EPD Congress 2009

TMS (The Minerals, Metals & Materials Society), 2009

ELIMINATION OF CRYSTALLINITY IN FRACTURED SURFACE

OF MEDIUM CARBON LOW ALLOY STEEL PLATES THROUGH
PROCESS IMPROVEMENT
Ram Avtar* and G Singh#
*Research & Development Centre for Iron Steel, Ranchi-834002, India
Ph.916512411089, Fax 912411072, e-mail-dra@sail-rdcis.com
#
Rourkela Steel Plant, Rourkela, - 679011, India
Keywords: Fracture, Quenching, Martensite, Tempering, Crystallinity, Hardness

ABSTRACT
High tensile thick plates (>80mm, weight ~3000 Kg) of medium carbon low alloy
steel, when heat treated, manifested higher percentage of crystalline area (>20%) in
fractured surface. Such problem was not encountered in thinner plates. The genesis of
higher crystallinity in fracture was examined. It was observed that the thicker plate
undergone slower rate (Average 0.9oC/Sec.) from soaking temperature to Ms temperature)
of cooling after austenising during oil quenching and thereby quenched microstructure had
upper bainites. During tempering of as quenched bainite, additional precipitation took
place at the lath boundaries of bainite. This led to weakening of grain boundaries and aided
easy crack propagation during fracture and resulted in formation of higher percentage of
crystalline area in fractured surface. Enhancement in cooling rate (Average 1.8oC/Sec.
from soaking temperature to Ms temperature) of austenised plate by switching over from
oil quenching to water quenching practice resulted in complete transformation of austenite
into martensite and produced ductile fracture (zero Crystallinity). Plates conformed
improvement in mechanical properties between 2-5%.

INTRODUCTION
Medium carbon low alloy steel compositions are well known for producing high
strength and tough steel plates for strategic applications. These steel plates have stringent
quality requirement with respect to high mechanical properties, Charpy impact and lower
Crystallinity in fractured surface. Therefore, plates are appropriately heat treated to achieve
desired properties in the final product. During the heat treatment of the plates, various
factors like plate transfer time, quality of quenching oil, scale formation on plate surface,
heat transfer rate from plate to quenching oil effects the phase transformation in the plate.
In general, the transfer time of the plate is maintained uniformly for each plate through
electronically guided system. Scale formation is minimized by controlling the air/gas ratio
in side the furnace. But the quality of the oil may not be consistent during prolong use.
Therefore it may adversely affect the heat transfer rate from plate to oil. In the present
work, efforts have been done to study the oil characteristics and its effect on heat transfer
through surface hardness control and phase transformation study.

675

EXPERIMENTAL PROCEDURE:
The existing heat treatment process line at Rourkela Steel Plant consist an on linehardening furnace, oil quenching tank and a tempering furnace. Plates of all thicknesses
ranging from 4-85mm are quenched in the same tank. Under such cooling conditions
cooling rate of the plate slowed down with the increase of plate thickness. It was observed
that as the plate thickness exceeds 60mm, the incident of failure in fracture test increased
(three point bend test) and in 80mm and above thick plates the condition was alarming.
About 60% plates of the total production are produced in 80/85mm thickness. Present
study has been carried on 80mm thick plates. Though the mechanical properties and
Charpy impact of the steel sample met the specifications, the Crystallinity in the fractured
surface seem to be higher then the specified limit of 20%. The fractured surface of the test
sample (80x80x200mm), tested under three point bend test, showed excessive crystalline
area as shown in fig.1 which is more than the specified of limit of 20 % of the total area
of cross-section.

200 mm

80 mm

Mag. X1
Three point bend test
Fig. 1- Fracture test of thick Plate
Production data, of previous months for 80/85mm thick plates, were collected and plotted
in Fig. 2. Success rate of accepted plates in fracture test with respect to time was varying
between 26-50%

Fractured surface

% Passing in fracture test

120

100

80

60

40

20

Oil Quenched

Water Quenched

0
1

10

11

12

13

14

15

16

17

18

19

Period (Month)

Fig. 2 - Fracture test failure analysis in 80/85 mm thick plates

676

20

21

The plates were being produced as per the process chart provided by Rourkela Steel Plant
and Defence Metallurgical Research Laboratory, India. In order to understand the problem,
processing condition of failed plate samples were analyzed in detail with the help of optical
microscope, Electron Probe Micro-Analyses (EPMA) and Transmission Electron
Microscopy (TEM). Temperature profile of the hardening and tempering furnaces were
studied. Temperature gradient across plate thickness was examined during heating and
quenching process. Physical and chemical characteristics and the cooling efficiency of the
quenched oil were also evaluated.
Microstructure Examination
The micro structural studies were made on 80mm thick plate samples. Samples
were collected from center of the plates showing excessive crystallinity as well as zero
crystallinity. The surface of these samples was prepared by standard technique of sample
preparation. Polished surface of the samples was etched with 2% nital solution. Optical
photomicrographs of failed as well as accepted plate samples are shown in Fig. 3. Failed
sample showed strong banded structure compare to that of accepted plate. These bands
were related to the formation of different phases in the steel during heat treatment.

Mag. X200
(A) - Sample from Failed plate (B) - Sample from accepted plate
Fig. 3 - Optical microstructure of plates
Elemental analysis was performed across the band by Electron Probe Micro Analyzer
(EPMA). It was observed that distribution of Mn, Si, Mo, and Ni was quite uniform across
the band. However, Cr was observed to be in excess in the dark bands of the failed as well
as accepted plate samples as shown in the Fig. 4.

Fig. 4 - Chrome distribution across the band

677

To study the formation of banded structure, samples from the centre of the plates were
prepared for Transmission Electron Microscopy. Identification of phases was carried at
magnifications of 15-25K. Photographs of both the samples are shown in Fig. 5. The failed
samples have a mixed structure of bainite and carbides. The pass samples show precipitates
of the carbides
Heat Treatment of the plates
According to the process chart [1], the hardening temperature of the plates should
be 9100C. Heating rate of the plate and the soaking time together may be maintained at the
rate of 2 minute/mm of the plates thickness. During the tempering, the temperature of the
plate should be maintained between 640-6800C and tempering time should be maintained
at the rate of 4 minute/mm of plate thickness (limited upto 200 minutes).
In order to verify the hardening and tempering temperature across the plate
thickness, three drilled holes each 40mm depth at different locations were made in 80mm
thick plate to fix the copper Constantine thermocouples. The temperature of hardening
furnace was maintained at 9000C and that of tempering furnace was maintained at 6250C.
In each case the temperature of the plate was measured after its complete soaking. The
temperature of the plate, just before the quenching, was recorded as 8700C and the
tempered plate was recorded as 6200C. In both the cases the temperature has been lower
than the targeted temperature as per the process chart.

.
(A) - Sample from Failed plate

(B) - Sample from accepted plate

Fig. 5 - TEM photomicrographs of samples

Cooling Rate measurements in plates
Formation of oxide scale on the surface of the plate during heating suppresses heat
transfer in the plate and as a result slows down its cooling rate while quenching. A study
was conducted on 60 and 80mm thick plates. Thermocouples were embedded on the
surface and at the center of the plates. These plates were heated till the center of the plate
attained ~9100C. The hot plate was taken out on the roller table along with the
thermocouples and quenched in the oil. Temperature v/s time was recorded continuously
during the quenching. The cooling curves of both, 60 and 80mm thick plates are shown in

678

Fig. 6. It can be seen that the center of the 60mm thick plate attained martensitic
transformation temperature (~3450C) in 320 seconds whereas it took 570 seconds for
80mm thick plate.
1000
900

Plate Thickness
80 mm

Temperature in C

800

60 mm

700
600
500
400
300

345

200
100

570

320

0
0

200

400

600

800

1000

Time in Seconds

Fig. 6- Temperature profile at the core of plates in quenching

These curves show that the average cooling rate in 60mm thick plate is almost two times
thats of 80mm thick plate. The cooling curves of 60 and 80mm thick plates were
superimposed on the CCT curves [2] and shown in Fig. 7. As shown in this figure (Fig.7)
the cooling curve of 60mm thick plate passed through

Fig. 7 - CCT diagramme of Cr-Mo steel

martensitic transformation region, where as for 80mm plate it passed through the nose of
martensitic transformation loop. It might have caused excessive bainite formation in 80mm
plate and also the possible reason for the formation of banded structure at the plate center
of 80mm thick plate (Fig.3). This microstructure [3] was prone to produce crystalline
fracture during the three-point bend test.

679

Cooling Efficiency analysis of quenching oil

Special quenching oil VM-48 marketed by M/s oil Aral Gutting, Germany was
used for heat treatment of the plates. Prior to quenching, the plate was heated in the
temperature range of 900-9300C. During quenching, there was some loss of oil due to its
burning and decarburization. Such loss of oil was met by replenishing with fresh oil.
Though the physical properties were being maintained but the chemical characteristics
were never studied. In order to assess the cooling efficiency of fresh and used oils, cooling
rates were evaluated. Cooling curves for fresh and used oils are shown in Fig.8. Used oil
had manifested poor cooling efficiency. The figure shows that the cooling rate was slowed
down by ~29% in case of used oil. This was preliminary due to depletion of volatile
components of the oil. Also efficiency of oil was evaluated in terms of

Fig. 8 - Quenchability study of Aral VMm-48 quenching oil

hardness value attained in the as quenched plates. In this kind of exercise the plate after oil
quenching was shifted to the cooling bed for hardness measurement. Surface of the plate
was prepared and hardness was measured at deferent locations of the plate.
60

Crystallinity

50
40
30

(%)

20
10
0
365 375 385 395 405 415 425 435 445 455 465 475

Hardness of plate (BHN)

Fig. 9 Hardness variation in plate v/s percentage crystallinity
with oil/water quenching.

680

In order to conduct fracture test, the samples of required size were drawn from
opposite corner of the plate. Each sample was fractured in three-point bend test machine
and crystalline area was evaluated in the fractured surface. A relation obtained between
surface hardness of the as quenched plate and percentage area of Crystallinity in the
fractured surface is shown in Fig.9. As shown in the figure crystalline area decreased with
the increase in surface hardness of the as quenched plate. It may be observed that there is a
transition in crystallinity corresponding to surface hardness value of plate ranging between
400-415BHN. This study revealed that the hardness of as quenched plate should be above
400 BHN to achieve crystalline area within the specification limits i.e. <20%.
RESULT AND DISCUSSION
The tensile and toughness of medium carbon low alloy steel depends largely on
quenching & tempering process evolved for particular chemistry and section size. The
microstructure of quenched plates must transform to 100% martensite prior to
transforming. It has been observed that cooling rate slowed down significantly when plate
thickness is increased beyond a particular value and bainite structure appeared in lieu of
martensite. As the ratio of bainite to martensite increased in the structure above a critical
value which correspond to hardness value of 400-415 BHN, weakened bainite the grain
boundaries and aided easy crack propagation resulting formation of higher percentage of
crystalline area in the fractured surface. In order to increase cooling rate of plate, agitation
in the oil bath may be effective, owing to removal of vapour blanket formed on the plate
surface. Also it was confirmed that replenishment of used oil with small quantity of fresh
oil improved cooling efficiency of oil. As shown in Fig. 8, cooling efficiency of the oil
reduced by 29% due to evaporation of volatile constituents of the oil which are responsible
for maintaining cooling efficiency of the oil. Fig.6 shows that the cooling rate at the center
of the 80 mm thick plate was just half that of 60mm thick plate. The above studies showed
that cooling rate at the center of 80 mm thick plate was low and was not adequate to
produce martensite. Fig. 7 shows cooling curves of 60 & 80 mm thick plates are
superimposed on the CCT curve of similar composition. Cooling curve of 60 mm thick
plate cuts the martensitic loop whereas the cooling curve of 80 mm thick plate passes
through the nose of the martensitic loop. This observation was confirmed by the micro
structural studies of failed and accepted samples. Fig. 5, demonstrate the microstructure of
accepted plate consisted of tempered martensite and that of failed sample showed a
mixture of bainite lathes and tempered martensite.
In order to overcome the problem of slower cooling rate at the center of 80 mm
thick plates, three quenching media were selected for experimental purpose i.e. Water,
1%Brine water and 2.5% Brine water.
A plate of dimension 80x800x2000 mm was quenched in above mentioned media.
The surface hardness of each plate was measured and the hardness values achieved are
given in Table 1. It may be noted that the plate quenched in brine water showed highest
hardness. Samples collected from all the three plates were fractured under three-point bend
test. Fractured surface of all these three plate samples showed zero Crystallinity on the
fractured surface. It was observed that water as a media of quenching showed slowest
cooling rate comparable to other two quenchants and thus water was considered as a
suitable media for quenching. Based on the results, all plates of 80x800x6000 mm size
were processed through water quenching, satisfying mechanical properties requirement as

681

well as Crystallinity criteria on three points bend test. Surface hardness of quenched plates
was measured and a plot is shown in Fig.9. It was observed that as quenched hardness of
plates was quite consistent and varied between 415-425 BHN. Mechanical properties of the
water quenched plates samples are shown in Fig.10. In case of water quenching, Yield and
ultimate tensile strength of plates were higher than those quenched in oil and impact
toughness energy was also higher. The microstructures of plates are shown in Fig.11.
Fractured surface is free from Crystallinity and the banded structure.
TABLE I, Hardness of quenched plates
Sl.No.

Plate Hardness
(BHN)

% Crystalline Area in
Fractured Surface

Quenching Media

1
2
3
4
5
6
7
8
9

365
380
397
408
415
420
425
443
473

50
40
30
10
2
0
0
0
0

Oil
Oil
Oil
Oil
Oil
Oil
Water
1% Brine Solution
2.5% Brine Solution

O il Q u e n c h e d
W a te r Q u e n c h e d
O il Q u e n c h e d
W a te r Q u e n c h e d

20

14
12

60

10
8

40

6
4

20

16

80

Charpy Energy, (kg.m/cm )

18
100

2
0
)
C

40

io
%

lo

LT

(-

ng

at

TS

0
Y

Strength in kg/mm and Elongation in %

120

M e c h a n ic a l P r o p e r t ie s

Fig.10 Mechanical Properties comparison of 80/85 mm thick plates

Produced through oil and water quenching Process

682

MACROSTRUCTURE Mag. 1X

MICROSTRUCTURE Mag. X300

Fig. 11- Macro (1X) and microstructures (300X) of water quenched plates
CONCLUSIONS
1. Genesis for formation of excessive Crystallinity (>20%) in fractured surface of
three point bend test sample was linked with formation of bainite at the center of
the plate corresponding to slower cooling rate of 10C/sec.
2. The hardness of plate surface of as quenched plate must be higher than 415BHN
which is easily attainable by replacing oil with water as quenching media. This
ensured 100% transformation of martensite at center of the plate eliminating risk of
excessive Crystallinity in three point bend test in as quenched and tempered plates

REFERENCES
1. Avtar R, Saxena A, Sinha S N and Patnaik B.B. RDCIS Report No.
45:02:2319:94, March1994.
2. Austenite Transformation Kinetics of Ferrous Alloys, I. Wrought Construction
Steels Climax Molybdenum Company, pp I-127.
3. Bergman H.Robort , Metals Engg. Quarterly, May, 1971, p205.

683