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LA-7972-MSInformal Report

LASL Fabrication Flowsheet for

GPHS Fuel Pellets

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LOS ALAMOS SCIENTIFIC LABORATORYPost Office Box 1663 Los Alamos. New Mexico 87545

DISTRIBUTION OF THIS DOCUMENT IS UNLIMITED

LA-7972-MSInformal Report

UC-23 and UC-25Issued: August 1979

LASL Fabrication Flowsheet for

GPHS Fuel Pellets

R. A. Kent

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P. A. Kent

APAiRACT"

The- rieru.'TrT] I ' i j r i v r . f ' H o . i t r o u r ( . i ' ' G P H S ; b e i n o'If- "• 1 ( i | ! f - l ',; l\\f I n s A l a < o s ' . c i e n M f i c L a b o r a t o r yf o r t h e [ j f p a r t . r o n t o r [ n c - r g / , D i v i s i o n o f A d v a n c e d' , ' u ' 1 e i r O y s t e r s a n d P r o j e c t s , o o n s i s ^ s o f a s e r i e so f M I > M J M i f.<" : - 'P / ! ' . J1 C S , e a c h h a v i n g o t h c n - o i p u w e ri n v e n t o r y o f f>? .rj w a t t s , f a r . ! ) m o d u l o i s l o a d e d

v / i t . h f o u r c y l i n d r i c a l 6 2 . 0 - ' / ? f - P u 0 ; f u e l p e l l e t s .T h i s r e p o r t s u p i r i a r i z e s che s p e c i f i c a t i o n s f o r t h e s ep e l l o t s u j ' i L ' l . ' n i . ' r w i i . i i Lru.1 f a b r i c a L i o nr l e v o l o p e d a t LAc-1 .

i. rrThe Los Alamos Scientific Laboratory (LASL) has been involved for a number

of years in a continuing pronrai" to develop and characterize :'3'Pu0-: fuel formsused in rad ioi sotopic thermal-electric nencrators (RTGs) to [.irovide electric|)ov/or for spacecraft. Once a specific fuel form has been selected and charac-terized, the LACL fabrication parameters and flowsheets are generally trans-ferred to another Department of Energy (DOE) contractor for production. Pre-viously, LASL supplied fabrication information to Mounds Facility (MF) for theplutonia-molyfidenuin-cormet fuel form (PMC) used in the PIONEER, TRANSIT, andVIKING missions and for the 100-W spherical plutonia fuel form (MHW) used in theLES and VOYAGER missions. Subsequently, LASL supplied fabrication informationto the Savannah River Plant and Laboratory (SRP and SRL) for the improved MHWfuel form to be used for the GALILEO mission.

In addition to developing and characterizing specific fuel forms, LASL hasbeen involved in a lonq ranne developmental program to determine the effects offabrication parameters on fuel microstructures and, in turn, the effects ofmicrostructural changes on fuel properties.

The flowsheet, discussed below, for the fabrication of 2 3 8PuO 2 GPHS fuelpellets is the result of the experience aained at LASL, both in the develop-mental program^"4 and in the continuing development and characterization ofspecific fuel forms.^ The initial version of this flowsheet was presented at

[)r;L h e a d q u a r t e r s b y ''. W . Z o c h f r in .July, 1 9 7 ' ; ar;d a s l i n h t l y a m e n d e d v e r s i o nw a s p r e s e n t e d b y c. f. B - ' o n i s z in A p r i l , 1 V 7 0 - l.-ich s t e p in t h e f l o w s h e e t ,i n r l u d i n q ; o d "> f i o a t i o n s , h a s b e e n d i 'j .us s o d in d'-tail in r f e t i n n s b e t w e e n L A C I,-ir,H C,D[ /r:,| |,r.vc,nnnr;i . T h e M n / i l v e r s i o n < / ̂ hr- M o w s h e f f , p r e s e n t e d in t h i sr e ; i o r ' , w a s m o d i f i e d s l i g h t l y b a s e d o n t hf; L A M e , p ^ r i ^ n c e in f a b r k . a t i n q';< i f ! / t h i r t y rii"'Mr, ;.*--! ] et.s f o r t h e desi rin-;>has<-- !••;:-!''. t e s t s e r i e s .

i r i r ^ - . M q [ ' f j j i P T J o : ; A ? ; ; . ; ; i 7 , r ! O P ' 1 f ,"T

•;• s e l e c t e d r / ' i . \ f i j c - 7 f n r " i ' - s h o v / n i n '• '•;. ' . - i - i d c o n s i s t s o f a . " i i h ti f r y l i r i d c r w i t h f a d i u s e d f ' n o c r j p s a n d r< ' ' , ' • • • d 1 i r> y ' : n t s> r / f ; r 6 ? . J v / a t t s .• e n s i o n , ' o r t h ? > e n d c n . s w f r ^ s f l o f . ' r . - d f o d i : - ' i s a t r - f . h ' . ' t " h i c ^ n r - s s / r a d i u s -jnt->r(: r,i f. i o f o> t h r - i r i d i u r ' . n n t . , 1 i n e r . "••' • " u o l ; r . - l U ; t i s ^ a b r i c a t c - d b /

:••-in J ! o s s n - j s o n c d a ' l l ^ O 0 ! " lf,Ct w t ) a n d M'Y)f)C ' ?*'' w t ''. Th.-; r a d i j s o d o n d c a ; si r- r. 'i)r(:ii d . r i n n h o t [ i r o s s i n q a n d n o ' V K . M nins- o r - hf p e l l e t , is r o q u i r o d .,."('rr- h o t |.n :•-,-, i n q , t h e p e l l e t i s s i n t e r e d f o r f h ,i t-. 1 5 ? 7 ° C t o sta.'.ilizp t h e•• i s r o s truf.t -ire- a n d ; > r o d u c e t h e d e s i r e d q r a i n s i z e , ?'-'-.'' ,.v . H r a n u l ^ s e a s o n i n s" -( nr^iir. t ^ ' I ' M - i n n ,-.̂ r> •-,•> tn" rin s a r e lie r f n p v c i i ri r!ii O ' , " : e n - i r a t r o i p h p r e t oM'".' ;.' (• ?.>•"•' !if: i t r o n e; issi r u ' r a t e d u e t o ( ;,nNi r e a r f i o n s v. i th t'ne ' ' 0 a n d :''0: ^top--'1 i r'--sr-nt in n o t r a l o v y n e n . T h e a s - p r e s s e d p ^ l l o t h a s a c e n t e r ! i n f H j _• v ' . e r o* ,-/./'•; ctr: a n d a c e n t e r i i n e l e n q t h o f ? 7 . T . "i> . o u r i n q t h e s u b s e q u e n t;.o'-•-pross •, i P i t ' e r m q , t h e s e d i m e n s i o n s w i l l u s u a l l y s h r i n - O . S t o •).' p e r c e n t>"f-s.iltinq in a p;:ll'"'t d e n s i t y o f al)O'jt '-V\> T O .

T o u r -i'.S'ir;,!. i n n s a n d c o n s t r a i n t s , b a s e d o n t h e L A M e / p e r i e n c e n a i n e d in' :<•} f o r r df'Vf.-lO'nienf a n d in t h e l o n q r a n q e devf'lo[ii"ent"a 1 s t u d i e s , w e r e a p p l i e d'-• ; '')(• d e y e l r . ' p n e n t of t h e fiPi!r. f u e l forp 1. T'lese w r r - fa'; t h e f u e l w o u l d c o n -r!" , ) r p u r e p l u t o n i u r ; o x i d e ( P P O ) . ( b ) t h e f u e l d e n s i t y w o u l d b e in t h e r a n q e

f o '•;£ p e r c e n t o r \ f i e o r e t i c a 1 d e n s i t y 'TT:;, (r.' t h e th e r » , a l i n v e n t o r y p e r- d i v i d u a l f u e l forii- w o u l d b e g r e a t e r t h a n I f w a t t s b u t l e s s t h a n 1 0 0 w a t t s a n d': " n e f u e l w o u l d h a v e a b e t t e r i r p a o t r e s p o n s e t h a n '1!!'.-,' f u e l . T h e d e n s i t y>•!:;'!<• w a s s e t f o e n s u r e a d e n s i t y e q u a l t o o r q r e a t o r t h a n t h a t f o r M H H f u e l ,I1;' ' o'w o n o - K i h t o li;i;it p r o h l o r s (issof;iated w i t h h e l i u r ; r e l e a s e . T h e t h e r m a lm y n t o r y ranne was set to produce a reasonable power density and clad/fuelweiuhf ratio while prnvidino a fuel wit1' lower then-ial Gradients, and consequent'.herMfil stresses, thar, those far '*\',\i fuel. The radiused endcaps are intended toelii'iinatc thermal stress points and to enhance irnacf response.

Prior to the development of" the IPP'S fuel ^orr, three types of fuel werefabricated and tested at LACL to deternine the innact response. These consistedo^ hinh density pellets (F,6 T D ) , low density pellets (61 T D ) , and oarticulatefuel with a 55 nackinn density, [ach type of cuel was sintered at the sanetemperature to eliminate qrain size as a variable. The high density Del lets,when inpacted, proved to be sionificantly stronqer than the other types of fuelan!, consequently, had a better impact response.

The results of additional developmental studies performed at LASL indicatedthat as fuel riicrostructures were made more uniform, the impact responseimproved. An early result of these studies was the development of the flowsheetfor the fabrication of homoneneous lVW spheres. Three such spheres were madeat LASL, sent to MF for encapsulation and returned to LASL for impact testing.All three spheres survived the usual MHW impact test. The fabrication flowsheetfor these spheres was transferred from LASL to SRP in 1977.

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' o r >re f r t . l . ^ 1 | ! ' f u o ! n v i i ' - l ' . c o n s i s t - , o f " • ] I ' l iO i K i w d o r: • "•• i i c n c ! a t ( i [ : ' i ' p h y <j.J i r! i ' v : o y a l i r . n . i f ! t o r > 1 '.f t o n i ; i r " n i t r a f f s o l i i t i o n a n d t h e n"•• ; ' . •• n i ' v ; f h t - o x o l a l c : r e c i j • i f n t o a t 7 3 0 t o 7 r > f i ° r . t o f o r r . p l u t o n i a . U a s e d o n a' ' ' 1 J at.! ["f.'CMiion t h o t . vivv'.\ D O T . " i ' ' : , a " d L A ! L , t h e - l i m i t s f o r t h e p r e c i ' r ' i t a t i o n s

.- . ' . • r ( ' s o t a t l . C • ' i . ? '•! a o i d . *•-(• ' . ' / i i f c r p l M i . o n i u ! ' s o l u t i o n a n d 3C • C ^ C . T h oi s o t o n u ; C O I ^ P O S i t i o n f n r a t y ; n c ; : l l o t o f • ; ' r j u 0 f e e d p o w d e r u s e d a t L A S L i si ' T V " 1 ! i n T a b l e 1 . T h e ri T u t o n i u;1 i n t h i s n a t c - r i a l i s e n r i c h e d a t •••••() a t . • ' ' P u .• • r o - ! i i r i rv. a t h e n w a l o o w e r d e n s i t y o f 0 . 3 9 ' ' , ' • i / r ; o f p l u t o n i u m .

I n l i - 'O f u t u r e , p r o d u c L i o r i - n r r " i d e p e l l e t s w i l l b e f a b r i c a t e d a t SRP f r o r ;• 1 " r uCi_. t e e d p o w d e r w h e r e i n t h e n l u t o n i u i " w i l l b e e n r i c h e d a t 8 3 . 5 a t . ; ' 3 u P u .T h e v a l u e s l i s t e d i n T a b l e I w i l l b e s l i g h t l y d i f f e r e n t f o r t h i s m a t e r i a l . P r o -d u e ' i o n o f t h e i i x i r e h i g h l y e n r i r l i e d f e e d p o w d e r w a s r e c e n t l y i n i t i a t e d a t S R P .' b w e v e r , a t t h i s t i i " e , n o n e o f t h e n e v , r v i t e r i a l h a s b e e n r e c e i v e d a t L A S L f o rc h a r a c t e r i z a t i o n s t u d i e s . A c c o r d i n c i l y , t h e d i e s f o r a l l G P H S p e l l e t s r.iade atL A S L f o r t h e D e s i g n P h a s e i m p a c t t e s t s h a v e b e e n c h a r g e d a t 1 5 2 . 4 4 q . T h i sc h a r g e w i l l p r o d u c e a t h e r m a l i n v e n t o r y o f a b o u t 6 3 . 2 w a t t s a s p r e s s e d a n d 6 2 . 5w a t t s d u r i n g " M s s i o n l i f e i f t h e f e e d e n r i c h e d a t 8 3 . 5 a t . : ' 3 " P u i s u s e d . T h es i z i n g o f t h e p e l l e t c h a r g e b a s e d o n t h e c i o r e h i g h l y e n r i c h e d f e e d e n s u r e s t h a tt h e d e n s i t i e s a n d m i c r o s t r u c t u r e s f o r f h p p p l l e t s u s e d i n t h e L A S L D e s i g n P h a s e

i-.y i r . i t Ri'i',', r r r i a s

Sintered at 135O"C - H7 TDXI OP

Fiq. 2. Cross sections for developmental pelletsnade without GROG-type feed.

DEVELOPMENTAL STUDIES PELLETSEFFECTS OF wnr. FEFH

r

m.Sintered at 1350°C - 85", TD

X1OP

r

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Sintered at 1600°C - 85̂ .: TDX1OP

Fig. 3. Cross sections for developmental pelletsmade with GROG-type feed.

GPHS62.5-VJ TELLETGROG-TYPE FEED

Core

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1OOXP

Edge

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S i n t e r e d a t J527OC500XF

4 . M e t a l l o g r a p h i c d a t a f o r 6 2 . 5 - W GPHS p e l l e t .

TABLE I

PLUTONIUM CONTENT FOR TYPICAL

SRP 2 3 ePu0 9 FEED USED AT LASL

IsotopeAbundance

0.0001

80.0

16.5

2.5

0.8

0.2

Half-Life

2.8

B7.80±0.02

2.4x10''

6.6xlO";

13.0

3.7xlOr

Radiation

aDaughter products (:1'Pb, 7 1 ?Bi, andmoderate qamma radiation.

t>The alpha decay of ?3fiPu produces ?3L

month).

n

a

a

^Tl) produce

(525 ppm/

TABLE II

ACTINIDE IMPURITY LEVELS

FOR TYPICAL LASL PELLET

Element

Th

U

Np

Am

Abundance(wt?')

0.03

0.64a

0.12

0.05

aChanges with time due toalpha decay of 2 3 8Pu.

impact tests are r e p r e s e n t a t i v e of those that will occur for SRP p r o d u c t i o npellets i f the LAV.L f a b r i c a t i o n flowsheet is followed.

•-. Actinidr- ContentThe typical a c t i n i d e c o n t e n t of a fuel pellet m a d e with SRP feed m a t e r i a l

enrichart at '•") at. • '"'^u is listed in T a b l e II. Production o e l i e t s m a d e w i t hfeed e n r i c h e d at s3.S at.' :3!;:Pu will c o n t a i n slinhtly m o r e :>3''U which is p r o -duced V. / tv\<- alpha decav of :''-'"Pu at the rate of 5?r> n p m / m o n t h . The actual• ""\l c o n t e n t for any g'ven fuel pellet w i l l , of c o u r s e , depend on the aqe oftrie pellet and the initial isotopic c o m p o s i t i o n o f the feed m a t e r i a l .

(. !"puri ty LevelsThe specified impurity levels for the GPHS fuel art a s s u m e d to be the same

as r o r the '-V.'-V. ^ u e l . ^ T h e s e impurity l e v e l s , t o g e t h e r with LASL s p e c t r o c h e m i c a ldata ^or several lots of a s - r e c e i v e d SRP f e e d p o w d e r , are listed in T a b l e III.The anal/fir.al data listed in this table indicate that the i m p u r i t y levels inthe feed powder are g e n e r a l l y lower than those specified r o r f-lHl,' f u e l .

'•Vjst p r o c e s s e d fuel f o r n s contain fewer i m p u r i t i e s than the feed p o w d e rbecause of the removal of light e l e m e n t impurities durinn hot p r e s s i n g (inv a c u u m ) and p n s t - p r e s s s i n t e r i n o o p e r a t i o n s . The p o s t - i m i a c t s p e c t r o c h e m i c a ldata for LASL sphere STT-71 are listed in T a b l e IV. This s p h e r e , f a b r i c a t e da c c o r d i n g to the LASL h o m o q o n e o u s MH!\! f l o w s h e e t , was e n c a p s u l a t e d at 'flF andimpacted at L A S L .

A n a i n , it should be noted that the s p e c t r o c h e m i c a l data are for feede n r i c h e d at 80 at. ' '"Pu. None o r the new ^eed e n r i c h e d at °';.5 at. -"^"Puhas been c h a r a c t e r i z e d at LASL.

IV. P R O C E S S I N G fLni' cM[F~ A!;D P P O C F S ' U P L S

A. GeneralAll o p e r a t i o n s reqiiirinn the handling of u n e n c a n s h l a t e d : i~'Pu0- are p e r -

formed in 'iiovoboxos. These n l o v e b o x e s are c o n s t r u c t e d with s t a i n l e s s s t e e l -l o a d - s t a i n l e s s steel s a n d w i c h - t y p e w a l l s and have hinhly polished i n t e r i o r s tof a c i l i t a t e c l e a n i n g . G l o v e h o y w i n d o w s are safety g l a s s held in p o s i t i o n byvifon g a s k e t s that are provided with s t a i n l e s s steel ^ire s h i e l d s . The g l o v e sc o n s i s t of two layers of hypalon separated by a thin layer of lead. N e u t r o na t t e n u a t i o n is provided by 4 inches of h y d r o g e n o u s s h i e l d i n o located o u t s i d e then l o v e b o / . This shieldinn c o n s i s t s of L u c i t e panels over the n l o v e b o x w i n d o w sami w a t e r - f i l l e d steel tanks e l s e w h e r e .

'.-.'itfi this o l o v e b o x - s h i e l d i n g c o m b i n a t i o n , we have been able to p r o c e s s 16kq of • 3 " P u O . including r e s i d u e s , w h i l e limiting personnel e x p o s u r e s to lessthan I RTft per year.

All processinq n l o v e b o x e s are provided with inert q a s , arqon or h e l i u m ,a t m o s p h e r e s . This is a c c o m p l i s h e d by e i t h e r a c o n t i n u o u s inert aas pass t h r o u g h(•- 10 pom o x y n e n ) or a closed loop r e c i r c u l a t i n n system (< 1 ppm o x y q e n ) usinga V a c u u m A t m o s p h e r e s C o m p a n y Model MO^O 2HA D r i - t r a i n unit. G l o v e b o x e s areattached to one a n o t h e r via v a c u u m / i n e r t - n a s a i r l o c k s . T h u s , if any g l o v e b o x isb r e a c h e d , the a t m o s p h e r e s of n e i g h b o r i n g boxes are not a f f e c t e d .

For the purposes of d e s c r i p t i o n , the p r o d u c t i o n of e n c a p s u l a t e d G P H S p e l -lets from raw SRP feed powder may be separated into 8 c h a r a c t e r i z a t i o n and p r o -cessing s t e p s . T h e s e s t e p s , each of which is d e s c r i b e d in detail b e l o w , are

' i'.-iM'j-

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ino

200

200

50

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13

.-

10

1025

555

10052

1025

5100

a!_ess than sensitivity limits

SRP lot numbers (and No. of containers) are: 353(6), 361(1),362(4), 363(6), 364(3), 365(6), 367(5), 368(5), 369(4), 371(4),and 372(4).

•-••;. 1C.

A]

r.rt

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Mo

Nd

Hi

Pb

Si

Sn

Ti

Zn

Ir

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1b

20

C

15

aLess than sensitivity limits.

n

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! , ] • • ' . ••. I ' ' ' ' ' • I r ! ! I i • 7 1 • ; i ' ' . i ' • ' • : ' . . : i ; ' . ' : '• . ' , ' ' . ] ' . . .•• i ' ' • : ' . • • ' ' ' ' ' '

• r ; . ! ' • ' . ; . i / , r , ' : > • • • . • , ! ' • • - . • ' ' ; - ; . • , , • > '•' , • • • ! < • • • • ' . > • • • '. ! . • • - , • : ' \ '• ' \ , ; > - . . : . ; > •• ' • : ' -

,-, > ' < • < ' I ' . I ! . i i I J M ( ; : i • [ i ' • ' ! l I i ' ! ' ' , ' • ' ' • i • | • : i | i , / i • r • • t , i , . • • : ' , , • ' • ; i ' : . - . . : ' • ' . * ' ' ' / . : ' , ' .

' i i v i ' l r - ! ! « / t l ; « . (

, ! f ' . i i • • . ' - . ( . • ; • ' . • ' • ' : , / ! • • • • ! • . ' ( , . • . , . • • • ; > ' ' • ' - , . / • - ! • . • > - r . , ; • , • r . . • , / .

f M f • • ' ) ' ' ! ' • ! ' , ! i i | I ! I i n r : ' ' • ' . ' • ! i ! , ( • > i ' . i r ' t ' I M ' H <••'. ' •. ' ':• • ! • / , ' • • : . • > • ' ' n < - - n ; 1 ! ' . ' . ' • ' . • • ' . • . ' • : ' : • " ,

' n i : ! i \ i r , ( : r i ' . ' . i i v j i ' 1 ' ! f > : i f - i • - i n < ! •! i r . r , : r • 1 r • • ! . ( • < > ' < • r ' ' ' • ' < < ' > < • < : M M ' ! r ; - | ^ r ,\ - ; i - ' i : / . -

: • ! ! • • ' . i r / r . o i i t . , i i i n • > ' ' i t " ] ' ) v c i ' f i / \ } ' > ' j < - ' . . ' , ' " . < • ; j r i ' " - : r . ' ' ' i ' : 1 •! j w - y i ' . o ; , ' ' i i ( - ' i , " i > . ' i ' > ••

f t . , , , ! : i r j w f j r - r i ' . f . r . n r . ! f • r r i •' 1 ' f j . < t < i r ' - < ! • . f . i i i i l ' - ' • ' • • < • ] ; a n - M I ' 1 v ; f . - i r ] h > - ' ' , . < • < . ? < •

r i l ' . ' l i C 1 , 4 f ' l i I I ) l i C ' V l ' l i t f . i i l - : : i f ' f , i ] ' ] • > . ' . - f i ! I • ••! ' : - l ' i l i ( | f - i l l i l i ' i i n t f y M j ( . : , r . . - , •'.- r r . r ,

I ' c r . i j j i r l ( . f i ' i j i ' . 1 ! ' , ] l . u t •• r i ' . f ( . n ; ' „ - 1 : j ' , r • ! . [ ; ' • ' / - ' ' i i i ' : ' • > • ; , i r i •! , M i ' i l i i r r 1 , ' . ';'.<• i ' : ' i i n o '

• I f f : p r . T f n n n e r l O i l A i l i ' , W f i r I ! l C i f - H - ' P - - I I i , ' • ' ( ) • ! . ' r . ! i , l i t , - ' , - " , i • i ( | i , i 1 / H i C P ' , :-. r j r j r_- t . f ) [ J - . ' A

' . p o c i f i C O t i D N ' I . T f c . c l).i 1 ( i t u . f . h . i v f ' .i '..i;i'i'.i'.y '.f ̂ rf; <•; v / i M i ,i '.'.'ii'. i'. i v i t. / c'I ').'; i.'iq. T i n (.yii!.'-c- w o i ' j h l ' , u ' . c i <'.n- c c r L i f i ' - ' i !•/ r .ru-; > t < r" i s o n f:o 'ia t i (inr: 1[ ' u r i ' d u o f S t r T n d d r i i ' i (fJ!'(-,) s t r i n d a r f ] v/f'i'jlif.1.. I h c t'ull- W ' i ' i h t o f t.hf.' f f f d [,rr.-;MfMi'-, c.oM'ti i n e d w i t J i i . h e c a l n r i r i o t e r v a l u e t o d e l . f r : i n c t h e t f ' e r ' v i l i n v e n t o r / (V,/r))f o r t,h i r, m a t e r i a l . A t t i n ' s p o i n t , a S h i p p e r - R e c e i v e r d i f f e r ' T i C C i s w r i t t e n i frequired for account, i In 1 i ty .

2. Analyses. Next, analytical sample, are '.rilen if desired. !.7e qonoral-Iv take 4 samples to determine the (a) actinide content, (h) trace i^ipuritylevels, (c) neutron einission rate, and M ) particle size distribution. Typicalactinide content and spectrochemical values for fresh SRI' feed are listed inTables JI and III, respectively. The neutron emission rate and particle sizedata are discussed below. Each 1-g analytical sample is weighed on a chain-o-matic balance and transferred to a tantalum container. These containers arecleaned ultrasonically in ethanol and baked in vacuum at 200°C prior to intro-duction of the analytical sample. The containers are then welded shut and trans-ferred to the analytical group.

12

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. •• : ' • • , ' • • • . . : : . • . ' • ! " , I ' .: ' • •" . ' • ' : ' ' / • ' , f , r <• 1 1 : d i i . i t " ' n s p h o r o

' . . • ' • • • • . • • • • • : . - . • • • • • • • . , , i r • • • ' i • • ' • . - • - • , ' ' ; : ! • , ! • : > , , ' • ' ( >

. • • • • • • • • : : . ! . • • , ! ] ; : : ; • • : ' ' . ' • • • • • • ' < \ • • • ' . . ; r • • ' : , • ' ' > ' t * • * - p r o d u < -

• • •, : . - • i .'• ; • : , - ( • ' . ) p . : • • . ' . . • ! ' , . • : • . . : : , - . . ! , , v . . ; f ! ' o r ^ h a t

: > • • • • ' • , . . • ( . • • • ' • . t ; o • , • , , . ; , . . • , . • ' , , - • : ' . . • ] i r . " , < ; < • f u r n a c e

; . . . . • • , . . . • • : , , •• - r , ] M • : ! - . < i . • ' "• ' • ' - . - 1 ; , . , " . t - - i ; ": ! ; , f l c w i ^

• • • • • • ' , •• , • • • - , i . i j - , : : ; ; f- - - - i • . : " • 1 . • ' ' "' ' ; • ' '' •! n • u r , c < i p c r 7 0 f ;

' • • • •• , ' • ; • . : • > I i • • : . i - r i f ' ; r ' • ! , : • | , ' . ' ; ' ••.• - 1 * ' < T ; i m - ' h e r i e u t r o n o i n i s -

• : • • : : ' r • : ' • '" . • • . - ' . , ! ' ! . • ( • ' i : - < - , - x < - l i ' ' " ' ! H i T d M c V . T h f . - ' j p d a t a

• • • ' ' . • : * • • • • • : • • . ' • ' < i . - i - i f j r r . : 4 . ' - • ',.<•'. i • i ('•'. f ' > r ! ' " > v , ' * r u o l f H 0 0 ' ) n / s - g

. :• : • : • - : • < • • : , . - . . - i . r , •: i r , . : r . h < . ; ] : ; t . c i ; i , i < " r f , h a t 7 7 ' J 0 C f o l l o w e d b y

: ' ' " . ' • • • • : . : ' • : • • . ] • ' i r i d i r . , i • ..:• - . ' i f ' i r v r r - < : ' . < • i n ( - y c f a r K j o f f f i c i e n c y w i t h

. i - ' ' < • • • • • ; . * ' • • • • i i ; ' r - ;. r , - -. i : I f r . • • , ; ' - , i o n r < > . \ . < - \ r , \ , ( - f . b y t h e s p o n t a n e o u s

' ' ! ' • • : ' ' • ' • ' • - : • ••',. \ n •,)'.•.{ ' } ' _ < • . : - ' i i . i : - - . i : f / ; i - / , i o n r a t e s n e a r 4 5 0 0. • : ' . • : " • ,'. ' • • : v , < - ' . ! / ( • . • < . * , a i . ' i i i r j f i i t ; - r i t o f i a l l o r ?A h a t 7 7 5 ° C f o l l o w e d'• •'" ' '•" . '. ' i • : < < • ' . \ \ A <• t . o i n r r o , i r , ( . ' U i o c / f . h d i K j t - r a t e b y i n c r e a s i n g

''•' '•'•' ••' ••• . i - . ' ' ' i ' '••!'. ' J f l c t o r i f i r - , e f f e c t s o n s u b s e q u e n t f e e d b e h a v i o r .' . < • . ' < - • i . • • • ; . • i , - . r , i - , - i f . r . ' . f r , r ' . f - v r - r a 1 l o t s o f S R P f o o d p o w d e r , b o t h a s -

: .'••! • : ! , < : i ( 4 . f r ( / f • n:<]<: a t L A M . , a r r - l i s t e d i n T a ! ) l e V I . S l i g h t d i f f e r e n c e si • - i M ) - • ' , ' . < ' , ' u \ - . ' • y r . h r i n q e d 1 ' j t . s r a n b e a t t r i b u t - . ' . ' d t o l o t - t o - l o t v a r i a t i o n si- . ' . ! !* ' • - ; ' . r , f 1 i q t i t o l f . - ' - - r : n t i I ' f j u r i t i e s t h a t c a n c a u s e ( a , n ) r e a c t i o n s .

i. f '{u fp'̂ .-fi1.. T;-/CJ '••(<<]<:}', of furnaces are used, -Astro Industries, Inc.,'•ViM l':'/A and r.f.-nt.orr Associates, Inc., Model 10-4X16-G-0-17. Both furnacei-iodf'ls <\r<: \:<;\-izonU) 11 y nounted and are provided with alumina core tubes mountedbr-f.vef'n frv.» rosi stnace-hoated graphite elements. While the Centorr furnaceshevo been adequate- for the exchanoe reactions they have proved unsatisfactoryfor th? rjrariulc- seasoning and post-press sintering operations performed athigher temperatures. Two gas streo1 s are introduced into the furnaces at oneend. pass through the furnace and then exit to the glovebox exhaust. The coregas consists of Ar containing 6 vol lip. This is passed between the graphiteheating elements and the alumina core to protect the heating elements shouldthe core tube break. The reaction gas consists of Ar passed through a bubblercontaining H:

!''0 and then through the aluminum core. Before these gases areintroduced into the exchange furnace, they are purified by passing them throughLindberg Model 70 tube furnace containing titanium beds at 750°C. Valves andflowneters are used to regulate gas flows. Alumina baffles are placed at bothends of the alumina tubes to moderate the flow of the Ar-H 2

1 G0 required. Inaddition, when the Astro furnaces are used in the high-temperature post-pressingsintering operations, the baffles prevent cold gases from coming in contact withthe hot pellets and. thus, producing thermal shock to the pellet.

The platinum boats used to contain the plutonia powder are made by deepdrawing (no welded seams) to facilitate cleaning. Two ̂izes are used. Theboats for the Astro furnaces are normally loaded with 40 to 70 g plutonia, those

13

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( • ' • . ! ' ! ' . " . ! . r j . i ' . ! ! • • ! ' ^ • • • ! • o r / , - J ; I 1 1 ' . \ ' \ ' • i r n - i ' . i • . ' • • • • > ) '•• u \ \ i i ' - . ' • .

f . ' > ( • • • i- ' <;-i t •'. r 1 1 " r ' • •' ' f h - i r ' . ' ' , < ) ' ; ' J < ' i t •: ! • ' - ! ' . • • ' ' J ' .

' t . f . f j - » . ) ; , i t . , . r ! r - . ' ; ! M » (• f - r - . , r , - l •• ' / r ) r ' - r , ' / , ! j \ ; i 1 ' - . " M / , , " ' ) ; l ! ' T ; ] . / . - | .

! , ! ! ' • ( . I f . h f l ' . f i ' ' . f i T ' l ' t " ' i > ] ' . i \ ' \ i ' ' \ H i \ \,< f . l i f l i " ' ; • 1 1 ; , f • r .

J ' r . ' f . o r - i - j f s j r r i ' : r. f • n i j ' 1 ' ! ; ' " < i ( f ! r u n ( J i w \ i '. i o n ' , .

l l r . ' f j i n ' ] ' j ' , f l o v ; i - i r i ' l M r f ) ' : r ' . r ;r f " ! r u n ( . / ( . ! ' • .

' • ' f . - f i ^ . - d f . r , t c \ ' \ I: • . \ \ r n \ i " j \ }i ' i l l r i l l ; • / ) ' . f - r i - i ' i \ 1 o ^ H r - ' ) .

, r v - n o v f . ' i - ' i ' i ' ' r r i ' - r j r»<• - f u r n - i c c j . W r - i n i :

-'! < ) n ' i i j r ; f . o f : ' • ' < : u ' , f : H .

t . i ' "I c J r ; r • r o c o r d c . t u i r f . f o r r" • j r , i n l o t . f o l d f - r .

1 . ' ' , : ' . > i r | f ; r t r i - ' j n . ' f . o r ' ! 1 <\ -•! n - i I / f . i r . d 1 ' . • ) • • p l o i ' r K M t r o n r - i n i ' / i r m r a t f - i '

• / i i ' - < \ ' : l f \ - " \\-,<,:'\ .

r . P f . - f j c - i t . ' , f . ' j i > r . j • ) ! ) ' ] I ' f f i r c j t . i i c r t i o r j t . o .

• 1 . I r a n 1 . f r r r ; y r ; h r i n r i ' - " ' ! p l u t o n i , ] ' . r , I , o i l ' • • i l l ' . ! ' : i l l ' , - i r e n u \ . a v d i l -d t i l r . ' , s t o r e n o t o r i / i l i n d o a n , l ; \ r < - < \ r, t a i n l o ' , ' , s L i - o l c m r . , . - i p j i r o x i i ' M t e l y l r ! r ) qi ' : o r c a n .

o . F r o i " i n i t i a l a n ' ) o / c h a t i ' i ( : d w i g h t ' . , r l e t o r i i i n o : i r o c o ' . s i n r : l o ^ c o s , i fa n y . R e c o r d r , a ; : i c .

D.__ _ Sal 1 -Mil 1 jnqThe second LASL processinq stfp involves millinq the feed powder to pro-

duce the desired particle size and powder morphology. This is, to some extent,a normalizing step to eliminate differences in surface activities from one lotof feed powder to the next. Particle size data for several lots of SRP feedpowder, both as-received and after ball-milling at LASL, are listed in Table VII.The as-received powder consists of two types of particles and has a mass-mediandiameter of about 2.1 ui". One type of particle is rosette-shaped, the other islath-shaped. The lath-shaped particles have an extremely high surface activityand cause the material to shrink excessively when sintered. Milling the powderconverts most of the lath-shaped particles to the less reactive rosette-shapedones. The results of developmental studies performed at LASL indicate that thereactivity of the feed will be adequately adjusted if the powder is milled toproduce a mass-median diameter of about 0.6 pm. This requires 40 h in the LASLball-mi 11.

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, : • . [ : : ! i P ' M i f • : : r : i [ . ( - r r : . i • |.. f • r ' '; ! ! ' . ! ' I ' .

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• ! . I ! l - i i i j . l t •!' ! ' I ' l ' . ! . . ! i n ! ' • ' . ' , I i : C ' • i F i r . i ' ' I ! , I ' ! •'; ' •'• . I I : ' ] ' , ' • - ) • ; r ! r " ,

' i : ' '.' i ! i i i • ; I J ( j ! ' . ' , i • v f • 1 1 I / .

( . I - 1 ! . ; ( \ ! » . - , t . i ' p - . • , ( [ ! • ! ' I ' H I 1 • . * . t i " i ; ' • : • • . I I ' . ; ! ••.'.', • n ? i - > ; i ! i ' , I < > . : • ' . < • • ' .

' . ' , • ' r u j - t j f r ( j ' i . i r 1 1 . • i t i V . ' ' i ' 1 f . h - n : ; • ; i f - t j - 1 ' • ' " • • ! ' • ! ! • • . > . • ! " ? f . f ! • " , ' , . : ' . t o ^ ' t / ' 1

f . ' , ' : ! • > ; i : . . ' . ' . I ! I i . - t r . . i ; > - ' i ' • ' < • ' • , - M i ' ' - ' • ; ( • • , - i i r ' i ! ! ' • • ' • • . , ' , e ! ' . i ' - . - - . - i n ' i

: ' • • • ; : : • i ! ! i > i : . ; ; f - i r > • • ! ' i : - • • , < r , r j : • ; . - .

: . r-. ! ! . • • • • i 1 I i i i : i • f f i ; - ; : i ; • ' c ! . ? • • i ^ t , / • ; > i 1 1 - n t • , . - , ; . - j M f • i - ' i r o n t ' i . J c 1 e o n

. , ' ; r - !••! .̂ f . j i n [ < " - , ' . , ! . • ! • ; •/. i I ' f M <y.\- i i . i ' ; r i ' " l i ! > . • ) v " •! r ? (.• n r i , f . a r o ' ! r, t a i r i l r ^ . ' ,

, ' ; • ; • ! ; ' . : • : . ' ' • , •• - i • ' r i r r 1 1 ( • ' . ' . - . ' f c l i i r - i / n f . u •.. i " n n * . ! M - I : - : M ' , . p a r , ' , i r v : t h e f e e d

' r - . ^ - i ;•:•: ' . r i " s c r c ' i i ! . < > t h i • I J - H I l . c i o w . '--'•"• l - 1 • i c f • ! v i 1 1 r i n i , ~ i r a r u i ' , o a 1 l i : l .

» : . . • , ' e i ] h i - i i ! i ^ l i - u w f l c r . H K ! I ' ' . " n r d w o i q h f .

i . W e i f ) ' i • i i i ' ! r K i ' r d <i 1 r\ i i t i - i 1 y t i c . o 1 ' . a i n p l e i c U i e p r i r L i d n s i z u i s l . o

: . ( • : > • , . ! • . u r e c l . I f i i i ' . u M i i i i ' i i t - • i l l i r i ' ! l i a r j c . c u r r o c i , r f l n a f l t h e e i r p t i e d j a r a n d

" i i i a i 1 j c i r s 1 o t K i e r .,i . I f p a r t i c l e ',!.;•;• ; l, i t .,. i i r . ^a I i r , 1 a c l o r y , o r i s n e t o b t a i n e d , r u p e a t

s u - p s ri a n d h f o r t f i e n t . h e r j a r s .V. L c a u t h e r : i ! l e ; ! i m w r l c r i n t n ( . l e a n s t r i i n l e s s s t e e l c o n t a i n e r s , a p p r o . " i -

i : c i t e l y ; 1 0 0 q p l u t o n i a pr>r r u n t a i n e r , f o r s t o r a g e o r t r a n s f e t - t h e s l u g q i n q a n dsc r e o n i w\ a r e a .

1 . f ' r o c ! t f i f . ' i n i t i a l an<\ r i l l e d w e i r j h t s d e t o r n i n e t h e p r o c e s s i o n l o s s e s ,i f a n y . R e c o r d s a m e .

L. S l i j i j ' i i n f ] a n d S c r e e n i n qT h e s l u q q i n q a n d s c r e e n i n g o p e r a t i o n s a r c p e r f o n : ' o d t o c o n v e r t t h e ba 1 1 -

m i l l e d p o w d e r t o q r a n u l e s o f t h e s i z e d e s i r e d f o r h o t p r e s s i n g . T h e p l u t o n i a

1 8

: . . : > • • : ; . - ; : • : i r ' - : ' •• . i ; i n j " ' o r : . * " i ; : r o • y ] ' » • ' . • • : . _ ' < C ! • ' . r - - , ' l e p e r , - : i r r :

• ' • • • • : : . ' ' . ] . • • • . i n - . ' . ' • ! • : < i ' . • ' . ' . I d •>••'•'•-.'<•'. •?.'. •"•''' '•"•'" - i * ' ' o r " < i o r e e ) ; p ' - ] ] f T

: • • ' ' . ' • ••• : e ' : ( • : , ! > • ' • ' . o e r < ! . r i r i - r ' i i i ' i '.-~ r • ' • ! • ! i f d • • • • ; . ' f a n d t h e •• 1 '. '•,- .::•

i . : \ " j i ; • ' - n * . '.''• ' ' I ! : • • ( • s ' . i n : j . : i . - r ! ; . ' » ' • i - ' .-. i ' ; ,1 f i r v f r M o d f 1 '.: : : • : ' . , ! . : >.-(••. . " • ! ' c . : ! : '• '•:•'• r < • e ! • . i > u i - ! 1 i • o r ' n I > '• / - ! r . t . . i 1 i ; : a l 1 y p i L I " t i e d

• • i < • ; ' ',:•'•' ' J ' . ' • < • . T ' • > • • o 1 d ; " • ( • • ' ' , i n :• ! i r - i • h r ' w r • ' i ' \ i v : i n o • ' ( " V - 7 < •• 7 . ' [ , 1

: • • • • ' • • • ' i r . *. ' " • ; : ; • - ' ' i • * ' " • d r • w i N : > i l l ' . • r • » : ( • - r • • * i -. r •• a t o r i a ! . h o w e v e r ,

.-.•• • : / • • - • ; ' . . • • • • . • i l l . - - j - ' - : - l i e . - ' - i d ' f r ; , - ' ; . i r d i - M - ! ' : • ' • . M i - : . r h ' - ' - . o d i f . t - a v

: ••• ' : : : • . . ' . • • : ! . ' h > - I ' • ' 1 i i ' • r a f f t / f c •• i ' . ' - < • ' i r • , - . ' • f r ', . 1 i ' i n . i . T h e d i e

: , • • ' • . . , : • • • • ] , : i i : . . i : , ( • • : ,•; i t ' • o l / ! d f r - j : : i .••> ] * i d f , i r ; • ! ' ; ' . ! ' • • ! ' • • ' ' " . i d r i t - d t o t h e

: ' • . ' ' > ' . ' • . : i . - . •'.• i ; " • ! ! ' . ' r - c i / , . p a r s , M • 1 ] . ' r ' . . f : , : ' : > ! . ' • > r - f > • : , a r , i l i r ' . i S h c s u s e d

1 ' • • . . • • • ; ; . ' • • • • ; . ' - . : > ' , • : i i n l e ' ' , M M 1 .

: , ,.. , . , ] j , - . . . .

•: . : - ( - r • , ) - • : l o r . i i i . n r ! ' . . i , \ > v . i ^ A A ,.. • i m s f e r r ' - - ! : - f . c r P a 1 ! - " i 1 1 i n ' i .: . ' ] < • , . , ; . ; i , - . : ; o ! i - . h - ! i " , r , ( - ! 1 , .-. i t * 1 ( . l e a n < •, < . , - . ' . , . ( ! : , t . i ; .

'.. i i i " i ( . : ! . • • • P ' l M ' ' " • ' . p ' M i ' , ] ' : ' ,' v , \ ' r; • o 1 .•! d e n i d i ",;• 1 f i - i " t t i I- i n g c a r e' ' : ' ' . i i i i i - i t ' • ; ; • t • ( n ;• \ \ y \\ \ ,\: ( ; ' , .

•:. : ' ' i ' . i ' . i ! ' . ' ' - . • : • i f f . ^ i n ' i f . ! . o , i . . : j p p r o p r - i .•: * i - y - . u i * o f f e e d p o w d e r

i . ; ' ! ' i c d ; < - • : ' • • : : .• o n I - O l ' o : 1 [ . ' r e ' . s p l - i f . e n . - I T : ' ! ' i o w l / r - j i s o a s s e j ' i b l y' i i 1 '.<:': : j " r , h t o j ' . ! " ' . a n - : i ' . ' / i ^ a r ' ' : ;•, i l h L o p [ i l a f f r i .

f . ' " ' i p l v ' o r o ' / o f ••/•..'-: \'',, h o l d f o r 1 J1 i n a n d r r - 1 f , i - , f .•:. ;'•:•: 1 / < : i r - " - o f f / . r k 1 ; , n o l d f o r 1 p . i n a n d ' ' f i e a s e .v . • " : ; • ! / '<>>-<.'• o f 1 •••!..'. r ; , h r , l d f o r 1 " i n a n d r e i " a s e .i . .'.'tien ;;'••'••,', ifr: c / o l e i'. c o r ' p l e t e d , r e n i o v e a n d i n v e r t d i e a s s e m b l y .

'•":••••:<• r.op' p-ji.;.'. , j n d p o s i t i o n s p a c o r . R e p o s i t i o n d i e a s s e r ' b l y a n d e j e c t p e l l e t ,r , i ivi •• i r )'•: ...i" f o r o e .

i. Pf'o,'" p e l i e t wi'fi f o r c e p s and p l a c e on 600-;;!•; s c r e e n p o s i t i o n e d'iio/e 'i \?:J-.:: -.c'fft ttiat in turn is p o s i t i o n e d a b o v e a tare d p a n .

k. 'Jpo• r o l l e r i.i,' g e n t l y break u p p e l l e t . U s e r o l l e r and b r u s h to p a s sill " a t e r i a l t h r o u g h the f/10-..r. s c r e e n and c o l l e c t g r a n u l e s on 1 2 5 - u m s c r e e n .

I. l'','i roll'-r tf; ;ja',' ":aterial t h r o u g h l?5-;;m s c r e e n to pan b e l o w . U s el.r.j'.'i fii>" rr.-' idual t a i l i n g s o n l y .

if t h e r e a r c ;;iny g r a n u l e s :• 12f,--,iiii, w e i g h and t r a n s f e r them to a r e s i -du': '.on:.a i iv.-r .

n. Woi'ih t a r e d pan to deteri-ine w e i g h t of < 1 2 5 - p r g r a n u l e s . R e c o r dw e i g h t .

o. R e p e a t s t e p s b t h r o u g h n until all m a t e r i a l is s l u g g e d a n d s c r e e n e d .p. F r om initial w e i g h t a n d w e i g h t of s l u g g e d and s c r e e n e d g r a n u l e s ,

d e t e r m i n e p r o c e s s i n g l o s s e s , if a n y . R e c o r d s a m e .

F . Granule SeasoningThis is the most important pre-press processing step. After the < 125-ym

granules are made they are thermally seasoned to form the reactive and nonreac-tive components of the GROG-feed mixture. The majority of the green granules,60 wt , Are seasoned for 6 h at 1100°C in flowing Ar-H ?

l fO. The remaininggranules, 40 wt , are seasoned fo> 6 h at 1600°C. Heating and cooling ratesfor both seasoning operations are 300°C/h. Seasoning the granules in Ar-H 2

1 60prevents the back exchange of the ru l r0 ? and, in addition, frequently leads toa further reduction (5 to 10 ) in the neutron emission rate.

* ' • ' ' < • 1 ' • * : ' . ; • ' , ' . ' . - ' '

• • , . < - , : ' • • : r i • r , . ; • , ' ; . , . • ; , , , ; ' • - - . • • : . • • . V , , :< > . i < • " ' • ' . * . : .

! . • ; , ! ; , < • ' , ' . ' < < ' ; • ! . : • • . : .• ' ' . • '. • ' r , • • > ' r , 1 i - r ' . , ( ' . , . f 0 ' . ' ; . J | . 1 ' • , ..

! • • • • • • i , ' • ! . ' ! O r ! ' • ' • • • • ' • / : i • ' ; i '' . . , • • > . . i , ; i • r - ( - - ; ? . ) • ' . • : f - ! ? . . i r r l ' < • ( • ] 1 f i ' ! r . i t ' ' . - ! ! : ' ]

. ' • ' - - • • • ' ' J ' i f j V . r " . , ' ' •'• , .,' 1 ' I i • . ' : i . f I • • ' , • : ( • .' • . '."•' • • • ' ' " ' . T i e 0 • / ' ; ' : ' ! - 1 C f • / ' . ' - i V, ''.' • ' . t ' " I .

' , . . ' • • t . * i , ! * 0 1 ; ! / ' . ' '• / ' • ' , ! ( ' . f i r ' • ! • • • • • . • • : " ' I ' " ' ( ' - r ' . ' : < • \ t ' ' ' ' ' . ' . e . i ' , r , r , i r r : 0 ; . - r . r . - , t . j < , r r , .

i ' f ; i '• i • d J r ' • .

• i . : - ' i - ( ' i r ^ i ' j ' .','; i ' . . ' > : ' • ! , ' ' .-.•' ; ; ' ; 1 •<.'. t , - . : ' : ' . ' ' ' f ' r ' ' - - i , i ! * " ! • • ', j r r : i ' ' r : ^ w r !

, • i i • " n i n •; .

! , . l . - j . i d •! . f . ' . / ' • \ r , ! - ; , - i t • ! : • • • . I r i ' . ' , -. ... i . - • - j r • - m d t - : - - c d ;• ; , i t i r i i i " h o - i f i f

i n . ' • , ! t ' i t u r n i ' ' ' i . ! ' i .'••'• u s ' - d . ! r . - ' i d • ' . ' , t . . . ' . " r : ': i n ' / ; • ) ! - i r ; ! " r b o , i t i ' . i

•' i • • • ' • ) r j ; / f ( , , . • , • | , ( . . i . ' • • " i ; ' . / • ' .

'. . ' O ' , 1 ' i ' •! ' I 0 . : • ' i r i d • 1 1 ' - I T ' i - ' I ' i p l ' : ' . i r , f I n ' - ! ' . ' • . ' / v " i I f l i r l : - i r r . .

! . ( h i - 'r t r . . ! t i f , r i ' i - ' ' f i M i f ' o r 1 1 ' ; • ' ' . ' J f . • , ( _ • • : ! ' . ^ 1 1 i r i < : r u n i r o n ' J a f a T r ^ i c r

» . I h i - t ]• !. ! i , j t . - i d ' - . ' i i j / i t . i ' /•,• . ; n d i • - ' 0 ' i r i 1 , i v , i i 1 a b 1 ' • . : j e i . f ' r d ; 1 • ' '•) l e ; r - l .

' . C f i e c l - t f i - i t r e ' r j r ' ! ' •• r " i ; , r a l c i i u a t e c l , r i r ( . i j a i ' f M " .

h . !ieg i r, 'iaj, f](iw ,ind pt :"',i '-n ;'• ed r u n eye!'.-.i. Repeat - J e p , b through h till al! !;:atoriai to hf seasoned at 1100°C

ha\ ')0en loaded.j . Repeat step', b thruu'ih 1 for material to lie seasoned at 1600°C. Note

that different programmer char!, is used and only the Astro furnaces are usedfor the 16fiO°C seasoning runs.

k. At end of programmed run cy c l e , shut of ; gas flow and remove boatfrom furnace. Weigh boat and record seasoned granule weioht. Record amount ofH/ : f Q used.

1. Repeat step k for all boats. Place recorder charts in lot folder.;i.. Combine all granules seasoned at 1100°C and pass then1 throuoh a 70-

n:esh (?J)H-\i\i-.) screen. Weigh and store granules in labelled stainless steelcontainer. Do not store more than about 150 g of granules in a single container.

n. Combine the granules seasoned at 1600°C and pass them through a 3 0 -mesh (600-um) screen and then through a 70-mesh ( 2 0 8 - M I H ) screen. Weigh andstore granules in a labelled stainless steel container.

20

r - . \ •:• :'. - . < ' • ' . ' . ( , ' . ( • • : • . - , ' < • i - : h t - ' , ; ! ' • ' . • " i n e p r o r e s s i n n l o s s e s ,

" r .. ,:• , _ • , ; , . • , , - • ; , c i t •, < , - , ; , i • - i * i - :. <>,>• '/• ••' i J - 1 : > < • ! ' i - t s i s o b t a i n o d b y

• ; , • ' . ; V . - . - : • : • < • ' ! • < ! - > . o f - l . ' : . - ; . - : < , i > - - i } < - ' < v . • r , i , M . : ? l l i . . - f i C ( 6 0 w t ) a n d

•- ' ' •'.".' ,-,- . * r i • • ! . . i n : i , •;< < <•• ; } i ' , ' - • ! ! : i ! . t i ' . - : ' h e : i m u l e s i n t o a

: - . ' ] - • ; ; i : - : r ,-. : , ' • . ] • • , • . i f ' ' >• 1 ; > f c •• • ' ' : • < . ' . 7 ' ;•' . ' > ' " ' > < . 1 1 s a r e u s e d .

' ' • - • ; - : - i • ' : • : > . ( • • • : ,-. i ' • } [ / : . ' • • ' • : ! > f : r i r ; . j ! < • ' , . A i ' c J h * - r d l l i r v . i s c o n . p l e t e d ,

' • •• ; ' : : ' ! * • • • '. • ; • • ( • , ; r . ; ' I i >•• i . f ' ' . : :>• '. w i ' '; : ; . .-"'•"• ': <>' t h ( - f . T a n u l 0 " : i x .

" • ' • : i ( - ::-, . • • • : ! . • • . • • , r - , i ' t •, '•' •>. -. / "I i r r i r i c s 1 i c . ( - ; • : , S U M f - p t . o r , 1 o c k i n • j p i n ,

; . , : .•- ' .••• ,:- : ••!; :' - i : ' , . > . < • ; j ^ l i ? ' * i r , f o r m e d i r : •; ' i - . ] f - h n r f d U m u ' j h t h e i n -

• r 4 • ! ' • : . . . • , - . , - ; . ' ! f , r . ' f ! r . : ,• ] i i - , - | t- i : . , i 1 , ! • ! ' , . T h ' - •• j ' , < ( . ' ] • t r . r i ' , s i z e d " o t h e i n s e r t

: u : ' ' ••• ] [ • : , ' * j o r : ' . f - ! f . " ' n ; ! . i , i l ' , r , / I ' . * o : • • : • ! ' 1 / r t | f - , [ 4 i i r ; f f f l C l P n c v . T h p S U S -

' . ' • ; • i : . ; • • ' . . ' : -[•>• ', , ; i v 7 ; . l < r !• ! ^ , - i / ' i ( ; l ' ' . 4 o r ' . ( • • • \ - i - \ - < t . j r > ' ;• ( • , ' i s i i r ( j i i ; e n t w i 1 1 - 1 a n

• . i . ' - ' - . - : ! : . • • ' • • • • r " . ' ' > • i n " . f c ? u i i - i r , L < - : . ' : • ' ' < t r < - ;n> , j '. i c n o - i r e l a t i v e t o o n e

• : r . - . ' . •• . : , > • : ' , • • •, ' •: l i r . M r r . ; i i , . " w . : i ! j i i ! . t i f - s . i n - " i n t . » - ; , . j ' j ( . f r i i n t o t h e i n s e r t ,

•.!.•• - r , ( . • • : • ' f ' ! , ! . I ' ; ? ' ? . ' • - ! . ' • ' ! ' i ' * ' • ' • : •.-, r i ' ' h f ' S d w r i r ) ' ; [ .• r ( - ' - , s i n < ; i s f i e t e r r i n e d b y

* > • • : ( • ; ' . • • ' • ' . ' • • • • r , : ' , ! . ' I 1 , - ' . T i " - ! • ' • ' ! ' l i e . r , r , e ; ' : ! l / h , i ' , 1 - f - c n ' ] < • ' , i q n e d t o c i l o v ; 2

•.. r f • -, •. i r . : , . r , , , -,, . r • . T f : i " . i ' . - i • ' ' ' f I • 1 l s h o d ! • > ' e " ; i ) f ; , i ( ) • : f - n d ( . H , ' ' S w i t h d i f f e r e n t

! ' • ; • • • ' , -,•• * ' : ' ' . ' i ' - : - f - l l i - ' i - , < r . - • > • ' ! n t , o v e r i r b e l i ' v . t h e r . p n t . f f r o f t h e i n s e r t

: • , ' • • . ' - f t ' . - i f . • M r f. ; i f - M c - i . i s I ' r ^ s s e d , n e w \ ' n n ( } , c , a r e e r p l o y e d a n d t h e e n d -

' •;: • ) ! ' • r e , ; r - r s " d f o r U : < - S f c o n d [ . r s ' S s i r v j . T h i s e n s u r e s t h a t t h e s e c o n d p e l l e ti s ''.-" <•] i r . - i n - i r i S ' s e d r e g i o n o f t h e i n s e r t .

i . J f ; i j i ;.•• o r , t . T r i e t j a l ' - i i l l i a r u s e d t o r i / t h e G R D G - t y p e f e e d g r a n u l e si s s - ' f ' , - ; ' : o r d r - " ; v : i i v ; ? ^ V - 7 ' ) ? n ^ l [ J ! . " h e r o l l e r a s s e m b l y i s s h o w n o n d r a w i n g s ? 6 Y -/ r ' f . / • ; ' 1 r i n d > r': ' - / ' * f: 7 ' ; [ > ? . A l l '' d t v i v n ' n g s a r c p r e s e n t e d i n t h e a p p e n d i x . N o t e' • ••,' n o : . - - i l l s - l i e '.•:• : 1 r r / e d d u r i r o • • . i x i n g . T h e - - o t o r a n d s p e e d c o n t r o l l e r u s e df o r " ' <>(• ( i }}!•<- l i s s e - \A i , i r e o f t h e s a n e t y p e a s t h o s e u s e d f o r b a l l - r i l l i n g t h ef f . ; f ' d ;•• r i . - . ' i c • r" .

The die a s s e - b l / is shewn on drawings 26Y-74791 Cl and 2 6 Y - 7 9 7 5 0 Dl p r e -sented in frit; ai.r.'S-ndiy. All die parts dre machined from A X M - g r a d e g r a p h i t eproduced !•/ '<)!)<'r\ Ciranhite, Inc. T hi -, material has c o n s i s t e n t l y proved to befree of flaws rind sufficiently pure to preclude significant d e g a s s i n g . Use of*his die asse'1,1/ will produce a hotpressed pellet with a ce n t e r l i n e d i a m e t e rof 'L"I .!'••'. in" and a centerline length of 27.R8 mm. Individual pellet d i m e n s i o n swill Vcir/ slightly dnpr-nd i nn on the tolerances obtained in mac h i n i n g the dieand the reactivity of the plutonia feed g r a n u l e s . The LASL shops r o u t i n e l yproduce dies machined to tolerances of 0.005 to 0.012 pim.

'( . P r o c e d u r e .a. Wei'oh 92". 064 g of - 125-;.m granules seasoned at 11 00°C. Place these

i n the mixi ng-mi11 jar.b. Weigh 61.376 g of - 125-um granules seasoned at 1600°C. Place these

in the same jar.c. Record lot IDs and granule charges placed in jar.d. Secure ball-mill jar lid. Place jar on roller assembly and roll for

15 to 30 min at 27 rpin.e. While the GROG-type feed material is being m i x e d , select the insert

and punches to be used.f. Visually inspect the insert and punches. Measure the punch d i m e n s i o n s

with a m i c r o m e t e r and record the d i m e n s i o n s . Do not use p u n c h e s w i t h d i m e n s i o n stnat are outside the tolerances listed on drawing 2 6 Y - 7 9 7 5 0 D l .

21

q. Clean the insert and :;ur:chr", with fi'jrrj r thor..,! usinq lint-fV.--«.•f hei-cc loft.

h. Wrap thf- insert and 'junchcs with -•-! 1: J • - i r. -jr- foil to kf'C-p rhr.-- rlean andi '.\tr'od j'.f' t.hfjT'• into the q l o v o b o / line.

i. for the first p r e s v n q with a now ins e r t , i n t r o d u c - the bottom punch•i'id p o s i t i o n the- lone o n d o a o , detail 7 on d-awinc '/'(, •' - /' 0 7 r/J Lil , at the base of'.fi" in',f'i' t.

;. A f t e r t h e OPOfl-tytjf; f e e d i'. m i / e d , w o i q h o u t ,, l c j ? . 4 4 q c h a r g e - . T h er e s i d u a l t ^ i l i n q w i l l b o 1 q , If;',', t h e a m o u n t ddcf""" i ns; t o thf- w a l l ' , o f t h e •<•}/.-[w. ; •• r. ". r<r '.'<-f t.hf t.'iilinq t o a ro r , i d o o c o n tn i n o r . P c o o r d t h e t a i l i i v ; a n d

'.*••! I ' ' i f - W - ! ' j h t ' , .

k . (,hr\rr:i- t h ' - d i ' : ! j , i r i q a ' • .• ' i ! •.•',', r J . f ; c l f u n n e l t a M n q c a r e t h a t - a t e r i -

ri 1 i - , i n t r o d ' j f . f d i n t ' j p a l l e t c a v i t y a r e a w i t h o u t r . o a t i n ' ; t h e T n c e r t b o r e .

1 . I n t r o d u c e t h e t o ; . \ > I I < \ O > a n d i n t r o d u C ' - t h e i n o f : r t i n t o t h e j U r , c e | j t o t

a ' , ! e r : ' ; , " K ' l o c k i • i u. f t i c i t i o r . t t i e c h o r t " " ' n d c a p , d f - t a i l 1 o n d r a w i n g ? f , 7 - 7 0 7 5 Q! l , a i . r ; . i t t ; f ' i r i ' , f - r i. a r i d v j ' . c o p t o r .

i; . '• <>r t h f - c e c o n d p r c ' ' , ' , i r r ; v ; i t ' r i ' i n i r r , o r t , r e [ ; e a t c t e i r , a t h r o u g h 1

"••• . " p t t h . - i t o n i / t h e p . j n . h e t r i ' - f ' d t o \><- c V - ' i n f - d , : n A , t . h e p o c i t i o n c o f t h e ? e n d -

' . ' i : , a r e r e - v e r ' . o d .

!he rii'ii'. pellet 1, are prev,ed orv- at M t. i r e in the ! A M . hot prect a c e m i . l /. o'i-, i cf. ino; of <i hy d r a u l i c './cteif, a vocuim ty.te- and an indue t ion-hea tirrsc / . te:'- cone i c t i nq of a work coil powered by a mo t o r q e n e r a t o r . The h y d r a u l i c•./•.'em powfrc the ? i-iain p r e c i n q cervora.-c and j actuator'.. The cervora-:'", are:-nui;t('d verticrilly and e/tond into the vacuuir; c h a m b e r c o n t a i n i n g the wfjrk c o i l .The actuator', a r e w,<-cl to rni'j: and lower the vacuui-; can r,o that the die a s -r,e:!!!ily may be int r o d u c e d and re m o v e d . The die ar, r,emM y i \ c e p a r a t e d from the•.frvoramc by q r a p h i t e s p a c e r s ',o that, durinq preciri'], thf' die a s s e m b l y isc :n f('red in the work c o i l .

A f t e r the die is positioner], the system is eva c u a t e d by mea n s of a d i f f u -• ion p u m p . T y p i c a l l y we load (.he press in the a f t e r n o o n , e v a c u a t e o v e r m ' q h t'Hid press the ne/t. r'orninq. The o v e r n i q h t evacuatirin results in a vacu u moh.v!-er p r e s s u r e of G.7 to 13 ;.Pa.

Aft e r the c h a m b e r has been e v a c u a t e d , the s e r v o r a m s , p r o v i d e d with w a t e r -eouii'd load c e l l s , are po s i t i o n e d so that the b l a c k b o d y holes in the s u s c e p t o rarc c e n t e r e d on the slot in the w o r k c o i l . A slight p r e l o a d , 517 k P a , ispro v i d e d . The timer is then started and the m o t o r q e n e r a t o r is br o u q h t on toC/.'J full p o w e r . The t e m p e r a t u r e is m o n i t o r e d with an optical p y r o m e t e r .When the t e m p e r a t u r e reaches 1 3 0 0 ° C , a b o u t 4.1 ruin into the r u n , the p r o q r a m m e dload c y c l e is ini t i a t e d . When the s u s c e p t o r t e m p e r a t u r e r e a c h e s 1 5 3 0 ° C , a b o u tt :•!in into the r u n , the m o t o r q e n e r a t o r is reduced to 50 po w e r for the r e m a i n d e rof the run. The full p r o g r a m m e d load, 11.8 kN c o r r e s p o n d i n g to 19.5 MPa forGP H S p e l l e t s , is att a i n e d in 8 to 9 min from the initiation uf the load c y c l p .The die is held at 1530°C u n d e r full load for 15 m i n , a l t h o u g h punch c l o s u r e isty p i c a l l y a t t a i n e d in less than 10 m i n . At the end o f the p r e s s i n g c y c l e , them o t o r q e n e r a t o r is turned off and the load is removed from the die a s s e m b l y .T h e c h a m b e r is allo w e d to cool for a b o u t 1 h and then the v a c u u m s y s t e m isvalv e d off and dry ar g o n is introduced into the c h a m b e r to f a c i l i t a t e c o o l i n g .A f t e r a s u i t a b l e cooling p e r i o d , the va c u u m can is raised and the die a s s e m b l yis r e m o v e d . T y p i c a l l y , we press in the m o r n i n g and remove the die in the a f t e r -noon .

' n - ' - h o t p r e s s s v s t o " i s c o r p l e / ( J n d a n u - b o i o f f n i r i r - ; :, w e n - e n c u u n t e r e dd . - r i r y : i n i ;. i a i J S O T h o w a t e r c o e i i n s f o r t h e l o a o c o l l " . , w o r t ; . o i 1 a n d v a c u u m'.•:••: ; « - , * ' ' i j r r . ! t o h e i n a d e q u a t e . T i i o l o a d - c o l ' n e a s i s s w a s s o l v e d b y a d d i r v j as i n ; i < - ; J / » - r j "1 / t i c s r n p h i t e s p a s o r t o t h e s t a a s -• L c ' v c a n ' ! b e l o w t h e d i e a s s e : > h W .; , r . ' j v ' - r t ' f . v j r. j •,••; o ' t h < - w o r k c o i l a n d v a c u u m c a r , v . . , - v . s o l v e d b y t h e a d d i t i o n o f a

' • > < s s t e r i . - j v j ; U i t ^ s ' k i t e d - v o r i m e ( . ( > ( , l i !!••'. v i i i t e r s v s N ^ . I n < i d d i t i o n , h e a t i n ;' • - ) * ' • ' , f o r t ' e d i e i s s e r L ; / w e r e t o o s l o w . T h i s w a s . < - l v e d !•/ w r c i p p i n - j a l a y e r• i f r, ..'.-•••:• - t h i s ^ s r a p h i f - " e l t a r t ; j n d t h e • , i s c e ; : t o r a : . . ; ','••! 1 i ' . • • : i ! i f : ' l a ( . o w i t h

/ ' • ' ' t o r M i ; - s . - •• o d i f i s.! f i o n o w p r r - M a d e , t h o s / s i c - r . w a . ' j s i - d . .-. i ' h o u t ^ u ^ t h s ' r.' -,-: ri - ; f , t.o ••'!»'.• /.'•• fW'>-:. p e l l e t s a c c r ; ^ ; ! i r v ; ' o t f i e f ! n w . v - ' d e s f r i !->vj i n t h i s• •'•sort .

!. : O|!ji;i-sait. T h e L A S L h o t c r o s s syste;- is .ii ilai t o arid h a s f v Sri^e<•]•>•<.'. i i i t i o s a s t h e i , r e d a c t i o n u n i t , a t f,pp e / s o ; , ! tJu'* t h e [..-'I. p r e s s i s l o a d e d ,o[;(-> .-i ' o d . ar,d idlf; -idorl m a n u a l l y . T h o " a t e r - h l s Tr-st '.;stf'-s / - c y c l e p r e s : j u n i tc s n - . i s t s of ' s o r v o r d : - a c t u a t o r - in a cl o s e d - c y d (; t e s ' 7 o i •; J a n d '- s a f e t y -i r; '.c-r 1 f;C M'-' i f i o t j ' i t o r s ?.h.i+ tire j s e d t o r a i s e , l o w e r , a n : c i-i"!1 t h e s t a i n l e s s•.'.oi-1 v - : s . us c h a r : . o r i n t o p o s i ' i o n . T o p c o n t r o l s -jriri h y ' . ^ ) w l i c r.anif o l d i n q a r ed'-s isTied s o t h a t h o t h a c t u a t r i r looi'S c a n h e o p e r a t e d . i' • • u 1 t a n e o u s l y o r i n d e -s'-ndoi, t i y . frich ot t h o ; • r j in s e r v o r a : - ' is u r o v i d e d w i t h , a w a t e r - c o o l e d l o a d c e l lo< tnc- t y p e s h o w n o n d r a w i r r ; ? f • Y - 7 f-< i 5 S H I , p r e s e n t e d in t h e a p p e n d i x . C i t h e rs e r v o r - r •• ,iy h e u s e d a s t h e :'!ain c o n t r o l r a m . T h e p r o s c i n o c y c l e i s d e t e r m i n e d\./ 'jso o f d Dtita T r a k prr/|rai rii -er a n d t h e i n t e g r a t e d s i q n a l f r o m t h e l o a d c e l ll o c a t e d i n t h e m a s t e r s e r v o r a n . T h r e e H e w l e t t - P a c k a r d M o d e l 7 1 0 0 E 2 - p e n r e c o r d -e r s dft: u s e d t o d i s p l a y t h e d i s p l a c e i r e n t o r s t r o k e , ran 1 v e l o c i t y a n d l o a d e d c e 1 !o u t p u t f o r b o t h s e r v o r a - s . T h e h y d r a u l i c f l u i d u s e d i s F y r q u e l p h o s p h a t e e s t e r ,m i l i t a r y s p e c i f i c a t i o n 'Jo. M I L - H - - C ; 3 2 H 2 , a n d t h e s y s t e m , a s p l u m b e d , i s c a p a b l eo f p r o d u c t n o a ma/. l V u r l o a d f o r c e o f 1 6 . 3 kfj.

The heafin'i systet1 consists of a 100 kVA motor generator and associatedcontrols, viator-cooled leads carry the. rf current froiv. the capacitor bank tothe work coil. Temperatures are measured by sighting with a Micro Optical pyro-meter throuoh an optical quartz window into 1 of 7 blackbody holes drilled intothe susceptor. Water cooling for the load cells, double-wall vacuum chamber,capacitor bank, rf leads and work coil is provided with a limited-volumepositive-pressure water system with a capacity of 30?..

The vacuum system consists of a Varian 102-mm-diam Model M4 diffusion pumpbacked by a Welch Model 1397B mechanical pump. Convoil No. 20 oil is used inboth pumps. Suitable manifolding is provided so that the vacuum chamber may beevacuated to 6.7 Pa prior to opening the gate valve to the diffusion pump.Chamber pressure is measured by thermocouple gauges and a Granvi1le-Phi11ipsModel 270 ion guage controller connected to a Bayard-Alpert guage connected toa high vacuum flange by means of a kovar seal.

2. Procedure. Assume that prior to the pressing cycle the hydraulicsystem and"the motor generator are off and that the chamber is evacuated.

a. Turn off ion guage and close gate valve between vacuum chamber anddiffusion pump. Open valves to dry argon sypply and bring vacuum chamber toambient glovebox pressure.

b. Turn Master Control power ON. Reset interlocks if necessary. Turnon channels 1 and 2 and set at HIGH RANGE.

c. Check that servorams are in fully retracted position.d. Switch by-pass clamp interlock to BY-PASS position.e. Turn Lift-Clamp switch to LIFT and raise vacuum chamber.

23

-; ' 1 • ' '. •, i

r . • k ' • . ' r • . r i •' '

i ' ' -' I •••

'.''!'• •'•'.'••:' i ' -i ' : i :. ,.•: i '. '', ' i '. . t ' ' - r ,

; . l ' • ' . ' . i ' i ' ! 'i . V: '. '• ''•',''.< <•''. \\<- / ' ' •' ' lii '•'! .

', . ' ' ' • ' , < • ' ; '; ' ' - r , ' ' ' '. ! ' ' ' i ' • ' ', •; f

/ T J '" F

M • ' ' • • ) ' !

f : .

! ' i i ' • : ' r , ' , ' > • > ; , • : <\ '. ' . ] < " . . - , i .- • ' • , / ' • ' ' • ' . • " r - i ' . i t ; t . i ! '. ' , / ' , ' . < • • • i ' . 1 '

r • < • : . • , ] ' . < • : ::•: ' < • ! ! i . • • ; • ! ' • • ; . J 1 ' '.'•', ' • : • • < . J < \ \ \ ' ! - ' . < ! ' . h < - ' . ; " ' - ' • • " •

'. . ' "• ' ' . ' :"• 1 , • ' .• • .1 { • ' < • I . i I .', r : r : ; ! -! i ' ' r , v I T , t , ' . . V / 0 I " J [ • ' •'; r ' , r i I I .

' < • • • • • • ' • : . i \ . ' < ' • ] ' • " - ' i - r . - ' * . , . ) - , > . / . , , r ' ' . T ' . ' . ' M r ' t . ^ - f j V ' l n ' ' • [ ) ! • ' , > • " \ ' ) ' • ' ' • U > \ I i i 1 . 1 -

: ' ' . . - ' • ' ; H i " i - : • : . - d r • J t • , " . } < • . ' . - : \ l i . \ : ' ' < • . • . * > • ) • r . ' , ! ' , ' f h ) I ' r i f i f l t o I 1 i - l ' ! r j t ' 1 " - V r ' , ; ,

• : ' ! ' : f : ' . < ': I ' . ! 1 , ' ! . . • ' . ? ( ' • ( ( ,! i ] ' ••'• ' , 1 l l ' f , f f j l V ' l , [ . • ! ) j I I I . , :| ' . ' i i l i l - f 1 I " ) . - ; .

r . ' • . ! • ; . '. i ' i - i . M i ' I ! J r ' i r • •. , f . ( n ' 3 ' - r i * - r - i t . n : t o *",''.%• ' j i 1 : i f j ' . - . ' f • r ' .

' • " > < ! • i n ' / I ' , ' ' - : . 1 ! i r ! . r - : • < • . • r -"• t . u t ~ f • <•.'. ] ' ; ' , ' J 1 : ^ ', i n t . f - i v a 1 ' . w i t h V <• ' . : t i c r j l

; • i t ' i " > • ' • ' .

;.. V . ' n i M . * . [ • : • ; f t •: t.'it >• r i j t i t h i / ' , V - ; f ! ' ' ; ( ) f ''. f . j f - ) i r • i t _ i . , t o ;•, ,-; ; c - i ir ! ! (-d l o a d c . y c l r ;

: ,• - . w ; ! ' . h i n ' ; [!>•".;'• I ! - ' , " ' • • i, R ' i ' , .

J. M o n i L i . i .I'r' ifc.'i'.-i t.f'i; p(;rri L u r e a r i d l o a d t h r t j i i ^ h o u f . t'ic r u n .v . V J h c i : '.("'.•.''•r.)' irt' r f i u . h f ' ' , ] r i ° / l ° r ' t n i o ) t c d ' j i f - f i t ' i r ' j e r v - r . i t o r t u r J 0

f • - 1 ' j ' O w j i" * o r r'f-"i,) i •• i' f r -»- '] t r i n .

fi'iff- w'if'n ', v", t < v i'. -1*. iirn;r,)y:: (H] I n / i d . T h i s w i l l o c c u r a t - o u t ^ n i nI I ' ' - I i n i t i ; ! ' i o n o f 1 < M O r / c i f . M-j i nt,i i n \>r'()",r<>f-:\tjri l o a d a t 1 v ; 0 ° C t o n p e r a t u r e' > !': •• i n .

Turn off -int(<r ii'-nc-rri t nr -.'.mi rotat(' DATA TRACT, to down slope to re-\t:.rif load, '.••hen sorvorai;:', art- fully retracted, introduce a neqative si'qnal to'..ie r c ! Point Control and turn off the hydraulic syster:.

y. When vacuum chanber has cooled for 1 h, repeat steps a throuqh e andrp::o'.'c dio assembly. Note that argon should be introduced 1 h before proceedingto step b.

z. Repeat steps h throuqh k to leave vacuum chamber evacuated. Placerun sheets and record charts in appropriate folders.

I. Post-Press Sjnjiering and Pellet StorageAfter the pellet is removed from the die insert it is stored in a graphite

container for 16 h or longer (overnight). We have stored pellets for as long as2 weeks prior to sintering with no deletorious effects. After storage, thepellet is weighed and the dimensions are measured. The pellet is then sinteredin flowing A r - H ;

l r O for 6 h at 1000°C followed by 6 h at 1527°C. Heating andcooling rates are 150°C/h. The same Astro furnaces are used for the sintering

24

...••• : ..... , . • • . '>•.,• ' , . . - : e r - l ( o / c u i n q e a n d g r a n u l e s e a s o n i n g o p e r a -• . • - . . . • ' ..:•'., • i ] * -: -i ' - i e d , i n A i ' l a t v s r ! o : i t f i l l e d w i t h h i g h -

• •• •• • .. . • . .'.--.. • ' • • . ; [ ; : . t » e :.»-1 I*--* i s i - z - i s h e d a r i d t h e d i m e n s i o n s

• • • . ' , • : ' • : :••'•• :*. •':)->• t h e n c a 1 <s; 1 a t . e d . T h e s i n t e r e d• •• • • *•• :• ::• i''• i r.fi tii i n c r j t / i l • <~ a r s f e r r e d f o r u s e . D u r -

.••'... ;,.'•,.• ij.'<.r-',i.;n' w i l l s h r i n k h y a b o u t 0 . 5 t o

• • • • • • • . •' • : I ,' •• r ; : i1 r e d . j < e d t o 'i ' t o i L h i c u r e t r y o f a b o u t• • • • • . • ]. - * . . . . - ? - ' . ! .' ' ••; f 'ia t i t w i l l b f r e n / i d i z e d t o P u O

• • • . • . • . . • • . •; ,.r •.: - . i i : :• ' i..' i ' i f . ' . i - i 1 a r l v . t h e A r - l l - -' 0 q a s• •••• ••• > • • ••• ' ('!.-:•.•• ; '. J i ' : ( • • : i.'i '•:• i - n , . ; > ' ' • a s t n i c h i o r e t r y o f

• • •. ••. ..';.• • , i ' : ' . f . - : . T v : ( - : ; s e r.,< ' r - - '••••• f l n w o a s , o f c o u r s e ,

• • . . • •• :> ; • • . ( • ; ' . - r i a i , i n d r 'il <•<•'•; if-r. t i n c r e a s o f i n e u t r o n e - i s -

• • ••• . '•• i .-, •• :• : r , : jr..i , •,,- ] jt,•.- r . - i ' e s •!!''• f.-'•; l o v e d t o ( " ( ' d u c c t h e

• •• • • •••• •''. • • • ' f i : ' ' . ( • ; i - l l ' - ' . '• i r; t o r i w\ t h e [ ' d i e t i n a p l a t i n u m

•• • • .•,;•• •• i ! .• ;••,,•, ii.|- : i " t ; V " n ' . . f h e r ; . ( i l s t r ' - ' s p o i n t - - t h a t c a n o c c u r i f1 • • ; - • • - .- i n '.':••••.' i ' n t a e t ',-.'' !i t h e ;••] a t i n u 1 1 .

'•• . •'.'••.*;.••••• . - • ? h f ,'• r j ; . e i M t i t j n s i s i n d i c a t e d b y t h e f a c t t h a t f l o w:•••!!••• • ' . ,i '.: >• •< <•.'••. d u r i n g s i n t e n t 1 / : a n d t-.y t h e i r p a c t t e s t r e s u l t s .

:.•••-. ' : ."• : ,: •• ; . . - 1 ' ' * s <•(,• ri'isu 1 a t(.-d i n i r i d i u r c o n t a i n e r s h a v e b e e n i n : -: : • > • : . •'• I ! ;- :-! ' t ' - ' s wer - - - S'jcf.f.-ss f u l a n d i n n u c a s e d i d t h e f u e l b r e a c h• •.'• ' ! • : ' • . ( • r • ; • • r i a ] .

1. • V ' i; • ••!. t. "';(• " f j u i i ' - n t u s e d f o r t h e s i n t e r i n g a n d w e i g h i n g o p e r a -'.!;'. s.i, .'""i. -if.-'.t ii-ed rit;ovf. r'w,s f l o w s arr : t h e sai"e a s t h o s e u s e d f o r t h e',//'•.!•' -' ( '•-••:'::' -iir! iranulr- s e a s o n i n g o p e r a t i o n s . N o t e t h a t o n l y t h e A s t r o*.iri;-!C-s -if. ,','••[ r':r t n c s i n t e r i n ' : o p e r a t i o n s . T h e p l a t i n u m h o o t i s f i l l e d t o•'.\"'i' ,' f.•! :•.!•' i',•• wifti t h o r i a p o w d e r p r e v i o u s l y s i n t e r e d a t 2 0 0 0 ° C . T h e p e l l e ts t o r a ;< cni'.'i in'-r is s h o w n o n d r a w i n g ? 6 Y - 7 9 o 2 9 Cl . T h e m e a s u r e m e n t s t a n d i ss h o w n -.1- d r a w i n v . '•'< >'- 7n::'^ !)1 a n d P 6 Y - 7 9 5 9 4 \)2. L a c h o f t h e s e d r a w i n g s i s p r e -sijfi *".ed i fi '. h'.- a;.j•'•v.'\ i / .

a. Transfer the die assembly to the pellet storage and dimensioning area.!.-. Re;sove the endcaps and the susceptor. Remove 1 punch. Note that if

the insert is to be used for a second pressing, the pellet must be pushed outof the end of the insert farthest from the bore region to be used for thesecond press ing.

c. Place insert on Carver press and use stainless steel rod to push outpellet. Secure pellet with stainless steel forceps before it can fall to thepress platen.

d. Place pellet in graphite storage container and leave it there for16 h (overnight).

e. Weigh the pellet. Check the micrometer with the standard block andmeasure the pellet dimensions. Record the weight and dimensions.

f. Transfer pellet to furnace qlovebox. Place pellet in platinum boatfilled with thoria so that pellet is half-buried with endcaps facing the furnaceends.

g. Place boat in Astro furnace, seal furnace, position thermocouples andinitiate gas flow.

h. Check that correct chart is on the DATA TRACK programmer. Beginprogrammed run cycle.

i. When sintering cycle is complete, remove boat from furnace. Removepellet from boat and brush off any thoria particles with a stainless steel brush.

25

,. ; .-• ', ] f - f I , ] - . ' ' '• ' ' ' '• . ' • : : • i ' . ' •

' ' •• i ' • ; . f - ! ! i •' i r . r .-: • , ' • • '

' . • • : ; . ; ! • ; ' ! • , ! • . : ' . ! ' I • ' • : ' . ' • • / i » •: ' . i ' ; l

i r . ( I T ' • ' ! ; , [ • ! | i - ' i . ! f j - j . - i f - ! i n 4

. • - - ' . . . : • • . i ! - - ' : . , ; . - . ; < : . - T ' - / • • ' / .

, . - . ; , , ' , [ , ] ' , : ' • • • : . : • • ! ' . • ; < • • / i - r . ' ' .

: « • • . . . ' • . • • - - ! ! • ! ( / / . ) ' ; - - r ! ' , r

• i • ( ' • ' : : . / - . • • ! • • ! • ! ' : M ' . > ! • - : - . * • - r „ • - '

: . • , T . - . : ' • • : ; : , • ' • ' , .-. ' I ; ! ••• - . " •

- . ' . : • • - • ' i - • . - , ! : ' , ! ' • '.< • _, i ! < • • [ •

1 , , . . , , I I , ,1 . • ' , . . . ,-. , 1 . . . . r / . ' i

, • . ' • ' , ' . ' . / I ' " ' ' ' . • ' . ' • ' .' ' ''•• ' '•• 1 i : ' • ' ' ' • ' < • ! '.' • ' '• i '

•< < , ' ' ' . . , ' * ' < > • • • • . : • • . , ' • > • ' • . - ' ' i •'. i ' - ' ' ' . < > : • < ' -

1 i t - i ' . ' . '• i ! •. :\ - 1 ' •'. -! ' '• ' . I f •, 1 r ; ( • •! * / , <<-.•!<•<:

-,]•• ' • . • . • , • ! ; • ' • ; ! . • • • ' ' . ' • • t ' - i ' i ' ! ' r " . : r . - . • " - . r - . < - . ; > , . t , . , .

, , : : • • ( • • . ' . : - < • • : : • , ! ' • • I ' - : - , i n : • : ' • ' : ' : • ' • ' - : . ! • • • • ' . ' ! ; ' • i . I f " ! V M * • • • -

•• '; / ' i i ' : '• ; i ' , ' i ' . .! T i ' ! ' i ' I ! ' . I ' ' ' , \ , ' , ' • ' ' ; ] ' ' < • : ' ' • I K ' ' ' " . , ' ' •' •'' '. ' •'. I ' • ' - '

' ! ( . ' • ' ) , T ' • . ' , i n ' " ' . > / ' • ' 1 ' • ' ! ! : i I : 1 : ( ; ; . • ' • • , i t i f i r , i n y , 1 ; < • ' , ' > : < • ' r . i - < ' •'.'. i : :

. . , ] ! i . l ; i i f i / . i i ' , : •. r j r i i t . r . T h e I I < ' . < • ' . I H t -: I ! ( !•• ( • • . .f ) ' ; •! r , f i i . ' . ' , •!' • I ' , f i 1 " ; ' : . - i r - ' l •">''. - 1 o f l i f i n • )

: - j : . • • • ! M / I ' • [ ! ( • l i i ' i l ' T . ' [ ' , < • - , n n - f . i / ! ' ' i i j r ' ; K ' , i f i ' l i n t . o t . h c w - ' i t . T .

: , . [ - ' ( • ; i " , i f m i ! i i •; r i r i ! [ , ( v " i f f r " r , f w i v f - ( . r • r - n [ . I ' f i M r r - r l .

P ' i j r } ' ' , ( i r.'] •>' ' l i ' . t i l l f ' ] w - i l . f r i n ! o o f o M > ~ : . h h f < i h - f .' . f ' f j j f I ' ; ' ! ; : i l o * p u r e f t j i f i n o l i n t . r i -i f i H h l i f ^ k c r .

f . U s ' 1 U i f n i t \ c 1 - | i I a f f < l f r n " f ( • [ ) ' . l . o I T P O V 1 o i p s u l r ; f r o c - r t i r l o r J ' d n < j j ; l f i ' . oi t i r t . h f j f i r ' , t . i K . i i ] t i f ' a i ' f - r . ! ' p f | 5 f r i j i ' ^ u l < • i i i i i i i o r s o d f o r ? t . o 3 i i i i n .

f . R o m n v f . ' ( . o i i r , u l f f r o r f i r ^ t . r ' i r . i d h n f i k o r , w i [ > e w i t h w o t c h p f - s o c l o t hi ' w . - i L ( ' r ) a n d p l a c r : c i i ' . u l f i n \ f ( o n d , i c . i d ( I C I K T . T h e h a t f r o r : t h e C f i p s u l e w i l lo i j i c k l y d r y t h e c h f f . f c l n t . h .

<\. R f | . ) f ? ' i t s t e p f , i i i o v ' i M M c a p s u l e t o t h i r d a c i d m j a k e r .

f i . C o n t i n u e siK.ce^. ' . i VP immerc , i o n s i n w a t e r dm\ e t h a n o l , 2 t o 3 i ; i in e a c h .i . A f t e r i i : nner r , i on i n e t h - m o l , c a p s u l e s h o u l d have f e w e r t h a n 50 c o u n t s

p e r s e c o n d ( s w i p e ) . I f s w i p e c o u n t i s q r e a t e r , r e p l a c e c a p s u l e i n t h i r d a c i db a t h and r e p e a t i m m e r s i o n s .

j . When c o m p l e t e d d i s p o s e o f c h e e s e c l o t h i n p r o p e r c a n , p o u r a c i d andw a t e r i n t o l a b e l l e d p o l y e t h y l e n e b o t t l e . R e p e a t f o r t h e e t h a n o l . Do n o t m i xe t n a n o ! and n i t r i c a c i d .

K. F l o w s h e e t SummaryThe f l o w s h e e t d e s c r i b e d i n t h i s r e p o r t has been used t o f a b r i c a t e 25 GPHS

f u e l p e l l e t s a t LASL. The s i n t e r e d d i m e n s i o n s f o r t h e s e p e l l e t s are l i s t e d i nT a b l e V I I I . These p e l l e t s have a v e r y homoqeneous n n ' c r o s t r u c t u r e , an e x c e l l -a n t r e s p o n s e t o i m p a c t and a h i g h e r d e n s i t y t h a n p r e v i o u s l y used f u e l f o r m s .

26

1 .00 91.0,0 f.1.0';',

1 . ').>:•',

"0003

1 ''•'••'•

i .0001 .'];•:,:1 .003l or<31 .07'-1 .Of-;11 .0931 ,0''G

1 .090•0.006

lo

15

1115?.11/1 '':•:•'. 3 2 5-

. -11 ,0

.351

. 397

. 200

.356.. -307

152 377 b

• 0.051

'•',( . 1

M5.1VA . 3R5.705.1-05.1KG. 684.8' > /i n

86. 785.685.1J5_5.4_

85.01 0.7

'^Jui^oroir. <idjij%ti':ents v/ere made to hot-press after pressing eachof the first 3 pellet lots. Dimensions for lots 4, 7, and 11 arenot included in the averaoes.

Standard deviation in weight corresponds to 4.0.02 watts.

27

; I ( • • i ; • i t . ! ' i ',• ; • • • • ; i ' , r ( • .

: r i > - ! i ( • - ; •• - i ' . I T - i . i ! w i l l : •> < • ! ! r i ' .

' . ' 1 | ; . ; • , ' • : , . v h ( - t f i t - , ! : a d i • .

'-.. - ; j ! i t /

1 1 i f 1 p i i t i ' .• -.; •••'• i ! :: r . 1 ' i i j r i •. f o r f h f - ! < • • < • ' ! ; i o w d < ' t - i r i d S w b ' . e ' i j " n '. ( ' j * • ] : " • '• 1 < • ! . ' ,

'.-v i I I [ J C 1 » ] : ; ' , ' • I r . ' i ' d ! o f M i i ' . . 1 f i i " l i n " a b l e i l l . r o l u s - r . ? , o r t f . i s r u p - i f f .

' • . ' . t f . i I . i o n I :• i ' , ' , i o n f - ' . i f f

[ h e r v ' i i t r o i i ( • • " ] ' . • i o n r a t . f f o r i . h ( - - . i n f o f o d f i j f • 1 p e l l e t ' , w i l l b e 1 ' " , ' , t h a n

L . F a b r i c a ti on F I fn-r.Fief.'t.T h e f a b r i c a t i o n f l o w s h e e t used to p r o c e s s the feed '-'a'erial and ;-:aie the

GPH r; p e l l e t s will be l.hat d e s c r i b e d in this r e p o r t .

F. Fuel C h a r g e and Th e r m a l I n v e n t o r yT h e g r a p h i t e d i e s used for hot p r e s s i n g the p e l l e t s will be ch a r g e d w i t h

1 5 2 . 4 4 + 0.01 g of G R O G - t y p e feed g r a n u l e s s e a s o n e d at 11 DO + 15 ° (60 w t ) and160 0 + 15°C (40 w t ) . T h e thermal i n v e n t o r y for the p e l l e t s will be 6 3 . 0 !•: org r e a t e r as p r e s s e d .

The sintere"d dimensions for the fuel pellets will be 27.64 ± 0.15-nnii-dian:by 27.69 + 0.25-mm-length. The density will be set by the dimensions and thecharge weight and will be 85 + 1 TD.

28

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i i ' • • . :• j . < • '

' IM '.< j , r , _

• 1 ' ,

. i lt '• '

' ' '. ' u [ .:'. ' < r d t i n •.• ' • ' ' • ; ' O r I. L A -

: : . ."•. • ' ' • < ' , • ' • ' • [ • • • . i ! ! ••• [ • si r i •". i 11 r i o f • ' " T ' u f )

•> , : ' ' - ; - - • I • • - > '• . - " • n e l r . i . n / , T - 7 6 ) .

• ' < • : • ' \-' \ '•• - i :.-",: -'•" ' ' • " , ! / . 1 f ) 7 f , " ' .

. I ' ' / / , ' • ' • i ! ? . : - ' V i . i r v f i 1 . - , 1 . i t . t . r u e ! ^ [ . c c i f i c a -

i ' - n ' . i f !•:. ! ( - : ; ! > ' > ( " ( ! f . r j r y . i i n n : j !• 1 i c ; h c d w o r k , 1 9 7 9 .

APPENDIX

PROCLV.I ' .C : 0U IPM[ ' ,T DRAWINGS FOR LASL CPHS PROCESSING FLOWSHEET

T h i o af.pc.Ti-! i / ir. r. l u d f j ' , t h e f o l l o w i n g d r a w i n g s :

^ Y - 7 9 2 34 Cl 26Y-79204 Dl 2 6 Y - 7 9 3 5 5 Dl

26Y-79394 Dl 26Y-7967.; . Dl 26Y-79594 Dl

26Y-79394 C2 26Y-79673 D2 26Y-79594 D2

26Y-74491 Dl 2 6 Y - 7 9 7 5 0 Dl 2 6 Y - 7 9 8 2 9 Cl

26Y-74o72 Dl 26Y-74791 Cl 26Y-79902 Dl

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