Dual Phase Steel Online Processing Trials: Microstructure and Mechanical Properties Inter-relation

Ahmed Refaee1, Sabbah Ataya2 and Samir Ibrahim2

arefaee@ezzsteel.com.eg , sabbah.ataya@s-petrol.suez.edu.eg , saibrahim@link.net

1) Ezz Eldekhela (EZDK) Steel Company, Alexandria, Egypt. 2) Department of Metallurgy and Materials Engineering, Suez Canal University, 43721, Suez, Egypt.

Abstract
The application advantages of dual phase steels in automobile industries motivate further studies on the effect of processing parameters on the properties of dual phase steel. Trials were performed using a thin slab casting unit (TSC) in producing dual phase steels. The effect of inter-critical temperatures (790 and 800C) and coiling temperatures (120, 150 and 180C) on the final microstructure were investigated. Dual phase steels with the composition (in wt. %) 0.057 C, 0.277 Si, 1.38 Mn, 0.027 Nb, 0.036 P, 0.63 Cr 0.39 Al were produced in sheet thickness of 3.2 mm. Characterization of the dual phase steels mechanical properties was carried for different martensite volume fraction at quasi-static tensile loading and impact testing. The final mechanical properties were correlated with the different microstructure constituents. Key words: Dual phase steel, Cooling regime, On-line processing, Mechanical properties, Martensite volume fraction

1. Introduction
Dual phase (DP) steels were developed in the mid-seventies in order to satisfy the increasing needs of automotive industry for new high strength steels which combine significant weight reduction and improved crash performance, while keeping the manufacturing costs at affordable levels. The high commercial potential of the newly developed alloy has motivated extensive research in numerous laboratories, resulting in DPgrades having a wide range of chemical compositions and being produced with various processing routes 1. Dual-Phase (DP) steels composed of martensite islands dispersed in a ductile ferrite matrix were developed to provide a good balance between strength and ductility. In order to reach this goal, it is of prime necessity to control their final microstructure, in particular phase volume fraction, carbon composition and banded structure 2. The high-strength and good formability characteristics of high strength steels (e.g. Dual phase steel) when compared to conventional grades make them attractive in applications involving high rates of loading combined with a demand for low weight. Typical examples include light-weight protective systems, crashworthiness of automotive and aerospace structures, and high-speed machining 3. These properties are only possible through the appropriate controlled rolling followed by controlled cooling to the coiling temperature. Both parameters should be design in function of the steel chemical composition. The resulted mechanical properties changes are associated with different strengthening mechanisms 4. In low carbon DPsteel, the carbon strengthening mechanism is partly substituted by grain refinement through controlled rolling treatment in addition to martensite phase strengthening. It is established that martensite volume fraction, size and distribution will have a significant influence on the properties of the produced steel 5.

The present work is an on-line trial to study the effect of the processing parameters, mainly cooling and coiling conditions on the microstructure and subsequently on steel mechanical behaviors.

2. Experimental procedures 2.1 Dual phase steel production trials

Dual phase steels produced in this study were processed at EZDK (by Steel Making, Thin Slab Casting and Hot Strip Mill). The chemical composition of the used low carbon heat is shown in Table 1. Based on the online pyrometer temperature measurements, the production line length and the rolling speed, the cooling regime is determined as shown in Fig. 1. After finishing the rolling process at a temperature ranging between 800-790C, the rolled sheet was cooled down to a temperature of 650 C, then a holding time (~3 - 5 sec) in air is applied before the final cooling step to reach the coiling temperature which has changed in this work to be 120, 150 and 180C. Under the present cooling and coiling conditions, the highest cooling rate was calculated and found corresponds to the highest coiling temperature as shown in Table 2.
Table 1: Chemical composition (in Wt%) of dual phase steel materials

C
0.057

Si
0.277

Mn
1.38

P
0.0036

S
0.002

Cr
0.63

Ni
0.02

Cu
0.04

Nb
0.027

Ti
0.01

Al
0.05

N
0.0049

F4

F5

F6
1 2

Cooling zone (run out table)

3 4 5 6 7 8 9 10 11

Transport

Coiler

Temperature
800 -790 C

= Pyrometer
850 C

680 C

500 C

< 200 C

Length of cooling line

Fig. 1: Applied cooling regime for dual phase production. Table 2: Cooling regime of the dual phase steel production trials

Trial No. DP1 DP2 DP3

Finishing rolling temperature (C) 800 800 790

Holding time (sec) at 680 C 4.68 3.78 3.52

Cooling rate (C/sec) 113.26 132.29 136.36

Coiling temperature (C) >120 150 180

2.2 Materials Characterization 2.2.1 Microstructure

Microstructure investigation was carried out to reveal the produced structure, to determine martensite volume fraction and grain size. Samples were taken from sheets cross section perpendicular to rolling direction. A double etching step is used to reveal the martensite. Pre-etching in methyl alcohol Nital (2% nitric acid) for 5 sec. then rinsed in distilled water and etching for 20 sec. in 8 g Na2SO4 + 100 ml water according to ASTM E407-07. Microstructure was captured using an Olympus optical microscope equipped with a digital camera (AXIOCAM MRC5). Grain size was measured according to ASTM E112. Martensite area fraction was measured depending on the brightness difference between the ferrite and martensite.

2.2.2 Mechanical tests

Tensile test samples according to the standard JIS Z2241 were used for quasi-static tensile tests (b = 33 mm, Lo= 50 mm), which were carried out using the tensile testing machine Model Zwick/Roll (250 KN). Impact test was conducted on small size impact samples (10 mm height, 2.5 mm thick and 2mm V-notch depth) according to the standard EN 100045-1. Charpy impact testing machine Type RKP 300/450 was used. Tensile and impact specimens were cut in the rolling direction discarding the un-cooled and off-gauge parts.

3. Results and discussions 3.1 Micro structural evolution analysis

The cycle of cooling used in the sheet processing line implies that water quenching is carried out after a preliminary air cooling, i.e. from 800 to 650oC, before immersion into water. The various high cooling rates by water quenching to coiling temperature are shown in Table 2. The obtained microstructures then generally consist of mainly two phase structures, ferrite and martensite. The martensite volume fraction is observed to increase with increasing the coiling temperature, as shown in Table 2. The range of variation is between 30% to 35% volume fractions. The martensite islands in the microstructure exhibit an irregular shape even though they are roughly equiaxed and inhomogenously distributed, as shown in Fig. 2. The martensite islands are dominantly formed along ferrite boundaries with a change in their morphology when the rate of cooling is changed. However, no banded structure is observed and the ferrite grains are generally slightly elongated parallely to the rolling direction. Since the intercritical deformation finishing temperature is the same for the various microstructures, the different martensite volume fractions (MVF) can only be attributed to the adopted cooling rates. Retained austenite is quite likely to be formed in the microstructure following the quenching treatment and, in low carbon steels, is generally estimated to occupy 1-2% of the austenite volume fraction before transformation. Also, during the intercritical treatment, austenite enrichment by carbon from ferrite matrix may facilitate bainite formation 6. Assuming a complete partition of carbon between ferrite and martensite, the carbon content of martensite Cm (wt%) can be given by 7:

Cm Wt %

C Alloy Wt % Vm

(1)

Where: CAlloy is the carbon content of the steel and Vm is the martensite volume fraction. From this relation, the carbon contents in martensite for Vm = 0.306, 0.32 and 0.35 are 0.186, 0.178 and 0.163 wt% respectively, i.e. carbon content decreases with increasing MVF. Moreover, in a low carbon steel, the crystal structure has a low degree of tetragonality (c/a ratio), compared with a higher value in a high carbon steel. The degree of tetragonality has been shown to increase linearly with the carbon content and is given by 7:

c/a= 1.005 + 0.045 C(wt%)

(2)

Using this equation, values of c/a equal to 1.0134 and 1.012 for MVF of 0.306 and 0.35 are obtained respectively. This will give a unit cell volume difference of 2.77% due to the increased martensite volume fraction. Subsequently, these volume differences will have different effects on the surrounding ferrite matrix. Therefore the MVF difference is expected to be higher, the higher the martensite carbon content is. A higher dislocations density is therefore expected at the ferrite martensite interfaces in order to accommodate this volumetric expansion due to the transformation from austenite to martensite and the accumulated dislocations density in the ferrite matrix will depend on the martensite volume fraction. The martensite volume expansion has been estimated to be 2.9 4% at the martensite starting temperature 8.

Fig. 2: Microstructure of the processed dual phase steel Martensite area fractions: a) DP1 = 0.306, b) DP2 =0.32 and c) DP3=0.35

3.2 Mechanical properties.

The engineering stress-strain curves of DP steels with MVFs of 0.306, 0.32 and 0.35 obtained with different cooling rates are shown in Fig. 3. The three curves show a continuous yielding behavior without appearance of the Lders band. It has been reported that a minimum of 4% martensite is needed to achieve a continuous yielding 9. Fig. 3-b shows the increase in both yield stress (Y) which is determined by the onset of plastic deformation, and ultimate tensile strength (UTS) with increasing MVF, however both total elongation and uniform strain decreased. An increased strengthening span which represented in low yield stress and a high ultimate tensile strength confirms the low Y/UTS ration of 0.55 to 0.565. This ratio reaches ~ 0.9 in many tempered and low carbon steels especially those having discontinuous yielding 10. The observed strengthening of DP-steel as a function of MVF can be attributed to two contradicting effects. The first is due to the presence of a hard martensite phase and increase of the tensile strength with increased MVF, and the second due to the carbon content decrease in the martensite with an increase of the volume fraction. As indicated before, reducing the carbon content in the martensite will reduce the structural tetragonality and therefore its strength i.e., the martensite intensity as a hard phase strongly depends on its carbon content. Therefore, the degree of martensite transformation effect on the ferrite grains is expected to be stronger the higher is the carbon content of the martensite. On the other hand, a higher martensite volume fraction increases the ferrite-martensite interface and subsequently increases the possibility of dislocations generation at the interface which affects the DP-steel yielding behavior. These dislocations are generated in order to accommodate the martensite volume expansion and are assumed to facilitate plastic flow. Since, these dislocations (at least partly) are mobile mainly at the early stage of strain and will contribute to work hardening. It has been also indicated 11 that during dual-steel deformation, geometrically necessary dislocations (GND) would be generated to maintain lattice continuity at interface and add to the statistically stored dislocations which are mainly due to dislocations interaction. For a constant MVF, for each of the

examined cooling rate, tensile results of tests in longitudinal, as shown in Fig. 3-a, b, indicated mainly a slight difference in strength values; however, a relatively important change in the total strain to fracture as well as in the homogenous strain is observed. This behavior can be attributed mainly to the martensite morphology, which is also observed to change with present differences in MVF with cooling rates. Moreover, a reduction in ductility is obtained in the case of fast cooling and can be related mainly to a higher dislocation density adjacent to the martensite areas. At a moderate rate of cooling (Table 2), ductility improves (Fig. 3) which has been attributed to a possible growth of epitaxial ferrite within austenite 12 likely to give a good combination of strength and ductility.
800
800

a)

600

DP3 DP2 DP1

Stress (MPa) and Strain (x 10 %)

700 600 500 400 300 200 100 0

Stress [MPa]

Yield stress Ultimate tensile stress Strain at fracture ( x 10 %)

400

200

10

20

30

DP1

DP2

DP3

Strain [%]
Fig. 3: Tensile properties of the processed dual phase steels.

The impact test was carried out on small standard specimens (2.5x10 mm), so that the results were recalculated to be comparable with the other results which carried out using the standard (10x10 mm) specimens. Fig. 4 includes the results of Charpy impact test. It is shown that the higher martensite content dual phase steel has a lower toughness compared to those with lower MVF. This result agrees with the results of the tensile curves shown in Fig. 3. DP1 steel which contains lower MVF has a combination of high strain at fracture with moderate strength; consequently, the area under curve up to fracture is larger.
270 Absorbed energy, [J] 250 230 210 190 -80
o

DP1 (120 C) DP2 (150 C)

o

DP3 (180 C)

-60

-40

-20
o

20

40

Test temperature [ C]

Fig. 4: Absorbed impact energy of the produced dual phase steels.

4. Conclusions: Based on the results of PD steel processing trials at the conditions of the current work it can be concluded that: 1- The experimental results of the investigation indicate that it is rather the cooling rates are responsible for microstructures changes than the measured coiling temperature. 2- Martensite phase strengthening effect depends on the delicate balance between martensite carbon content, volume fraction and morphology. 3- The impact toughness values of microstructures DP-steel are martensite volume dependent, and a superior toughness is obtained at lower martensite content. 5. References: [1] Prodromos Tsipouridis, Mechanical properties of Dual-Phase steel, Ph. D. (Dr.-Ing), Mnchen University 2006. [2] B. Krebs, A. Hazotte, L. Germain and M. Goune', Quantitive analysis of banded structures in dual-phase steel, Image Anal Stereol, 29 (2010) 85-90. [3] V. Tarigopula, O. S. Hopperstad, M. Langseth, A. H. Clausen and F. Hild, A study of localisation in dual phase high-strength steels under dynamic loading using digital image correlation and FE analysis, 45(2008) 601619. [4] N.K. Balliger, T. Gladman, Work Hardening of Dual-Phase Steels, Metal Science, 15 (1981) 95-108. [5] Denise M. Bruce, "Dynamic tensile testing of sheet steels & influence of strain rate on strengthenining mechanisoms in SFIEET steels, Ph. D. thesis, Colorado School of Mines, 2003. [6] H.K.D.H. Bhadedshia: Bainite in steel: Transformation, microstructure and Properties, 2nd edit, by IOM Communication Ltd, London, (1992). [7] Z. Nishiyama, Martensitic Transformation, edit. M. E. Fine et al., 13, 1978, New York, Academic Press [8] T. Sakak, K. Sugimoto, T. Fukuzato. Acta Metall. 46 (1983).1737. [9] .M. Rigsbee, J.K. Abranam, A.T. Davenport, J.E. Frankline, J.W. Pickens, JMS, N.Y(1979), 304-329. [10] Suleyman Gunduz , Mat. Sci. Eng. A488 (2008) 63-71. [11] J. Kadkodaponv,S. Schmander,D. Raabo,S. Ziaei-Rad, U. Weber, M. Calcagnotto, Act.Mat.59 (2011) 4387-4394. [12] F.B.Pickering. Constitution and properties of steel, Materials Science and Technology, 7 (1992) 77-79.