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CFETI WCES

ORNL-4123

Contract No. W-7405-eng-26 METALS AND CERAMICS DIVISION

MSRF, CONTROL ELENEXt"T: MA"ACTURE, INSPECTION, DRAWINGS, AND SPECIFICATIONS

G. M. Tolson and A. Taboada

JULY 1967

e -

OAK RIDGE NATIONAL LABORATORY Oak Ridge, Tennessee operated by UNION CARBIDE CORPORATION for the U.S. ATOMIC ENERGY COMMISSION

ti"

iii

CONTENTS

........................... Introduction . . . . . . . . . . . . . . . . . . . . . . . . . Development of Specification and Fabrication Methods . . . . . Component Manufacture . . . . . . . . . . . . . . . . . . . . Control Element Assembly . . . . . . . . . . . . . . . . . . . Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . Abstract

.......................... Appendix B . . . . . . . . . . . . . . . . . . . . . . . . . . Appendix C . . . . . . . . . . . . . . . . . . . . . . . . . . Appendix A

1 2

4 6 9 11

35 39

MSRE CONTROL ELEMENTS: MANUFACTURE, INSPECTION, DRAWINGS, AND SPECIFICATIONS G. M. Tolson’ and A. Taboada2 ABSTRACT The control elements f o r the Molten S a l t Reactor are Gd203-Al203 bushings canned i n Inconel. The report includes material s e l e c t i o n and development of f a b r i c a t i o n methods. The can w a s made from f u l l y inspected Inconel closed by four TIG welds. The Gd203-Al203 bushings were made by conventional pressing and s i n t e r i n g methods after a s p e c i a l prereaction s t e p was used. The bushings were given thermal shock t e s t s , weighed, dimensionally inspected, and given a f i n a l v i s u a l inspection f o r chips or crack$. As-built drawings, s p e c i f i cations, and manufacturing procedures a r e included. By methods described i n t h i s report, 160 MSRE control rod elements were manufactured.

INTROlXTCTION The Molten S a l t Reactor Experiment (MSRE) i s a high-temperature (675°C) low-pressure ( 5 0 p s i ) system designed t o provide a thermal output of about 10 Mw.

A f u e l mixture of LiF-BeF2-ZrF4-UF4 i s circulated

through a c y l i n d r i c a l 5 - f t - d i m r e a c t o r vessel (containing a graphite

core) t o a heat exchanger, where heat i s t r a n s f e r r e d t o a n unfueled f l u o r i d e salt and then t o t h e atmosphere. Gd2O3-x)$

The control elements are

A1203 bushings clad with Inconel as shown i n Fig. 1. They a r e

about 1 1/2 i n . long with an inner diameter s l i g h t l y l a r g e r than 3/4 i n . and a w a l l thickness of about 3/8 i n .

The MSRE has three control rods,

each of which has 36 control elements strung on a f l e x i b l e s t a i n l e s s s t e e l hose t o form a 56-in.-long

control rod.

The f l e x i b i l i t y of the control

rod prevents binding due t o misalignment or thermal expansion.

Although

’Present Address, Oak Ridge Gaseous Diffusion Plank. 2Present Address, Division of Reactor Development and Technology, USAEC, Washington, D. C.

2 UNCLASSIFIED ORNL-DWG 64-1105R

\INNER

TUBE

OUTER TUBE

Fig. 1. A Cutaway of an MSRE Control Element. cooling a i r w i l l be blown down the inside of t h e f l e x i b l e hose and control element and then back up over the outside of the element, the element must be designed t o withstand the temperature generated a t f u l l power without cooling, about 8 1 5 째 C .

DEVELOPMENT OF SPECIFICATION AND FABRICATION METHODS To prove the f e a s i b i l i t y of t h e control rod design, f o u r prototype elements were manufactured on a research contract with Dresser Products. The prototype elements d i f f e r e d from the f i n a l element i n t h a t t h e prototype p e l l e t s were produced by hot pressing and were canned i n stainless s t e e l r a t h e r than Inconel.

The prototype elements were subjected t o

x-ray, penetrant, and dimensional inspection and t o t e s t i n g t h a t included exposure i n a r i g 3 designed t o determine under simulated reactor conditions soundness, dimensional s t a b i l i t y , and general s u i t a b i l i t y f o r reactor use.

3R. B. Briggs e t al., MSR Program Semiann. Progr. Rept., Jan. 31, 19&> ORNL-3626, pp. 2 + 3 7

* t

I n t h e control-rod t e s t i n g r i g , two canned elements were exposed t o repeated thermal and mechanical shocks.

They were examined radiograph-

i c a l l y and dimensionally a f t e r 24, 350, and 600 hr of t e s t i n g t h a t included approximately 11,000 cycles and 1700 scrams.

Holes were made

i n one can t o expose t h e Gd203-AJ-203 t o a i r f o r t h e f i n a l 250 h r of testing

Dimensions of the metal cans were not a l t e r e d by the t e s t i n g .

Axial

cracks i n t h e p e l l e t s were observed radiographically a f t e r the f i r s t cycle, and severe cracks i n both t h e a x i a l and transverse directions were observed a t l a t e r stages.

However, no crumbling o r ratcheting was evident,

and no condition was observed t h a t might a f f e c t the nuclear o r mechanical performance of the control rod elements. Inconel was chosen as a canning material f o r t h e poison bushings because of i t s high-temperature strength, good weldability, and availability.

Inconel w a s chosen over s t a i n l e s s s t e e l f o r t h e following

reasons:

1. Inconel w i l l not catastrophically oxidize, while many s t a i n l e s s s t e e l s w i l l under c e r t a i n conditions. 4 2.

Inconel w i l l not stress-corrosion crack.

Inconel i s more r e s i s t a n t t o n i t r i c acid a t t a c k than i s sensi-

tized stainless steel.

N i t r i c acid can form i n radiation f i e l d s by

reaction of t h e nitrogen and water vapor i n the air.5

j j f

If salt should leak i n t o t h e control element, Inconel would

have b e t t e r corrosion r e s i s t a n c e than stainless s t e e l . Although t h e r e was only a s l i g h t p o s s i b i l i t y t h a t these conditions might occur, t h e s m a l l c o s t f a c t o r i n favor of s t a i n l e s s s t e e l did not warrant t h e r i s k involved. Boron and boron-containing materials were ruled out as poison mate-

rials, since under c e r t a i n conditions they r e a c t with s t a i n l e s s s t e e l

4J. H. DeVan, Catastrophic Oxidation of High-Temperature Alloys, ORNL-TM-51, (Nov. 10, 1961)

W c

-.i

5J. J. Stobbs and A. J. Swallow, "Effects of Radiation on Metallic Corrosion," Met. Rev. 7(251, 95-131 (1962).

4 and nickel-base alloys.

I n addition helium i s one of t h e products when

boron i s i r r a d i a t e d , which would require a venting system on t h e element o r design f o r high i n t e r n a l pressure.

A rare e a r t h oxide was chosen as

t h e poison material on the b a s i s of work done by O m 6 and Knolls Atomic Power Laboratory7 and i r r a d i a t i o n t e s t i n g by General E l e c t r i c on dysprosium oxide mixtures. 8 Since t h e cross section of dysprosium oxide was not s u f f i c i e n t l y high, the choice of materials was between GdpO3 and Eu2O3.

Gadolinium

was chosen because it w a s from one-third t o one-fourth less expensive than Eu2O3. Because pure gadolinium oxide r e a c t s with water i n t h e air,

it w a s d i l u t e d with aluminum oxide. I

A s e r i e s of t e s t s w a s run i n boiling

water and water-saturated air a t 700째C t o determine t h e aluminum oxide content needed.

Although 20% A1203 performed s a t i s f a c t o r i l y , 30% A1203

w a s chosen as added protection.

To prevent t h e "self welding" of the elements during operation, a

preoxidation was specified.

It was necessary t o perform t h i s operation

on t h e finished element t o avoid contamination of t h e closure welds. From experience gained i n t h e manuf'acture of the prototype control rods, specifications (Appendix A) and drawings (Appendix B) were prepared. Quotations were obtained from several control rod manufacturers and were carefully evaluated.

The prime contract f o r manufacturing t h e control

elements w a s awarded t o Westinghouse Atomic Power Division.

COMPONENT MANUFACTURE *

The top and bottom closures were machined from Inconel bar stock. The inner and outer tubes were made from tubing drawn t o t h e correct size.

The manpfacture and inspection procedures f o r the Inconel p a r t s

%.F. k i t t e n , Jr., The S t a b i l i t y of Europium Oxide i n SiliconBearing S t a i n l e s s S t e e l , ORNL-2946 (Aug. 9, 1960). 7G. L. Ploetz e t al., "Dysprosium Oxide Ceramics," J. Am. C e r a m .

SOC.43, 154-59

(19w'

8F. H. Megerthand and D. L. Zimmerman, VBWR I r r a d i a t i o n of Reactor Control Materials i n Tubes Containing Simulated Defects, GEAP-3927 (June 1963).

=bd are given i n Appendix A.

I n t h e case of the tubing, t h e ORNL Tubing

Specification (JS-81-183, Part 11) was rewritten by the vendor, who

added additional manufacturing requirements and purchased the material from a tubing vendor.

The tubing vendor performed the inspection and

c e r t i f i e d the material t o ORNL specifications.

I n the case of t h e bar,

Westinghouse purchased the material t o ASTM specification, performed the necessary inspection, and c e r t i f i e d t o the ORNL specification (JS-81-183, Part 111). I n both cases, the material was inspected by u l t r a s o n i c and penetrant methods a s r a w stock and examined by p e n e t r m t methods a f t e r f i n a l machining. ,

All of t h e raw material had certifiedr chemical analyses

and mechanical properties, and samples of each heat of material were

i I

retained.

A flowsheet f o r cladding components i s given i n Appendix C,

Procedure 1. The Gd203-Al203 bushings f o r t h e prototype control element were hot pressed, but Westinghouse proposed t o manufacture the production bushings by conventional pressing and s i n t e r i n g .

I n work performed previously a t

ORNL, a chemical reaction occurred a t 165OoC, and the p e l l e t s became severely distorted; a t 1750°C they melted.

Westinghouse could manufac-

t u r e bushings t h a t would meet the specifications except t h a t they were Experiments a t ORM;

so hygroscopic t h a t they dissolved i n boiling water.

showed t h a t bushings could be made t h a t were not hygroscopic by prereacting t h e powder a t 1650°C and then pressing and s i n t e r i n g .

To manufacture a

bushing t h a t w o u l d not r e a c t w i t h water, Westinghouse used a prereacting s t e p on a l l production bushings. The manufacturing procedure used f o r t h e bushing i s outlined i n i

Appendix C, Procedure 2.

The process s t a r t e d with mixing the A1203 and

Gd203 powder, pressing, and prereacting a t 1700°C. were crushed, ball-milled,

The reaction products

sized, pressed i n t o bushings, presintered,

and then sintered a t 1450°C.

Bushings made by t h i s method were boiled

i n w a t e r f o r 48 hr without any,appreciable weight loss.

Each bushing

w a s then given a thermal shock t e s t by heating t o 1400°C and quenching ~~

1963, -

9R. B. Briggs e t al., MSR Program Semiann. Progr. Rept., July 31, ORNL 3529, p. 78.

6 i n water.

G-

After s&face grinding, t h e bushings were v i s u a l l y inspected

f o r chips o r cracks.

Bushings were reJected i f they had chips longer

than l/8 i n . o r d e e e r than 1/32 i n .

Each bushing was weighed and dimen-

s i o n a l l y inspected with go-no-go gages;

The content of Gd2O-3 w a s a l s o

determined spectrographically f o r each batch. Three bushings were selected f o r each control element so t h e i r combination would y i e l d the proper stack height and t o t a l weight of Gd2O3.

The Gd2O3 content was computed from t h e weight of t h e bushing a

and the results of the spectrographic analysis f o r Gd2O3. Experience Showed t h a t even a f t e r a 150째C bake, t h e bushings could a c t u a l l y release enough gas t o bulge t h e Inconel can during t h e preoxidation of it.

To prevent bulging, it was necessary t o outgas t h e

bushings a t 815째C before loading. CONTROL EIBMENT ASSEMBLY Before production assembly, welding procedures were written and qualified f o r eacn of the four weld j o i n t s required i n a control element. It was necessary t h a t t h e procedures consistently producea defectf r e e weld with a minimum of 0.20 i n . penetration.

The weld must not

contain buildup o r d i s t o r t t h e kan s u f f i c i e n t l y t h a t the element would not pass f i n a l dimensional inspection.

Appendix C, Procedure 3, gives

the welding procedure used, and Fig. 2 shows sections through t y p i c a l top and bottom welds.

If the outer t o p weld was made l a s t , t h e weld

would blow out due t o buildup of gas pressure inside the element.

t h e inner bottom j o i n t was welded last, no d i f f i c u l t y was encountered. This was probably because less gas was heated during welding as a r e s u l t

of t h e configuration of t h e weld j o i n t (see Fig. 2). "he assembly i s described i n Appendix C , Procedure 4 .

After both

t o p welds were made, the bushings were loaded i n t o t h e subassembly i n a helium-filled dry box, and t h e bottom closure w a s pressed i n t o place. The f i n a l two bottom welds were then made.

The element w a s then dimen-

s i o n a l l y inspected with go and no-go gages, and, if necessary, excess weld buildup was removed.

An i d e n t i f i c a t i o n number was electro-etched

bj e

Fig. 2. Sections Through Closure Welds on MSRF: Control Elements. (a) Top closure. (b) Bottom closure.

W-

Fig. 3. Bushings.

Radiographic of MSRE Control Elements, Showing Cracked

i n t o each of t h e elements, and each p a r t used i n the manufacture of t h a t element was recorded.

The element was given a c a r e f u l v i s u a l inspec-

t i o n , helium l e a k checked, and inspected a t t h e welds with postemulsified fluorescent penetrant.

To /prevent s e l f -welding of t h e seg-

ments o r components during service, t h e elements were oxidized by heating t o 927OC.

They were then given a f i n a l v i s u a l and dimensional inspection,

packaged, and shipped. During receiving inspection a t ORNL, radiographic examination (see Fig. 3) revealed t h a t 5 1 of t h e elements contained cracked bushings. These cracks had developed during welding o r during preoxidation.

Since

tests on t h e prototype element showed t h e bushings would crack during t h e f i r s t f e w r e a c t o r cycles i n any event, t h e elements were accepted. The control elements t h a t w i l l be used i n t h e MSRE were run i n t h e control rod t e s t f a c i l i t y f o r a t o t a l of 2000 cycles. changes were noted.

No dimensional

The elements were then put i n t o position i n the

MEBE, where they are presently operating.

SUMMARY By the methods described i n t h i s report, 160 MSFC3 control rod

elements w e r e successfully manufactured.

Figure 4 shows a group of t h e

f i n i s h e d elements.

Fig. 4 .

Three MSRE Control Elements.

APPENDIX A Master Specification f o r the Control Rod Elements f o r the Molten S a l t Reactor

Tentative Specification f o r Seamless Inconel Tubing f o r Molten S a l t Reactor Control Rods

.......................

................ Tentative Specification f o r Inconel Rods f o r the Molten Salt Reactor Control Rod .................... Tentative Specification f o r Gadolinium Oxide - Aluminum Oxide Bushings for Molten S a l t Reactor Experiment

........

27 30

f 4

13 . , MSR CONTROL ROD SPECIFICATION METALS AND CERAMICS DMSION OAK RIDGE NATIONAL LABORATORY

Spec. No. JS-81-183 Part I Date: September 21, 1962 Page 1 of 10

Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee

MASTER SPECIFICATION FOR THF: CONTROL ROD ELEMENTS FOR THE MOLTEN SALT REACTOR

Subject: I.

scorn This s p e c i f i c a t i o n covers the control rod elements f o r the Molten S a l t Reactor. The element consists of Inconel-clad gadolinium oxidealuminum oxide bushing.

11. RliFEmNcEs A.

JS-81-183, P a r t 11, "Tentative Specification f o r Seamless Inconel Tubing f o r Molten S a l t Reactor Control Rods

JS-81-183, P a r t 111, "Tentative Specification f o r Inconel Rods f o r t h e Molten S a l t Reactor Control Rod"

JS-81-183, Part IV, "Tentative Specification f o r Gadolinium Oxide-Aluminum Oxide k s h i n g s f o r the Molten S a l t Reactor Experiment

ASTM Designation: E 2 - 49 T, "Methods of Preparation of Micrographs of Metals and Alloys"

ASTM Designation: E 3 - 58 T, "Methods of Preparation of Metallographic Specimens"

Mil-C-19874 (Ships), 14 May, 1957, ?Military Specification

C l e a n i n g R e q u i r e m e n t s for N u c l e a r P r i m a r y C o o l a n t Eq-lipment

Including Piping Systems" c

MET-NDT-4, Revision 2, "Tentative Methods f o r Liquid-Penetrant Inspection"

Dwg. D-BB-Bb0600,

%SRE Control Rod Assembly a d Details"

111. MANUFACTURING REQtrrREMENTS

The eleaents s h a l l be manufactured i n accordance with O m - D W G 64-1104, 64-1197, 64-1108, and 64-1106 and i n accordance with t h i s specification.

14 \

MSR CONTROL ROD SPECIFICATION METALS AmD CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

Subject:

Spec. No. JS-81-183 Part I Date: September 21, 1962 Page 2 of 10

WTER SPECIFICATION FOR THE CONTROL ROD ELIBENTS FOIi THE

MOLTEN SALT REACTOR

N. MATERIALS Each element s h a l l consist of t h e following components: Item No.

Component

Material

ORNL DWG. No.

Bushing Gd2O+-U203 Inner Tube Inconel

64-1108 64-1104

Outer Tube

Inconel

64-1107

Top Closure- Inconel

64-110 6

Bottom Closure

64-1106

Inconel

Specification No.

Quantity

MET-RM-C 301 JS-81-183, P a r t I1 JS-81-183, P a r t I1 JS-81-183,* P a r t I11

1 1

JS-81-183,* Part I11

V. WEIXIING â&#x201A;ŹEQUIREIvENTS A.

The closures s h a l l be joined t o t h e inner and outer tube by means of a fusion weld made by t h e TIG process.

A l l welds s h a l l have a minimum of 0.020-in. penetration and determined according t o Section X I of t h i s specification.

The welds s h a l l be t i g h t s o t h a t no l e a k w i l l be detected by a mass spectrometer c a l i b r a t e d t o d e t e c t a standard helium leak of 7 x lo-' s t d cc/sec a t room temperature, as specified i n Section VI11 of t h i s specification.

Each closure weld s h a l l be f r e e of surface cracks, surface porosity, o r c r a t e r s t h a t can be detected v i s u a l l y o r with t h e a i d of dye penetrant as specified i n Sections XIV and I X of t h i s specification.

E. Each weld s h a l l be smooth, bright, and f r e e of contamination as determined by v i s u a l inspection.

VI.

WELO Q X L I F I C A T I O N A. The welding procedure shall be submitted t o the Company f o r approval. No q u a l i f i c a t i o n w i l l be performed before t h e Company has approved t h e welding procedure.

No production welding s h a l l be performed before t h e welding procedure has been qualified. ,-

*The closure may be manufactured from heavy w a l l tubing i n accordance with JS-81-l83, Part I1 a t t h e s e l l e r ' s option.

15 MSR CONTROL ROD SPECIFICATION METALS AND CERAMICS DIVISION OAK R I X E NATIONAL LABORATORY

Spec. NO. JS-81-183 Part I D a t e : SeptemSer 21, 1962 Page 3 of 10

Subject:

MASTER SPECIFICATION FOR THE COYTROL ROD ELEMENTS FOR THE MOLTEN SALT mACTOR

WELD Q J A I D I C A T I O N (Continued)

The welding procedure s h a l l be qualified by making three welds of each type.

The welding parameters on the q u a l i f i c a t i o n t e s t s h a l l be set t o give the minimum penetration with the range of parameters allowed i n t h e procedures.

Qualification welds s h a l l meet the requirements of Section V of t h i s specification and s h a l l be inspected i n accordance with Sections XIV and I X of t h i s specification.

i j ~

F. A l l q u a l i f i c a t i o n welds s h a l l be sectioned by the S e l l e r longitudinally through t h e weld area a t approximately 90-deg i n t e r v a l s , thus permitting four penetration measurements on each weld. (One section s h a l l be made a t t h e location where welding was stopped.) One half of the sample elements s h a l l be sectioned a t the i n i t i a l closure weld and the remainder a t t h e f i n a l weld. The sections s h a l l be prepared f o r examination, metallographically measured, and photographed a s specified i n ASTM Designations: E 2 - 49 T and E 3 - 58 T unless otherwise specified i n t h i s specification. The photographs s h a l l become t h e property of the Company and s h a l l be delivered with o r p r i o r t o f i n a l shipment. 1. The sections s h a l l be f r e e of cracks. 2. The sections s h a l l be f r e e of voids, porosity, or inclusions g r e a t e r than 0.005 i n . i n t h e i r l a r g e s t dimension. VI1

INTERNAL ATMOSPHERE A.

The atmosphere within t h e welded element s h a l l not exceed atmospheric pressure by more than 2 psi at room temperature.

The atmosphere within t h e welded element s h a l l contain a t least 504 He.

L)' MSR CONTROL ROD SPECIFICATION METALS AND CERAMICS DMSION OAK RIDGE NATIONAL LABoIiATORY

Subject:

Spec. NO. JS-81-183 Part I Date: September 21, 1962 Page 4 of 10

MASTER SPECIFICATION FOR THE CONTROL ROD EIZNENTS FOR THE MOLTEN SALT REACTOR

VITI. IXAK TESTA.

Each element s h a l l be helium-leak t e s t e d before penetrant inspection o r oxidation i s performed. Helium-leak testing s h a l l be carried out i n accordance with the following procedure :

1. Scope: This section applies t o t h e b e l l - j a r method of t e s t i n g the assembled, helium-containing elements after t h e f i n a l closure weld has been accomplished.

2. Reference: The Manufacturer's operating manual f o r t h e p a r t i c u l a r instrument used i n the inspection. 3. Equipment: A mass-spectrograph type, helium-sensitive instrument, similar t o the Veeco Type Us-9 o r Consolidated Engineering Corporation Type 24-110, which includes t h e following as incorporated i n t h e instrument o r as additions o r modifications:

A cold t r a p (liquid nitrogen o r l i q u i d a i r ) .

A helium-leak source of 7 x ' 0 1

s t d cc/sec.

c. An external o r a u x i l i a r y roughing vacuum pump connected t o t h e instrumen$ manifold and t o t h e specimen o r t e s t chamber through a vacuum valve. d. A t h r o t t l i n g o r modulating valve between the i n s t r u ment manifold and t h e instrument.

e. A low-pressure supply of helium with a nozzle l e s s than 1/16 i n . i n diameter f o r use i n checking f o r leakt i g h t connections. One o r more leak-tight chambers, each of which i s capable of accommodating an element f o r t h e f i n a l closure weld inspection and having no l e s s than 3/8-in. diametral clearance between the element and t h e w a l l of t h e chamber. f.

4. Technical Requirements: a. The instrument s e n s i t i v i t y s h a l l be such t h a t the s t a b l e s i g n a l from t h e standard leak, as determined i n Section VI11 A5c of t h i s specification, i s a t least two times as large as the signals produced by background noise.

17 MSR CONTROL ROD SPECIFICATION

METALS AND CERAMICS DMSION OAK RIDGE NATIONAL LABORATORY

Spec. No. JS-81-183 Part I Date: September 21, 1962 Page 5 of 10

Subject:

MASTER SPECIFICATION FOR THE CONTROL ROD l3lXI'ENTS FOR THE MOLTEN SALT REACTOR

LEAK TEST (Continued) b. The inspection shall be performed i n a force-ventilated location t o f a c i l i t a t e the removal of any helium background. c. The connecting l i n e s between the t e s t chamber and the instrument manifold s h a l l be as short a s i s p r a c t i c a l and should have a minimum inside diameter of 1/2 i n . A l l connections s h a l l be leak-tight. d. Care s h a l l be exercised t o avoid plugging leaks with any sealant p r i o r t o attempted detection with helium. e. A l l assembled elements s h a l l be e i t h e r helium-leak t e s t e d within 48 h r a f t e r t h e f i n a l closure weld i s completed or stored i n a helium atmosphere of pressure equal t o or g r e a t e r than t h e i n t e r n a l pressure of t h e element u n t i l such time as they can be helium-leak t e s t e d . I f an element i s t o be r e t e s t e d or i f the t e s t i n g procedure i s interrupted, as i n Section VIIIM-a, -f, and -g of t h i s specification, t h e element s h a l l be stored i n a helium atmosphere as described u n t i l such time as t e s t i n g can be completed. No assembled element s h a l l be allowed t o remain i n a non-helium atmosphere f o r more than a t o t a l of 48 hr between t h e t i m e of i t s assembly and the completion of helium-leak t e s t i n g . 5.

Testing Procedure : a. The performance of t h e leak-detector equipment s h a l l be v e r i f i e d after each inspection. If a t any t i m e t h i s equipment f a i l s t o function properly as described i n t h e Manuf'acturer ' 8 operating manual, and/or i f t h e s e n s i t i v i t y as determined i n Section VIIIMc of t h i s specification decreases below t h e minimum l e v e l prescribed i n Section VIIIUa, t h e equipment s h a l l be readjusted t o function as specified and recalibrated, and a l l elements which have been inspected during the interim since the l a s t satisf a c t o r y performance v e r i f i c a t i o n of t h e equipment s h a l l be inspected again.

18 MSR CONTROL ROD SPEClFICATION METALS AND CERAMICS D M S I O N OAK FUDGE NATIONAL LABORATORY

Subject:

Spec. No. JS-81-183 Part I Date: September 21, 1962 Page 6 of 10

MASTER SPECIFICATION FOR THE CONTROL ROD EUDvEWB FOR THE MOLTEN SALT KEACTOR

b. The element s h a l l be inspected as f o l l o w : The assembled, helium-containing elements s h a l l be inspected a f t e r t h e f i n a l closure weld has been accomplished by placing the element i n the inspection chamber, evacuating the chamber, and searching f o r helium leaks as prescribed i n the instrument Manufacturer's operating manual. c. The instrument s h a l l be calibrated as follows: The standard l e a k source (7 x 10'' s t d cc/sec) shall be connected t o one end of t h e t e s t chamber. The opposite end of t h e t e s t chamber s h a l l be connected t o t h e manifold, and the time which i s required t o produce a s i g n a l two times as l a r g e as t h e background noise s h a l l be measured. This measurement s h a l l be accomplished while examining a loo$ sample from t h e t e s t chamber and with a l l valves between the standard leak source and t h e helium-sensing device completely open. This portion of t h e c a l i b r a t i o n s h a l l be continued u n t i l t h e s i g n a l from t h e standard leak reaches a s t a b l e amplitude. The s i g n a l amplitude and manifold pressure s h a l l be measured a t t h i s point. d. The inspection s h a l l be made taking a sample from t h e t e s t chamber. A l l valves between t h e element and the helium-sensing device s h a l l be completely open and the time of inspection s h a l l be no less than one minute and a t least twice as long as t h e time, as determined i n Section VIIIASc of t h i s s p e c i f i c a t i o n f o r t h a t p a r t i c u l a r method, required f o r t h e standard l e a k t o produce a s i g n a l t w o times as large as the background noise.

e . The manifold pressure a t which the inspection i s made s h a l l be the same as t h e pressure a t which t h e instrument i s calibrated, as measured i n Section VIIIASc of t h i s specification. Excessive pump-down time s h a l l be i n d i c a t i v e of an external leak. The leak s h a l l be located and corrected before f u r t h e r t e s t i n g i s accomplished.

19 MSR CONTROL ROD SPECIFICATION METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

Subject:

Spec. No. JS-81-183 Part I Date: September 21, 1962 Page 7 of 10

MASTER SPECIFICATION FOR THE CONTROL ROD ELEMENTS FOR THE MOLTEN SALT mACTOR

LiEAK TFST (Continued)

g. During the inspection, any s i g n a l which produces an indication two times as large as t h e background noise l e v e l s h a l l be indicative of a through path o r leak i n t h e element being inspected and t h a t element s h a l l be rejected. If more than one assembled element i s k i n g inspected a t the time a leak i s detected, the elements s h a l l be inspected again such t h a t t h e leaking element or elements are i d e n t i f i e d and rejected. h.

A l l rejected, assembled elements s h a l l be disassembled.

Any salvageable p a r t s of the rejected elements may be

reused i n t h e assembly of other elements. A salvageable i t e m i s one t h a t i s reinspected and found t o conform t o t h e specification. IX.

PENETFUIIT INSPECTION OF ELEMENT Each element s h a l l be loo$ examined f o r d i s c o n t i n u i t i e s by means of penetrant inspection i n accordance with MET-"-4, Revision 2. The process times s h a l l be t h a t l i s t e d i n Table 2 of NDT-4 f o r 11 All forms with machine f i n i s h 125 rms o r b e t t e r . " The penetrant inspection s h a l l be performed before the elements a r e oxidized and before t h e elements a r e leak t e s t e d . /-

SURFACE OXIDIZING RE91JIREMl3NTS A.

The outer surface of t h e closures s h a l l be oxidized with a black, adherent high-temperature oxide film t o prevent selfwelding of t h e elements. The e n t i r e outer surface of t h e element may be oxidized.

The process and procedure u t i l i z e d by the S e l l e r t o provide the oxide coating on t h e required surfaces s h a l l be subject t o t h e Company's apkroval.

For,each oxidizing operation, t h e S e l l e r s h a l l include a control s m p l e f o r t e s t i n g purposes. The sample s h a l l be material of i d e n t i c a l s i z e and composition t o t h a t specified f o r the closure. The sample s h a l l be processed with and s h a l l receive the same treatment as t h e production p a r t s . The samples s h a l l become t h e property of t h e Company and s h a l l be delivered with o r p r i o r t o f i n a l shipment.

20 ~

MSR CONTROL ROD SPECIFICATION METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

Subject:

XI.

Spec. No. JS-81-183 Part I Date: September 21, 1962 Page 8 of 10

MASTER SPECIFICATION FOR THE CONTROL ROD EIEMEXTS FOR THE MOLTEN SALT IiEACTOR

DESTRUCTIVE TEST OF WEIlDMENT A.

A sample of I$ of t h e elements w i l l be selected by t h e Company's inspectors. The sample may be selected itmediately a f t e r welding o r a f t e r a l l nondestructive t e s t i n g has been performed a t the S e l l e r ' s option.

All the welds on t h e elements selected f o r t e s t w i l l be sectioned, examined, and photographed i n accordance with Section VIF of t h i s specification. The photographs and sectioned samples s h a l l become the property of t h e Company and s h a l l be delivered with o r p r i o r t o f i n a l shipment.

XII.

The sections s h a l l be f r e e of cracks. The sections shall be f r e e of porosity o r other inclusions greater than 0.005 i n . i n t h e i r l a r g e s t dimension.

The welds s h a l l show a minimum of 0.020-in. a l l sections.

If one o r more elements of t h e 1% random sample are rejected, then double t h e number of elements s h a l l be selected f o r t e s t i n g . If one o r more of the second group a r e determined t o be rejectable, then t h e e n t i r e l o t w i l l be considered r e j e c t a b l e and the S e l l e r w i l l be responsible f o r i n i t i a t i o n of corrective action. After i n i t i a t i o n of corrective action, sampling s h a l l again go i n t o e f f e c t a s described above.

penetration on

DIMENSIONAL INSPECTION A.

After oxidization, t h e elements s h a l l be inspected f o r inside and outside diameter and length, using the following gages: Inspection Area

ID OD Length

Go Gage (in.)

No Go Gage (in.)

0.785 min

0.795 max

1.150 m a x 1.578 m a x

1.130 min 1.547 min

Length of Gage (in.) 1 3/4 min 1 3/4 min

The gages s h a l l become t h e property of t h e Government.

Any reworking performed on t h e element t o pass t h e above test must be approved by the Company.

21 MSR CONTROL ROD SPECIFICATION METALS AND CERAMICS D I V I S I O N OAK RIDGE NATIONAL LABORATOIiY

Subject:

XIII.

Spec. No. JS-81-183 Part I Date: September 21, 1962 9 of 10 Page

MASTER SPECIFICATION FOR THE CONTROL ROD EI;EMENTS FOR THE MOLTEN SALT RJ3ACTOR

IDENTIFICATION AND RECORDS A.

Immediately after assembly, each element s h a l l be given an identifying number. The number s h a l l be marked on each element by means of an e l e c t r o l y t i c etch.

The S e l l e r s h a l l be responsible f o r maintaining a complete record of a l l materials and process treatments which are required i n t h e f a b r i c a t i o n of t h e completed element. The information t o be included s h a l l be such as t h e following: heat numbers, batch o r blend numbers, process numbers, weight and density of t h e GdzO3-AI.203, inspection r e s u l t s , t e s t results, dimensional measurements, and process treatments. A complete report of a l l such data on each element s h a l l be furnished i n f i v e copies t o t h e Company p r i o r t o shipment of the completed elements. Additionally, t h e S e l l e r s h a l l submit t o t h e Compaw f i v e copies of c e r t i f i e d chemical analyses, physical properties data, and such other t e s t reports as are required i n the individual component specifications immediately upon r e c e i p t of these o r upon completion of f a b r i c a t i o n i n h i s shop. The maintenance and submission of these records along with a c e r t i f i c a t e of compliance t h a t t h e elements conform t o the requirements of t h i s specification s h a l l be a condition of acceptance of the elements.

XIV.

The S e l l e r s h a l l submit t o t h e Company f o r information any i n t e r n a l procedures used i n t h e manufacture of t h e elements o r any s p e c i f i c a t i o n w r i t t e n f o r a subvendor, provided t h e information i s not considered proprietary.

VISUAL INSPECTION A.

Each element w i l l be given a c a r e f u l v i s u a l inspection by a qualified inspector under 100 footcandles j u s t p r i o r t o , shipment. Any v i s u a l indication questioned by the Company's inspector

If t h e element w i l l not meet any provision of t h e s p e c i f i c a t i o n a f t e r removal of t h e indication, t h e element s h a l l be rejected. After removal of the indication, t h e element w i l l be completely inspected.

must be removed.

MSR CONTROL ROD SPECIFICATION METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

Subject:

Spec. No. JS-81-183 Part I Date: September 21, 1%2 of 10 Page 10

MASTER SPECIFICATION FOR THE CONTROL ROD EXEMFXFS FOR THE MOLTEN SALT FEACTOR

VISUAL INSPECTION (Continued)

The element s h a l l be free of o i l , grease, d i r t , o r o t h e r foreign matter as specified i n Mil-C-19874.

xv. s w m s A.

XVI.

Samples from each l o t of I n c o n e l m a t e r i a l used n t h e element s h a l l be furnished by the S e l l e r with o r p r i o r t o f i n a l shipment.

FINAL INSPECTION F i n a l inspection w i l l be performed a t Oak Ridge by t h e Company.

23 REACTOR MATERlAL SPECIFICATION

METALS AND CERAMICS DMSION OAK RIDGE NATIONAL LABORATORY

Spec. No. JS-81-183 P a r t I1 Date: September 21, 1962 Page 1 of 4

Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee Subject:

TENTATIVE SPECIFICATION FOR SEAMLESS INCONEL TUBING FOR MOLTEN SALT mACTOR CONTROL RODS

SCOPE 1.

(a)

This specification covers seamless Inconel tubing f o r t h e control rod elements f o r t h e Molten S a l t Reactor.

Tubing s h a l l be produced i n s t r i c t accordance with requirements f o r t h e specified grade of Tentative Specifications f o r Nickel-Chromium-Iron Alloy Seamless Pipe and Tube (ASTM Designation: A 167 - 61 T) except as modified herein. ASTM A 167 - 61 T s h a l l be considered p a r t of t h i s specification. Modifications are arranged under corresponding headings, sections, paragraphs, and t a b l e numbers of t h a t standard. Additional requirements are given under appropriate headings. MANUFACTURE

(a) The tubes s h a l l be cold-drawn and annealed

CHECK ANALYSIS 6.

(b)

A check analysis s h a l l be made by t h e Manufacturer o r S e l l e r on one tube from each l o t of finished material.

SPECIAL mâ&#x201A;Ź&JI#EMENTs I

15.

(a) Ultrasonic t e s t i n g shall be performed on a l l tubes as given below:

(1) Technical Requirements: The tubing s h a l l be inspected a t t h e completion of t h e manufacturing process. No drawing operation s h a l l be accomplished after t h e ultrasonic inspection. (2) Inspection Eqyipment: The instruments and accessory equipment s h a l l be of t h e pulse-reflection type with s u f f i c i e n t s e n s i t i v i t y t o d i s t i n g u i s h t h e reference notches as required during calibration. The transducer employed s h a l l have no dimension g r e a t e r than 1 i n .

24 REACTOR MATERIAL SPECIFICATION ' METALS AND CERAMlCCS DIVISION OAK RIDGE NATIONAL LABORATORY

Subject:

TENTATIVX SPECIFICATION FOR SE-SS SALT REACTOR CONTROL RODS

Spec. No. JS-81-183 P a r t I1 Date: September 21, 1962 Page 2 of 4

INCONEL TUBING FOR MOLTEN

SPECIAL RE$IJIREMENTS (Continued)

( 3 ) Calibration Standards: A c a l i b r a t i o n standard s h a l l be prepared from tubing taken from t h e same heat and manufactured by the same processes as t h e tubing t o be inspected and s h a l l be f r e e of defects; t h e tubing used f o r t h e c a l i b r a t i o n standard s h a l l be the same s i z e as the tubing t o be inspected and s h a l l be i n the as-polished condition. A longitudinal reference notch, 1/4 i n . long w d with a maximum depth of 0.0025 i n . (the depth s h a l l include t h e highest point of the metal due t o upset, although "deburring" i s permitted), s h a l l be machined on the outs i d e and inside surfaces of t h e standard. The notch may be made by t h e e l e c t r i c a r c discharge method. If both reference notches a r e on t h e same end of the standard, they s h a l l be a t least 120 deg apart. The width of t h e reference notch s h a l l not exceed twice i t s depth.

(4) Equipment Calibration: Using the c a l i b r a t i o n standard specified i n Section 15 (a) (3), the equipment s h a l l be adjusted t o produce indications t h e same height from both the inside and outside reference notches. The r e j e c t i o n alarm s h a l l be adjusted t o s i g n a l a t the indication of t h e lesser amplitude. The equipment s h a l l be calibrated a t the same circumferential speed and rate of t r a n s l a t i o n (feed helix) of t h e c r y s t a l with respect t o t h e tube s h a l l be the lesser of 3/8 i n . per revolution o r 1/2 t h e c r y s t a l or collimator width o r diameter.

(5) Inspection Procedure: The material s h a l l be t e s t e d f o r radial-type defects i n both circumferential d i r e c t i o n s under i d e n t i c a l conditions which a r e used f o r c a l i b r a t i o n of t h e equipment.

The equipment s h a l l be recalibrated as specified i n Section 15 (a) (3) after t h e inspection of 10 lengths of tubing o r when any adjustment t o t h e equipment i s made. When s i g n i f i c a n t adjustment of the equipment i s required during the c a l i b r a t i o n check (any time t h e i n s i d e and outside reference notches do not present a reJectable s i g n a l ) , t h e preceding t e n tubes s h a l l be reinspected i n accordance with Section 15 of t h i s specification. I

25 Spec. No. JS-81-183 Part I1 Date: September 21, 1962 Page 3 of 4

REACTOR MATERIAL SPEC~ICATION METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

SubJect:

TENTATIVE SPECIFICAmON FOR SEAMIESS INCONEL TUBING FOR MOLTEN SALT REACTOR CONTROL RODS i

SPECIAL R E G X J ~(Continued) S

(6) Defects and Rejection: All indications of d i s c o n t i n u i t i e s equal t o or g r e a t e r than t h e l e s s e r indication of the reference notches as described i n Section 15 (a) ( 3 ) s h a l l be considered as defects and s h a l l be rejected. If the defect i s reworkable, it may be removed and reinspected u l t r a s o n i c a l l y . Reworked material s h a l l conform t o the dimensional requirements of t h i s specification. (c) The material i s intended f o r use i n nuclear applications. SUIiFACE FINISH AND WORKMANSHIP 16.

The f i n i s h e d tubing s h a l l be f r e e from oxide o r scale and any other foreign material. The f i n i s h e d tubing s h a l l be f r e e of cracks, seams, laps, gouges, t e a r s , o r other defects which exceed 0.002,in. Such defects of l e s s depth which have sharp contours s h a l l be removed a t request of the Company. Defects may be removed by grinding, provided the w a l l thicknesses are not decreased t o l e s s than 0.018 i n . Ground areas s h a l l have t h e same surface f i n i s h requirements as unground areas of the tube. Ground areas s h a l l merge smoothly with t h e adjacent surface.

MARKING 17. Each length of tubing s h a l l be marked w5th the following information:

(1) Specification No. (JS-81-183) (2) Lot number, ( 3 ) Manufacturer s private identifying mark, and (4) Heat number.

CERTIFICATION AND INSPECTION

18.

(b)

The S e l l e r s h a l l submit t o t h e Company the Manufacturer's c e r t i f i e d statement of compliance t h a t a l l tubing conforms t o requirements of ASTM B167 - 61 T and JS-81-183, Part 11.

26 ~

REACTOR MATERIAL SPECIFICATION METALS AND CERAMICS DMSION OAK RIDGE NATIONAL LABORATORY

Subject:

TENTATIVE SPECIFICATION FOR SEAMLESS INCONEL TUBING FOR MOLTEN SALT KEACTOR CONTROL RODS

CERTIFICATION '

Spec. No. JS-81-183 P a r t I1 Date: September 21, 1962 Page 4 of 4

AM) INSPECTION

(Continued)

(c)

The S e l l e r s h a l l submit t h e r e s u l t s of a l l required tests. Each t e s t report s h a l l i d e n t i f y form, s i z e , heat number, and l o t number. The following test reports s h a l l be furnished by . t h e Seller: (1) Chemical analyses (ladle and check), (2) Tensile properties, (3) e d r o s t a t i c test, and (4) Ultrasonic t e s t .

(e)

The S e l l e r s h a l l n o t i f y t h e Company f i v e days i n advance of date s e t f o r t e s t i n order t h a t the Company's inspector may be present t o w5tness u l t r a s o n i c inspection, t o review t e s t reports, t o check dimensions, and t o v i s u a l l y inspect t h e tubing.

! 3 ~

LidT

27 FUWCTOR MATERIAL SPECIFICATION METALS AND CERAMICS DMSION OAK RIDGE NATIONAL LABORATORY

Spec. No. JS-81-183 P a r t I11 Date: September 21, 1962 Page 1 of 3

Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee i

Subject:

TENTATIVE SPECIFICATION FOR INCONEL RODS FOR THE MOLTEN SALT REACTOR CONTROL ROD

SCOPE This s p e c i f i c a t i o n covers Inconel centerless-ground rods f o r the Molten S a l t Reactor. The rods s h a l l be produced i n s t r i c t accordance with requirements of t h e Tentative Specification f o r Nickel-Chromium from Alloy Rod and Bar (ASTM Designation: B 166 - 61 T) except as modified herein. ASTM B 166 - 61 T s h a l l be considered p a r t of t h i s s p e c i f i cation. Modifications a r e arranged under corresponding headings, sections, paragraphs, and t a b l e numbers of t h a t standard. Additional requirements a r e given under other appropriate headings. MANUFACTURER

(a)

The rod s h a l l be hot-worked,

annealed, and centerless-ground.

(b)

Dimensional requirements are a t the S e l l e r ' s option. p a r t s must be i n accordance with Dwg. D-BB-E40600.

Finished

SAMFL ' ES FO2 CHEMICAL ANALYSIS

(b)

A check analysis s h a l l be made by the Manufacturer or S e l l e r on each l o t of finished material.

SPECIAL R E 16.

(a)

An u l t r a s o n i c t e s t w i l l be performed as follows: 1. The reference standard s h a l l consist of two 1/16-in.-diam flat-bottomed holes positioned a t l e a s t 2 i n . apart, one of which s h a l l be d r i l l e d t o a depth of one-fourth of t h e bar diameter and t h e other t o a depth of three-fourths of t h e bar diameter; a 1/32-in.-diam hole d r i l l e d t o a depth of a t least 3/4 i n . i n t o t h e end of t h e standard, p a r a l l e l t o t h e axis, and a t a distance of one-fourth of the bar diameter from the axis; and a notch 0.005 i n . i n depth (of optional cross section) cut p a r a l l e l t o t h e longitudinal axis.

2. The reference standard s h a l l be made from bar material similar t o t h e bars under t e s t i n s i z e , type, temper, form, and surface f i n i s h . A l l surfaces, except t h e ends, s h a l l be scanned i n a c i r cumferential d i r e c t i o n with a minimum overlap of 50% of the c r y s t a l width and a t a surface speed not t o exceed 6 in./sec.

6@J. IIEACTOR MATERIAL SPECIFICATION METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

Subject:

Spec. No. JS-81-183 P a r t I11 Date: September 21,' 1962 3 Page 2 of

"TATIVE SPECIFICATIONFOR INCONEL RODS FOR THE MOLTEN SALT REACTOR CONTROL ROD

SPECIAL REQUIREMENTS (Continued)

The transducer s h a l l be no l a r g e r than 3/4 i n . i n diameter.

5. The equipment s h a l l be calibrated with the use of the appropriate reference standard. Clear indications s h a l l be demonstrated from t h e f l a t bottom of each r a d i a l hole, from t h e s i d e of the hole p a r a l l e l t o t h e axis, and from the side of the reference notch. The response f r o m t h e hole p a r a l l e l t o t h e axis s h a l l be discernible when the hole i s rotated approximately 90 deg from t h e c r y s t a l position. 'If adequate indications from a l l notches and holes can be demonstrated with a single t e s t setup, t h i s shall be considered s u f f i c i e n t f o r t h e required inspection. However, it may be necessary t o make separate inspection setups and c a l i b r a t i o n s t o achieve t h e ,specified s e n s i t i v i t y f o r a p a r t i c u l a r reference standard. The amplitude of t h e back surface r e f l e c t i o n a t a reduced-sensitivity s e t t i n g s h a l l be noted f o r determination of differences i n u l t r a s o n i c attenuation properties i n t h e t e s t material as comi pared t o t h e reference standard. "he equipment s h a l l be calibrated a t t h e same speed and rate of t r a n s l a t i o n t h a t w i l l be used f o r t h e inspection. 6. The maximum indication from any detected discontinuity s h a l l be r e l a t e d t o t h e reference defect which i s most nearly comparable i n regard t o cross-sectional position and with t h e reference and detected d i s c o n t i n u i t i e s being, as near as p r a c t i c a l , t h e same distance from the transducer. Bars containing d i s c o n t i n u i t i e s which produce indications equal t o or g r e a t e r than t h e proper reference defect, after consideration of differences i n u l t r a s o n i c attenuation properties between the standard and the t e s t material, s h a l l be rejected.

WORKMANSKIP AND FINISH

17.

A l l defects s h a l l be explored f o r depth. When the depth encroaches on t h e minimum specified dimensions, the bar s h a l l be rejected.

c \

REACTOR MATERIAL SPECIE'ICATION METALS AND CERAMICS DMSION OAK RIDGE NATIONAL LABORATORY

Spec. No. JS-81-183 P a r t I11 Date: September 21, 1962 Page 3 of 3

Subject:

TENTATIVE SPECIFICATION FOR INCONEL RODS FOR THE MOLTEN SALT REACTOR COPJTROL ROD

CERTIFICATION AND INSPECTION

18. (b) The S e l l e r s h a l l submit t o t h e Company t h e Manufacturer's c e r t i f i e d statement of compliance t h a t a l l bars conform t o t h e requirements of ASTM B 169 - 61 and JS-81-183, Part I11 and s h a l l a t t a c h c e r t i f i e d r e p o r t s of results of a l l required

tests. (c)

Each test report s h a l l adequately i d e n t i f y the material as t o form, s i z e , and heat number. The following reports s h a l l be furnished by the S e l l e r : (1) Chemical analyses ( l a d l e and check), (2) Tensile properties, m d ( 3 ) Ultrasonic t e s t .

(e)

The S e l l e r s h a l l n o t i f y the Cumpany f i v e days i n advance of date set f o r t h e t e s t i n order t h a t t h e Company's inspector may be present t o witness the u l t r a s o n i c and fluid-penetrant t e s t s , t o check dimensions, t o v i s u a l l y inspect the bars, and t o review the t e s t reports.

30 Spec: JS-81-183, P a r t IV Date: September 3 , 1964 Rev. No: Page : 1 of 5

NUCUAR IiEACTOR SPECIFICATION METALS AND CERAMICS DIVISION 'OAK RIDGE,NATIONAL LABORATORY Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee 1 Subject:

ALUMINUM TENTATIVE SPECIFICATION FOR GADOLINIUM OXIDE OXIDE HJSHINGS FOR MOLTEN SALT IiEACTOR EXPEXIMENT

SCOPE: -

This s p e c i f i c a t i o n covers gadolinium oxide aluminum oxide (Gd2O3 Al203) bushings f o r use i n control rods f o r nuclear reactors.

11. RF3FEmcEs: ,

ORNL Dwg. 64-1108. 111. MANUFACTURING RE68JIREMENTS:

Individual gadolinium oxide aluminum oxide (Gd2O3 - A l 2 O 3 ) bushings and stacks of bushings ready f o r canning s h a l l be manuf'actured i n accordance with t h i s specification. IV.

DEFINITIONS: A.

A l o t of gadolinium oxide power consists of a l l GdpO3 powder i d e n t i f i e d by t h e same l o t number.

A l o t of aluminum oxide powder consists of a l l A1203 powder of t h e same grade designation received a t t h e same t i m e .

A blend l o t consists of a l l A1203 Gd2O3 powder and recycles sintered o r green material which a r e mixed together a t the same t i m e f o r pre-reacting.

D. A pressing l o t consists of a l l shapes pressed from a blend l o t t o t h e same green density range.

E. A s i n t e r i n g l o t consists of all shapes pushed through t h e s i n t e r i n g furnace a t t h e same t i m e .

CHEMICAL COMPOSITION: A.

S t a r t i n g aluminum oxide powder s h a l l be 99.9$ minimum p u r i t y based on i g n i t e d weight and aluminum oxide content.

S t a r t i n g gadolinium oxide powder s h a l l be of 99.9$ p u r i t y based on i g n i t e d weight and r a r e e a r t h content.

31 Spec: JS-81-183, P a r t IV Date: September 3, 1964 Rev. No: 2 of 5 Page :

NUCI;EAR REACTOR SPECIFICATION

METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee Subject:

AIUMINUM TENTATIVE SPECIFICATION FOR GADOLINIUM OXIDE OXIDE BUSHINGS FOR MOLTEN SALT FEACTOR EXPERIMENT ~

VI.

~~~

CHEMICAL COMPOSITION:

(Continued)

Finished shapes ready f o r canning s h a l l consist primarily of A1203 and Gd2O3 or compounds thereof and s h a l l have a completion of 65-14 w t $ Gd2O3.

DENSITY: A.

For purpose of density calculations, the following parameters s h a l l be used: Theoretical density of A1203 Theoretical density of Gd2O3

Theoretical density

3.96 gm/cc

7.407 gm/cc

29% A1203 - 71% Gd203 28% A1203 - 72% Gd2O3 -

Theoretical density 30$ A1203 Theoretical density

70% GdzO3

5.873 gm/cc 5.914 gm/cc 5.955 gm/cc

The sintered bushings s h a l l have a minimum density of 95% of theoretical.

A stack of bushings ready f o r canning shall have dimensions f a l l i n g within the envelope defined by ORNL-Dwg. 64-1108 and s h a l l weigh a minimum of 41.100 gms.

The t o t a l Gd2O3 content of t h e stack s h a l l be computed by multiplying t h e s t a c k weight by the average analyzed Gd2O3 content. The analyzed Gd2O3 content i s t h a t obtained by analysis of sintered bushings from each blend l o t (Par. 9 . b . 3 ) . If more than one blend l o t i s represented i n a stack of bushings, the Gd2O3 content s h a l l be computed f o r each bushing and the results then summed t o g e t t h e t o t a l stack Gd2O3 content. I n e i t h e r case the minimum t o t a l stack Gd2O3 content s h a l l be no less than 28.770 gms.

NUCLEXfl REACTOR SPECIFICATION

METALS AND CERAMICS DIVISION 9AK RIDGE NATIONAL LABORATORY

Spec: JS-81-183, Part IV Date: September 3, 1964 Rev. No: Page : 3 of 5

Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee Subject: VI1

VI11

TENTATIVE SPECIFICATION FOR GADOLINIUM O X I E AIUMINUM OXIDE BUSHINGS FOR MOLTEN SALT REACTOR EXPERIMENT

DIMENSIONS: A.

Not more than three bushings may be stacked t o make an assembly (stack) f a l l i n g within the envelope defined by ORNLDwg. 64-1108.

Individual bushings and stacks of bushings s h a l l be shown i n Om-Dwg. 64-1108.

SURFACE FIIVISH AND CONDITION: Chipping on t h e inner and outer cylinder surfaces shall not exceed 546 of t h e inner and outer c y l i n d r i c a l surface areas, respectively. Chipping on t h e surface of each end of the bushings s h a l l not exceed 546 of the surface area of one end of the bushings. No chipped area s h a l l be greater than 1/16 i n . i n l a r g e s t l a t e r a l dimension nor greater than 1/32 i n . deep. The finished material s h a l l be f r e e of cracks. TEST REQUIREMENTS: A.

Non-Destructive

1. Visual All bushings s h a l l be subjected t o v i s u a l inspect i o n under d i r e c t daylight-type fluorescent l i g h t i n g of a t l e a s t 100 footcandles t o insure conformance with t h i s specification.

2. Dimensional

All individual bushings s h a l l be subjected t o dimensional inspection t o determine conformance with w a l l thickness v a r i a t i o n requirements s e t f o r t h i n ORNLDwg. 64-1108. All stacks of bushings s h a l l be subjected t o dimensional inspection t o determine conformance with o v e r a l l envelope dimensions s e t f o r t h i n ORNL-Dwg. 64-1108.

All stacks of bushings s h a l l be weighed t o determine conformance with stack weight requirements set f o r t h under ' b n s i t y " above.

3. Weight

Destructive

1. A sample of each l o t of aluminum oxide powder s h a l l be analyzed t o determine conformance with p u r i t y set f o r t h under "Chemical Composition. "

33 " 3REACTOR SPECIFICATION METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

Spec: JS-81-183, Part N Date: September 3, 1964 Rev. No: 4 of 5 Page :

Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee Subject: IX.

TENTATIVE SPECIFICATION FOR GADOLINIUM OXIDE ALUMINUM OXIDE BUSHINGS FOR MOLTEN SALT mACTOR EXPERIMENT

TEST REâ&#x201A;Ź&JIRE3ENTS:

(Continued)

2..

A sample of each l o t of gadolinium oxide powder s h a l l be analyzed t o determine conformance with p u r i t y set f o r t h under "Chemic a l Composition 'I.

Two sintered bushings from each blend l o t (one each from two d i f f e r e n t s i n t e r i n g l o t s ) s h a l l be broken i n t o quarters and two opposite quarters analyzed separately t o determine t h e Gd2O3 content. "he remaining quarters s h a l l be forwarded t o the Company f o r check analysis.

CERTIFICATION AND INSPECTION: A.

The S e l l e r s h a l l submit t o t h e Company t h e c e r t i f i e d statements and reports required i n Section 10 (b) of t h i s specification.

Statements t h a t the material complies with requirements of t h i s s p e c i f i c a t i o n s h a l l accompany t h e t e s t reports which s h a l l include the following results: 1. Chemical analyses on s t a r t i n g v i r g i n aluminum oxide powder and s t a r t i n g v i r g i n gadolinium oxide powder.

Chemical analyses on sintered bushings.

Visual inspection of sintered bushings.

Results of GO-NO GO I D and OD bushing inspection.

Individual heights and summation of heights of bushings i n eacQ stack.

k s h i n g stack weight.

Remaining quarters of s i n t e r e d bushings Section 9.b.3. s h a l l be i d e n t i f i e d and supplied t o the Company f o r check analysis.

The S e l l e r s h a l l n o t i f y the Company f i v e ( 5 ) days i n advance of date s e t f o r s t a r t i n g of production t e s t i n g i n order t h a t Company's inspector may be present t o witness t e s t i n g .

34 MTCUAR REACTOR SF'ECDICATION METALS AND CERAMICS DIVISION OAK RIDGE NATIONAL LABORATORY

Spec: JS-81-183, P a r t IV Date: September 3, 1964 Rev. No: Page : 5 of 5 ~

Union Carbide Nuclear Company A Division of Union Carbide Corporation Oak Ridge, Tennessee Subject:

TENTATIVE SPECDICATION FOR GADOUNIUM OXIm - AIUlWWM OXIDE BUSHINGS FOR MOLTEN SALT REACTOR EXPERIMENT I

XI.

THERMAL CYCm TEST: A.

A thermal cycle t e s t s h a l l be performed by t h e Seller on each bushing from a temperature of 1475 k 25째F t o room temperature i n 10 sec. The method of thermal cycling shall be as follows:

1. Heat Gd2O3 - A1203 bushings ie a i r i n a furnace operating a t 1475 k 25V f o r a t l e a s t the time necessary f o r t h e bushings t o approach t h e same color as t h e i n t e r i o r of t h e furnace as judged by eye. As an a l t e r n a t i v e , bushings may be placed i n a cold o r a warm furnace and both furnace and bushings r a i s e d i n temperature t o a furnace temperature of 1475 k 25 "F before bushings are removed (next s t e p ) .

2. Remove bushings from furnace one a t a t i m e and quench immediately i n a container of cold t a p water. Allow bushings t o remain i n water f o r a t least 1/2 min. 3.

D r y bushings by a i r drying and/or heating f o r a minimum of

one hour a t 250째F o r higher i n air. 4.

Inspect bushings f o r cracks.

Any bushings having cracks s h a l l be r e j e c t e d .

APPENDIX B Fig. 5 . Fig. 6. Fig. 7 . Fig. 8.

I i

.......... Dimensions of Inner Tube . . . . . . . . . . . . . . . . Dimensions of Outer Tube . . . . . . . . . . . . . . . . Assembly and Closure of Control Element . . . . . . . . Bushing and Bushing Stack Dimensions

37 37 38 38

37 UNCLASSIFIED ORNL-DWG 64-4108

0.010 MAX. PERMISSIBLE VARIATION IN WALL THICKNESS

Q I

I-

1.330 4.315 NOM. MIN. MAX. (SEE NOTE 1 I

0.040?gt:0ID

INDIVIDUAL BUSHING

BUSHING STACK

NOTE: TOTAL LENGTH SHALL BE DETERMINED BY THE DIMENSION OF THE MINIMUM LENGTHS OF EACH BUSHING IN STACK. BUSHING MINIMUM LENGTH TO BE DETERMINED BY INDICATING OUTER PERIPHERY OF EXPOSED F L A T FACE OF BUSHING LYING ON F L A T FACE, USING EQUIPMENT SIMILAR TO STARRETT BENCH GAGE N0.652. DIMENSIONS ARE IN INCHES

Fig. B-1.

Bushing and Bushing Stack Dimensions.

UNCLASSIFIED ORNL-DWG 6 4 - ! 1 0 7

0.0207

1.465 NOM.-

TOLERANCE: k0.002 U.O. S. I

OD AND ID TO BE CONCENTRIC WITHIN 0.002 TIR.

i! w 1

DIMENSIONS ARE IN INCHES.

NOTE: NO SURFACE DEFECTS GREATER THAN 0.002 DEEP PERMITTED

REMOVE A L L BURRS

Fig. B-2.

Dimensions of Outer Tube.

38 i

UNCLASSIFIED ORNL-DWG 64-!104

L J

0.020

4.537 NOM.

DIMENSIONS ARE IN INCHES.

OD AND ID TO BE CONCENTRIC WITHIN 0.002 TIR.

Fig. B-3.

NOTE: NO SURFACE DEFECTS GREATER THAN 0.002 DEEP PERMITTED

Dimensions of Inner Tube.

UNCLASSIFIED ORNL-DWG 64-tI06

ID TO GO OVER 0.785 MANDREL; NOT-GO OVER 0.795 MANDREL

TOP

CLOSURE DIMENSIONS ARE IN INCHES. BEFORE WELDING

I-

OD TOGO THRU 4.450 BORE; NOT-GO THRU 1.130 BORE '

FINISHED ASSEMBLY

NOTE: MACHINING OF WELDS TO MEET DIMENSIONS PERMITTED PROVIDED THAT WELD METAL IS NOT MACHINED BELOW THE LEVEL OF SURROUNDING UNMELTED METAL AND THAT METAL IS NOT MACHINED. I

Fig. B-4.

Assembly and Closure of Control Element.

APPENDIX

. . . 41

Westinghouse's Manufacturing Procedure for Cladding Components Westinghouse's Welding Procedure for MSFE Control Elements Westinghouse's Manufacturing Procedure f o r the Gd203-Al203 Bushings. Westinghouse Assembly Procedure for the MSRE Control Elements .

. . . . . 42 ..

47 50

Westlnghouse 's Manufacturing Procedure f o r Cladding Components

,I Inconel Tubing,

"'I"

Incono1 fib%, %all

Inconel Dar Stock (Purchase t o A!3I:-S-166-61T)

(Purchase t o spec. AFD-ORL-~O~) smple t o OWL Retainer sample dinensions a t ends, sample

AClean -

Deerease Wash i n Alccnox + hot wa%er Rinse i n .lot water Alcohol dehydrate (U necessary) Air D r y

clam

Sanple t o ORVL Retainer sample

Inspcct-

Inspect-

Mmensions, Surface Defects

Dimensions, Suxface Defects

A Clean

Decrease Wash i n Alconox + hot water Itlnse i n hot water Alcohol dehydrate (if necessary)

Degrease Wash In Alconox + hot water Rinse i n hot watcr Alcohol dehydrate (if necessary)

Air D r y

Air Dry

Clean Degrease Wash In Alconax + hot water Rinse i n hot water

Alcohol dehydrate (tf necessary)

Westinghouse's Welding Procedure for MSRE Control Elements

Four welds will be made on each control element assembly. The top welds w i l l be made using copper chills. The control element assembly will be positioned in two different planes to make the top closures. The inner weld will be made first and the electrode will be positioned as shown:

Copper Chill

c P

On the bottm rlnp, the outer weld w i l l be made first. Chills w i l l be used to make both welda. The electrodv w i l l be positioned as shownt

Outer Tube > --

Tube w(TpE?

The eleatrode w i l l be positioned over the I.D. of the bottam closure Just as it I s shown for the O.Do

I. tfeldinp: Speciffcations

The follanng parametera have been found t o produce welds of. desired widt,h and penetration with acceptable characteristics. Where a r a q e occurs, the operator may adjust settings within the range given. !&ere settings are marked fixed, the operator will not make changes without specific engineering approval, 11. Welding Operating Parameters A.

Welding Current lo

I h

Top C ~ O S U ~ Battan Closure

4lt-91 amperes (ranee 30-hO mperes (range

Bo Welding Voltage l o TOP C ~ S U ~ 20 Bottan Closure C.

Rotatlorn1 Speed

1, Top Closure 2, Tcp Closure 3o Bottun Closure I, Bottom closure

inside weld outside weld ,fnside weld outside weld

‘

1102 seco/mvo 1102 seco/revo 13.2 geco/rev. l2,2 secc/revo

(fixed) (fixed) (bed) (fixed)

Do Weid T W 1. Bottom Closure 2, Bottom CImwre 30 TGP Closure bo Top Closure

15.5 13 15 U

outside weld inside weld outside wold inside weld

8eCo

(fixed)

Beeo (fixed) see. (fixed) 8eco (fixed)

E, TailTime 1.

outaide weld

inside weld

3,1 seco (fixed) 2.25 see. (fixed)

outside weld i n s i d e weld

2,25 seco (fixed 2,25 sec, (fixad

Bottm Closure Botton Closure 3- Top Closure t o Top Closure

F. Arc Gap Arc gap fixed Go

before welding With a u t m a t i c head at

Vickers Welder Control

1, Arc Control 20 current C O n t F o l 3,, Switchea 80

Panel’ H i - f requency/hanual

Current do Voltage e,,’ Polarity

Crr

0.025 h,

10 (fixed) 90 (fixed) Off (fixed) H i - f requency (fixed)

Remote (fixed) Remote (fixed) Strairht (fixed)

H, Vickors Walder Remote Control 1. Arc Control 2,

9-XI (range) use for m a l l changes in w l d b g ch-8nto

Current Control (use outer calibration only) Bottan Closure Bottom Closure co Top Closure de Top Closure

outside inside outside inside

weld weld weld

weld

.,so5 (range) s& range)

2,O 200 e-

-- -0

6,O 6,o

9,s !range) 9,,5 (ranm)

I e Slope Control 1, Top Current Dial 2*

Top T h e M a l Bottom Current Dial Bottom Time Ma2 SWitChQS

Up (Plixad) On ( f b d ) T a i l Slope only (fixed)

a, Start Slope bo S t a r t and Tail C, Start and T a i l do TailSbp~i

Dawn (fixed)

Control Panel Internal Settims f o r Autmatic Head

1, Stability 2., Hanu& Speed Control 3. Start Compensator be AC/DC A r e Switch

KO Remote Control

outside weld

inside weld outside weld i n s i d e weld

Top closure

0,7 0,7 0,7 007

L O (Range) L O (Range) loo (Range) 1,O (Range)

Hi-Frequency Oscillator

1, Mal

AC/DC Swltch 3e On/Off Snitch 2,

3*2 (fked) 1,s (fixed) 0 (fked) DC Arc (ffxed)

Arc Voltage

1, Bottan Closure 2, 3ottom Closure 3 e TOP C b s ~ ~ e Le

Inert Gas

1, Purity Flow

* Flow of flowing,

each gas i s t o be adjusted with the other gas Gases are in approxjmately a 50-50 ratio,

1, Mahrial Slm3

30 *int Projection from Noazle

70 100 (Range) Ix: (fixed) On (fixed)

Welding grade ( f i x e d ) 10 CF" of He* 10 CFH of A r

No E l e c t m d e 2,

2% Thoriated Tungsten, centerless ground (fixed) l,/14" diameter ( f i x e d )

Rounded

1/16" 1/L" (rmge)

. 46

Material

Size

Ceramic 3 P openine

47 Westinghouse's Manufacturing Procedure f o r the Gd203-Al203 Bushings

Powder 0 ~ :

A1203 Powder

F.S.S. Size Customer Sample Analytical Sample Sample

Custmer Sample

Batch -Welph

! E

Plater and binderwater solution

80 to 10o째C

mrrdte, l?Oo*Cin H2 or cracked MH3 Jaw crusher

h I? HC1,

hr60 ~

Wet Hsgnettc Treat

2 u/o carbo to00 1 u/o PVA

Dry

80 to W 0 C

Gramlate

Dry I

Weigh Individual Charges

â&#x20AC;&#x2DC;3 Presinter

,---

sample

- Visual DiBlenaions

Hoat t o a 7 5 2 25oF, quench in cold tap water

OD Grind

Wmh and A i r Dry I

b Make Stacks and Inspect

Inspect

End Grind

I n d i ~ B i a Iength l

If mcessary, to make stack height.

OD, ID Emlope Wall Thickness

Variation

suundness Chipe

To Assembly

Westinghouse Assembly Procedure f o r t h e EIISRE: Control Elements

Cleaned Outer Inner (large) (small)

Baked Gd203-Al203 r i n g s

Cleaned

Top Sealing Ring

Bottom Sealing Ring

Clean Chill

t Weld

Inspect

OD and I D welds a t t o p For p o r o s i t y ana blow holes

I D Weld Expand Identify

Remove from Store Helium- f i l l e d

OD and I D welds a t bottom

I D Weld Expand

GO-NO-GO Weld OD and I D GO-NO-GO Length

Visual f o r weld and surface defects

Helium Leak I

Dye Penetrant Inspect

Oxidize

Minimum 1 h r a t 1700 t o 1800째F, a i r cool

GO-NO-GO for Inspect

i I

I D , OD and Length

, e

Visual Inspect

Check Records

Ship

UC-25

- Metals,

OWL-4123 Ceramics, and Materials

INTERNAL DISTRIBUTION 1-3. 4-5. 6-25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 4042. 43.

Centra Research Library ORNL - Y-12 Technical Library Document Reference Section Laboratory Records Department Laboratory Records, ORNL R.C. ORNL Patent O f f i c e G. M. Adamson, Jr. J. W. Arendt (K-25) R. J. Beaver H. Beutler G. E. Boyd Ji Young Chang W. H. Cook F. L. Culler J. E. Cunningham D. E. Ferguson J. H Frye, Jr. V. 0. Haynes M. R. H i l l C. E. Iarson

44. 45. 46. 47. 48. 49.

A. P. Litman

H. R. G. H. C. 50. C. 51. J. 52. M. 53. A. 54. C. 55-64. G. 65. T. 66. A. 67. W. 68. M. 69. M.

G. E. B. E.

K. J.

A. W. E. E. M. N. M. J.

B. 76. A. R. 71. J. A.

MacPherson MacPherson hrrow McCoy, Jr. McGlothlan McHargue Parsons (K-25) Rosenthal Richt Sessions Tolson Washburn Weinberg Werner Winton Bever (consultant) Kaufmann (consultant) Krumhansl (consultant)

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75. W. J. Larkin, AEC, Oak Ridge Operations T. W. McIntosh, AEC, Washington , H. M. Roth, AEC, Oak Ridge Operations J. Simmons, AEC, Washington W. L. Smally, AEC, Oak Ridge Operations E. E. Stansbury, University of Tennessee D. K. Stevens, AEC,'Washington J, A. Swartout, Union Carbide Corp., New York A. Taboada, AEC, Washington Given d i s t r i b u t i o n as shown i n TID-4500 under Metals, Ceramics, CFSTI) and Materials Category (25 copies

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