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JOURNAL OF IRON AND STEEL RESEARCH, INTERNATIONAL. 2011, 18(2): 64-69

Effect of Heat Treatment Process on Properties of

1000 MPa Ultra-High Strength Steel
Y U Wei, QIAN Ya-jun, W U Hui-bin, YANG Yue-hui
(Metallurgical Engineering Institute, University of Science and Technology Beijing , Beijing 100083, China)

Abstract: Two types of steel, C-Mn-Cr-Mo-B microalloyed steel and C-Mn-Mo-Nb-Cu-B microalloyed steel, are de-
signed to develop 1000 MPa ultra-high strength steel. Two kinds of processes, thermomechanical controlled process
(TMCP) combined with traditional off-line quenching and tempering (QT) process versus controlled rolling process
(CR) combined with direct quenching and tempering (DQS-T) process, are applied. The effect of heat treatment
processing mode on the microstructure and mechanical properties is studied. The relationship between microstructure
and mechanical properties is investigated by SEM and TEM. After tempering at 450 to 550 'C for 1 h, the steel pro-
duced by TMCP+ QT process shows combination of excellent strength and low temperature toughness. The yield
strength is above 1000 MPa, elongation above 15% and impact energy at -40 *C more than 30 J. After tempering at
450 OC , a large number of E-CUparticles precipitated in C-MrrMwNb-CwB steel produced by CR+DQ+T process lead
to a significant increase in yield strength. And after tempering a t 500 to 600 'C , the yield strength of the steel is fur-
ther improved to 1030 MPa because of precipitates, such as nitride or carbide of niobium, carbide of molybedenum
and vanadium. When the tempering temperature is increased above 620 'C , the yield strength is still higher than
1000 MPa and elongation is above 20% and impact energy at -40 'C is more than 35 J. After tempering at above
500 'C , the toughness of the steel treated by TMCP+QT process is superior to that of steel by CR+DQ+T process.
Key words: heat treatment; high strength steel; microstructure; mechanical property

High strength steel plays an important role in im-
proving efficiency and service life, reducing weight and
energy consumption of engineering structures. But
alloy content of traditional high strength steel is at
high level. T h e total alloy content (in mass percent)
in the high yield strength steel, such as HY80-
HYlOO [Re = 550 - 690 MPa, C 0.17% - 0 . 1 8 % ,
Ni 2.35% - 2 . 5 % , Cr 1.32% - 1 . 5 % and Mo
0.25%-0.5%], HY180 and AF-1410 (Re=1250-
1500 MPa) is more than 10%"'. With development
of HSLA steels, HSLA80-HSLA 100 copper-bear-
ing series steel ( HSLA-100, CGO. 06% , Cu 1.61 % ,
Ni 3.41 % , Cr 0.55%, Mo 0.6%) are developed and
used to replace HY80 - HY130 (Re = 690 - 890 MPa)
in the United States, whose toughness and weldability
are improved while strength is not significantly low-
ered[']. These steels have good comprehensive me-
chanical properties, but they are mainly produced by
off-line quenching and tempering, which requests
high cost and long production cycle. With development
and application of TMCP ( thermomechanical controlled
process) and microalloying, low carbon bainitic steels
with low carbon or ultra-low carbon and microalloy have
been developed in recent years and ultilized in structure.
As a part of TMCP, DQ (direct quenching) process,
which refers to directly quench hot plate or rod to lower
temperature after deformation via on-line quenching
units, is another new technology and has been used
to produce high-strength steel in recent yearsC3].
Compared to conventional off-line reheating quench-
ing, DQ process takes advantage of good strength-
toughness balance and good weldability for steel, re-
duction of energy consumption and lower cost for
manufacturing ~ t e e l [ ~ - ~As
] . a measure of improving
steel toughness and stability, tempering is still an
indispensable step after DQ process.
1 Experimental Materials and Methods
1.1 Chemical composition
Two kinds of high strength steel are made in a

Biography:YU Wei(1968-), Male, Doctor, Associate Professor; E-mail: yuwei@nercar. ustb. edu. cn; Received Date: March 22, 2010
Issue 2 Effect of Heat Treatment Process on Properties of 1000 MPa Ultra-High Strength Steel 65

vacuum induction furnace with different chemical
compositions listed in Table 1. C-Mn-Ni-Mo-B steel
is treated by TMCP and off-line QT (quenching and
tempering) process ( T M C P + Q T ) , with less con-
tent of alloys in order to improve the toughness and
weldability. C-Mn-Mo-Nb-Cu-B steel is treated by
CR+ DQ+ T process, with ultra-low carbon, mi-
croalloy and an amount of copper and nickel in or-
der to enhance strength and low temperature tough-
ness.

Table 1 Chemical composition of experimental steel (mass percent, %

Steel C Si Mn Mo Cr Cu Ni B S P MA CE3' Pa4)
C-Mn-Ni-Mo-B 0. 16 0. 25 1. 1 0. 5 0. 4 - 0. 8 0.0018 0.005 0.008 0.066l' 0. 63 0.35
C-Mn-Mo-Nb-Cu-B 0.06 0.24 1.8 0.3 - 0.8 0.79 0.0014 0.005 0.008 0.124'' 0.58 0.30
Note: 1) W ~ ~ = W v + w i i2) W M A = W N b + W V + W i ; 3) ~ c ~ = w c f ( w ~ . + w ~ ) / 6 + ( w c . + ~ ~ i ) / l 5 + ( w ~ , + ~ v4)) /WPcm=
5i
wc + Wsi /30 + (WM" +wcu+wcr)/20 + WNi /60 + wMo / 15 +Wv/ l o +'~WB.

1.2 Process
1.2. 1 Hot rolling and cooling
As shown in Fig. 1, ingots with dimensions of
90 mmX 90 mmX 120 mm are austenized at 1250 "C
for 2 h , then hot rolled into 13 mm thick plates by 7
passes ( 4 passes in the recrystallization temperature
zone and other 3 passes in the non-recrystallization
temperature zone, respectively), and finished at about
850 "C. T h e total reduction ratio in the non-recrys-
tallization zone is more than 60%. After rolled, the
specimens are air-cooled down to 780 'C in about 20 s
to enhance the strain-induced precipitation and to re-
lax the dislocations. Then, in TMCP+QT process,
the specimens are accelerately cooled down to 450 "C
at a cooling rate of 15 C / s and finally cooled to am-
bient temperature; while in CR+DQ process, they
are directly quenched to ambient temperature, as
shown schematically in Fig. 1.

1250%,2h TMCP+QT
I. loo
.loot
930 .
-
I t Off-line quenching

780 . Relaxa\

450 Cooling rate 15 %is

Air cooling
I -
Time Time
Fig. 1 Schematic diagrams of hot rolling and heat treatment of two processes

1.2. 2 Heat treatment pact properties change with the heat treatment
T h e steel plate produced by TMCP process is process. T h e microstructure characteristics are eval-
further off-line quenched at 900 'C. Then, from each of uated using scanning electron microscopy ( SEM )
the two steel plates, the plates are cut to specimens and transmission electron microscopy (TEM).
with the demensions of 13 m m X 13 m m X 150 mm,
2 Experimental Results
and of 13 mmX 13 mmX 55 mm. T h e specimens are
tempered subsequently at different temperatures 2.1 Mechanical properties before and after heat treatment
from 400 to 700 'C for 1 h , followed by air cooling Fig. 2 shows that C-MrKrMoB steel with TMCPf
to ambient temperature. T h e tempered steel plates QT performs better in both ultimate tensile strength
are machined into $5 mm standard tensile samples ( U T S ) and yield strength (YS) before tempered,
and 55 mm X 10 mm X 10 mm impact samples. T h e comparing to C-Mr-Mo-NbCu-B steel with CR+DQ+
tensile properties are determined on rod samples using T. In the early stages of tempering (<500 "C) , the
standard procedures. T h e impact properties are ob- U T S of C-Mn-Cr-Mo-B steel decreases rapidly in
tained from full-size Charpy V-notch specimens with both process, but then it decreases more slowly
the notches perpendicular to the rolling-plane direc- from 500 to 600 O C (only 25 MPa) with TMCP+QT
tion. The average properties of three samples in the process, while U T S of C-Mn-Mo-Nb-Cu-B steel
same process are used to analyze the tensile and im- slightly rises and shows a peak at 550 "C , followed by
 66 Journal of Iron and Steel Research, International
2040350 400 450 500 550 600 650
(a) T M C P f Q T process;
Fig. 2 Effect of tempering temperature of two processes on average mechanical property
a small decline with CR+DQ+T process. When the
tempering temperature is higher than 600 "C, UTS of
both steel decreases rapidly, but C-Mn-Cr-Mo-B steel
is even faster than C-Mn-Mo-Nb-Cu-B steel. YS
changes are even more different between the two
processes. When tempered at 400 "C , YS increases
slightly for C-Mn-Cr-Mo-B, and then the trend is
basically same as UTS. While in CR+DQ+T process,
the YS change of C-Mn-Mc-Nb-Cu-B steel shows an M-
shape. When tempered below 450 "C , there is a rap-
id increase (ranges up to 150 M P a ) , and then a
slight decrease. The peak of YS ( 1040 MPa) is
reached after tempering at 600 OC.
Fig. 2 also shows a decrease of the elongation of the
two steels in the early stages of tempering, along with
the increase of YS. As the tempering temperature
. increases, the elongation of C-Mn-Cr-Mo-B steel
displays a rapid linear growth from 500 to 600 'C,
up to 1 9 % at 550 'C. As indicated in Fig. 3 , when
tempering temperature is below 600 "C in TMCP+
QT process of C-Mn-Cr-Mo-B steel, the toughness
improves constantly and impact energy at -40 "C in-
80 . tains the quenching state of the basic morphology of
70 . lath martensite in the matrix retains [Fig. 4 (a)] and
60.
50. CR+DQ+T
2040350 400 450 500 550 600 650 700
TemperaturdC
Effect of tempering temperature of two pracesses on
average impact energy ( -40 'c )
Vol. 18
24
22
- 18
$
20
Ei
18
. 12 800 I _ . # 16
700 2040400 450 500 550 600 650 700
Ternperaturdt
(b) CR+DQ+T process.
creases from 25 to 40 J. However, the elongation of
C-Mn-Mo-Nb-Cu-B steel fluctuates when the tempe-
ring temperature is from 450 to 600 'C in CR+DQ+
T process, but still more than 17%. When the tem-
pering temperature is higher than 600 "C , the elon-
gation rises rapidly. The CVN impact energy at -40 "C
also goes through a rising followed by a reducing, only
that the change is small under a tempering tempera-
ture of 500 to 600 "C. Overall, the plasticity of C-
Mn-Mo-Nb-Cu-B steel treated by CR+DQ+T is su-
perior to C-Mn-Cr-Mo-B steel treated by TMCP+QT.
2.2 Microstructure
Fig. 4 shows the changes of the microstructure
along with the increase of tempering temperature in
the two processes. Due to the presence of high hard-
enability elements such as B, Mo and other alloying
elements, the microstructures in the two steels have
high austenite stability and hardenability. After
quenching, C-Mn-Cr-Mo-B steel by TMCP QT +
process obtains an obviously fined microstructure,
and the matrix microstructure is main quenched lath
martensite. When tempered at 400 'C, matrix re-
the original austenite grain boundaries become clear.
There are some bigger rods and granular carbide
precipitations within martensite clusters, but the
large carbide precipitations do not occur along the
grain boundary. When tempered at 600 'C, mar-
tensite lath is merged, coarsened and the matrix re-
covers, but the lath feature still could be found
[Fig. 4 (e)], which ensures that the steel tempered
at 600 'C still shows high strength. While for C-Mn-
Mo-Nb-Cu-B steel by CR+DQ+T process, the ma-
trix microstructure is mainly quenching martensite-
Issue 2 Effect of H e a t Treatment Process on Properties of 1000 MPa U l t r a - H i g h Strength Steel 67

( a ) , (c) , (e) Microstructure of hot rolled state, 400, 600 O C by TMCP+QT process, respectively;
( b ) , ( d ) , ( f ) Microstructure of hot rolled state, 450, 620 'C by CR+DQ+T process, respectively.
Fig. 4 SEM micrographs of evolution of structure with increasing tempering temperature

bainite lath with a small amount of acicular ferrite

(AF and granular martensite-austenite ( M-A )
islands [Fig. 4 (b)]. Martensite lath grows from the
austenite grain boundaries and the lath is thin and
long even throughout whole grain. After tempered
at 450 C , the matrix structure conversed the hot
rolled state, but the M-A islands decomposed and
reduced significantly [Fig. 4 (d)]. With the tempe-
ring temperature rising, partial martensite-bainite
lath was connected and was coarsened, but many
lath-beam still could be seen. As the temperature in-
creased to 620 'C , M-A islands and carbide were al-
most decomposed, and lath continued to coarsen.
Meanwhile, a small amount of polygonal ferrite gen-
erates along the grain boundaries [Fig. 4 (f)].
3 Analysis and Discussion
3.1 C-Mn-Cr-MeB steel after TMCP-kQT
Due to the relatively high carbon content
( 0 . 1 6 % ) in C-Mn-Cr-Mo-B steel, which is pro-
+
cessed by TMCP QT process, the quenching mi-
crostructure is typical martensite lath [Fig. 5 (a)].
T h e solid solution strengthening is caused by car-
bon, as well as the large number of poor mobility
dislocation generated by phase transformation during
quenching. The quenched steel shows high strength.
However, such transformation dislocations are rela-
tively flat and not pinned mostly. When specimens
are tempered at 400 'C , the dislocations would merge or
rearrange. As a result, there would be a rapid fall of

( a ) , ( c ) , ( e ) , ( g ) Microstructure of hot rolled state, 400, 500, 600 .C in TMCP+QT process, respectively;
( b ) , ( d ) , ( f ) , (h) Microstructure of hot rolled state, 450, 500, 600 O C in CR+DQ+T process, respectively.
Fig. 5 "EM micrographs of the evolution of microstructure and precipitates in two processes
 68 Journal of Iron and Steel Research, International
ultimate tensile strengthc5'. Meanwhile, the diffusion
ability of carbon and nitrogen atoms would be enhanced,
and the atoms would cluster around dislocations and
formed the atmospheres to pin movable dislocation,
which caused a slight increase in yield strength and
decrease in plasticityc6]. When tempered at 400 to
500 "C, carbon atoms would be emitted from mar-
tensite to form needleshaped carbide with fixed ori-
entation related with the lath or to diffuse into the
residual austenite [Fig. 5 (c)]. Carbon diffusion
0
r Fe
i
cu
2 3
(a) EDS of the particle of Fig. 5 (d) ; (b) EDS of the particle of Fig. 5 (g) ;
Fig. 6 EDS of the particle
tempering temperature is higher than 600 "C, the
dislocation pinning ability is reduced, and the hinde-
ring ability to the matrix recovery is weakened in
tempering due to the precipitate particle coarsening.
Furthermore, the dislocation mobility is enhanced,
so matrix strength decreases rapidly but plasticity
and toughness are enhanced.
3.2 C-Mn-Mo-NbCu-B steel after CR+DQ+T
C-Mn-Mo-Nb-Cu-B steel specimen is directly
quenched after rolling in CR -I- DQ +
T process,
therefore, bainite and martensite lath in quenched
steel has a large number of transformation disloca-
tions and the dislocation recovery is weak because of
faster cooling rate, so the dislocation density in mi-
crostructure of directly quenched steel is relatively
high, which made the quenched steel has an ultra
high strength ( U T S up to 1160 MPa). As the steel
is controlled rolled in non-recrystallization zone with
severe deformation, the microstructure is refined and
the bainitemartensite lath width is about 300 nm, with
highly dense deformation dislocations. Meanwhile,
between deformation passes, especially during relax-
ation time, a large number of fine N b , V , T i carbo-
nitrides precipitate on the dislocations [Fig. 5 ( b ) ]
that pined the dislocations. Because the dislocations
Vol. 18
from martensite makes further strength decline of
martensite. In addition, higher tempering tempera-
ture activates more movable dislocations, which re-
sults in the decrease of yield strength. When tem-
pered at 500 to 600 'C , strength reduction is accom-
panied with plasticity increase, and little change in
toughness, since the thermal softening effect is greater
than precipitation strengthening effect caused by in-
teraction between ( C r , Mo) C particles and disloca-
tions, as shown in Fig. 5 (g) and Fig. 6 (b). When
Fe
4 5 6 7
EnergyIkeV
i 8 9 2 3 4 5 6 7 8 9
(c) EDS of the particle of Fig. 5 (h).
are inherited during the phase transformation and re-
main pinned laterc7], the yield strength is high (up to
845 MPa) in quenching state. As tempered at 450 OC,
the carbonitride and E-CU particles continue to pre-
cipitate, preferentially on the dislocations [Fig. 5 ( d )
and Fig. 6 (a)], and enhance the pinning effect. MO-
reover, the high density of dislocations in bainite
martensite lath also provides a multitude of nuclea-
tion sites for precipitation. Hence, finer and more
homogeneously distributed particles and a better
precipitation strengthening effectCB1are achieved.
Therefore, yield strength is largely increased (about
150 M P a ) and the first strength peak appears.
Then, E-CU particles begin to merge and coarsen,
and its role of pinning is weakened [Fig. 5 (f)]. Be-
sides, more movable dislocations are activated with
the temperature rising, which decreases the yield
strengthCg3.When the tempering temperature rea-
ches 500 'C , alloy elements, such as Nb, Mo, V ,
are precipitated [Fig. 5 ( h ) and Fig. 6 (c)], which
creates a new strengthening. Furthermore, the dis-
locations do not disappear, which forms the second
yield strength peak in curve, plasticity and tough-
ness correspondingly decreases. T h e CVN impact
fracture a t the temperature of - 40 'C mainly is
cleavage fracture at SEM. When the tempering tem-
Issue 2 Effect of Heat Treatment Process on Properties of 1000 MPa Ultra-High Strength Steel
perature is higher than 600 'C , change of mechanical
properties is similar to that by TMCP+QT process.
4 Conclusions
1) Good comprehensive mechanical properties are
obtained in both kinds of steels with different com-
positions and different processes. T h e change trends
of mechanical properties in tempering process are
different, indicating that the original microstructure
before heat treatment plays an important role in the
mechanical properties after heat treatment. In TMCP+
QT process, for a tempering temperature of 450-
600 "C, C-Mn-Cr-Mo-B steel has the yield strength
beyond 1000 MPa, the elongation over 1 5 % , and
the -40 'C impact energy more than 30 J. When
specimens of C-Mn-Mo-Nb-Cu-B steel subjected to
+ +
CR DQ T process are tempered at 620 'C , the
yield strength reaches 1030 MPa, the elongation is
18%, and - 40 'C impact energy is also more than
30 J.
2 ) The strengthening mechanism of the two
processes is different. T h e main strengthening mecha-
nism includes phase transformation strengthening,
solid solution strengthening, solid solution and pre-
cipitation strengthening of other alloying elements
such as molybdenum, chromium and niobium in the
+
steel treated by TMCP QT process. But for the
+
steel treated by CR DQ+ T process, precipitation
strengthening of copper, especially E-CU precipi-
tates, and carbide of molybdenum is the additional
69
strengthening mechanism. C-Mn-Mo-Nb-Cu-B steel
with relatively lower carbon and alloying element
content has excellent mechanical properties and sig-
nificant weldability after tempering at high temperature.
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