The Effect of an Intercritical Heat Treatment on

Temper Embrittlement of a Ni - Cr - Mo- V Rotor Steel

T. WADA A N D D . V . D O A N E
The e f f e c t of an i n t e r c r i t i c a l h e a t t r e a t me n t on t e mp e r e mb r i t t l e me n t h a s b e e n i n v e s t i g a t e d
f o r a r o t o r s t e e l c o n t a i n i n g 0. 25 p c t C, 3. 5 p c t Ni , 1. 7 p c t Cr , 0. 5 pc t Mo, 0. 1 p c t V, and d e -
l i b e r a t e a d d i t i o n s of p h o s p h o r u s , t i n, o r a n t i mo n y . Bot h ma r t e n s i t i c and b a i n i t i c s t e e l s we r e
h e l d a t t he i n t e r c r i t i c a l t e mp e r a t u r e of 1380~ (750~ f o r t i me s up t o 40 h and we r e t he n
que nc he d o r c o o l e d t o o b t a i n ma r t e n s i t i c o r b a i n i t i c t r a n s f o r ma t i o n . The s t e e l s we r e t he n
t e mp e r e d , f o l l o we d b y wa t e r que nc hi ng o r s t e p c ool i ng f r o m t he t e mp e r i n g t e mp e r a t u r e .
The r e s i d u a l f e r r i t e ma i n t a i n e d a f i n e p l a t e - l i k e s h a p e e ve n a f t e r 40 h a t t he i n t e r c r i t i c a l
t e mp e r a t u r e . E mb r i t t l e me n t i n d u c e d b y s t e p c o o l i n g f r o m t he f i na l t e mp e r i n g wa s ma r k -
e d l y r e d u c e d by t he i n t e r c r i t i c a l t r e a t me n t a s c o mp a r e d t o t he e mb r i t t l e me n t o b s e r v e d
a f t e r c o n v e n t i o n a l h e a t t r e a t me n t ; f o r e x a mp l e , AF ATT, t he i n c r e a s e i n t he Ch a r p y V- n o t c h
50 p c t s h e a r f r a c t u r e t r a n s i t i o n t e mp e r a t u r e c a u s e d b y s t e p c ool i ng, wa s r e d u c e d b y a t l e a s t
80~ (45~ a s a r e s u l t of t he i n t e r c r i t i c a l t r e a t me n t of s t e e l s c o n t a i n i n g 0. 02 p c t P. Mo l y b -
de num e f f e c t i v e l y r e d u c e d AF AT T i n i n t e r c r i t i c a l l y h e a t - t r e a t e d s t e e l s a s we l l a s i n c o n -
v e n t i o n a l l y t r e a t e d s t e e l s . P o s s i b l e me c h a n i s ms f o r r e d u c i n g t e mp e r e mb r i t t l e me n t wi t h
t he i n t e r c r t t i c a l t r e a t me n t a r e d i s c u s s e d .
T E MP E R e mb r i t t l e me n t of s t e e l s h a s b e e n a s u b j e c t
of r e s e a r c h f o r s e v e r a l d e c a d e s , ~'z and i t ha s b e e n e s -
t a b l i s h e d t ha t s uc h i mp u r i t i e s a s p h o s p h o r u s , a n t i mo n y ,
and t i n c o n t a i n e d i n a l l o y s t e e l s a r e p r i ma r i l y r e s p o n -
s i b l e f o r t he e mb r i t t l e me n t . Re c e n t i n v e s t i g a t i o n s wi t h
Au g e r s p e c t r o s c o p y 3-5 ha ve r e v e a l e d t ha t t h e s e i mp u r i -
t i e s a r e p r e s e n t at a s u b s t a n t i a l l y h i g h e r c o n c e n t r a t i o n
i n p r i o r a u s t e n i t e g r a i n b o u n d a r i e s t han wi t hi n t he
g r a i n s of e mb r i t t l e d s t e e l s .
It i s a l s o known t ha t c o n t e n t s of n o r ma l a l l o y i n g e l e -
me n t s , s uc h a s ma n g a n e s e , c h r o mi u m, o r n i c k e l , i nf l u-
e nc e t he e x t e n t of e mb r i t t l e me n t b y i n d i v i d u a l i mp u r i -
t i e s . 8 Some e l e me n t s , f or i n s t a n c e mo l y b d e n u m, a r e
known t o r e d u c e t he e mb r i t t i e me n t . 7-9
Though t he ma j o r e f f o r t s t o r e d u c e t e mp e r e mb r i t -
t l e me n t ha ve b e e n d i r e c t e d at c o n t r o l l i n g t he c h e mi c a l
c o mp o s i t i o n a nd t he i mp u r i t i e s of t he s t e e l s , s o me
p h y s i c a l t r e a t me n t s ha ve a l s o b e e n i n v e s t i g a t e d . A
t h e r mo me c h a n i c a l t r e a t me n t , f or i n s t a n c e , ha s p r o v e d
t o be e f f e c t i v e , ~~ but i t s a p p l i c a b i l i t y t o p r o d u c t i o n
ma y be r e s t r i c t e d b y t he s i z e and s h a p e of t he f i na l
p a r t .
In t h i s i nve s t i ga t i on, , an i n t e r c r i t i c a l h e a t t r e a t me n t ,
i . e . , a t r e a t me n t a t a t e mp e r a t u r e b e t we e n t he A 1 and
A a t e mp e r a t u r e s , wa s a p p l i e d t o a t u r b i n e and g e n e r -
a t o r r o t o r s t e e l c o n t a i n i n g 0. 25 p c t C, 3. 5 p c t Nt , 1. 7
p c t Cr , 0. 5 p c t Mo, and 0. 1 p c t V, and i t s e f f e c t on t he
s u s c e p t i b i l i t y of t h i s s t e e l t o t e mp e r e mb r i t t l e me n t wa s
d e t e r mi n e d . A mo l y b d e n u m- f r e e s t e e l wa s a l s o e x a m-
i ne d t o d e t e r mi n e t he e f f e c t of mo l y b d e n u m on t he i n t e r -
c r i t i c a l l y t r e a t e d s t e e l .
Al t hough t he a p p l i c a t i o n of an i n t e r c r i t i c a l t r e a t me n t
t o r o t o r s t e e l h a s not b e e n r e p o r t e d p r e v i o u s l y , s e v e r a l
i n v e s t i g a t o r s 13-2a ha ve shown t ha t t h i s t r e a t me n t ma y
T. WADA and D. V. DOANE are St aff Metallurgist and Manager of
Research, Ferrous Metallurgy, respectively, Research Laboratory,
Climax Molybdenum Company of Michigan, a subsidiary of American
Metal Climax, Inc., Ann Arbor, Michigan. 48105
Manuscript submi t t ed March 23, 1973.
METALLURGICAL TRANSACTIONS
i mp r o v e l ow t e mp e r a t u r e t o u g h n e s s of a l l o y s t e e l s . The
f i r s t d e t e r mi n a t i o n of t he b e n e f i c i a l e f f e c t of t he i n t e r -
c r i t i c a l t r e a t me n t on t he t o u g h n e s s and on t he r e d u c t i o n
of e mb r i t t l e me n t wa s ma d e b y Sazonov. 14 Roux 1B and
Bo r n and Ha a r ma n ~6 a p p l i e d t hi s t r e a t me n t t o p r e s s u r e
v e s s e l s t e e l s of Mn - Mo - V and Mn - Ni - Mo - Nb t ype , r e -
s p e c t i v e l y , and s i g n i f i c a n t i mp r o v e me n t s i n l ow t e m-
p e r a t u r e t o u g h n e s s we r e o b t a i n e d . Re c e n t l y , s u c c e s s -
f ul a p p l i c a t i o n s of t hi s t r e a t me n t have b e e n ma d e t o
5. 5 p c t Ni - 0 . 2 5 p c t Mo s t e e l f o r c r y o g e n i c s e r v i c e , .7,18
Th e s e s t u d i e s and b a s i c wo r k by L~g e r et al . ~9 i n d i c a t e
t ha t t he mi c r o s t r u c t u r e b e c o me s a f i n e l y d i s p e r s e d
f e r r i t e - a u s t e n i t e a g g r e g a t e upon h e a t i n g t o a t e mp e r a -
t u r e b e t we e n A~ and Aa. Subs e que nt que nc hi ng and t e m-
p e r i n g r e s u l t i n a s t r u c t u r e c o n s i s t i n g of f i n e l y d i s -
p e r s e d f e r r i t e and t e mp e r e d ma r t e n s i t e , whi ch e x h i b -
i t s hi gh t o u g h n e s s at l o w t e mp e r a t u r e s .
The t ype of s t e e l s t u d i e d i n t h i s wo r k i s a g r a d e u s e d
f o r r o t o r s of l a r g e s e c t i o n s i z e . 2~ Be c a u s e bot h ma r t e n -
s i t i c and b a i n l t i c s t r u c t u r e s a r e i mp o r t a n t i n r o t o r
f o r g i n g s , t h e s e t wo s t r u c t u r e s a r e i n c l u d e d i n t he c u r -
r e n t i n v e s t i g a t i o n . Th e s e s t r u c t u r e s we r e p r o d u c e d b y
oi l que nc hi ng o r c o n t r o l l e d c ool i ng, r e s p e c t i v e l y , a f t e r
c o mp l e t e a u s t e n i t i z a t i o n . The s t e e l s of bot h s t r u c t u r e s
we r e t he n i n t e r c r i t i c a l l y h e a t e d , and e i t h e r o i l - q u e n c h e d
o r c o n t r o l - c o o l e d , r e s p e c t i v e l y , f r o m t he i n t e r c r i t i c a l
t e mp e r a t u r e . Su s c e p t i b i l i t y t o t e mp e r e mb r i t t l e me n t
wa s d e t e r mi n e d f o r t he c o n v e n t i o n a l l y h e a t - t r e a t e d
s t e e l s a s we l l a s f or t he i n t e r c r i t i c a l l y h e a t - t r e a t e d
s t e e l s .
EXP ERI MENTAL PROCEDURES
Ma t e r i a l s
The t e s t s t e e l s we r e me l t e d a s 55-1b ( 25- kg) h e a t s
i n a v a c u u m- i n d u c t i o n f u r n a c e . The s t a r t i n g ma t e r i a l s
we r e e l e c t r o l y t i c i r o n , hi gh p u r i t y n i c k e l , s p e c t r o -
s c o p i c g r a p h i t e , and f e r r o a l l o y s ; s p e c i f i c i mp u r i t i e s ,
a s f e r r o p h o s p h o r u s , p u r e t i n p e l l e t s , and p u r e a n t i -
mony p e l l e t s , we r e a d d e d . The c o mp o s i t i o n s of t he
VOLUME 5, JANUARY 1974- 231
T a b l e I . C h e m i c a l C o m p o s i t i o n o f T e s t S t e e l s
Element, Pct
Heat No. C Si Mn Ni Cr Mo V s Sn Sb
P630B 0.22 0.12 0.34 3.49 1.69 0.50 0.13 0.054 (0.008)* (0.001)
P679 0.27 0.08 0.29 3.42 1.71 <0.001 O. 12 0.022 0.002 0.001
P682 0.25 0.04 0.30 3.40 1.66 0.51 O. 13 0.021 0.010 <0.001
P683 0.25 0.08 0.27 3.41 1.64 0.51 O. 12 0.003 0.021 <0.001
P684 0.25 0.09 0.30 3.43 1.63 0.52 O. 13 0~003 0.010 0.015
*The value in parentheses is the composition of a typical steel of the series to which Heat P630B belongs.
st eel s ar e shown in Table I. Heat P630B contains
0.05 pct P, while ot hers contain 0.015 to 0.02 pct i m-
pur i t i es, as i ndi cat ed by the underl i ned per cent ages
in Table I. Heat P679 does not contain molybdenum.
The basi c composi t i on of t hese st eel s meet s the r e -
qui rement s for Cl asses 6 to 8, ASTM Designation
A469-71, except that the si l i con content of Heat P630B
is sl i ght l y high.
The st eel s were poured into 3 89 (89-ram) di am
ingot mol ds, ei t her 6 or 12 in. (150 or 300 mm) high.
1 9
The ingots were forged into l ~m. (32-mm) sq bar s
from a t emper at ur e of 2050~ (1120~
Heat Tr eat ment s
CONVENTIONAL TREATMENT
All st eel s were nor mal i zed by aust eni t i zi ng at 1850~
(1010~ for 2 h, ai r cooling, and then aust eni t i zi ng at
1550~ (845~ for 40 h followed by oi l quenching or con-
t r ol l ed cooling to obtain mar t ensi t i c or bai ni t i c s t r uc-
t ur es, r espect i vel y. The cont rol l ed cooling was con-
ducted by pl aci ng four bar s, 188 in. (32 mm) sq by 7 in.
(180 mm) long, in an i nsul at i ng br i ck encl osur e with a
-~ -in. (19-mm) wall t hi ckness. A t hermocoupl e was
pl aced in the cent er of the group of bar s to moni t or the
t emper at ur e. When the st eel bar s and br i ck encl osure
were put in a hot furnace, about 4 h were r equi r ed to
r each the furnace t emper at ur e of 1550~ (845~ After
40 h, the as s embl y was withdrawn and cooled in ai r .
The cooling curve of the bar s is f ai r l y cl ose to the
cooling curve of the core of a wat er-quenched forgi ng
of 40-in. (1000-mm) di am, as shown in Fig. 1. The
aust eni t i zi ng t i me of 40 h was sel ect ed to si mul at e
conventional pr act i ce in r ot or heat t r eat ment .
The mar t ensi t t c and bai ni t i c st eel s were both t em-
per ed. The condition of t emper i ng was sel ect ed to give
the ai med har dness aft er t emper i ng. The st eel s were
usual l y double t emper ed at t emper at ur es up to 1175~
(635~ except for mol ybdenum- f r ee st eel s at a har d-
ness of Rockwell C 32 to 35. A si ngl e t emper at a t em-
per at ur e around 1070~ (575~ was used for the l at t er
case. The conditions of t emper i ng ar e l i st ed in Table
If. The aust eni t e grai n si ze of the st eel s was in the
range from ASTM Grai n Size Numbers 6.7 to 7.7 aft er
the heat t r eat ment s.
INTERCRITICAL TREATMENT
The st eel s to be i nt er cr i t i cal l y t r eat ed were f i r s t
convent i onal l y heat - t r eat ed by nor mal i zi ng at 1850~
(1010~ for 2 h, aust eni t i zi ng at 1550~ (845~ for
40 h, and oil quenching or cont rol cooling to obtain
mar t ensi t i c or bai ni t t c st r uct ur es, r espect i vel y. They
were then heat ed to 1380~ (750~ a t emper at ur e
about 60~ (33~ below the Acs, and held at that t em-
per at ur e for 40 h (for some speci mens, 80 min). The
mar t ens i t i c st eel s were quenched in oi l from that t em-
per at ur e. The bai ni t i c st eel s were cont r ol - cool ed in
the same way as from 1550~ (845~ using the br i ck
1500
t
1ooo
500
I I I I I l I
< ~ TYPICAL COOLINSCURVEOFTNECORE
~ ~ BAINITIC COOLING
FROM 1380 F { 750 C) ~ ~ , ~ . . . . . . . . . . . . .
I I I I I I I
30 60 90 120 150 180 210
TIME, MIN
Fi g. 1- - Cool i ng c ur ve s of ba i ni t i e t e s t s t e e l .
800
o
600 w"
#_
400 ~
,.=,
200
240
40
3O
2 5
2o
u~
~= 1 5
Tempering Parameter = [T(C) + 2 7 3 ] (20 + log 0
, 17 18 19 x 10 ~
zero'Mo, CT ' ~ ' '
i ~ ' - , . [ 2 " - 0 ~ 0. 5 Mo, CT
, - 1 8 0 , } 5 7 0 5 c )
O 9 Mo Steel, IT ~ ~ 4 ~ j ~ 1340' F [ C]
9 / -o~ 0.5 Mo
r~ImMo Stee~ CT ~ ~-~-1380F(750C1
' ~ . ~ zero Mo
A 9 Mo-Free Steel, IT
60 F (740 C)
v v Mo - F r e e Steel, CT
zero Mo
pen: M a r t e n s i t i c S t e e l
Closed: Balnitlc Steel
"A
~ 3 4 0 F" ~725 C)
( ( l ~ r o M o I
30 31 32 33 34 35 103
TemperingParameter = IT{F) 4- 460j (20 + le~ t)
Fig. 2--Hardness and tempering conditions of test steels.
Conventionally treated and tempered steels are labelled CT;
intereritioally treated and tempered steels are labelled IT.
The point (a) was intereritteally treated for 80 rain at 1380~
(750~ and ot he r s we r e t r e a t e d f or 40 h at t e mpe r a t ur e s i n-
di cat ed.
232- VOLUME 5, JANUARY 1974 METALLURGICAL TRANSACTIONS
Tabl e I I . Heat Treat ment , Hardness, and Temper Embr i t t l ement of Test Steels
Heat Tr eat ment
Nonemhrittled State Emhrittled State
Condition of Tempering and
Intercritical Treatment,t Hardness, 50Pet FATT, Shelf Energy, 50 Pet FATT, Shelf Energy,
Heat No. Type* ~ (~ R e ~ (~ ft-lb (J) ~ (~ ft-lb (J) AFATT, ~ (~
Martensitic Steel
P630B C 1160 + 1150 (625 + 620) 33-34 - 3 0 ( - 3 5 ) 85 (115) +430 (+220) - 460 (255)
I 1 3 8 0 1060 33 8 0 ( 6 0 ) - + 1 0 ( 1 0 ) 75( 102) 90( 50)
(750 8 0 mm + 570)
P679 C 1070( 575) 35-36 +190 (+90) 75 (102) +550( +290) - 360 (200)
1 1380 X 40 h + 1075 + 1050 29 +30( 0) 120 (163) +275 (+135) 245 (135)
(750 X 40 h + 580 + 565)
I 1380 40 h + 1075 + 25 - 2 0 ( - 3 0 ) - +195 (+90) 215 (120)
1050 + 1085 X 3 h
(750 X 40 h + 580 +
565 + 585 X 3 h )
P682 C 1150+ 1150 (620 + 620) 34-35 - 1 5 0 ( 1 0 0 ) 85 (115) +65 (+20) 74 (100) 215 (120)
C 1125 4 8 h + l l OOX 48 h 26 165 ( - 110) - +25 ( - 5 ) 190 (105)
(610 X 48 h + 595 X 48 h)
I 1380 4 0 h + 1075 26 - 1 7 0 ( - 1 1 0 ) 125 (169) - 6 0 ( - 5 0 ) - 110 (60)
40 h + 1050
(750 X 40 h + 580 X
40 h + 565)
P683 C 1150+ 1150( 620 + 620) 34-35 - 1 7 0 ( - 1 1 0 ) 90( 122) - 7 0 ( 5 5 ) 87 (118) 100( 55)
C 1 1 7 5 X2 h + l 1 5 0 X2 h 30 2 0 5 ( 1 3 0 ) 123 (167) - 7 5 ( - 6 0 ) 127( 172) 130( 70)
(635 X 2 h + 620 X 2 h)
I 1380 X 80mi n + 1060 33 - 1 3 5 ( - 9 5 ) 97 (131) - 1 5 0 ( - 1 0 0 ) 103 (140) - 1 5 ( - 5 )
(750 X 8 0 mi n + 570)
P684 C 1150+ 1 1 5 0 ( 6 2 0 +6 2 0 ) 34-35 - 1 6 0 ( - 1 0 5 ) 95 (129) - 4 0 ( 4 0 ) 80( 108) 120 (65)
1 1380 X 40 h + 1075 X 26 - 1 8 0 ( - 1 2 0 ) 138 (187) - 1 3 5 ( - 9 5 ) 127 (172) 45 (25)
40 h + 1050
(750 X 40 h + 580 X
40 h + 565)
Bainitic Steel
P679 C 1060 (570) 33-34 +200 (+95) 70 (95) +410 (+210)
I 1380 X 40 h + 1075 + 1050 27 +20 ( - 5 ) 100 (136) +185 (+85)
(750 40 h + 580 + 565)
1 1 3 8 0 X4 0 h + 1 0 7 5 + 25 2 0 ( 3 0 ) +165 (+75)
1050+ 1085X 3 h
(750 X 40 h + 580 +
565 + 585 X 3 h)
P682 C 1140 + 1130 (615 + 610) 34-35 +85 (+30) 78 (106) +175 (+80)
C 1125 X 48 h + 1100 X 48 h 25 - 3 5 ( - 3 5 ) - +100 (+40)
( 610X 4 8 h + 595 X 48 11)
I 1380 X 40 h + 1075 X 26 - 2 5 ( - 3 0 ) 122 (165) - 5 ( - 2 0 )
4 0 h + 1050
(750 X 40 h + 580 X
40 h + 565)
P684 C 1140 + 1130 (615 + 610) 34-36 +50 (+10) 78 (106) +140 (+60)
1 1 3 8 0 X4 0 h + 1 0 7 5 X 26 2 5 ( 3 0 ) 122( 165) - 1 0 ( 2 5 )
4 0 h + 1050
(750 X 40 h + 580 X
40 h + 565)
210( 115)
165 (90)
185 (105)
65 (88) 90 (50)
- 135 (75)
120 (163) 20 (l O)
75 (102) 90 (50)
120 (163) 15 (5)
*C = conventional heat treatment; I = intercritical heat treatment.
t Ti me of tempering is 1 h unless otherwise noted.
e nc l os ur e . The cool i ng curve f rom the i nt e r c r i t i c al
t e mpe r at ur e i s al s o shown in Fi g. 1.
After the i nt e r c r i t i c al t reat ment , the s t e e l s we r e
t e mpe r e d to obtai n the de s i r e d hardnes s . The rel at i on
bet ween t emperi ng condi t i ons and hardnes s was de t e r -
mi ned by pr e l i mi nar y e xpe r i me nt s , as shown in Fi g. 2.
The fi nal condi t i ons of t emperi ng are l i s t ed in Tabl e II.
EMBRITTLING TREATMENT
The nonembri t t l ed s pe c i me ns we r e obtai ned by wat er
quenchi ng f rom the fi nal t e mpe r i ng t e mpe r at ur e . The
embri t t l ed s pe c i me ns we r e obtai ned by st ep cool i ng
f r om the fi nal t e mpe r i ng t e mpe r at ur e , as de s c r i be d
by Low e t a l . , 6 by f ur nace cool i ng and holding in the
fol l owi ng s t e ps :
1000~ (540~ f or 15 h,
975~ (525~ f or 24 h,
925~ (495~ f or 48 h,
875~ (470~ f or 72 h,
Furnace cool i ng to 600~ (315~ and
Ai r cool i ng to r oom t emperat ure.
Impact Tes t Method
Twel ve st andar d Charpy V-not ch s pe c i me ns we r e
prepared f r om al l s t e e l s that had been t e mpe r e d and
wat er- quenched or t e mpe r e d and s t e p- c ool e d. The i m-
ME T AL L URGI CAL TRANS ACTI ONS VOLUME 5, J ANUARY 1 9 7 4 - 2 3 3
p a c t t e s t s we r e c onduc t e d s o a s t o obt a i n t he t r a n s i t i o n
c u r v e s f or t he s t e e l s . The a r e a of b r i t t l e f r a c t u r e wa s
d e t e r mi n e d on t he f r a c t u r e s u r f a c e by v i s u a l me a s u r e -
me nt , us i ng a s c a l e . Then t he p e r c e n t a g e of b r i t t l e
f r a c t u r e wa s c a l c u l a t e d . The i mp a c t e n e r g y a nd p e r -
c e n t a g e of b r i t t l e f r a c t u r e we r e p l o t t e d a g a i n s t t e m-
p e r a t u r e , and t he u p p e r s he l f e n e r g y and t he 50 p c t
f r a c t u r e a p p e a r a n c e t r a n s i t i o n t e mp e r a t u r e ( FATT)
we r e d e t e r mi n e d f r o m t he c u r v e s .
Ot he r Te s t s P e r f o r me d
Te n s i l e t e s t s of i n t e r c r i t i c a l l y t r e a t e d s a mp l e s t e e l s
we r e p e r f o r me d wi t h s p e c i me n s havi ng a r e d u c e d s e c -
t i on 0. 250 i n. (6. 35 mm) in d i a m by 1.25 i n. (31. 8 r am)
l ong, wi t h a gage l e ngt h of I i n. (25. 4 r a m) .
Mi c r o s t r u c t u r e s we r e o b s e r v e d wi t h a l i ght mi c r o -
s c o p e a nd wi t h an e l e c t r o n mi c r o s c o p e us i ng a r e p l i c a
me t h o d .
Di s t r i b u t i o n of a l l o y i n g e l e me n t s and p h o s p h o r u s b e -
t we e n t he r e s i d u a l a and t r a n s f o r me d y p h a s e s wa s d e -
t e r mi n e d on an e l e c t r o n mi c r o p r o b e a n a l y s i s uni t
( ARL- EMX- S M Mi c r o P r o b e ), Si nce t he c o n c e n t r a t i o n s
of e l e me n t s we r e r e l a t i v e l y l ow, c ount i ng of c h a r a c t e r -
i s t i c X- r a d i a t i o n wa s ma d e i n t he s t a t i c mode f or 50 s
and r e p e a t e d at l e a s t t h r e e t i me s . Me a s u r e me n t s we r e
ma d e at 20 kV and 10 nA. The b a c k g r o u n d was a l s o d e -
t e r mi n e d and s u b t r a c t e d f r o m t he c ount e d v a l u e s .
The s a me e l e c t r o n mi c r o p r o b e uni t c a n be u s e d a s
a s c a n n i n g e l e c t r o n mi c r o s c o p e by p h o t o g r a p h i n g t he
s e c o n d a r y e l e c t r o n e mi s s i o n i ma g e . F r a c t o g r a p h s of
t he i mp a c t - f r a c t u r e d s u r f a c e we r e o b t a i n e d wi t h t hi s
uni t .
EXP ERI MENTAL RESULTS
Ch a r p y I mp a c t P r o p e r t i e s
The 50 p c t F AT T and t he uppe r s he l f e n e r g y of non-
e mb r i t t l e d a nd e mb r i t t l e d s t a t e s of ma r t e n s l t i c and
b a i n i t i c s t e e l s of d i f f e r e n t h e a t t r e a t me n t s a r e s u m-
HEAT HARD-
NO, NESS,
R c -I00 0
I l I
MARTENSfflCSTEEL
P630B 1
(0.0Syo P) 3 3 - 3 4
P 6 7 9 3 5 - 3 6
( 0 . 0 2 % P ] 2 9 ~ p
ZEROMo) t 2 6 i
P682 3 4 - 3 5
(O.02Yo P) 2 6
2 e
p,,, I ,4-ss I m
{ o . o 2 7 o s . } I 30 I ~ "
P684 34 - 35
0"Q157~ Sb I 26 I
BAINITIC STEEL
P679 3 ~ 3 4
0.02% P
ZERO MD) 2 5
P682 3 4 - 3 5
(0.02% P) 2 5
2&
P684 3 4 - 3 5
0. 0L5% SI 26
FATT,C
I00
I
- - J
200 300
m CONVENTIONAL
~EAT TREATMENT
INTERCRITICAL
HEATTREATMENT
m
i I
[ i
I
Q
l l I I
- 2 0 0 0 200 4Q0
FATT, F
Fi g. 3- - AFATT of convent i onal l y and i nt e r c r i t i e a l l y heat -
t r eat ed t es t s t eel s .
ma r t z e d in Ta b l e II. The s hi f t of 50 p c t F AT T ( AFATT)
wi t h e mb r t t t ! i n g t r e a f me n t i s a l s o s hown i n Fi g . 3. Af t e r
c o n v e n t i o n a l he a t t r e a t me n t , ma r t e n s i t i c s t e e l s g e n e r -
a l l y show l o we r F ATT v a l u e s t han b a i n i t i c s t e e l s at
I d e n t i c a l h a r d n e s s , whi l e AF AT T i s u s u a l l y g r e a t e r i n
ma r t e n s l t i c s t e e l s t han in b a l n i t i c s t e e l s . Be c a u s e of
t he d i f f e r e n c e i n h a r d n e s s l e v e l s , d i r e c t c o mp a r i s o n
b e t we e n t he i n t e r c r i t i c a l l y t r e a t e d s t e e l a nd t he c o n -
v e n t i o n a l l y t r e a t e d s t e e l ma y be ma d e onl y i n a l i mi t e d
n u mb e r of h e a t s , He a t P630B s h o we d a ma r k e d r e d u c -
t i on i n t e mp e r e mb r i t Ue me n t a s a r e s u l t of t he i n t e r -
c r i t i c a l he a t t r e a t me n t when s p e c i me n s we r e t e mp e r e d
t o a h a r d n e s s v a l u e of 33 R c. In t he ma r t e n s i t i c and
b a i n i t i c P682 s t e e l s e x h i b i t i n g h a r d n e s s v a l u e s of 25
t o 26 Re , t he F ATT of t he e mb r i t t l e d s t a t e i s r e d u c e d
by 85 t o 105~ (45 t o 60~ a s a r e s u l t of t he i n t e r c r i t i -
c a l t r e a t me n t , whi l e t he F AT T of t he n o n e mb r i t t l e d
s t a t e r e ma i n s e s s e n t i a l l y t he s a me , s o t ha t AF AT T d e -
c r e a s e d a c c o r d i n g l y . The s a me t e n d e n c y ma y be o b -
s e r v e d i n t he ma r t e n s i t i c P683 s t e e l , i n whi ch t he F AT T
of t he e mb r i t t l e d s t a t e d e c r e a s e s b y a bout 80~ (45~
wi t h t he i n t e r c r i t l c a l t r e a t me n t . In t h i s c a s e , h o we v e r ,
t he F ATT of t he i n t e r c r i t l c a l l y t r e a t e d , n o n e mb r i t t l e d
P683 i s h i g h e r t han t ha t of t he c o r r e s p o n d i n g c o n v e n -
t i o n a l l y t r e a t e d s t e e l , and t he AF ATT i s n e g a t i v e i n t he
i n t e r c r i t i c a l l y t r e a t e d s t e e l . Ge n e r a l l y , t he i n t e r c r i t i -
c a l h e a t t r e a t me n t d e c r e a s e s t he F AT T of t he e mb r i t -
t l e d s t a t e , but i t d o e s not ma r k e d l y d e c r e a s e t he F AT T
of t he n o n e mb r i t t l e d s t a t e .
The e f f e c t of i n t e r c r i t i c a l t r e a t me n t on a mo l y b d e -
n u m- f r e e s t e e l , P679, ma y be e v a l u a t e d i n s p i t e of t he
d i f f e r e n c e i n h a r d n e s s b e t we e n t he c o n v e n t i o n a l l y
t r e a t e d s t e e l and t he i n t e r c r i t i c a l l y t r e a t e d s t e e l . The
r e s u l t s f o r t he c o n v e n t i o n a l l y t r e a t e d P682 and P683
wi t h d i f f e r e n t h a r d n e s s v a l u e s i n d i c a t e t ha t a d e c r e a s e
in h a r d n e s s doe s not a l wa y s r e s u l t i n a s i g n i f i c a n t d e -
c r e a s e i n 5 F AT T . F o r ma r t e n s i t i c P679, t h e r e f o r e ,
i t i s a l mo s t c e r t a i n t ha t t he i n t e r c r i t i c a l t r e a t me n t i s
e f f e c t i v e i n r e d u c i n g t he t e mp e r e mb r i t t l e me n t . I t i s
l e s s c e r t a i n i n b a i n i t i c P679. I t i s a l s o c o n c l u d e d t ha t
mo l y b d e n u m d e c r e a s e s t he t e mp e r e mb r i t t l e me n t i n
t he i n t e r c r i t i c a l l y h e a t - t r e a t e d s t e e l , a s we l l a s i n t he
c o n v e n t i o n a l l y h e a t - t r e a t e d s t e e l . F r o m t he r e s u l t s on
St e e l s P679 and P682, t he d e c r e a s e i n AF AT T by t he
a d d i t i o n of 0. 5 p c t Mo at t he 0. 02 p c t P l e v e l i s 105~
(60~ i n t he i n t e r c r i t i c a l l y t r e a t e d ma r t e n s i t i c s t e e l s
and 165~ (90~ i n t he i n t e r c r i t i c a l l y t r e a t e d b a i n i t i c
s t e e l s , whi l e i t i s 145~ (80~ i n t he c o n v e n t i o n a l l y
t r e a t e d ma r t e n s i t i c s t e e l s and 120~ (65~ i n t he c o n -
v e n t i o n a l l y t r e a t e d b a i n i t i c s t e e l s , t e mp e r e d t o h a r d -
n e s s l e v e l s of 34 t o 36 R c.
Ha r d n e s s and St r e ngt h of I n t e r c r i t i c a l l y
T r e a t e d St e e l s
Fi g. 2 s hows t he r e l a t i o n b e t we e n t he h a r d n e s s of
t he t e s t s t e e l s and t e mp e r i n g c o n d i t i o n s . The t e mp e r -
i ng p a r a me t e r , p = {T ( F) + 460){20 + l og t (h)}, wa s
t a ke n a s t he a b s c i s s a . The p o i n t s i nc l ude t h o s e of p r e -
l i mi n a r y t e s t s a s we l l a s t h o s e of t he s t e e l s u s e d i n t he
Ch a r p y i mp a c t s t u d i e s . The t e mp e r a t u r e of i n t e r c r i t i -
c a l t r e a t me n t a p p r e c i a b l y a f f e c t s t he r e l a t i o n b e t we e n
h a r d n e s s and t e mp e r i n g c ondi t i on. Thi s i s p r e s u me d
t o be c a u s e d b y an i n c r e a s e i n t he f r a c t i o n of f e r r i t e
wi t h d e c r e a s i n g i n t e r c r i t i c a l t e mp e r a t u r e s .
T e mp e r e d h a r d n e s s v a l u e s f or a l l s t e e l s a r e gi ve n
234-VOLUME 5, JANUARY 1974 METALLURGICAL TRANSACTIONS
i n Tabl e II. The t e ns i l e pr ope r t i e s of t wo of t he i nt e r -
c r i t i c a l l y t r e a t e d s t e e l s a r e shown i n Tabl e IT[. The
r e l a t i ons hi p be t we e n ha r dne s s , t e ns i l e s t r engt h, and
0. 2 pct of f s et yi el d s t r e ngt h in t he i nt e r c r i t i c a l l y
t r e a t e d s t e e l i s r e a s ona bl y c l os e t o t hat i n t he c onve n-
t i onal l y t r e a t e d s t e e l s . 2~
Tabl e II I. Tensile Properties of I ntercritically Heat-Treated Steels
0.2 Pet Offset Yield Strength, Tensile Strength,
Heat Structure Hardness, R c ksi (N/mm 2) ksi (N/mm 2) Elongation, Pet Reduction of Area, Pet
P683 Martensitic 26 104 (715) 122 (840) 32 76
P684 Bainitic 26 105 (722) 129 (888) 21 65
(a) (b)
(c) (d)
Fig. 4--Phot omi crographs of i nt er cr i t i cal l y heat - t r eat ed r ot or st eel . (a) Mart ensi t i c P683 st eel , oi l -quenched f r om 1380~
(750~ (b) Mart ensi t i c P683 st eel , oi l -quenched f r om 1380~ (750~ and t empered. (c) Bainitic P683 st eel , oi l -quenched
f r om 1380~ (750~ (d) Bainitic P684 st eel , cont rol -cool ed f r om 1380~ (750~
METALLURGICAL TRANSACTIONS VOLUME 5, JANUARY 1974-235
Mi crost ruct ures
The light mi crographs of the i nt ercri t i cal l y t reat ed
steels are shown in Fig. 4. Fig. 4(a) and Fig. 4(b) are
mart ensi t i c P683 steel as-oi l -quenched and oil-quenched
and tempered, respectively, after an i nt ercri t t cal t reat -
ment for 40 h at 1380~ (750~ The white plate-like
phase is ferri t e retained at the i nt ercri t i cal t emper a-
ture, and the mat ri x is mart ensi t e or t empered mar -
tensite t ransformed from austenite. The phot omi cro-
graphs of Fig. 4(c) and Fig. 4(d) are the mi cr ost r uc-
t ures of bainitic P683 and P684 steels, which were oil-
quenched and control-cooled, respectively, after the
i nt ercri t i cal t reat ment . The ferri t e phase is slightly
l ess distinct in the batnitic steel than in the mart en-
sitic steel, but a fine dispersion is maintained.
Figs. 5 and 6 are the electron mi crographs of the
same steels as in Fig. 4. As indicated by an arrow in
Fig. 5(a), an ar r ay of small austenite grains is often
observed on pri or austenite grain boundaries in the
t nt ercri t i cal l y t reat ed steels. Fig. 5(b) shows that
dense carbide precipitation occurs during tempering,
especially in the pr i or austenite region adjacent to
ferrt t e part i cl es. Fig. 6(b) indicates that some of the
residual ferrt t e grows into austenite during slow cool-
ing. One such grain is shown by an arrow.
Fract ographs
Scanning electron mi crographs obtained from impact
fract ure surfaces of st ep-cool ed speci mens are shown
in Fig. 7. The conventionally heat -t reat ed mart ensi t i c
steel with 0.05 pct P, P630B, t empered to a hardness
level of 33 to 34 Rc, showed al most exclusively Int er-
granul ar fract ure at - 160~ ( - 107~ After i nt er cr i t -
ical heat t reat ment , the same steel showed i nt ergranu-
lar fract ure only partially, even at - 320~ ( - 196~
as shown tn Fig. 7(b). A conventionally heat -t reat ed
barnitic steel with 0.02 pct P, t empered to a hardness
of 25 Rc, showed partial i nt ergranul ar fract ure, as
shown in Fig. 7(c), while the t nt ercri t i cal l y heat -
treated steel of the same composition and hardness
levels showed al most complete t ransgranul ar fract ure
at - 320~ (-196~ as shown in Fig. 7(d).
Distribution of Alloying Elements
The resul t s of the electron mi croprobe analysis are
shown in Table IV for two st eel s. The resul t s suggest
that nickel and, to a l esser degree, chromi um and mo-
lybdenum concentrate in the austenite phase. Phos-
phorus is concent rat ed in the ferri t e phase.
(a) (a)
fb)
Fig. 5--El ect ron mi cr ogr aphs of i nt er cr i t i cal l y t r eat ed r ot or
st eel . (a) Mart ensi t i c P683 st eel , oi l -quenched f r om 1380~
(750~ (b) Mertensi~ic P683 steel, oil-quenched from 1380~
(750*C) and tempered.
(b)
Fig. 6- - El ect r on mi cr ogr aphs of i nt er cr i t i cal l y t r eat ed r ot or
st eel . (a) Bainitic P683 st eel , oi l -quenched f r om 13S0~
(750~ (b) Bainitic P684 steel, control-cooled from 1380~
(750~
23b-VOLUME 5, JANUARY 1974 METALLURGICAL TRANSACTIONS
(a) (b)
(c) (d)
Fig. 7--Fraetographs of step-cooled test steels. (a) Conventionally heat-treated P630B (0.05 pet P), martensitie (33 to 34 Rc),
fractured at - 160~ ( - I07~ (b) lntereritieally heat-treated P630B (0.05 pct P), martensitic (33 Rc), fractured at - 320~
(- 196~ (c) Conventionally heat-treated P682 (0.02 pct P), bainitic (25 Rc), fractured at - 320~ (- 196~ (d) Intereritieally
heat-treated P682 (0.02 pct P), bainitie (26 Rc), fractured at - 320~ (- 196~
METALLURGI CAL TRANSACTI ONS VOLUME 5, J ANUARY ~974- 237
DISC USSION
The i nt ercrt t i cal heat t reat ment applied in this in-
vestigation markedl y reduced the t emper embri t t l e-
merit of the t est steels with both mart ensl t i c and bain-
ltlc st ruct ures. The t nt ercri t l cal t emperat ure used,
1380~ (750~ is on the high side of the range between
A 1 and A s t emperat ures, so that the fraction of austen-
ire at the Int ercri t i cal t emperat ure was sufficiently
l arge to obtain the desi red strength after the t reat ment .
In this condition, the i nt ercri t i cal t reat ment did not ap-
preci abl y lower the FATT of the nonembrtttled state,
but did lower that of the embrittled state of the test
steel.
Though the detailed mechanism for the effect of the
l nt ercrt t i cal t reat ment on reducing t emper embri t t l e-
ment is not yet certain, three important feat ures of
the i nt ercri t t cal l y t reat ed steels may be noticed. First,
the mi crost ruct ure, part i cul arl y austenite grain size,
is refined by this t reat ment . As shown in the electron
mi crographs, small grains of austenite often nucleate
on austentte grain boundaries formed in the previous
austenitlzing t reat ment at a higher t emperat ure. The
average austenite grain size after the i nt ercri t i cal
t reat ment has not yet been determined, but probably it
is much l ess than the grain size after conventional heat
t reat ment at a higher t emperat ure. Also, f er r i t e/ pr i or
austenite grain boundaries in the i nt ercri t i cal l y t reat ed
steels probably have an area about 10 to 50 t i mes
l arger than that of the austenite boundaries formed as
a resul t of conventional t reat ment . Thus, si mi l arl y to
the refinement of the austenite grain size, z the i mpuri -
ties segregat ed may be diluted in the l arger boundary
area. The smal l er grain size may also impede crack
propagation.
The second effect is the distribution of impurity el e-
ments between ferri t e and austenite grains. Because
the embrittling impurities, such as phosphorus, anti-
mony, and tin, are all ferri t e st abi l i zers, they are ex-
pected to concentrate in the ferri t e phase. The resul t s
of the el ect ron mi croprobe analysis indicate that the
enri chment of phosphorus occurs in the ferri t e phase.
The experimental distribution ratio of alloying el e-
ments between ferri t e and austenite phases may be
compared with those predi ct ed by t hermodynami cs.
The partial f r ee- ener gy difference of an alloying ele-
ment, i, in its dilute range, (7i ~/- G-~, is known for
some elements, z2-z6 Neglecting the interactions be-
tween alloying elements, the distribution rat i o
(pct i)~/(pct i) ~/may be calculated as shown in the
fourth column of Table V. The experimental values,
as shown in the fifth column of Table V, are qualita-
tively in agreement with the t hermodynami c cal cul a-
tion, except for molybdenum. The weak partitioning
of molybdenum to austenite at the i nt ercri t i cal t em-
perat ure is l ess certain. In general, the experi men-
tally observed distribution ratio was cl oser to unity
than that indicated by t heoret i cal considerations. This
Table I V. Results of Electron Microprobe Analysis of Distribution of Alloying Elements Between Ferrite and Austenite
Intensity of Characteristic X-Ray, Count s/ 50 s Distribution Rat i o
Standard Deviation Pct in a
Element Phase Average Counts Standard Deviation Background of Background Pct in 3' Standard Deviation
Ni* a 6713 121 (890) (2) 0.70 0. 04
9217 208 890 2
Cr* a 8410 101 (549) (27) 0.91 0.05
9210 272 549 27
Mo* ~ 521 9 288 11
551 35 301 4 0.93 0.3
505 5 329 5
Pt 1.6 0.6
421 11 313 13
*Determined for Steel P683, intercriticaUy treated to martensitic structure.
t Det er mi ned for Steel P630B, intercritically treated to martensitic structure.
Table V. Comparison of the Distribution Rati o of Al l oyi ng Element Between Ferrite and Austenite, Calculated and Experimentally Determined
(Pct i in a) / ( Pct i in 3')
Alloying Element, i C,7 - ~ , cal/mol Reference Calculated from C,~ - C,~ Experimental Values
Standard Deviation of
Experi ment al Values
C - 7600* 22 0. 024
Mn - 1700* 23 0.43
Si 480"~ 24 1.3
Ni - 1 4 0 0 " 23 0.50
Cr - 5 5 0 * 25 0.76
Mo 1000t 23 1.6
V 1OlOt 26 1.7
P 2250t 24 3.0
Sb 1200t 23 1.8
Sn 1 6 0 ~ 23 2.2
0. 70
0.91
0.93
1.6
0. 04
0.05
0.3
0. 6
*The value around 1380~ (750~ determined from known temperature dependence of G..
t Averaged value at temperatures 1830 t o 2370~ (1000 t o 1300~
2 3 8 - VOL UME 5, J ANUARY 1974 ME T AL L URGI CAL TRANS ACTI ONS
difference may be due to the fact that the phases are
so finely di spersed that the el ect ron beam may not
have always been exclusively i rradi at i ng one phase.
The ferri t e plate width and the thickness of the austen-
ite between the plates were approximately equal to the
effective beam diameter.
This scavenging effect of ferri t e may reduce the seg-
regation of impurities in pri or austenite grain bounda-
ri es, possibly being combined with the grai n-refi ni ng
effect mentioned above.
Third, the carbide morphology in the i nt ercri t i cal l y
t reat ed steel is apparently different from that in the
conventionally t reat ed steel. As shown in Fig. 5(b),
carbides in the i nt ercri t i cal l y t reat ed and t empered
steel are coar ser than those in the usual t empered
mart ensi t e. An extrapolation to 1380~ (750~ of the
solubility of vanadium carbide in austenite 27-z8 shows
that precipitation of vanadium carbides is possible in
the t est steel at that t emperat ure. Therefore, it is
highly probable that some alloy carbides st art preci pi -
tating at the i nt ercri t i cal t emperat ure and supply nu-
clei for further precipitation in tempering. McMahon z
proposed a model for temper embrittlement, in which
fract ure takes place at boundaries between the ferri t e
and the carbides in pri or austenite grain boundaries,
so that the presence and morphology of carbides in
pri or austenite boundaries are important for t emper
embri t t l ement susceptibility of steel. Additional r e-
search may be requi red to clarify the behavior of car -
bides in the i nt ercri t t cal heat t reat ment .
The Int ercri t i cal heat t reat ment is a promi si ng pro-
cess for pract i cal application. However, because this
t reat ment generally decreases the strength level of
steel, 18'29 especi al l y yield strength, it is necessar y to
use a sufficiently high i nt ercri t i cal t emperat ure to op-
timize the amount of residual ferri t e so that high
strength is achieved upon t ransformat i on of the austen-
ire. The optimum t emperat ure range in this sense may
not exceed 100~ (55~ below the A3 t emperat ure. As
indicated in Fig. 2, the addition of a sufficient amount
of t emper - r esi st i ng elements, such as molybdenum, is
beneficial in retaining the strength level and extending
the optimum t emperat ure range for i nt ercri t i cal t reat -
ment to lower t emperat ures.
SUMMARY
The effect of the i nt ercri t i cal heat treatment, a t r eat -
ment at a t emperat ure between A 1 and A3, on t emper
embri t t l ement was det ermi ned for mart ensi t i c and
bainitic rot or steels, which contain 0.25 pct C, 3.5 pct
Ni, 1.7 pct Cr, 0.5 pct Mo, 0.1 pct V, and deliberate
additions of phosphorus, tin, or antimony. The resul t s
may be summari zed as follows:
1) The t nt ercri t i cal heat t reat ment at 1380~ (750~
markedly reduced the embrittlement. The AFATT in-
duced by step cooling decreased by at least 80~ (45~
with the i nt ercrt t i cal t reat ment of steels containing
0.02 pct impurity.
2) Molybdenum reduces the embri t t l ement suscept i -
bility in the t nt ercri t l cal l y heat -t reat ed steel as well
as in the conventionally heat -t reat ed steel.
3) The residual ferrt t e maintains a fine plate-like
shape even after 40 h at 1380~ (750~ Nickel, and
to a l esser degree, chromium and molybdenum concen-
t rat e in the austenite phase. Phosphorus was observed
to concentrate in the ferri t e phase.
4) The fract ographt c study shows that the i nt ercri t i -
cally heat -t reat ed steels exhibit l ess i nt ergranul ar
fract ure than the conventionally heat -t reat ed steels.
5) The refinement of mi crost ruct ure, the concent ra-
tion of impurities to the ferri t e phase, and the change
in precipitation processes of the carbides may be con-
sidered as possible mechani sms for reducing t emper
embrittlement by i nt ercrt t i cal heat t reat ment .
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ME T AL L URGI CAL TRANS ACTI ONS VOLUME 5, J ANUAR Y 1 9 7 4 - 2 3 9