIBUTION

 

   
 
 
 
 
    

 

 

ORNL-2373
¢-84 - Reactors-Specifl
Features of Aircraft Reactors

7. W. H. Jdbrdan
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120.
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EXTERNAT, DiSTRIBUTION

   
   
  
 
 
  
   
   
 
 
   
    
 
    
    
     
   

Aerojet-General CRrporation #F
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Division ofJ search and Dey fflopment AEC, ORO

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Abstract

A survey of the experimental methods used in testing the radiation
stability of molten salts and their corrosion properties is presented.
The effects of irradiation on the corrosion on Inconel exposed to fluoride
fuel mixtures and on the physical and chemical stablility of the fuel
mixtures have been investicated by irradiating in the MIR capsules
filled with static fuel and by operating in-pile forced-circulation loops
in the LITR and in the MTR. In the many capsule tests and in the three
in-pile loop tests made to date, no major changes have occurred in the
fuel mixtures that can be attributed to irradiation, other than normal
burn-up of uraniumf Metalluregical examinations of the Inconel capsules
and tubine have likewise shown no chanees in corrosion that can be the
result of radiation damaese. The low corrosion results obtained for the
in-pile loops have been confirmed by chemical analyses for corrosion

products in the fuel mixtures.
-D-

The use of molten fluorides as reactor fuels (1) requires that they be
stable both thermally and in intense radiation fields. The fission process in
the salt causes resions of hish ionization density to exist, as well as very
hich heat fluxes. However, since molten salts are eenerally ionic liquids,
there is no crystalline lattice to disrupt, nor are there.covalent bonds to
sever. Thus, fast neutrons, fission fraemsnts, and ecamma radiation cannot
cause severe damage of the type found in crystalline materials. However, the
interface between the molten salt and its container offers a site where
radiation effects mieht meake themselves evident in an acceleration of the
corrosion process. With this possibility, it has been necessary to test the
compatibility of various salts with structural metals in the hichest neutron
fluxes available.

The principal methods used in in~pile testing of molten salts are listed
in Table I. Capsule tests were performed first because of their simplicity
and their ability to produce information susceptible to statistical analysis.
The successive techniques listed in the table are of increasine desrees of
complexity and approach closer and closer to the desien conditions of a
practical nuclear power plant. Each step, however, introduces new variables
and requires far ecreater expenditure of effort and time than the previous
step does, rapidly decreasine the number of tests which can be performed.
Although consideration was eiven to their use, rockineg capsule tests and
thermal convection loops have not formed a part of the work described hers.

Capsule tests have been made with nickel, types 316 and 347 stainless
steel, and Inconel. The salts employed and their compositions are listed
in Table II. The first salt irradiations were conducted by Van De Graaf (2)

and cyclotron (3) bombardments. Proton bombardments {3b)were employed to

 
 

TABIE T

METHODS OF STUDYIN~ RADIATION EFFECTS ON CORROSION BY MOLTEN FLUORIDE FUELS

1,
2.
3.
Lo
5.

In-Pile Capsule Tests
Rocking Capsule Tests
Thermal Convection Loops
Forced-Flow loops

Experimental Reactors

 
i

TABIE II

MOLTEN SALTS TESTED IN RADIATION EFFECTS PRONRAM

System
KOH

NaF-KF--UF4

NaF—Ber-UF
NaF-BeFZ-
NaF-BeF ~UF

NaF-ZrF ,=UF

I~

NaF=ZrF, -UF

,F\
&7 e

o~

NaF=2rF, -

NgF~ZrF -

=~
w o

Compogition (molgi)
100

46,5-26.0-27.5
25,0-60,0-15.0
47.0-51,0-2,0
50.0-46.0-4.0
63.0-25,0-12.0
53.5=-40.0-12.0
50.0-48.0-2,0

50,0-48.0-2.0
-5~ | S
supplement parallel experiments in the ORNL fraphite Reactor because of the high
gspecific power attainable in this way. These irradiations were continued for 1
to 92 hours, usineg 20 to 22 Mev. protons in the ORNL 86-in. cyclotron. Specific
power generation ranged from 500 to 4700 watts em™>. With the starting of the
MTR, a sufficiently hish-flux reactor became available for these experiments.
Irradiation with fieutrons, gamma rays, and fission fragments obtained in this
way are far more realistic than those using elementary charced particles. The
emphasis was therefore shifted to reactor irradiations.

A typical capsule used in the MIR irradiation prooram is shown in Fie. 1.
It is 0.100 in. i.d. with & 0.050 in. wall. The length of the salt column is
1 in. In salts with hich o35 contents, the diameter of the fuel column is
reduced to 0.055 in. This avoids excessive temperatures at the center Sf the
salt colums when working with fuels penerating as hish as 8000 watts em™ (4)
Fie, 2 illustrates the arranrement of control instrumentation on the north
balcony of the MIR, Electrical and cooling-air lines extend from the instrument *
panels to the top of the reactor. The capsule is loaded through the reactor
inlet water line. It is inserted down an aluminum tube into a beryllium
piece located in the reflector recion. Fig. 3 shows the MIR irradiation
facility. The temperature of the fuel is controlled by a variable flow of
air, the outer surface temperature of the capsule being monitored with
thermocouples. The weicht of salt is chosen so that about 250 watts of
fission heat are cenerated in the capsule. This requires about 3 c¢fm of
cooling air. Usine 45 psig air, the velocity throuesh the capsule restriction
is about 700 ft.sec.™t,

It was necessary to develop special thermocouple junctions for use in

such hich=-velocity cooline air streams. The air produces a large thermal
-6
gradient in the capsule wall and in the thermocouple heads. In poorly censtructed
thermocouples, errors as pgreat as 30000 have been observed., The thermocouple shown
in Fiec. 4 wes made by a resisténce spot-weldine technique. The bead 1is desigmed to
have & laroe area of contact with the capsule and to be very thin, thus ensuring
that the part which measures temperature is at the same temperature as the surface
of the capsule.

After irradiation, capsules are returned to ORNL where detailed examinastions
are made in the Solid Btate Division hot cells, Fir. 5 shows a cell equipped
for chemical analyses. Right-to-left are a vertical lathe for opening capsules,

a master-slave manipulator, a drill press for removine salt samples, and a
chemical hood. Operations involvine radioactive powders are enclosed in lucite
cases which are exhausted through a filter system. Fie. 6 shows a tool for
slittine capsules longitudinally (5), to obtain specimens sometimes desired for
metalloeraphic studies. Fig. 7 shows the hot cell in which metalloesraphic
specimens are prepared (6). Some salt samples have been examined using the *
shielded petroeraphic microscope (7) shown in Fie. 8,

The principal variables studied in the static corrosion program have been
flux, fission power, time, and temperature. In a fixed neutron flux, the fisaion
power is varied by adjusting the U235 content of the fuel mixture. Thermal
neutron fluxes have raneed from 1011 to 1014 neutrons em 2 sec.™t and fission
power-densities from 80 to 8000 watts em™, Capsules have generally been
irrediated for 300 hours at 1500°F (815°C), although in recent tests the
experiments have been extended to 600 to 800 hours. The techniques used for

examinine capsules after irradiation are listed in Table III.

 
1,

2o

TABLIE III

TECHNIQUES FOR EXAMINING IRRADIATED MOLTEN FLUCRIDES

Pressure Tests (In-Pile)
Melting Point Determinations
Petrooraphic Analyses

Chemical Analyses

Mass Spectroscopic Assays
nemma-Ray Spectroscopic Studies

Metallopraphic Exemination of Containers
_8-

In the many capsule tests to date (over 100), no major chanees have been
observed which can be attributed to irradiation, except the normal burn-up of
U235. Metallooraphic examinationa (8) of Incbnel capsules tested in NaF-ZrFL-UFA
and in NaF-ZrFA-UF3 at 1500°F for 300 hours have shown corrosion comparable to
that foupd in unirradiated control tests; 1.e., penetrations to depths of less
than 4 mils, In capsules which experienced accidental excursions to 2000°F and
atove, there was penetration to depths of more than 12 mils, accompanied by
srain erowth. These results stimulated extensive development work on control
instrumentation and thermocouple construction. Chemical determinations of

chromium in irradiated salts have been shown (3) to bte seriously affected by

the intense beta radiatlon of the accompanyine fission products. Work is
currently in proeress on the circumvention of this problem.

Three typesof forced-circulation in-pile loops have been.studied. A larece
loop was operated in a horizontal beam-hole of the LITR (1Q). The pump for
¢irculating the fuel in this loop was placed cutside the reactor shield. A
smaller loop was operated in a vertical position in the lattice of the LITR
(11), its pump mounted just above the lattice. A third loop was operated
completely within a beam-hole of the MIR (12). The operating conditions for
these loops are presented in Table IV. The dilution factor for a reactor may
be defined as the ratio of the total volume of fuel in the system to that in
the reactor core. A more useful definition for in-pils loop use is the ratio
of the maximum specific power to the averace specific power. 1In th;a two LITR
loops, metalloeraphic examinations showed less than 1 mil penetration of the
Inconel fuel tubes. Fipgs. 9 and 10 show drawings of these two loop models,

The MIR horigontal loop is shown in Fig. 11, Examination of etched and unetched
metallo~raphic sections of Inconel tubing from this loop showed no attack to a

depth ereater than 3 mils. A slicht amount of intersranular corrosion was noted,

 

e BB e w
 

..9_

but this was neither dense nor deep. Measurements of wall thickness showed no
variations attributable to corrosion. The loop was examined carefully for effects
of temperature variations between inside and outside walls of the tubine at the
bends, but no effects of overheatine were observed. The low corrosion is
attributatle to careful temperature control of the salt-metal interface and to the
maximum wall temperature beine below 1500°F at all times. The larger corrosion
value in the MTR loop results from the ereater fuel-temperature differential
(155°F) which was obtained during operation. Ioops operated in the absence of
radiation show similar effects, Studies of the behavior of fission product |
elements in these loops are discussed elsewhere (13).

The experiments described above show that, within the limits of tests to
date, there is no acceleration by radiation of the cofrosion of Inconel by
molten fluoride reactor fuels. Experiments are planned to extend the prosram to
cover new salt compositions and new alloys and to oberate in-pile loops for much

longer times with hicher flow-rates and orester fuel-temperature differentials,
 

-10-

TABIE IV

OPERATINA CONDITIONS FCR INCONEL FCRCED-CIRCULATION IN-PIIE LOOPS

Fuel Composition (mole%)

Max. Fission Power,
watt cm=3

Total Power
Dilution Factor
Mex, Fuel Temp.,°F.

Fuel Temperature
Differential, °OF.,

Fuel Reynoldas'! Number
Operatine Time, Hours
Time at Full Power

Depth of Corrosion
Attack, mils

LITR "LITR
Horlzontal Vertical
Ioop l1oo
NaF~ZrF -UF, “aF-irF,-

(62.5~12. 5-25) (63-25=12

400 500
208 5.0
180 10
1500 1500

30 71
6000 3000
645 130
475 30
<1 <1

MIR

Horizontal
oo
NaF—ZrFA-U
(53.5-40-6.5

800

20

5

1500

155
5000
467
271
{3

1
-1~

ACKNOWLEDCEMENTS

The work reported here has been obtained over the past six years with the
assistance of many members of the staffs of ORNL and of the Phillips Petroieum
Company, Idaho Falls, Idaho. We wish to acknowledes particularly the assistance
of the followines:

In-Pile Experimental Proorams: H. E. Robertson, P. R. Klein, M. ¥, Gsborne,
D. E, russ, H. L. Hemphill, H. V. Klaus, D. D. Davies, D. F. Weekes, W. R. Willis,
J. F. Mardock, C. D. Cac~le, J. T. Delorenzo, W. H. Tabor.

Post-Irradiation Studies: C. C. Webster, A. E. Richt, E. J. Manthos,.

Petroeraphic Studies: T. N. MeVay, 7. D. White.

Analytical Chemistry: J. H. Edeerton, L. C. Henley, J. E. lee

Mass Spectroscopy: C. F. Baldock, J. R. Sites, L. G. ~ilpatrick.

 
2.

3.

6o

9.
10.

11,

12.

13,

-12-

REFERBNOES
A. M, Weinberg, American Nuclear Society Meetins, Pittsbure, Pa., June

10-12, 1957,

W. E, Brownine, TID-5021, p. 44, March 6, 1951 (Secret); V. P. Calkins,

W. E. Prownine, and Saul Siegel, NEPA-1869, April 15, 1951 (Secret).

(a) W. V, Goeddel,.NAA—SR-ZOS, January 26, 1953 (Secret); (bt) W. J. Sturm,
R. J. Jones, and M. J. Feldman, ORNI-1530, April 3, 1953 (Secret).

P. R. Klein, personal communication, 1953.

L. N. Howell and G. C. Webster, Fourth Annual Symposium on Hot Laboratories
and Equipment, Washineton, D. C., September 24-30, 1955.

M. J. Feldman, Metal Prosress, p. 97 (November, 1953); S. E. Dismuke, M. J.
Feldman, 7. W. Parker, and F. Ring, Jr., Intl. Conf. on the Peaceful Uses
of Atomic Enerey, Meneva, Switzerland, Au~ust 2-20, 1955, Proceedines 7,

6

-3

(Paper P/732).

M. T. Robinson, ORNL-1606, p. 43, November 20, 1953 (Secret).

M. J. Feldman, A. E. Richt, and E. J. Manthos, Solid State Division
Metallurey Reports, 1952 to 1957 (Secret).

R. P. Shields and R. E. Adams, ORNL-2221, p. 306, March 12, 1957 (Secret).
O. Sisman, W. W, Parkinson, and W. E. Brundage, ORNL-1965, January 16, 1957
(Secret).

W. R. Willis, M. F. Osborne, H. E. Robertson, D. E. nusa, C. C. Webster,

A. S. Olson, and C. D. Baumann, ORNL-1944, p. 16, November 3, 1955 (Secfet).
D. B. Traucer, L. P. Carpenter, C. W, Cunningham, J. A. Conlin, P. A. fnadt,
C. C. Bolta, and D. M, Haines, ORNL-2012, p. 27, n.d. 1956 (Secret).

M. T. Robinson, W. A, Brooksbank, Jr., S. A. Reynolds, H. W. Wricht, and

T, H. Handley, American Nuclear Society Meseting, Pittaburg, Pa., June 10-12,

 
=-13-

 

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UNCLASSIFIED
ORNL—LR—DWG 201470

INSTRUMENT CUBICLE TOP OF REACTOR

ELEV 420.5 ft

   
 
 
 
   
  

TESTING FACILITY
HOUSING

AIR EXIT

 

TESTING FACILITY
INSTRUMENTATION

 

 

Fig. 2. Installation of Control Instrumentation for MTR Capsule Program,

 
 

UNCLASSIFIED
SSD-C-1097
ORNL -LR-DWG-4407

   

AIR PATH

IRRADIATION TUBE WITH CAPSULE INSTALLED

 

 

 

 

TYPICAL

 

 

CAPSULE ]ANNULUS SLEEVE

 

CAPSULE IRRADIATION TUBE

 

IRRADIATION TUBE WITH CAPSULE REMOVED

INSTALLATION OF
IRRADIATION TUBES IN MTR
REFLECTOR A PIECE

Fig. 3. Facility for Irradiation of Molten Fluorides in the MTR,

_gl_
 

UNCLASSIFIED
ORNL-LR-DWG 20172

 

    

.

- ” -

 

O O 0.2 0.3 04 WD

INCHES

Fig. 4. Thermocouples for Use in High-Velocity Air Streams.

_Ql_
 

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UNCLASSIFIED
PHOTO 11972

 

 
 

PHOTO 15230

 

Fig. 6. Remotely Controlled Slitting Saw.
      

  

UNCLASSIFIED
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P.‘:‘#-—*-— - e & . T e W —— I. ‘:fl :
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Fig. 7. Hot Cell Equipped for Preparing Metallographic Specimens.
-20-

UNCLASSIFIED

D-17145

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Fig. 8. Shielded Petrographic Microscope.

 
 

OlL IN THROUGH SHAFT Ol'n'-lr-dwg 5969

 
 
 
 
  
 
 
  
 
 

HELIUM EXHAUST
JACKET ASSEMBLY OIL INLET FOR -SPARK PLUG PROBE

| RING COOLING ~—
' NOSE PIECE

   
  
  
   

 

- CENTRIFUGAL PUMP MODEL LFA
_—— CONTROL GAS

FUEL TUBING KOVAR SEAL

FITTINGS _—— PUMP ENCLOSURE
/

 

NOSE COVER
DRAIN TUBE SEAL

ALSIMAG 202 FREEZE TUBE " | HELIUM ATMOSPHERE

HEATER CORE EXPANSION BELLOWS

i NICHROME V
CORE HEATER

/

 

 

 

SECTION A-A

 

WATER OUTLET

 
   
 
    
  

EXPANSION BELLOWS

   
  

JACKET ASSEMBLY HEAT EXCHANGER LINER SEAL
CADMIUM SHIELD Yo-in DIA SUPPORT ROD AND FLANGE
HELIUM PURGE LINE / FUEL T CALRODS o
3, ~FUEL TUBING FUEL TUBING 0" RING
%-in. DIA SUPPORT RO / / (OUT)
£ AIR INLET

 

 

 

 

 

 

 

 

 

 

 

 

 

  

 

 

 

 

 

 

  

 

 

 

 

 

 

7

%

| ' , ;

NOSE PIECE A ANNULUS FOR \ \, VENTURI /
BORON SHIELD WATER FLOW—" “TRANSITION 4-in. DIA “—~FUEL TUBING {IN) KOVAR SEAL
NOSE COVER PLATE SUPPORT ROD FUEL LEADS PRESSURE FITTINGS
T¢ DIAPHRAGM TRANSMITTER CELLS WATER INLET
HELIUM LEADS TO
&0 in REF —————————— DIAPHRAGM

+ {2 ft 5in. REF + P =

 

Fig. ?. LITR Horizontal Forced-Circulation Loop for Dynamic Corrosion
Testing of Molten Fluorides.

_lz_
UNCLASSIFIED
ORNL-LR-DWG 18553

WATER INLET AND OUTLET

AIR IN '
=

AR OUT FLEXIBLE METAL HOSE

MOTOR
WATER COOLING TUBES
—TE-1 )
PUMP
— TE-2,2A
H “—TE -3, 3A
PN~ 1E-4.4A

|| ||||;=!

    
      
     
   
 

PUMP HEATERS —

> TR-1: TE-1—TE-2
~——TE-6

 
  
    

LOOP HEATER —— —
TE -]

TE-9 ON SWAGE-LOK—
TE—11 ON AIR TUBE— —~

TE-13,13A,138B _

gl LOOP HEATER
lI'H
II‘ |~ TE-8
i| pf N — TE-10 ON SWAGE-LOK
f¥ N ~—TE-12 ON AR TUBE
|il

N\ _TE-14, 144,148

   

 

 

 

 

 

  
  
   

 

 

 

AIR RETURN DUCT (OUT)—= @ AIR_ANNULUS (AIR IN)
e b —TE-16
TE-IS || ‘ > TRA-2: TE-13—TE-18,
LOOP HEATER —— —— \———Loop HEATER TE-25—TE-30
..'
1N
Te-17, 17,178 —— —— —J[l] ——TE"' 184188 J
v s
TRCA-{—— TE—19,19A 19B—— —— |\:}| [[™~—-TE-20, 20A, 208 TRA-3
TRA-5——TE-21,21A,21B — — |J \\—*—TE-22,22A.228 —— TRA-6
™~ Loop TUBE
DIRECTION OF FUEL FLOW— [k —— TRA
TRA-4 —— TE-23,23A,238 —— U —12‘246. 24A,248 —— TRA-H
TE-25 — A ~~— TE-28 TRA-2: TE-25 —TE-30
TE-29 i\
DIRECTION OF AIR FLOW ™/ g’gtfigi‘g“ TE-29
TE-25 —TE-26
SIMPLYTROLS (.
LEAK DETECTOR {TE—32 TE-27 —TE-28

——TE-30
DETAIL OF LOOP TIP

Fig. 10. LITR Vertical Forced-Circulation Loop for Dynamic Corrosion
Testing of Molten Fluorides.

 
 

FILL TANK

HEAT
EXCHANGER

   
  
 
 
 

AIR OUT,

AIR IN

Fig. T1. MTR Horizontal Forced-Circulation Loop for Dynamic Corrosion
Testing of Molten Fluorides.

Unclassified
ornl-lr-dwg. 20171