Materials Science and Technology (MS&T) 2011

October 16-20, 2011, Columbus, Ohio · Copyright © 2011 MS&T'11®

Steel Product Metallurgy and Applications

Properties of Low Carbon Steel with Various Microalloying Additions after

Particular Thermomechanical Processing
P. Podany
COMTES FHT a.s., Dobřany, Czech Republic

M. Balcar
ŽĎAS, a.s., Žďár nad Sázavou, Czech Republic

Keywords: microalloyed steels, thermomechanical processing, forging

Abstract

The article deals with production of the micro alloyed steel forged products for oil
industry. Customer requires high toughness in lowered temperatures, guaranteed weldability and
also relatively high yield strength. Applied heat of steel has 0,1 of carbon content and 1,5 percent
of manganese. Conventional alloying with conventional heat treatment not always lead to
consistency in mechanical properties. Application of usual heat treatment (quenching and
subsequent tempering) ensures only close compliance of requirements in yield strength. It is also
complicated to meet adequate toughness at -46°C by applying conventional heat treatment. New
heats with combination of several microalloying elements (Ti, V, Nb, Zr) were prepared.
Physical simulation of forging on real specimens was done on unique device with possibilities of
temperature and deformation controlling. The main goal of this experiment was to assess
mechanical and microstructural properties of steel after addition of various amounts of various
microalloying elements.
Introduction

High-strength low-alloy (HSLA) steels, or microalloyed steels, are designed to provide

better mechanical properties and/or greater resistance to atmospheric corrosion than conventional
carbon steels. They are not considered to be alloy steels in the normal sense because they are
designed to meet specific mechanical properties rather than a chemical composition. In order to
realize the full strengthening potential of microalloying additions, it is necessary to use a soaking
temperature prior to forging that is high enough to dissolve all vanadium-bearing precipitates. [1]
A soaking temperature above 1100 °C (2010 °F) is preferred. For Nb–Ti microalloyed
steel the single step austenite reheating temperature at 1150 °C provided better austenite
conditioning than the higher reheating temperature at 1240 °C [2]. According to [3] and [4]
complete dissolution of carbonitride precipitates based on Nb occurs at 1140 °C respectively in
interval between 1100 – 1200°C.[5]
Further processing after austenitization should consist of two phase forging. A higher
amount of deformation at elevated temperature (ca 1100 °C) facilitates dynamic recrystallization.
In this stage a critical amount of strain is required for austenite grain refinement through repeated
recrystallization. The second stage should be carried out below 900°C i.e. below recrystallization
temperature (TR) with an intention of making the austenite grain pancaked and to introduce
interfacial defects in hot austenite. These interfacial defects in turn lead to an increase in
effective grain boundary areas and enhances the nucleation potency of ferrite. Subsequently, the
microalloying elements come out of solution with decrease in temperature, which inhibit

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austenite grain growth by forming microalloying carbides or carbonitrides at these interfacial
defects. Controlled cooling after forging leads to desired microstructure. Subsequent tempering
could bring another strengthening due to the precipitation of microalloying elements. Tempering
temperature 600°C and holding time 4 hours are used in this experiment to meet customer
requirements.

Experiment

First part of experiment was focused on numerical simulation in DEFORM 3D software.

It consists of simulation of controlled last step of forging from 500 mm bar diameter to 460 (440)
mm bar diameter. Forging takes place in the range of 940 – 800°C interval. Numerical modelling
allows accurate computing of precise deformation and temperature distribution in every locality
of real forged product according to choice. One locality 40 mm below the bar surface was chosen
for further experiment - physical simulation. It is the locality, where samples for mechanical
testing are made from.

1200 3
2.5
1000
2

displacement [mm]
temperature [°C]

800 1.5
1 temperature
600
0.5 deformation

400 0
-0.5
200
-1
0 -1.5
0 500 1000 1500 2000
time [s]

Figure 1Physical simulator of temperature/deformation cycles and particular prescription of thermo-deformation

cycles for sample of heat 14

Second part of experiment - physical simulation - was focused on samples with various
microalloying additions. Physical simulator is a unique device with possibilities of temperature
and deformation controlling. It allows simulating similar conditions of one locality of real piece
from the view of temperature/deformation in the small specimen. The specimen is shape similar
to tensile test sample and it is resistive heated and loaded with tension and press. Device
parameters are: Maximum force of 250 kN; heating rate of up to 150°C/s; cooling rate of up to
150°C/s; maximum frequency of cyclic loading 30 Hz; maximum forming velocity of 600mm/s.

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 Cooling rate of physical simulator allows simulation of cooling in various environments.
There is possible to simulate cooling in the air, quenching in oil and water. Simulation of cooling
in the water was chosen to be the best for this task. Cooling of whole bar to the water is also the
simplest way of cooling for the producer.

Figure 2 Specimen in physical simulator and numerical simulation of real temperature/deformation distribution in
specimen for physical simulation

Different deformation process was applied on specimens in simulator. Base heat B (with
no microalloys) and heat 8 underwent physical simulation of forging in the range of 980 – 840°C
for forging from Ø500 mm of bar to Ø460 mm. Decreasing of finishing temperature (of forging)
to 940 – 800°C was applied on heats 8, 16, 19, 9 and 12. Heats 9, 15 and 12 were subjected to
simulation of forging in full range of deformation (from 500 to 440 of bar diameter). Last batch
of samples (10, 11 and 14) was processed after preheating on 1200 °C. Chemical composition of
heats is summarized in table 1. There were prepared samples for tensile and minicharpy (notch
toughness) tests after the physical simulation and subsequent heat treatment. The microstructure
was observed by means of optical microscope Nikon Epiphot 200 with quantitative image
analysis software NIS Elements 3.2. Detailed observation with EDX measurement was done on
scanning electron microscope JEOL 6380. Last experiment was focused on real experimental
forging on hydraulic press. One heat with no microalloys and one heat with Ti, Nb, V were
subjected to the identical forging process. The aim was to compare microstructure and
mechanical properties of nonmicroalloyed and microalloyed heat.

Table 1 Chemical composition of heats

Heat C Mn Si P S Cr Ni Cu Mo Ti Nb V Zr
B 0,10 1,47 0,14 0,004 0,001 0,15 0,09 0,11 0,04 - - - -
8 - 0,06 0,042 -
9 - 0,09 0,049 -
10 - 0,045 0,13 -
11 - 0,044 0,17 -
Identical composition (exept of microalloys)
14 - 0,051 0,12 0,13
15 - 0,13 0,051 0,195
12 - 0,13 0,042 -
19 0,17 0,11 0,045 -

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 Results and discussion

Physical simulation

Tensile tests according to CSN EN 10002-1 were performed. Tests were executed at room
temperature. Prior to testing specimen dimensions were measured and original gauge length for
the elongation A2 determination was marked on each specimen. The final gauge length and cross
section dimensions were also measured after the test so that the cross section reduction could be
evaluated. Impact tests were performed at the instrumented Charpy pendulum with the impact
energy 15J. There were tested samples with dimension 3 x 4 x 27 mm. Tests were executed at
minus 46 °C. Requirements on mechanical properties are following:
Rp02 = min. 415 MPa; Rm = min. 530 MPa; A = min. 20 %; KV mini(-46 °C) = min. 2 J

Table 2 Mechanical properties of specimen after physical simulation

KV mini
Rp0,2 Rm A2
Heat [-46 °C] Microalloys
[MPa] [MPa] [J] [%]
B – as quenched1 365 606 6,9 24 -
1
8 – as quenched 415 543 6,2 28 0,06 Nb; 0,042 V
2
8 – as quenched 430 538 6,9 26 0,06 Nb; 0,042 V
2
19 - annealed 422 547 10 54 0,11 Nb; 0,17 Ti; 0,036 V
9 - annealed3 480 624 9,3 44 0,09 Nb; 0,049 V
3
15 - annealed 482 625 3,3 44 0,13 Nb; 0,051 V; 0,195 Zr
3
12 - annealed 481 593 8 25 0,Nb Ti; 0,042 V
4
10 – annealed 581 721 2,1 37 0,045 Nb; 0,13 V
4
11 – annealed 600 732 2,2 42 0,044 Nb; 0,17 V
4
14 – annealed 474 710 0,6 31 0,051 Nb; 0,12 V; 0,13 Zr
1
– Simulation of forging from Ø500 mm of bar to Ø460 mm in the range 980 – 840°C
2
- Simulation of forging from Ø500 mm of bar to Ø460 mm in the range 940 – 800°C
3
- Simulation of forging from Ø500 mm of bar to Ø440 mm in the range 940 – 800°C
4
- Simulation of forging from Ø500 mm of bar to Ø440 mm in the range 940 – 800°C – preheating at 1200°C

Required values of mechanical properties were met in all samples which were annealed
(at 600 °C for 4 hours). Samples with higher deformation rate, which were simulated with full
deformation cycles (forging of bar from Ø 500 to Ø 440 mm) have significantly higher yield and
tensile strength. Figures 3 and 4 shows that the reason is in the decreasing grain size with higher
deformation ratio (change of grain size from 10.5 to 11.5). Highest values of mechanical
properties (YS, TS) were reached with samples 10 and 11. They were austenitized before
thermomechanical processing on the simulator at 1200°C. This led to increasing of tensile
strength up to ca 730 MPa. But notch toughness was lowered to ca 2 J. Nevertheless this value is
still acceptable.

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 Figure 3 Microstructure of heat 19 Figure 4 Microstructure of heat 9

Microstructure of all heats consists of fine grained ferrite, tempered bainite/martensite

and pearlite. Lower values of notch toughness in case of heats 14 and 15 are caused by presence
of coarse undissolved ZrCN particles, which were visible also on the fracture surface and in the
microstructure of minicharpy samples (see figure 5).

Figure 5 ZrCN particles in fracture surface of heat 15

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There were observed fine vanadium based carbides/carbonitrides in microstructure of all samples
(see fig. 6)

Figure 6 Precipitation of VC(N) in the microstructure

Forging experiment

Forging on the hydraulic press were performed according to the numerical simulation
calculation of deformation in the one locality of real forged bar. Result will be the sample with
the same amount of final deformation as it is in one locality of real forged bar. Model of forging
and specimen after forging is shown on figure 7.

Figure 7 3D Model of forging and specimen after forging

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 Forging of experimental ingots was done by means of hydraulic press Zeulenroda (PYE
40). Ingots were put in atmospheric furnace Heraus and heated up to 1150°C. Then they were
forged to finial dimension for ca 1 minute and 10 seconds. Final temperature on the surface of
ingots was measured by thermocouple and reaches ca 750°C. Ingots were then cooled on air.
Microstructure of ingots after forging shows substantial differences. Ingot with microalloys has
finer grains – 11.0 according to ASTM E 112 in comparison to 9.5 in case of ingot with no
microalloys (see figures 8 and 9). Also the yield and tensile strength of ingot with microalloys
are considerably higher - see table 4.

Figure 8 Microstructure of ingots from the heat with no Figure 9 Microstructure of ingots from the heat
microalloys (100x and 500x magnification) microalloyed with Ti, Nb and V(100x and 500x
magnification)

Table 4 Mechanical properties of specimens forged from ingots without and with microalloys
Rp0,2 Rm A5 KV (-46 °C)
Specimen
[MPa] [MPa] [%] [J]
Base heat 326 480 34 179
Heat with 0,19 Ti, 0,036 Nb and 0,09 V 433 534 32 155

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 Yield strength is more than 100 MPa higher thanks to grain refinement and precipitation
strengthening of microalloys. This experiment proved the ability of technological process
(designed by numerical simulation of forging of bar) to meet customer requirements.

Conclusion

The new technological processes of forging of steel for oil industry was designed by
means of numerical simulation in DEFORM 3D software. This process was applied on samples
in experiment with physical simulation. Samples were made from heats microalloyed with Ti,
Nb, V and Zr. Grain refinement and precipitation strengthening of microalloying elements led to
substantial increasing of yield strength and tensile strength. Also good notch toughness at
lowered temperatures was kept. Best mechanical properties were reached by microalloying with
vanadium and niobium and especially with samples 10 and 11 preheated before
thermomechanical processing at 1200 °C. This process led to dissolution of all microalloying
aditions during asutenitization therefore good yield and tensile strength was reached after
thermomechanical processing. Also notch toughness of these samples is acceptable.
Forging experiment with real forging on hydraulic press confirms the ability of designed
technological process. Yield strength reached thanks to microalloying was about 25% higher in
comparison to heat with no microalloys.

Acknowledgments
This project OE08009 is supported by European Union and Czech Ministry of education
youth and sports

References

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