Author’s Accepted Manuscript

Increasing yield strength of medium Mn steel by

engineering multiple strengthening defects

B.B. He, B.M. Huang, S.H. He, Y. Qi, H.W. Yen,

M.X. Huang

www.elsevier.com/locate/msea

PII: S0921-5093(18)30424-6
DOI: https://doi.org/10.1016/j.msea.2018.03.065
Reference: MSA36258
To appear in: Materials Science & Engineering A
Received date: 1 February 2018
Revised date: 15 March 2018
Accepted date: 16 March 2018
Cite this article as: B.B. He, B.M. Huang, S.H. He, Y. Qi, H.W. Yen and M.X.
Huang, Increasing yield strength of medium Mn steel by engineering multiple
strengthening defects, Materials Science & Engineering A,
https://doi.org/10.1016/j.msea.2018.03.065
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 Increasing yield strength of medium Mn steel by engineering multiple strengthening

defects

B.B. He1, B.M. Huang2, S.H. He1, Y. Qi1, H.W. Yen2*, M.X. Huang1*

1
Department of Mechanical Engineering, The University of Hong Kong, Hong Kong, China;

2
Department of Materials Science and Engineering, National Taiwan University, Taipei 10617,

Taiwan

homeryen@ntu.edu.tw

mxhuang@hku.hk

*Corresponding authors. Tel: +85228597906, Fax: +85228585415.

Abstract

In general, medium Mn transformation-induced plasticity (TRIP) steels have a low yield strength

due to soft ferrite matrix. Here we provide a strategy to improve the yield strength of medium

Mn steels by coupling multiple strengthening defects in an austenite matrix. Such strengthening

defects include V-precipitates, intra-granular ferrite, forest dislocations and nano-twins.

Consequently, the present medium Mn steel has an ultra-high yield strength of 1350 MPa due to

the collective contribution from these strengthening defects. Moreover, the present medium Mn

steel demonstrates a good uniform elongation of 15%, which is ascribed to enhanced work

hardening behavior due to the operation of both TRIP effect and twinning-induced plasticity

(TWIP) effect.

Keywords: Medium Mn steel, TRIP, TWIP, Austenite, Precipitates

1
1. Introduction

High-performance steel with both high strength and high ductility is desirable for weight

reduction in automotive industry without sacrificing passenger safety [1, 2]. The quest for-high

performance properties leads to the development of medium Mn steels with a Mn content in the

range of 3~12wt.% [3-6]. In general, medium Mn steels have a dual phase microstructure of

ferrite and retained austenite. By optimizing the mechanical stability of retained austenite grains,

the medium Mn steels could have both high ultimate tensile stress (>1 GPa) and good tensile

ductility (>30%) [4]. This is because the transformation-induced plasticity (TRIP) effect in

retained austenite grains will enhance the work hardening behavior of medium Mn steels [4].

Moreover, twinning-induced plasticity (TWIP) effect could also be adopted in some medium Mn

steels due to the proper stacking fault energy (SFE) of retained austenite grains. The combined

TRIP and TWIP effects can lead to an enhanced work hardening behavior over a broad strain

regime, achieving an exceptional tensile ductility (>45%) in medium Mn steel [5, 7, 8].

Despite high tensile strength and excellent ductility, the medium Mn steels have a relatively low

yield strength (550~850MPa) [4, 5], which could be ascribed to the soft ferrite matrix after

intercritical annealing [9]. The yield strength of medium Mn steel can be increased by choosing

the hard martensite matrix through either quenching and partitioning (Q&P) process [10] or the

combined intercritical annealing and Q&P processes [11]. Consequently, the medium Mn steels

with martensite matrix have a high yield strength beyond 1 GPa [10, 11]. However, it is difficult

to achieve martensite microstructure in medium Mn steels with relatively high alloying elements

by simple quenching [8, 12]. It is worth to mention that the origin of high strength martensite

results from its multiple strengthening defects, including ultrafine grain size, high dislocation
2
density, and super-saturated C atoms [13-17]. In fact, any defects that can resist dislocation glide

will improve yield strength of metallic materials [18-20]. Therefore, it could be possible to

increase yield strength of medium Mn steel by incorporating multiple strengthening defects

without resorting to the high strength martensite.

In this paper, we propose to increase yield strength by combining multiple strengthening defects

in a single medium Mn steel. Such strengthening defects include solid solutes, dislocations,

precipitates, and nano-twins. Although this medium Mn steel has a dual-phase microstructure

with ferrite embedded in austenite matrix, the collective contribution from each strengthening

defects could make the yield strength beyond 1 GPa. Moreover, both TRIP effect and TWIP

effect can be employed to improve the ductility of present medium Mn steel.

2. Experiments

A medium Mn steel with a chemical composition of Fe-10Mn-0.47C-2Al-0.7V (in wt.%) is

employed for investigation. It is cast by forging and hot rolled to a final thickness of 4 mm. The

entry and exit temperatures of the hot rolling are 1050 and 800 oC respectively after the soaking

treatment at 1150 oC for 2 h. Then the present medium Mn steel is subjected to a thermal

mechanical process as schematically illustrated in Figure 1. Specifically, the hot rolled product is

rolled at 150 oC with a thickness reduction of 44%, followed by cold rolling with 7% thickness

reduction to the final thickness of 1.96 mm (Figure 1). The rolling at 150 oC is to introduce

mechanical twins in the austenite matrix. The sub-standard tensile samples with a gauge length

of 25 mm are wire cut from the rolled sheets along rolling direction. The tensile samples are then

subjected to intercritical annealing at 625 oC for 5 hours followed by water quenching (Figure 1).

3
The tensile tests are performed on a universal testing machine with a quasi-static strain rate of

5×10-4 s-1 at room temperature. The interrupted tensile tests are used to investigate the evolution

of microstructure during tensile tests. The electron backscattered diffraction (EBSD)

measurement is performed in Leo 1530 FEG SEM at 20 kV with a step size of 0.1 m and the

corresponding data is processed by HKL Channel 5. The EBSD sample is prepared by electro-

polishing using a solution of 25% perchloric acid and 75% ethanol (vol.%) at room temperature

after the mechanical polishing. The scanning electron microscopy (SEM) observation and

energy-dispersive X-ray spectroscopy (EDS) line measurement are carried out on the electro-

polished sample in the Leo 1530 FEG SEM at 5 kV and 20 kV, respectively. The X-ray

diffraction (XRD) tests were carried out on the electro-polished samples using a Cu Kα radiation

with wavelength 1.5405(6) Å for phase identification. The volume fraction of austenite is

estimated based on the integrated intensities of the diffraction reflections including the (2 0 0)α,

(2 1 1)α, (2 0 0)γ, (2 2 0)γ and (3 1 1)γ peaks. The high-resolution transmission electron

microscopy (HRTEM) observation is performed in an FEI Tecnai F20 at 200 kV. The TEM

sample is prepared by mechanically thinning down to 0.1 mm using SiC paper. The small discs

with a diameter of 3 mm are punched from the thin plate. Twin-jet is employed to perforate the

small discs utilizing a mixture of 5% perchloric acid and 95% ethanol (vol.%) at -30 oC with a

potential of 30 V.

3. Results

The present medium Mn steel has a bimodal grained microstructure with the large grains (~30

m) elongated the rolling direction and the small grains segregated at the boundaries of large

4
grains (Figure 2 (a)). The large grains are majorly austenite () phase while the small grains

consist of both austenite and ferrite () phases (white circle in Figure 2 (b)). An orientation

gradient is observed in most of the large austenite grains (Figure 2 (c)), suggesting a non-

recrystallized state of these large austenite grains. There are also some small ferrite grains within

the large austenite grains interior (white circle in Figure 2 (c) and (d)). The austenite volume

fraction in present medium Mn steel is estimated to be 80.8% according to the XRD profile

(Figure 2 (e)).

The small austenite and small ferrite grains segregated at the large austenite grain boundaries

have a submicron size (Figure 3 (b)). The ferrite grains (~70-250 nm) at the large austenite grain

interior could be even smaller (Figure 3 (c)-(d)). These ferrite grains are termed as the intra-

granular ferrite [12]. There is no apparent element partitioning of Mn/Al between the small

ferrite and small austenite grains (Figure 4 (a)). Similarly, such element partitioning is also

negligible between intra-granular ferrite and large austenite grain (Figure 4 (b)).

The mechanical twins can be observed in the large austenite grain (Figure 5 (a) and (b)). The

mechanical twins are formed during the rolling at 150 oC, and they are stable even after

annealing at 625 oC for 5 h. A significant amount of dislocations are also observed in the twinned

area of large austenite grain (Figure 5 (c)), suggesting a non-recrystallization state of these large

austenite grains, which is consistent with the observed orientation spread in Figure 2 (c). A large

number of V-precipitates (V4C3) with an average diameter of 18.4 nm are observed in the

austenite matrix (Figure 5 (d)). The orientation relationship between V-precipitate and austenite

matrix deviates from the conventional cube-on-cube orientation relationship [21] (Figure 5 (e)-

(f)).

5
The present medium Mn steel has a yield point phenomenon with a Lüders strain of 8% (Figure

6). The lower yield stress estimated to be 1350 MPa for present medium Mn steel. Such a high

yield strength is desirable to design automotive components such as the B pillar [1]. The

austenite volume fraction decreases with strains during the Lüders strain, and then it almost

saturates till fracture. (Figure 6).

The mechanical twins in present medium Mn steel after the tensile test has a single twinning

system (Figure 7 (a)-(b)). The amount of mechanical twins in the fractured sample is increased as

compared to the sample before the tensile test (Figure 5 (a)-(b)), suggesting the formation of

additional mechanical twins during the tensile test. In adjacent to the mechanical twins, some -

martensite with a width of a few nanometers could also be identified in the same austenite grain

(Figure 7 (d)-(f)).

4. Discussion

The present medium Mn steel has a dual phase microstructure with the small ferrite and small

austenite grains segregated at the large austenite grain boundaries and ultrafine intra-granular

ferrite grains at the large austenite grain interior (Figure 2). The large austenite grains serve as

the matrix of present medium Mn steel and therefore shall determine the macroscopic yield

strength. Despite of its coarse austenite grain size, the present steel has an ultra-high yield

strength of 1350 MPa, which is about 800 MPa higher than that of 5 Mn steel with ultrafine

ferrite matrix [4]. Moreover, it is even higher than some medium Mn steels with hard martensite

matrix produced by Q&P process [10]. Such a high yield strength of present medium Mn steel is

ascribed to the incorporation of multiple strengthening mechanisms, including precipitation

6
strengthening from both nano-sized intra-granular ferrites (Figure 3) and V-precipitates (Figure 5

(d)), coherent twin boundary strengthening (Figure 5 (a)-(b)), forest dislocation strengthening

from intensive dislocations (Figure 5 (c)), and solid solution strengthening from C/Mn/V solid

solutes. Therefore, the present work demonstrates that it is feasible to increase the yield strength

of medium Mn steel by incorporating multiple strengthening mechanisms without resorting to

the hard martensite.

In addition, the present medium Mn steel also has a proper uniform elongation of 15% (Figure 6),

which could be ascribed to the operation of both TRIP and TWIP effects during plastic

deformation. The austenite volume fraction decreases during the Lüders strain (Figure 6),

suggesting the operation of TRIP effect at this deformation regime. Such TRIP effect can result

from the formation of either ’-martensite or ɛ -martensite. The XRD diffraction profile suggests

that formation of ’-martensite dominates over the ɛ -martensite because no noticeable ɛ -

martensite peaks are detected in the fractured sample. The formation of martensite can provide

additional dislocation density [22] and dynamic strain partitioning [23], inducing the localized

work hardening to ensure the propagation of Lüders band without subjecting to fracture [24].

Such TRIP effect could be mainly from the large austenite grains due to their coarse grain size

(~30m) [25].

The strain hardening in present medium Mn steel is improved after the Lüders strain (Figure 6),

which could be due to the TWIP effect induced by the formation of mechanical twins (Figure 5

(a)-(b)). It is found that both grain size [26, 27] and SFE [28, 29] could affect the formation of

mechanical twins. Nevertheless, the SFE may play a more important role than the grain size in

determining the formation of mechanical twins [26]. The SFE can be estimated by the following

equation [28],
7
 SFE  2G   2 (1)

where ρ is the molar surface density along the austenite close-packed plane. ΔG→ is the molar

Gibbs energy of transformation → and  is the interfacial energy. The SFE depends on the

chemical composition and temperature [28]. The C content in austenite is a result of partitioning

and V-carbide precipitation, which are two competing processes. The carbon content in the

austenite can be calculated from the XRD profiles as below [30]:

a  a0  0.00453 X C  0.000095 X Mn  0.00056 X Al (2)

where XC, XMn and XAl are the element concentration (in wt.%) of C, Mn and Al in retained

austenite, respectively. a0=0.3556 nm is the theoretical austenite lattice parameter without any

alloying element at room temperature (~20 oC) [30]. a is the austenite lattice parameter that can

be calculated by the following equation:

a  dhkl  h2  k 2  l 2 (3)

where dhkl is the faulted inter-planar spacing at austenite reflections (hkl). h, k, and l are the

Miller indices. dhkl relates to the angular position (hkl) and the X-ray wavelength () as below:

dhkl   2sin hkl (4)

Since there is no evident element partitioning (Mn/Al) between ferrite and austenite (Figure 4),

the nominal concentration of Mn and Al elements is chosen for retained austenite grains.

Consequently, the average carbon content in austenite grains is estimated to be 0.62±0.05 (in

wt.%). The SFE of austenite is calculated to be 18.9 mJ m-2 at 300 K according to Eq.(1).

Therefore, the austenite in present medium Mn steel has an SFE within a regime (12 mJ m-2 ~ 35

8
mJ m-2 ) where the formation of mechanical twins could be favorable [28]. The mechanical twins

can dynamically refine the microstructure and efficiently accumulate dislocations at the

boundaries, increasing the flow stress and enhancing strain hardening [31]. In other words, the

TWIP effect resulted from the formation of mechanical twins is responsible for the strain

hardening of a strain regime beyond the Lüders strain.

The present medium Mn steel has better tensile properties than other high strength steels (Figure

8). For example, the present medium Mn steel has a yield strength which is much higher than

that of dual-phase (DP) steel while maintaining a comparable or even better uniform elongation.

The ultra-high yield strength of present medium Mn steel is ascribed to the multiple

strengthening defects while the proper ductility is due to the operation of TRIP and TWIP effects.

The present strategy in developing strong and ductile alloys could be a combination of recent

different strategies including nano-precipitates in ferritic steel [20], dislocations and mechanical

twins in nano-twinned steel [19] and the combined TRIP and TWIP effects in 10 pct Mn steel [5,

7, 8].

5. Conclusions

Here we provide a strategy to increase yield strength of medium Mn steel by assembling multiple

metallurgical strengthening defects, which are introduced by using conventional rolling and

annealing processes. These strengthening mechanisms include precipitation strengthening from

V-precipitates and intra-granular ferrite, forest dislocation strengthening and coherent twin

boundary strengthening. Consequently, the present medium Mn steel has an ultra-high yield

strength of 1350 MPa. It is expected that the present medium Mn steel is desirable for designing

9
automotive components where the yield strength is the major design criteria. Moreover, the

present medium Mn steel has a good ductility with a uniform elongation of 15%, which can be

ascribed to the operation of TRIP effect and TWIP effect during plastic deformation.

Acknowledgments:

M.X. Huang acknowledges the financial support from National Natural Science Foundation of

China (No. U1764252, U1560204) and Research Grants Council of Hong Kong (No. 17255016,

17203014, C7025-16G). H.W. Yen acknowledges the Ministry of Science and Technology of the

Republic of China for providing financial support under Contract MOST-104-2218-E-002-022-

MY3.

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11
Figures

Figure 1: Schematic illustration of thermal mechanical processing route employed in present

work. WR: warm rolling; CR: cold rolling; RT: room temperature.

12
Figure 2: (a) SEM image of present medium Mn steel. TD: transverse direction; RD: rolling

direction. White rectangle marks the region for EBSD measurement. (b) EBSD phase map of

present medium Mn steel. Austenite () is in yellow, and ferrite () is in red. The dashed circle

marks the segregation of small austenite and small ferrite grains. (c) The corresponding

orientation map of the present medium Mn steel. The dashed circle marks the ferrite grains at the

large austenite grain interior. (d) SEM image of the white circle in (c). (e) The XRD profile of

present medium Mn steel before the tensile test. The color images can be obtained in the online

version of this article.

Figure 3: (a) TEM image of the present steel. (b) The magnified view of the small ferrite and

small austenite grains close to large austenite grain boundary. (c) The bright-field TEM image

showing the distribution of ferrite at the austenite grain interior. (d) The bright-field TEM image
13
showing the intensive dislocations surrounding the intra-granular ferrite. Dashed circle

represents the area for diffraction pattern analysis.

Figure 4: (a) SEM-EDS line measurement across on the small ferrite and small austenite grains.

(b) SEM-EDS line measurement across on the intra-granular ferrite and large austenite grains.

The yellow lines in insets of (a) and (b) show the position of line measurement.

14
Figure 5: (a) The formation of mechanical twins in the austenite grain. Dashed circle represents

the area for the selected area diffraction pattern analysis. (b) The magnified view of the dashed

rectangle in (a). (c) The bright-field TEM image showing the high dislocation density in the large

austenite grain. (d) STEM image showing the distribution of V-carbide precipitates in large

austenite grain. The EDS mapping of V element from the white rectangle is shown in the corner.

(e) The high-resolution TEM image of V-carbide precipitate in austenite matrix. (f) The

corresponding FFT diffractogram from the region with white rectangular in (e) and the

information of diffraction spots. The color images can be obtained in the online version of this

article.

15
Figure 6: The engineering stress-strain curves of the present medium Mn steel. The austenite

volume fraction at different engineering strains is calculated based on the XRD measurement of

interrupted tensile samples.

Figure 7: (a) TEM bright field image showing the mechanical twins in the fractured sample. (b)

The corresponding dark-field image. (c) The diffraction pattern of mechanical twins and

austenitic matrix. (d) The high-resolution TEM image for ɛ -martensite layers (-M) and twin
16
plate (T) in the fractured sample. (e) The FFT image of the region with a dashed rectangle in (d)

and the detailed information of the diffraction spots of ɛ -martensite. (f) The schematic

illustration of diffraction spots for ɛ -martensite and austenite matrix.

Figure 8: Uniform elongation versus yield strength of present medium Mn steel compared with

other high strength steels, including dual phase (DP) steels [32-34], martensitic steels [35] and

TRIP steels [36, 37]. The lower yield strength is defined as the yield strength of present medium

Mn steel. Error bar represents the standard deviation of two tensile tests.

17