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G. Kosec i dr.

Utjecaj toplinske obrade na Charpy energiju udara mikrolegiranog čelika

ISSN 1330-3651 (Print), ISSN 1848-6339 (Online)


DOI: 10.17559/TV-20150119110824

EFFECT OF HEAT TREATMENT ON CHARPY IMPACT ENERGY OF MICROALLOYED


STEEL

Gorazd Kosec, Jelena Vojvodič Tuma, Mirko Gojić, Aleš Nagode, Antun Stoić, Ivan Samardžić, Borut Kosec

Original scientific paper


In this paper the microalloyed high-strength low-alloy (HSLA) Niomol 490K steel with an addition of niobium (0,032 wt. %) has been investigated. Heat
treatment of the steel consisted of austenitisation at 1250 °C for 3 minutes and reheating up to 750 °C for 5 s. After austenitization the quenching was
carried out in water with temperature of 70 °C and then in a lead bath up to 400 °C following cooling on the air. It was found that Charpy impact energy is
higher and the transition temperature is lower for the transformation of austenite to bainite than to martensite microstructure. Experimental results showed
that different fracture surface was observed. It is shown that preferred cleavage fracture occurred in the lattice plane (001) independently of steel
microstructure.

Keywords: Charpy impact energy, Fracture surface, HSLA steel, Microstructure, Transition temperature

Utjecaj toplinske obrade na Charpy energiju udara mikrolegiranog čelika

Izvorni znanstveni rad


U ovom radu istraživan je niskolegirani visokočvrsti čelik Niomol 490K koji sadrži dodatak niobija (0,032 mas. %). Toplinska obrada čelika se sastojala
od austenitizacije pri 1250 °C u trajanju od 5 minuta i ponovnog zagrijavanja do 750 °C u trajanju od 5 s. Nakon austenitizacije provedeno je kaljenje u
vodi kod temperature od 70 °C i u olovnoj kupci do temperature od 400 °C uz naknadno hlađenje na zraku. Utvrđeno je da je Charpy energija udara viša, a
prijelazna temperatura niža za transformaciju austenita u bainit nego kod transformacije austenita u martenzitnu mikrostrukturu. Eksperimentalni rezultati
su pokazali različite prijelomne površine. Pokazano je da je preferentno cijepajući prijelom zapažen po ravnini rešetke (001), neovisno o mikrostrukturi.

Ključne riječi: Charpy energija udara, Prijelomna površina, HSLA čelik, Mikrostruktura, Prijelazna temperatura

1 Introduction welded plate. LBZ-s cause instable local fracture


behaviour of the steel in HAZ [15]. In highly constrained
High strength low alloy (HSLA) steels represent a geometries, the local toughness dominates the failure
group of low carbon steels that utilise small amounts of process and deviates the crack into harder and more brittle
alloying elements, such as Mo, Ti, V and Nb, to attain weld metal, while in low constraint configurations, the
high yield strengths in the as rolled condition [1÷3]. The size of the plastic zone promotes crack deviation into the
main properties of HSLA steels are: high strength and softer and tougher parent plate [16]. By testing of
toughness, corrosion resistance, weldability and cost simulated welds a linear relation between the inverse
effectiveness [4, 5]. They are used for different square root of the fracture facets size and the impact
applications (pipelines, offshore platforms, ship buildings, transition temperature was found [17]. LBZ were found
reservoirs for liquid natural gas etc.). HSLA steels are also in HAZ of welds of the cryogenic 9 % Ni steel [18].
used for petrochemical vessels because of their excellent It is concluded from the survey of references that the
weldability and resistance to hydrogen embrittlement. It is harmful effect of LBZ on toughness is well established,
known that the toughness and transition temperature are nevertheless, no experimentally verified explanation of the
very important for these steels and because of that Charpy propensity of different microstructure to form LBZ in the
impact energy is highly dependent on the microstructure HAZ of welds was proposed, so far. Based on the field of
[6, 7] experience and investigation [19], it was assumed that the
In the previously published study it was found that formation of LBZ is related to changes in particular
the toughness transition temperature of welded plates with constituents of HAZ microstructure. The aim of this
thickness 15 was by about 20 °C higher than for 25 mm investigation was to verify the effect of short reheat at a
plates [8]. This finding confirmed simulation results with temperature of partial transformation on notch properties of
different 800 °C to 500 °C cooling rate [9]. In the martensite and lower bainite microstructure [20].
scientific literature this problem has not been described
yet. It is well known that microstructures of the base 2 Experimental work
metal, heat affected zone (HAZ) and weld metal are
different [10]. It is the result of effect of heat flow and the All experimental work was performed on the HSLA
cooling rate of steel during welding process. For example, Niomol 490K steel produced by electric furnace in
in this case of multilayer welding the deposition of each industrial conditions. The chemical composition of the
layer includes heating of underlaying microstructure [11]. investigated steel is shown in Tab. 1.
Difference in transition temperature of HAZ of As can be seen from Tab. 1 the steel is microalloyed
weldments of structural steels is explained with the effect with niobium in order to accelerate the formation of
of local brittle zones (LBZ) [12, 13]. It was suggested that ferrite and due to grain refinement [21, 22]. The steel
the ability of Charpy tests to detect brittle zones was slabs were hot rolled into plate 15 mm thickness. Samples
questionable [14] and that for the same steel the welding cut from 15 mm plate were austenitised at 1250 °C with
procedure should be adjusted to the thickness of the holding time of 3 minutes. The first group of

Tehnički vjesnik 23, 3(2016), 761-767 761


Effect of heat treatment on Charpy impact energy of microalloyed steel G. Kosec et al.

Table 1 Chemical composition od steel investigated, wt. %


C S Al Ni Cr Si Mn P Cu Mo Ti Nb
0,11 0,004 0,019 0,15 0,54 0,36 0,50 0,012 0,29 0,34 0,014 0,032

samples was quenched in water. The second group of This pearlite can be formed by nucleation of cementite at
samples was quenched up to 400 °C in lead bath for 5 austenite/ferrite boundaries followed by carbide-free
minutes and then cooled in the air. After that the samples ferrite layers enclosing the cementite in the temperature
are reheated for 5 s up to 750 °C (with holding time of 3 range the formation of conventional lamellar pearlite and
s) with direct conduction heating and air cooled with the upper bainite [26]. After rapid heating up to 750 °C
cooling time t750÷500°C = 17 s using Gleeble 1500 device. microstructure consisted of accicular ferrite, degenerated
By this heat treatment of the steel the welding process at pearlite and secondary martensite (Fig. 1b). The
next deposition was simulated by means of short time quenching in water from 1250 °C produced a coarse
annealing (5 s) in intercritical temperature range (750 °C) microstructure with platelets of ferrite and lath of primary
where two-phase region (austenite and ferrite) exists. On martensite (Fig. 2a). After rapid heating of quenched
all specimens the Charpy V-notch was cut after heat samples up to 750 °C primary and secondary martensite
treatment. occurred (Fig. 2b). In Fig 2b stringers of cementite
The Charpy tests were carried out in temperature particles in ferrite grains and inserts of secondary
range from 196 °C to 60 °C. Hardness was measured by martensite at grain boundaries can be also observed. The
Vickers method (HV5). Samples for metallographic cooling in lead bath from 1250 °C up to 400 °C produced
analysis were prepared by mechanically grinding and the coarse grain of bainite microstructure that consisted of
polishing. Etching of samples was performed by nital stringers of cementite particles at borders of ferrite
solution. Metallography analysis was performed using platelets, (Fig. 3a). After reheat (up to 750 °C) lower
scanning electron microscopy (SEM) method. bainite which was obtained with cooling in lead bath from
Fractography analysis was carried on Charpy samples 1250 °C changed into a microstructure consisting of
fractured. The fracture surfaces were investigated with platelets of secondary martensite at the boundaries of
SEM Jeol JSM 5610 [23, 24], and the space orientation of coarse grains and bainite microstructure (Fig. 3b).
cleavage facets was determined with electron backscatter
diffraction (EBSD) method [25].
a)
3 Results and discussion

Representative scanning electron micrographs of the


Niomol 490K steel in different states are presented in
Figs. 1÷3. The microstructure of the as delivered steel
consisted of acicular ferrite and degenerated pearlite (Fig.
1a).

a)
b)

b) Figure 2 SEM micrographs of the steel after water quenching from


1250 °C (a) and after reheating (b)

The hardness values of the different microstructures


are listed in Tab. 2. The low hardness of the as delivered
steel increased significantly after reheat (248 HV5). After
water quenching from 1250 °C the hardness was much
higher in comparison to the initial hardness (hardness of
the as delivered steel). After water quenching from 1250
°C, the greatest hardness was obtained (383 HV5) that
Figure 1 Microstructure of the steel in delivered state (a), and after decreased significantly at reheat, still, it remained high.
reheating at 750 °C (b)
After quenching in lead bath from 1250 °C the hardness
was increased moderately (257 HV5) and it was higher
after reheat. The experimental findings on microstructure

762 Technical Gazette 23, 3(2016), 761-767


G. Kosec i dr. Utjecaj toplinske obrade na Charpy energiju udara mikrolegiranog čelika

(Figs. 1÷3) and hardness (Tab. 2) indicate that depending heat treatment is presented in Figs. 4÷6. It can be seen
on the initial microstructure three different processes may that Charpy impact energy is closely associated with the
occur at short reheat: (1) the dissolution of cementite with microstructure. The Charpy curves show that at upper
a formation of secondary austenite around cementite shelf range the microstructure behaves as 100 % ductile
particles in the interior of ferrite grains and its fracture, while at lower shelf the Charpy impact energy
transformation to secondary martensite at cooling, (2) the tends to minimum (brittle fracture). The transition
formation of inserts (grains) of secondary martensite at temperature can be expressed in different ways. One of
triple points and boundaries of ferrite grains and (3) the them is that the Charpy impact transition temperature can
decomposition of primary martensite. be estimated as the average of maximum and minimum
shelf energy values in Charpy curves [27]. In this
investigation the trend in shift in the transition
a)
temperature was observed.

b)

Figure 5 Charpy impact energy versus testing temperature for the steel
quenched in water from 1250 °C, and after reheating up to 750 °C

Figure 3 SEM micrographs of the steel after lead bath cooling from
1250 °C (a) and after reheating (b)

Table 2 Hardness of steel after different thermal treatment


Thermal treatment Hardness, HV 5
As delivered 205
As delivered + 750 °C 248
1250 °C / water 383
1250 °C / water + 750 °C 320
1250 °C / lead bath at 400 °C 257
1250 °C / lead bath at 400 °C + 750 °C 298

Figure 6 Charpy impact energy versus testing temperature for the steel
cooled from 1250oC in lead bath at 400 °C,
and after reheating up to 750 °C

The upper shelf Charpy V-notch impact energy is


high (about 240 J) and the Charpy transition temperature
is low (about −70 °C) for the as delivered steel (Fig. 4).
After quenching from 1250 °C Charpy imapct energy is
decreased, while transition temperature is increased (Figs.
6 and 7). After reheating up to 750 °C the Charpy V-
notch impact energy is decreased little for the as delivered
steel (by about 40 J), more for martensite (by about 60 J)
and the most for fine and coarse lower bainite
microstructure (by about 200 J). Also after reheating the
Figure 4 Charpy impact energy versus testing temperature for the transition temperatures are increased, especially for the
delivered, and reheated steel up to 750 °C fine and coarse lower bainite microstructure.
The results of Charpy tests (Figs. 4÷6) on the same
The correlation between Charpy impact energy and test steel cooled to fine and coarse martensite and lower
temperature of the steel in both delivered state and after bainite show that the fracture energy was greater and the

Tehnički vjesnik 23, 3(2016), 761-767 763


Effect of heat treatment on Charpy impact energy of microalloyed steel G. Kosec et al.

transition temperature was lower for lower bainite than composition that the investigated, slower cooling could be
that for martensite. After the applied reheat (up to 750 more harmful than faster cooling.
°C), the fracture energy was decreased and the transition
temperature increased much more for lower bainite than
for martensite. The difference reflects the change of both
initial microstructures at reheating temperature and air
cooling. For bainite, in areas of cementite particles in the
interior of ferrite grains secondary martensite was formed
at reheat, while, at reheat virtually only a partial
decomposition of primary martensite occurred in the
interior of grains. In the very short reheat time of some
seconds, secondary austenite rich in carbon was formed
with dissolution of cementite particles and then
transformed to secondary martensite at cooling. The
Figure 8 Microfractography of fracture surface of steel after Charpy test
extent and form of decomposition of primary martensite
at 40 °C
in the applied reheating are not clear, yet. The extent of
formation of secondary austenite with dissolution of
cementite particles was sufficient to produce a volume of
martensite that greatly diminished the notch toughness.
Also, the change of primary martensite at reheating
decreased significantly the fracture energy, however, the
decrease was much lower than for bainite. An opposite
effect would be expected after the completed
decomposition of martensite.

Figure 9 Microfractography of fracture surface of steel quenched from


1250 oC in water after Charpy test at −60 °C

a)

Figure 7 Microfractography of fracture surface of steel in delivered state


after Charpy test at 20 °C

The fast formation of inserts of secondary martensite


at grain boundaries of ferrite for the initial microstructure
of martensite and lower bainite grains suggests the grain
boundary carbon segregation and the piping diffusion of
segregated carbon to the points of faster formation of b)
austenite with high solubility for carbon. The effect of
these inserts is not clear, nevertheless, it is possible that
they are responsible for the decrease of Charpy impact
energy of martensite after reheat.
It is evident that the effect of short reheating in the
ferrite+austenite range is more harmful for notch
toughness of lower bainite than of martensite. Therefore,
it is expected that the propensity to form local brittle
zones (LBZ) is greater for lower bainite than for
martensite. The very different Charpy imapct energy for Figure 10 Microfractographs of fracture surface of steel quenched from
similar hardness suggests that the physical form of 1250 °C in water and reheated at 750 °C (a) and cooling from 1250 °C
in lead bath up to 400 °C and reheated at 750 °C (b)
presence of carbon, in precipitates or in solid solution in
martensite, affects differently notch toughness
temperature than hardness. Selected fractographic observations made on some
broken Charpy V-notch samples are shown in Figs. 7÷10.
The findings in this investigations show that for HAZ
the transformation of austenite to lower bainite is more As can be seen three fracturing mechanisms were
harmful for the weld quality, than the transformation to identified for the three levels of Charpy impact energy. At
martensite, in spite of the lower hardness of bainite. Also, high Charpy impact energy the fracture surface consisted
for notch toughness of HAZ of structural steels of similar of areas of normal and of shear decohesion with dimples
of different size (Fig. 7). Most of the fracturing energy in

764 Technical Gazette 23, 3(2016), 761-767


G. Kosec i dr. Utjecaj toplinske obrade na Charpy energiju udara mikrolegiranog čelika

ductile range is consumed for the plastic deformation the cleavage surface can have only the index
before the crack is started at the notch tip. Similar fracture corresponding to a simple lattice plane (001) or (011), it is
mode is observed on microalloyed cast steel after post- concluded that it occurred in the lattice plane (001)
forging heat treatment [28]. At temperature above −20 °C independently on steel microstructure.
fracture consisted of a mixture of brittle and ductile
surface (Fig. 8). After quenching from 1250 °C in water
the cleavage facets were coarse (Fig. 9) and without
details related to the presence of inserts of secondary
martensite at grain boundaries. After reheating up to 750
°C was observed brittle fracture by cleavage mechanism
(Fig. 10). The shape and size of brittle facets was related
to the size of ferrite grains. Brittle crack initiation is
probably associated with carbide particles at boundaries (a)
for bainite and martensite microstructures. It is in
accordance with previous fractography study [29] on
Charpy V-notch impact tests which showed that
microalloying elements can change the fracture mode
from ductile to brittle.
The cleavage could occur in (110) and (100) lattice
planes with a greater density of rivers for the (110)
planes. The examinations of the obtained fractures did not (b)
confirm this observation although on cleavage facets of αFe {3 -3 19}〈13 25 6〉
coarse lower bainite the rivers density was greater. The
accurate EBSD (electron backscatter diffraction) analysis
is achieved with the angle of approximately 70° between
the facet surface and the incident electron beam and a
small distance between the incident spot and the electron
collector. This geometry could not be achieved at the (c)
Figure12 SEM micrography of fracture surface (a), diffraction lines (b),
examination of the uneven fracture surfaces. and lattice indexing of the cleavage facet (c) of steel quenched from
1250 °C in water and reheated at 750 °C

4 Conclusions

On the basis of experimental findings in this


investigation and their analysis the following conclusions
are proposed:
- the Charpy impact energy is higher and the transition
temperature is lower for the transformation of
(a) austenite to bainite than to martensite microstructure;
- after short reheat at 750 °C and air cooling Charpy
impact energy was decreased for approximately ten
times and the transition temperature increased above
40 °C for bainite microstructure.
- particularly harmful for notch toughness and transition
temperature is the transformation of austenite formed
at reheat in the interior of ferrite grains with
(b) dissolution of cementite particles to secondary
αFe {14 -5 -3}〈4 19 -13〉 martensite;
- physical form of the presence of carbon in the
microstructure, as precipitates or in solution in
martensite, has a different effect on notch toughness
than on hardness. For this reason, at similar hardness
different notch toughness properties could be
(c) obtained;
Figure 11 SEM micrography of fracture surface (a), diffraction lines (b)
and lattice indexing of the cleavage facet (c) of steel cooled in lead bath - although beneficial in terms of notch toughness and
from 1250 °C up to 400 °C transition temperature, the transformation of austenite
to lower bainite in the HAZ of welds is to be avoided
In Figs. 11 and 12 the analysed surface, the because of its higher propensity to form local brittle
diffraction lines and their indexes are shown for the zones at short reheat in the austenite + ferrite range.
cleavage fracture of steel cooled in lead bath from 1250 - different fracture surfaces are observed and preferred
°C and quenched in water from 1250 °C and reheated. In cleavage fracture occurred in the lattice plane (001)
the first case the cleavage surface indexing is {14 −5 −3} independently on steel microstructure.
(4 19 −13) and in the second {3 −3 19} (13 25 6). Since

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Effect of heat treatment on Charpy impact energy of microalloyed steel G. Kosec et al.

Acknowledgement Fracture Mechanics, 74 (2007), pp. 2395-2419. DOI:


10.1016/j.engfracmech.2006.11.011
The authors want to thank professor Franc Vodopivec [14] Sconover, T. M. Evaluation of Local Brittle Zones in
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Smolej (University of Ljubljana), and professor Ladislav
(HSLA) Steels Weldments, American Welding Society,
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Authors’ addresses

Gorazd Kosec, Ass. Prof. Dr.


ACRONI d.o.o.
C. B. Kidriča 44, 4270 Jesenice, Slovenia
E-mail: [email protected]

Jelena Vojvodič Tuma, Assoc. Prof. Dr


Institute of Energetics,
Mesarska 24, 1000 Ljubljana, Slovenia
E-mail: [email protected]

Mirko Gojić, Prof. Dr.


University of Zagreb, Faculty of Metallurgy,
Aleja narodnih heroja 3, 44103 Sisak, Croatia
E-mail: [email protected]

Aleš Nagode, Ass. Prof. Dr.


University of Ljubljana,
Faculty of Natural Sciences and Engineering,
Aškerčeva c. 12, 1000 Ljubljana, Slovenia
E-mail: [email protected]

Antun Stoić, Prof. Dr.


J. J. Strossmayer University of Osijek,
Mechanical Engineering Faculty in Slavonski Brod,
Trg Ivane Brlić Mažuranić 2, 35000 Slavonski Brod, Croatia
E-mail: [email protected]

Ivan Samardžić, Prof. Dr.


J. J. Strossmayer University of Osijek,
Mechanical Engineering Faculty in Slavonski Brod,
Trg Ivane Brlić Mažuranić 2, 35000 Slavonski Brod, Croatia
E-mail: [email protected]

Borut Kosec, Prof. Dr.


University of Ljubljana,
Faculty of Natural Sciences and Engineering,
Aškerčeva c. 12, 1000 Ljubljana, Slovenia
E-mail: [email protected]

Tehnički vjesnik 23, 3(2016), 761-767 767

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