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    JO U R N A L O F M A T E R IA L S S C IE N C E 21 (1986) 3223-3226

    X - r a y a n a l y s i s o f m i c r o s c o p i c s t r u c t u r e i n

    d e f o r m e d b r a s s

    F. T U N G , S . Z W U I , Y . W A N G

    Physics Department, J i l in Universi ty, Changchun 130023, China

    The m ic roscop ic s t ruc ture o f brass i s sys temat i ca l l y s tud ied by X- ray d i f f rac t i on pro f i l e ana lys i s

    in th i s paper . The samples were heat t reated d i f fe rent l y and deformed in an un id i rec t i ona l ten-

    s i le s tate. Parameters such as the ef fect ive grain s ize, average dis locat ion dens i ty , d is locat ion

    conf igura t i on parameter and s tored deformat ion energy dens i ty are care fu l l y deduced f rom

    X- ray d i f f rac t i on data based on some recent theor ies and models . These parameters change

    wi th macroscopic s t ress and s t rain regular ly and i t i s poss ible to establ ish a quant i tat ive

    re la t i onsh ip between the m ic roscop ic s t ruc ture and macroscop ic proper t i es . There i s an un ique

    re la t i onsh ip between the s t ruc ture parameters and s t ress ra ther than s t ra in fo r d i f fe rent sample

    heat t reatments .

    1 . I n t r o d u c t i o n

    A f t e r p l a s t i c d e f o r m a t i o n i n m e t a l s t h e r e a r e a l o t o f

    d i s l o c a t i o n s w i t h v a r i o u s d i s t r i b u t i o n s r e g a r d i n g

    d i f f e r e n t d e g r e e s a n d w a y s o f d e f o r m a t i o n [ 1 ]. D i s l o -

    c a t io n s m a y b e a r r a n g e d t o f o r m s u b g r a i n b o u n d a r i e s

    o r t o c a u s e a ce ll s t r u c t u r e a n d t h u s m a k e t h e c o h e r e n t

    d o m a i n s i z e s m a l l e r w h i c h c a n b e e v a l u a t e d b y a n

    X - r a y m e t h o d . I n t h e c a s e o f d i s l o c a t i o n p i le - u p s o r

    r a n d o m d i s t r i b u t i o n t h e r e i s a l a r g e l o n g r a n g e s t r a i n

    f ie l d c a u s i n g a s p e ci fi c b r o a d e n i n g o f X - r a y d i f f r a c t i o n

    p r o f il e s [ 2 ]. T h e m a c r o s c o p i c m e c h a n i c a l p r o p e r t i e s

    c h a n g e c o r r e s p o n d i n g l y w i t h t h e m i c r o s c o p ic s t r u c t u r e

    w h i c h c a n b e s t u d i e d s t a t is t i c a l ly b y X - r a y d i f f r a c t io n .

    L ine p ro f i l e ana lys i s i s ab l e t o g ive t he ave rage

    c o h e r e n t d o m a i n s i z e , d i s l o c a t i o n d e n s i t y a n d c o n -

    f i g u r a t i o n . S t o k e s ' [ 3 ] d e c o n v o l u t i o n m e t h o d a l l o w s

    t h e s e p a r a t i o n o f t h e p h y s i c a l b r o a d e n i n g p r o f i l e s

    f r o m t h e i n s t r u m e n t a l o n es a n d t h e W a r r e n - A v e r b a c h

    [4 , 5] a n a l y s i s g iv e s t h e d o m a i n s iz e a n d m e a n s q u a r e

    s t r a in . W i l k e n s [6 ] h a s p r o p o s e d a m o d e l o f r e s t r ic -

    t e d l y r a n d o m d i s t r ib u t i o n o f d i s l o c at i o n s t o a n a l y s e

    t h e l i n e p r o f i l e s a n d h a s o b t a i n e d t h e d i s l o c a t i o n s

    d e n s i t y 0 , c o n f i g u r a t i o n p a r a m e t e r ~ r , s t r a i n f i e l d

    r a n g e R o a n d s t o r e d e l a s t i c e n e r g y (El V) f o r m o n o -

    c r y s t a l c o p p e r . L a n g f o r d [ 7, 8 ] h a s s u g g e s t e d t h a t e a c h

    p r o f i l e c a n b e c o n s i d e r e d a s a c o n v o l u t i o n o f s e v e r a l

    G a u s s i a n f u n c t i o n s w i t h C a u c h y o n e s [ 7 - 9 ] . B a s e d

    o n t h e a b o v e m e n t i o n e d i d e a s W a n g et al. [ 1 0 ] h a s

    w o r k e d o u t a p r a c t i c a l p r o c e d u r e a n d s o m e s t a n d a r d

    c u r v e s f o r l i n e p r o f i l e a n a l y s i s o f f c c p o l y c r y s t a l s .

    R e c e n t l y s a t i s f a c t o r y r e s u l t s h a v e b e e n o b t a i n e d o n

    h c p a n d b c c p o l y c r y s ta l s a n d o n m u l t i - p h a s e f c c

    a l l o y s a s w e ll [1 1] . I n t h i s p a p e r t h e r e s u l t s o n c o m m e r -

    c i a l u - b r a s s a f t e r u n i d i r e c t i o n a l t e n s i l e d e f o r m a t i o n

    a re p re sen t ed .

    2 . E x p e r i m e n t a l d e t a i l s

    S a m p l e s w e r e c u t f r o m t h e c o m m e r c i a l u - b r a s s c o n -

    t a i n i n g 3 1 .5 5 w t % Z n , 0 . 6 m m t h i c k , a l o n g t h e r o l li n g

    d i r e c t i o n . A f t e r p o l i s h i n g t h e y w e r e a n n e a l e d i n

    v a c u u m a t t w o d i f fe r e n t t e m p e r a t u r e s f o r 2 h, n a m e l y

    a t 6 17 K f o r s a m p l e s o f g r o u p A a n d a t 6 51 K f o r t h o s e

    o f g r o u p B . A s f o r g r o u p C , s a m p l e s o f f il in g s a t r o o m

    t e m p e r a t u r e w i t h o u t a n y a n n e a l i n g w e r e u s e d . T e n s i le

    d e f o r m a t i o n w a s p e r f o r m e d a t r o o m t e m p e r a t u r e w i t h

    a s p e e d o f 0 . 2 6 m m m i n - 1. T h e s t r e s s - s t r a i n c u r v e i s

    shown in F ig . 1 .

    X - r a y d i f f r a c t i o n l i n e p r o f i l e s w e r e r e c o r d e d b y a

    r o t a t i n g a n o d e X - r a y d i f f r a c t o m e t e r w i t h C u K u r a d i -

    a t i o n a n d a g r a p h i t e m o n o c h r o m a t o r . T w o p a i r s o f

    re f l e c t i ons 1 1 1 /2 2 2 an d 2 0 0 /4 0 0 we re m easu red on

    d e f o r m e d a n d s t a n d a r d ( a n n e a l e d b u t n o t d e f o r m e d )

    samp le s o f 18 m m x 10 m m s ize.

    A f t e r S t o k e s ' [ 3 ] d e c o n v o l u t i o n t h e p h y s i c a l

    b r o a d e n e d p r o f i l e s a n d i t s c o r r e s p o n d i n g F o u r i e r

    coe f f i c i en t s

    A(L)

    w e r e o b t a in e d a n d t h e n t h e t w o c o m -

    p o n e n t s , p a r t i c l e c o e f f ic i e n ts A P ( L ) a n d s t r a i n

    coe f f i c i en t s

    AS(L)

    w e r e s e p a r a t e d a c c o r d i n g t o [ 1 0 ] a s

    L

    A P ( L ) = a - - - ( 1)

    Do,

    AS(L) = e x p ( - 2 f l0 L - ~ /~2gL2) (2)

    w h e r e a i s t h e q u a n t i t y e x p r e s s i n g t h e h o o k e f fe c t,

    L t he spec i f i c l eng th pe rpend icu l a r t o t he r e f l e c t i ng

    p l a n e s , D ee t h e a v e r a g e e f f e c t i v e c o h e r e n t d o m a i n

    s i ze , and /~c and ~ g t h e C a u c h y a d G a u s s i a n w i d t h s o f

    s t r a i n b r o a d e n e d p r o f i le , r e s p e c ti v e ly . M a k i n g u s e

    of t he s t and a rd cu rves an d p roc edure s de s c r ibed i n [10],

    t h e a v e r a g e d i s l o c a t i o n d e n s i t y ~ a n d c o n f i g u r a t i o n

    p a r a m e t e r ~ r h a v e b e e n o b t a i n e d a n d t h e y g iv e d i r e c tl y

    t h e s t o r e d e l a s ti c e n e r g y d e n s i t y El V

    E ~ r

    -~ = AG~b 2 In ro(~)m (3)

    whe re A = 1 /4~ fo r sc rew d i s loca t i ons , A = 1 /4~z

    (1 - - v ) fo r edge d i s loc a t i ons , v i s Po i ss ons r a t i o , G i s

    t h e s h e a r m o d u l u s , B i s t h e d i s l o c a t i o n s t r e n g t h a n d r0

    i s t h e d i s l o c a t i o n n u c l e u s r a d i u s .

    0022-24 61/86 $03.00 + . 12 9 1986 Chapman and Hall Ltd. 3223

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    2/4

    o"

    ( 1 0 7 N m -2 )

    40

    2O

    A . ~ t _ ~ _ ~ - ~ " - - ~ -' - 4 : 3

    o j . . ~ - ~

    0 10 20 30 40 6(% )

    Figure 1 F l o w s t r e s s - s t r a i n c u r v e s f o r s a m p l e s o f

    g r o u p A a n d B . ( D ) G r o u p A a n n e a l e d a t 6 1 7 K

    b efo re d e fo rm a t i o n , (O) g ro u p B an n ea l ed a t 6 1 5 K

    b e f o r e d e f o r m a t i o n .

    3 . R e s u l t s a n d d i s c u s s i o n

    T h e f l o w s t r e s s - s t r a i n c u r v e s f o r s a m p l e s o f g r o u p A

    a n d B a r e s h o w n i n F i g . 1 . T h e d a t a f o r b o t h g r o u p s

    c a n n o t b e p u t o n a n u n i q u e c u r v e , i . e . f o r a d e f i n i t e

    e t he re i s b ig d i f f e rence i n a fo r samp le s ann ea l ed a t

    d i f f e r e n t t e m p e r a t u r e s .

    T h e D e fr -s c u r v e s a r e p r e s e n t e d i n F i g . 2 s h o w i n g

    tha t D~# ~ i s a lwa ys b igge r t ha n D~~ 1 7 6spec i a l l y a f t e r

    s m a l l d e f o r m a t i o n . A t v e r y s e v e r e d e f o r m a t i o n a s i n

    th e ca se o f f il in g s, a-,effirll

    1 a . - e fr l 2 0 0 .

    T h e

    De~-e

    c u r v e s f o r

    s a m p l e s o f g r o u p B ( e x p e r i m e n t a l p o i n t s i n f ig u r e s a re

    e x p r e s s e d b y s m a l l c i rc le s ) a re l o c a t e d h i g h e r t h a n f o r

    s a m p l e s o f g r o u p A ( e x p e r i m e n t a l p o i n t s i n f i g ur e s

    e x p r e s s e d b y s m a l l s q u a r e s ). T h i s i s i n c o r r e s p o n d e n c e

    wi th t hose i n F ig . 1 .

    O n t h e o t h e r h a n d , F i g . 3 s h o w s t h e Defr-a r e l a t i on -

    s h i p s w h i c h c a n b e e x p r e s s e d b y a n u n i q u e c u r v e f o r

    s a m p l e s o f b o t h g r o u p s , i .e . th e r e i s a o n e t o o n e

    c o r r e s p o n d e n c e b e t w e e n D e e a n d a i n s p i t e o f t h e

    h i s t o r y o f s a m p l e t r e a t m e n t s . S o i t m i g h t b e p o s s i b l e

    i n t h e f u t u r e t o e v a l u a t e f l o w s tr e s s b y o n l y m e a s u r i n g

    m i c r o s t r u c t u r a l p a r a m e t e r s s u c h a s D eer a n d o t h e r s

    w i t h o u t d e s t r o y i n g t h e s a m p l e .

    In F ig . 4,

    E / V )

    i s c a l c u l a t e d b y E q u a t i o n 3 a s

    f o l lo w s . S u p p o s i n g t h e 1 1 1 r e fl e c t io n i s a f f e c t e d o n l y

    b y s c r e w d i s l o c a t i o n s , o n e c a n o b t a i n

    E/V)~

    ~1 . T he n

    El V)~ ~ , E/V )s

    22 an d

    El V)~22

    c a n a l s o b e d e d u c e d i n

    t h e s a m e w a y , w h e r e t h e s u b s c r i p t e o r s d e n o t e s t h e

    e d g e o r s c r e w t y p e o f d i s l o c a t i o n s , r e s p e c t i v e l y . A

    c r u d e a v e r a g e i s m a d e a s

    ( E ) ~ '

    = -4 1 ( ~ ) l l ,

    Deft f

    (nm)

    200

    0

    5

    100

    E X ~ l 11

    +

    + ~ ~ V ) s q - ~ , , V , ] e J ( 4 )

    o

    \

    ok

    \ ,,

    \ \

    \ \

    \\ ~o\111-222

    \

    \ - .

    - \ \

    200_400~o~ \o~

    1 1 1 2 2 2 ~ o _

    o . _ ~

    - z~_ ~- v -_

    - ~ - - - o . . . . .

    2u0 ~40,0 i I . . . .

    15

    _ ] ~ 0 - -0 . . . . ~ 0 , . ," " " ' 9 .

    9 . . . . " . . : ~

    I I ~ i q I I , i ~ i ] ~ 1 -- --

    25 35 45 E ~- -

    a n d s i m i l a r ly t h e E/V ) 2~176t i s c l e a r l y s h o w n i n F i g . 4

    t h a t

    E/ V) l l~

    i s a l w a y s s m a l l e r t h a n

    E /V ) 2~176

    n d

    t h e d i f fe r e n c e in c r e a s e s r a p i d l y w i t h i n c r e a s i n g d e f o r -

    m a t i o n .

    C o m p a r i n g F i g . 4 w i t h F i g . 2 , o n e c a n n o t i c e t h a t

    a t e < 1 2 % t h e d e f o r m a t i o n w o r k i s m a i n l y u s e d

    t o d e s t r o y t h e o r i g i n a l c r y s t a l g r a i n s w h i l e a f t e r

    > 1 8 % t h e e n e r g y s t o re d i n s id e th e d o m a i n i n cr e a se s

    r a p i d l y b e c a u s e o f t h e i n c r e a s in g d i s l o c a t i o n d e n s i t y .

    T h e E l V ) - e c u r v e f o r g r o u p B i s l o w e r t h a n t h a t f o r

    g r o u p A , i n c o r r e s p o n d e n c e w i t h t h o s e i n F i g s 1 a n d 2 .

    O n e s h o u l d k e e p i n m i n d t h a t E / V ) o b t a i n e d b y u s

    f r o m E q u a t i o n 4 i s n o t a p r e c i s e a v e r a g e . I n o r d e r t o

    i m p r o v e i t t h e w e i g h t e d a v e r a g e o f re a l s c re w a n d e d g e

    d i s l o c a t i o n d e n s i t i e s a n d c o n f i g u r a t i o n p a r a m e t e r s

    h a v e t o b e c o n s i d e r e d .

    F r o m F i g . 5 o n e c a n s e en th a t d a t a f o r b o t h A a n d

    B g r o u p o f s a m p l es a g a i n m a y b e p u t o n o n e u n i q u e

    E l V ) - a c u r v e u n l i k e t h e c a s e o f E l V ) - e curves .

    I t i s c l e a r i n F ig . 6 , d i s l oca t i on d ens i t y a t f i r s t

    i n c r e a s e s w i t h i n c r e a s i n g e b u t s t o p s c h a n g i n g a t

    > 10~~ -2, wh i l e )Q rap id ly r educes a t l a rge

    de f o rm a t ion s , e spec i a l l y fo r _M (2 0 0 /4 0 0) . Th i s p rob -

    a b l y m e a n s t h a t d i s l o c a t i o n s e x i s t m a i n l y i n p i le - u p s a t

    s m a l l d e f o r m a t i o n t o f o r m a l o n g r a n g e s t r a i n f i e l d

    w h i l e w i t h i n c r e a s i n g d e f o r m a t i o n t h e d i s l o c a t i o n s

    w i l l g r a d u a l l y f o r m t h e r e g u l a r l a t t i c e o f d i p o l e s o r

    r o w s n o r m a l t o t h e g l i d e p l a n e a n d t h e l o n g r a n g e

    s t r a i n s c a n c e l e a c h o t h e r o u t .

    T h e r e i s s i g n if i c a n t d i f f e re n c e in t h e a b o v e s t a t e d

    s t r u c t u r a l p a r a m e t e r s b e t w e e n t h o s e d e d u c e d f r o m

    1 1 1 /2 2 2 a n d f r o m 2 0 0 / 4 0 0 . F o r o u r p l a t e s a m p l e ,

    an y h k l r e f l e c t i on i s g iven by t hos e c rys t a l g ra ins

    wh ose {h k l } p l anes a r e pa ra l l e l t o t he sam ple su r face .

    D i f f e r e n t r e f l e c t i o n s a r e a t t r i b u t e d t o g r a i n s o f d i f -

    f e r e n t o r i e n t a t i o n s w h i c h c e r t a i n l y h a v e d i f f e r e n t

    Figure 2

    Effec t iv e d o ma i n s iz e ag a i n s t s t ra i n cu rv es

    fo r samp l e s o f g ro u p A , B an d C (D ) g ro u p A o (O)

    group B, (A) group C (fi l ings).

    3 2 2 4

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    D e f t

    ( n m )

    2 0 0

    1 0 0

    2 0

    o

    \

    o

    \

    \\ \

    \\ \\

    \ ~ o 1 1 1 - 2 2 2

    k

    \ ,,

    \ k

    2 0 0 - 4 0 0 \ \

    - - - - o - o - o _ _ _ - - - ~ . . .. . ..

    3 0 4 0 5 0 60 cr ( 107N m 2 )

    F i gu r e E f f e c t i v e d o m a i n s i z e a g a i n s t f l o w s t r e s s

    c u r v e s .

    ( O ) 1 1 1 2 2 2 , ( E l) 2 0 0 - 4 0 0 .

    F igu re 4

    A v e r a g e s t o r e d e n e r g y d e n s i t y a g a i n s t

    s t r a i n c u r v e s .

    ( I O G J ~ - 3 , ~

    2 0

    1 0

    2 0 0 - 4 0 0 .

    ~ O ' -

    - - - - ~ - -

    - - O

    . . . o - - I I I - 2 2 2

    / 4 b l 0 . . . . . .

    0

    o ~ / ~ ~ o . . . .

    /

    O I I I O ~ ~ ~ ~ / /

    q I

    I I

    I I I I I I I I I I I ] I I { I

    1 5 2 5 3 5 4 5

    E ( )

    { 4

    ( 1 0 ~

    n~3)

    t

    1 0

    2 0 0 - 4 0 0 . "

    rq.C~ . . . E l"

    /

    /

    ~ d

    / . O '

    ~ o _ o ~ 1 1 1 - 2 22 . . . . . . . .

    /

    O ~ ~ _ _ O / ~ "O

    /

    O - - - - - - 0 - - - - - - 0 ~

    .ZX

    2 0 3 0 4 0 5 0 6 0 0 " ( 1 0 7 N m 2 )

    F igu re 5 A v e r a g e s t o r e d e n e r g y d e n s i t y a g a i n s t f l o w

    s t r e s s c u r v e s .

    F igu re 6

    D i s l o c a t i o n p a r a m e t e r s a g a i n s t f l o w st r e s s

    c u r ve s .

    ( l dOcm-2)

    30

    2 0

    1 0

    , ~ 1 1 1 - 2 2 2

    \

    \

    \\

    \ p 2 0 0 - 4 0 0

    \

    \

    \

    \ ~ [ 3

    \ rn~ n ~

    \

    B

    / N

    / - ' / \

    9 2 0 0 - 4 0 0 . . o / / \ \

    o - - / o ~ i 1 1 1 - 2 2 2

    - I : ] .

    . - o ~

    2 ~ 2 ' I , , ,

    3 O

    3 0

    2 O

    10

    . . . . . , 4

    ~ c ] , . " "

    , I , , , , I , , , ' 6 ~ 0 ' ' Q - - N O " 0

    [ 4 0 5 0 O - m 2 )

    3 2 2 5

  • 7/27/2019 Cu-Zn Deformed Brass

    4/4

    s t re s s and s t ra i n s t a t e s hence d i f f erent s t ruc t ura l

    param et ers .

    T h e d a t a o b t a i n e d f r o m t h e f il in g s a r e p u t t o g e t h e r

    o n t h e c u r v e s i n F i g s 2 t o 5 w i t h t h o s e o f te n s i l e

    s a m p l e s t o s h o w t h e r e a s o n a b le t e n d e n c y o f c u r ve s .

    B ut our da t a f o r fi li ngs are a l i tt l e d i ff erent f ro m o t hers

    [ 1 2 , 1 3 ] .

    4 . C o n c l u s i o n s

    T h e X - r a y m e t h o d f o r s tu d y i n g a d e f o r m e d s t ru c tu r e

    i s a n o n - d e s t r u c t i v e o n e w h i c h c a n g i v e t h e s t a t is t ic a ll y

    a v e r a g e d m i c r o s c o p i c p a r a m e t e r s a s s o c i a t e d u n i q u e l y

    w i t h th e m a c r o s c o p i c f l o w s t r e s s r e g a rd l e ss o f t h e h e a t

    t r ea t m e n t h i s t o r y o f th e s a m p l e . T h i s m a y a l l o w a

    p r e d i c t i o n o f t h e m a c r o s c o p i c p r o p e r t i e s f r o m t h e

    m i c r o s c o p i c s t r u c tu r e .

    T h e q u a n t i ta t iv e r e l a t io n s h i p b e t w e e n m a c r o s c o p i c

    m e c h a n i c a l p r o p e r t i e s a n d t h e m i c r o s c o p i c d e f o r m e d

    s tr u ct u re c o u l d p r o b a b l y i m p r o v e t h e w o r k - h a r d e n i n g

    t h e o r y f o r m e t a l s .

    R e f e r e n c e s

    1 . P . H A A S E N , i n P h y s i c a l M e t a l l u r g y ( C a m b r i d g e U n i -

    ve r s i t y Press , C a m br i d ge , 1978) p . 243 .

    2 . H . P . K L U G , in X - r a y D i f fr a c t i o n P r o c e d u r e s ( W i l e y ,

    N e w Y or k , 1974) p . 618 .

    3 . A . R . S T O K E S , Proe. Phys. Soc . 61 ( t '948) 382.

    4 . B . E . W A R R E N ,

    in Progress in Metal Physics

    (Pergamon Press , London, 1959) p. 147.

    5. Idem,

    X - r a y D i f f r a ct i o n ( A d d i s o n - W e s l e y , R e a d i n g ,

    Massachusetts , 1969) p. 25[ .

    6 . M . W I L K E N S ,

    Ph y s . S t a t u s S o l i d i A

    2 t ( 1970) 359 .

    7 . J . I . L A N G F O R D , J . Appl . Cryst . 11 (1978) 19.

    8 . J . I . L A N G F O R D a n d A . J . C . W I L S O N , i n C r y s t a l -

    l o g r a p h y an d Crys t a l P e r f e ct io n s ( Acad e m ic P re s s , Ne w

    Y or k , 1963) p . 207 .

    9 . J . M . C O W L E Y , in Dif fract ion Physics ( N o r t h - H o l l a n d ,

    A m s t e r d a m ,

    1975) p. 25.

    10. W A N G Y U M I N G , L E E S H A N S A N an d L E E Y E N -

    C H I N , J . Appl . Cryst . 15 (1982) 35.

    I 1 . S . Z W U I , J . Ma t e r . S c i . Le t t . 4 (1985) 1434.

    1 2. J . B . C O H E N a n d J . E . H I L L I A R D , i n L o c a l

    A t o m i c

    Arran ge m e n t S t u d ie d b y X - r a y Diffract ion (Gordon Breach,

    N e w

    Y or k , 1965) p . 289 .

    13 . E . M A G E E a n d W . J . K I T C H I N G M A N , J . Ph y s . D:

    Ap p l . Ph y s .

    9 (1976) 939.

    Received 19 September

    and accepted 30 October 1985

    3 2 2 6