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Corrosion behavior of plastically deformed high-Mn austenitic steels

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 VOLUME 43
ISSUE 1
of Achievements in Materials November
and Manufacturing Engineering 2010

Corrosion behaviour of plastically

deformed high-Mn austenitic steels
A. Grajcar*, W. Krukiewicz, S. Kołodziej
Division of Constructional and Special Materials, Institute of Engineering Materials
and Biomaterials, ul. Konarskiego 18A, 44-100 Gliwice, Poland
* Corresponding author: E-mail adam.grajcar@polsl.pl
Received 12.09.2010; published in revised form 01.11.2010

Properties

Abstract
Purpose: The aim of the work was the comparison of corrosion resistance in an aqueous sulfuric acid
solution of two high-manganese austenitic steels of the 0.05C-25Mn-Al-Si-Nb-Ti type in a plastically
deformed state.
Design/methodology/approach: Investigations were carried out on specimens obtained from a thermo-
mechanically rolled sheet and then plastically deformed through bending and immersed in corrosive
solutions (1N H2SO4) for 100 hours. The mass decrement was calculated by the gravimetric method,
whereas the character of corrosion damages was observed in metallographic investigations using light and
scanning electron microscopes both in the polished and etched states.
Findings: It was found that after the thermo-mechanical processing one steel is characterized by an
austenitic structure with numerous annealing twins, whereas in the second steel lamellar martensitic phases
in an austenitic matrix occur. The investigations showed that the examined high-manganese steels have
very low corrosion resistance in normal H2SO4. Higher impact on the corrosion resistance than the phase
composition has the chemical composition. The mass decrement of the steel with martensite plates is a bit
higher than that with
a single-phase austenitic matrix. The specimens were intensively dissolved due to general corrosion
accompanying by pitting and hydrogen cracking.
Research limitations/implications: To investigate in more detail the corrosion behaviour of high-manganese
austenitic steels, the polarization tests and the analysis of corrosion products should be carried out.
Practical implications: The obtained results can be used for searching the appropriate way of improving
the corrosion resistance of high-strength high-manganese austenitic steels.
Originality/value: The corrosion resistance of two types of advanced high-manganese austenitic steels
with different initial structures was compared. Hydrogen impact in austenitic steels was discussed.
Keywords: Corrosion resistance; high-manganese steels; gravimetric method; pitting corrosion; general
corrosion; hydrogen cracking

Reference to this paper should be given in the following way:

A. Grajcar, W. Krukiewicz, S. Kołodziej, Corrosion behaviour of plastically deformed high-Mn austenitic steels,
Journal of Achievements in Materials and Manufacturing Engineering 43/1 (2010) 228-235.

228 Research paper © Copyright by International OCSCO World Press. All rights reserved. 2010
 Properties

1. Introduction
1. Introduction passivation, independently on the steel structure after heat treatment
(supersaturated, aged or strain-aged). Higher corrosion rate of
deformed specimens than that of specimens in supersaturated state,
High manganese steels with austenitic structure belong to a
was a result of faster steel dissolution caused by annealing twins,
group of advanced high strength steels for automotive industry [1].
which show a different potential than the matrix. The highest
Their particular beneficial connection of high strength, good
corrosion rate was observed in strain-aged samples, as a result of
plasticity and the ability to energy absorption of construction
ferrite formation, which creates a corrosive galvanic cell with the
elements with suitable cross-sections, are a result of the great
austenitic matrix [14].
susceptibility of J phase to plastic deformation during which Studies on the corrosion resistance of high-manganese steels are
dislocation glide, mechanical twinning or strain-induced martensitic confined to following alloy types: Fe-Mn, Fe-Mn-Al and Fe-Mn-
transformation can occur. Besides 15-30% Mn, high-manganese Al-Cr. There are no results concerning steels with increased silicon
steels include 0.03-1% C, 1-4% Si, 1-8% Al [1-5]. Mechanical content. Initial structural examinations of Fe-0.05-25Mn-3.5Si-
properties of these steels depend on structural processes occurring 1.6Al-Ti-Nb steel [6, 11] showed, that the austenitic matrix contains
during cold plastic deformation, which are highly dependent on
some fraction of martensite H with a lamellar shape.
SFE (Stacking Fault Energy) of austenite [3]. If it is from 12 to 20
The presence of martensite is a result of the decrease of austenite
mJm-2, a partial transformation of austenite into martensite occurs,
SFE, reached by adding Si and also, to some extent, Ti and Nb,
taking advantage of TRIP (TRansformation Induced Plasticity)
which are fixing carbon and nitrogen, resulting in a decrease of J
effect. Values of SFE equal from 20 to 60 mJm-2 determine intense
phase stability. It was preliminary found [15], that the presence of
course of mechanical twinning connected to TWIP effect
the second, lamellar phase, has a slight impact on the corrosion
(TWinning Induced Plasticity) [4]. Utilization of these phenomena
progress acceleration in acidic and chloride media, but it is the
allows to achieve mechanical properties of high-manganese steels
reason of local microcracks, spreading out usually from non-
in a wide range, i.e. YS0.2 = 250-400 MPa, UTS = 500-1000 MPa,
metallic inclusions. Taking it into account, the aim of the present
UEl = 30-70% [4-6].
work is to determine the influence of cold plastic deformation on
Up to now the mean area of studies on high manganese steels
corrosion behaviour of two steels with single-phase austenitic
was their high-temperature deformation resistance [2, 5-7] and
especially, the cold-working behaviour [1, 3, 4, 8, 9]. Less attention structure and containing some fraction of H martensite in aqueous
has been paid on the corrosion resistance of these steels [10-16]. In solution of sulphur acid.
the eighties of the last century, some investigations
[8, 9] on Fe-C-Mn-Al alloys for cryogenic application were carried
out in order to replace expensive Cr-Ni austenitic steels. The role of 2. Experimental
2. Experimental procedure
procedure
manganese boils to Ni replacement and obtaining austenitic
microstructure, whereas aluminium has a similar impact as Examinations were carried out on two high-manganese steels,
chromium. Performed studies [9] showed, that Fe-C-Mn-Al steels vacuum melted in the Institute for Ferrous Metallurgy in Gliwice.
show inferior corrosion resistance than Cr-Ni steels and they can be The chemical composition of the investigated steels is presented in
used as a substitute only in some applications. Zhang and Zhu [10] Table 1. The steels are characterized by similar C and Mn content.
reported that addition of 25% Mn to mild steel was very detrimental Significant impact on SFE of austenite has the difference in Al, Si
to the corrosion resistance in aqueous solutions. The Fe-25Mn alloy and Ti concentration. A lower SFE of 24.5Mn-3.5Si-1.5Al-Nb-Ti
was difficult to passivate, even in such neutral aqueous electrolytes steel compared to 26Mn-3Si-3Al-Nb-Ti steel is a result of the
as 1M Na2SO4 solution. They further reported, that the addition of higher Si and lower Al content. Moreover, much larger Ti content
5% Al to Fe-25Mn, results in forming of a stable passivation region in a first steel provides a decrease of J phase stability, as a result of
on the anodic polarization curves in Na2SO4 solution, but there is fixing the total nitrogen and a part of carbon [6].
still no passivation in 3.5% NaCl solution [10]. Low corrosion
resistance of high-manganese steels in chloride solutions was Table 1.
confirmed by our preliminary results of potentiodynamic tests on Chemical composition of the investigated steels
Fe-0.05C-25Mn-3.5Si-1.5Al steel [11].
Mass contents, (%)
Recently, corrosion resistance of Fe-0.05-29Mn-3.1Al-1.4Si Component
26Mn-3Si-3Al-Nb-Ti 24.5Mn-3.5Si-1.5Al-Nb-Ti
steel in acidic (0.1M H2SO4) and chloride containing (3.5% NaCl)
environments was investigated by Kannan et. al. [12]. Moreover, C 0.065 0.054
they compared the corrosion behaviour of the tested steel with IF- Mn 26.0 24.4
type (Intersitial-Free) steel. On the basis of gravimetric tests and Si 3.08 3.49
anodic polarization curves they found [12], that Fe-Mn-Al-Si steel Al 2.87 1.64
has lower corrosion resistance than the IF steel, both in acidic and P 0.004 0.004
chloride media. However, the corrosion resistance of high S 0.013 0.016
manganese steel in chloride solutions is considerably higher than in Nb 0.034 0.029
acidic solutions. Ti 0.009 0.075
Described results of corrosion tests concern steels in the N 0.0028 0.0039
annealed or supersaturated state. The influence of cold plastic O 0.0006 0.0006
deformation on behaviour of Fe-0.5C-29Mn-3.5Al-0.5Si steel in Initial structure [6, 15]
3.5% NaCl was studied by Ghayad et. al. [14]. They showed, on the J JHD’
basis of potentiodynamic tests, that the steel shows no tendency to

READING DIRECT: www.journalamme.org 229

 Journal of Achievements in Materials and Manufacturing Engineering Volume 43 Issue 1 November 2010

The material used for the investigation was delivered in a investigations were performed on LEICA MEF 4A light
form of segment of steel sheet with following dimensions microscope, with magnifications from 100 to 1000x.
340x225x3.2 mm, obtained after hot rolling using the thermo- Fractographic investigations were carried using scanning electron
mechanical treatment method. The thermo-mechanical processing microscope SUPRA 25 (Zeiss) at the accelerating voltage of
of studied steels consisted of: 20kV. In order to remove corrosion products, the specimens were
x heating of a charge up to the temperature of 1100°C and ultrasonically cleaned before the analysis. Confirmation of
austenitizing for 15 minutes, a phase structure of the investigated steels in the initial state was
x rolling of the charge in a temperature range from 1050°C to carried out by the X-ray phase analysis, what was reported
850°C, according to conditions in Table 2, elsewhere [6, 15].
x isothermal holding of a rolled sheet segments at the
temperature of finishing rolling for 15s,
3. Results
x solution heat treatment of the flat specimens in water. 3. Results
Table 2. The structures of the investigated steels after the thermo-
Rolling schedule for the flats with a thickness of 5.4 mm mechanical treatment are shown in Figs. 1 and 2. The 26Mn-3Si-
Pass Deformation Thickness Thickness Relative 3Al-Nb-Ti steel exhibits a homogeneous austenite structure
number temperature, before the after the reduction, with grains elongated in the rolling direction (RD) (Fig. 1). The
°C pass, mm pass, mm % susceptibility to twinning confirms the presence of a great number
1 1050 5.4 4.3 20 of annealing twins. The lower stacking fault energy of the
2 950 4.3 3.7 15 24.5Mn-3.5Si-1.5Al-Nb-Ti steel results in the presence of the
3 850 3.7 3.2 15 second phase with a lamellar shape, distributed in the austenite
matrix (Fig. 2). The X-ray diffraction analysis performed in
Taking into account the high deformation resistance during [6, 15] confirmed also the presence of H and D’ martensites,
hot-working [5-7], the relative reductions during rolling were confirming low stacking fault energy of the steel. Martensite D’
equal from 20 to 15%. In these conditions, the process controlling has also a lamellar shape and its unequivocal distinction from
the work hardening during the last rolling pass at a temperature of lamellas of Hphase is complicated. Usually, privileged places for
850°C was the dynamic recovery [5, 6]. The corrosion test results martensite D’ forming are crossings of H martensite lamellas
of investigated steels in the thermo-mechanically processed state [8, 16]. This matter will be the topic of future studies. In both
were described in [15]. In the current work, the corrosion steels, immersed after deformation in 1N H2SO4 many corrosion
resistance in a cold plastically-deformed state was investigated. pits of various size were observed (Fig. 3). The amount and the
Samples with a size of 10x15mm and a thickness between 3.1 and size of pits are very high and they are formed along entire surface
3.2 mm were plastically deformed in room temperature trough of the specimens. Privileged places to pits creation are
bending to an angle of 90°, with a bending radius of 3mm. Before concentrations of non-metallic inclusions, which are also probable
immersion into the corrosive solutions, the samples were ground place of hydrogen penetration. Hydrogen also penetrates deeper
to the 1000-grit finish, washed in distilled water and ultrasonically into the steel, accumulating usually in a surroundings of elongated
cleaned in acetone. Corrosion resistance of investigated steels was non-metallic sulfide inclusions (Fig. 4).
assessed using the gravimetric method, by immersing the samples
into 1N H2SO4 solution for 100 hours. Before the test, the
specimens were weighed with an accuracy of 0.01 g. The
temperature of the test was equal 23±1°C. After the test, the
samples were secondly weighed. The percentage mass decrement
was determined as follows:
mi  mf m
mp = ˜ 100% = d ˜ 100% (1)
mi mi

where: mp – percentage mass decrement [%], mi – initial mass [g],

mf – final mass [g], md – mass decrement [g].

The corrosion rate was calculated using following formula:

md
Vcor [g / m 2 day] (2)
S˜ t
where: Vcor – corrosion rate [g/m2 day], S – surface of a sample
[m2], t – time of the measurement [day], md – mass decrement [g].

Metallographic observations of non-metallic inclusions and

corrosion pits were carried out on polished sections, whereas the Fig. 1. Austenitic structure with annealing twins of 26Mn-3Si-
microstructure observations on specimens etched in nital. The 3Al-Nb-Ti steel in the initial state (transverse section)

230 Research paper A. Grajcar, W. Krukiewicz, S. Kołodziej

 Properties

Fig. 2. Austenitic structure containing lamellar martensite Fig. 4. Regions of hydrogen accumulation around elongated
plates, annealing twins and non-metallic inclusions of 24.5Mn- sulfide-type non-metallic inclusions in 24.5Mn-3.5Si-1.5Al-Nb-Ti
3.5Si-1.5Al-Nb-Ti steel in the initial state (transverse section) steel (transverse section)

Fig. 3. Wide corrosion pits on the surface of 26Mn-3Si-3Al-Nb-Ti Fig. 5. Elongated austenite grains of 26Mn-3Si-3Al-Nb-Ti steel
steel immersed in 1N H2SO4 and probable places of hydrogen after cold plastic deformation and some places of hydrogen
penetration (transverse section) accumulation (transverse section)

Hydrogen failures were usually observed to the depth of about Absorbed atomic hydrogen penetrating the steel, accumulates
0.3 mm. Places of hydrogen accumulation are also visible on in places with non-metallic inclusions, lamellar precipitations of
samples revealing the steel structure after cold plastic the second phase, microcracks and other structural defects, where
deformation. Usually, these places are elongated non-metallic convenient conditions for recombining of atomic hydrogen to
inclusions and grain boundary areas (Fig. 5). The 26Mn-3Si-3Al- molecular H2 exist. The recombination of atomic hydrogen to
Nb-Ti steel keeps after plastic deformation the austenitic molecular state is a very exothermic reaction, which provides
structure, whereas a fraction of martensite in 24.5Mn-3.5Si-1.5Al- a pressure increase in formed H2 bubbles as well as nucleation
Nb-Ti steel is increasing (Fig. 6). and growth of microcracks (Fig. 6) [17-19].
Besides non-metallic inclusions, especially privileged to The results of the gravimetric test in acidic medium are listed
hydrogen accumulation are lamellar areas of H martensite. in Table 3.

Corrosion behaviour of plastically deformed high-Mn austenitic steels 231

 Journal of Achievements in Materials and Manufacturing Engineering Volume 43 Issue 1 November 2010

Comparable mass decrement of two steels both in non-

deformed and plastically deformed states indicates that the
initial structure does not have any meaningful impact on the
corrosion progress, which is 838 and 1030 g/m2 day -
correspondingly for the single-phase steel and the steel
containing martensite plates.

Fig. 6. Regions of hydrogen failures and hydrogen microcracks in

24.5Mn-3.5Si-1.5Al-Nb-Ti steel, plastically deformed and
immersed in 1N H2SO4 (transverse section)

Table 3.
Results of gravimetric analysis for the specimens immersed in
1N H2SO4
26Mn-3Si-3Al-Nb-Ti Fig. 7. Deep corrosion decrements and banding-like arrangement
mi, g mf, g md, g Vcor, g/m2 day of corrosion products in 26Mn-3Si-3Al-Nb-Ti steel, plastically
deformed and immersed in 1N H2SO4
3.12 1.57 1.55 842.4
3.37 1.83 1.54 837.0
3.25 1.71 1.54 837.0
24.5Mn-3.5Si-1.5Al-Nb-Ti
mi, g mf, g md, g Vcor, g/m2 day
3.76 1.92 1.84 1000.0
3.82 2.03 1.79 972.8
3.91 1.85 2.06 1119.6

After cold plastic deformation and 100 hours immersion in 1N

H2SO4 both steels show a meaningful percentage mass decrement,
among 47 and 49% (Table 4).

Table 4.
Percentage mass decrement of non-deformed specimens [15] and
immersed in corrosion solutions after cold plastic deformation, %
Fig. 8. Cracked layer of corrosion products with banding-like
Before cold deformation [15] arrangement in 24.5Mn-3.5Si-1.5Al-Nb-Ti steel, plastically
26Mn-3Si-3Al-Nb-Ti 24.5Mn-3.5Si-1.5Al-Nb-Ti deformed and immersed in 1N H2SO4
38.4±5.2 41.3±9.6
After cold deformation Cold plastic deformation rises the mass decrement, in
comparison with specimens investigated in undeformed state
26Mn-3Si-3Al-Nb-Ti 24.5Mn-3.5Si-1.5Al-Nb-Ti (Table 4) [15]. The high rate of corrosion progress of high-
47.5±1.6 49.5±2.4 manganese steels in acidic solution is a result of hydrogen
depolarization mechanism.

232 Research paper A. Grajcar, W. Krukiewicz, S. Kołodziej

 Properties

4. Discussion
4. Discussion

The obtained results confirmed the low corrosion resistance of

high-manganese steels in acidic medium. The mass decrement in
1N H2SO4 is near 50% (Table 4) and is more than 2 times of
magnitude higher in comparison with samples investigated earlier
in chloride solution [15]. A similar order of magnitude of
corrosion progress was observed for Fe-0.05C-30Mn-3Al-1.4Si
steel by Kannan et. al. [12], which showed that the corrosion
current values in acidic solution are more than 2 orders of
magnitude higher than in chloride solution. The plastic
deformation enhances a higher corrosion rate compared to
undeformed specimens (Table 4) [15].
Big dissimilarities in corrosion resistance of examined steels
in different solutions are due to a different corrosion mechanism.
The big mass loss in H2SO4 solution is due to the hydrogen
depolarization progress. This is a process of reduction (in cathodic
areas) of hydrogen ions (from the electrolyte) by electrons (from
Fig. 9. Numerous craters formed due to corrosion pitting and the metal), to gaseous hydrogen, accelerating the corrosion
probable hydrogen penetration in 26Mn-3Si-3Al-Nb-Ti steel, progress [20, 21]. In this process numerous, wide and deep
plastically deformed and immersed in 1N H2SO4 corrosion pits are forming (Fig. 3). Especially intensive corrosion
pits form in places containing non-metallic inclusions, which are
A precise definition of the character of corrosion damages more resistant than the rest of material and foster potential
was possible on the basis of scanning electron microscope differences and galvanic cell creation. This causes the absorption
observations. It is characteristic that corrosion cracks were not of hydrogen ions, which due to increasing pressure and
observed, whereas deep corrosion damages and band arranged temperature, recombine to a gaseous form and get out of the metal
corrosion products were perceived (Fig. 7). The corrosion creating characteristic craters (Figs. 9, 10).
products layer is not continuous and has many cracks (Fig. 8). Hydrogen Induced Cracking (HIC) is a problem in carbon
steels and especially in high-strength low-alloy steels. Typical
examples are hydrogen failures of gas pipelines containing
hydrogen sulfite [17-22, 25]. Conventional Cr-Ni austenitic steels
are not usually liable to such damages. One of the reasons is
relatively low diffusion coefficient of hydrogen in austenite as
distinguished from steels with ferritic or martensitic structures
[23-25]. However, enhanced permeation of hydrogen was
observed in cold worked austenitic steels what was attributed to
strain-induced martensitic transformation leading to promote
hydrogen diffusion as the diffusivity is much higher in the bcc
martensite lattice [23]. Additionally, hydrogen mobility is
enhanced in the presence of high-dislocation density due to cold
working [26]. It is important to note that hydrogen impact occurs
both in diphase (Figs. 4, 6) and single phase (Figs. 9, 10)
structures of the steels. In the investigated high-manganese
austenitic steels a high corrosion rate (Table 3) and uncovering of
metal surface by formed successively corrosion pits (Fig. 3)
should be taken into account. Uncovered active metal inside of
expanding pits reacts with the acidic solution with hydrogen
Fig. 10. Craters created as a result of corrosion pitting and probable emission [21]. In this regard hydrogen impact can influence the
hydrogen accumulation and corrosion products residues in 26Mn- corrosion behaviour of the investigated high-manganese steels.
3Si-3Al-Nb-Ti steel after the immersion test in 1N H2SO4 Indirect confirmation of this fact are numerous craters formed due
to corrosion pitting and probably hydrogen impact (Figs. 9, 10).
Besides remaining corrosion products, a numerous number of The effect of hydrogen can be further enhanced by the presence of
craters, created due to corrosion pitting and probably as a result of increased sulphur concentration (for example present as sulfide
hydrogen impact, is characteristic. They are forming both in steel non-metallic inclusions) [21].
with martensite H lamellas and in steel with single-phase Craters forming is accompanied by local cracking of
austenitic structure (Fig. 9). Similar craters and corrosion products corrosion products layer (Figs. 7, 8), uncovering the metal surface
residues were observed in the specimens immersed in 1N H2SO4 - and causing further penetration of the corrosive medium and
not subjected to cold deformation (Fig. 10). finally the intensive progress of general corrosion. Corrosion
products show the characteristic layout consistent with the

Corrosion behaviour of plastically deformed high-Mn austenitic steels 233

 Journal of Achievements in Materials and Manufacturing Engineering Volume 43 Issue 1 November 2010

deformation direction (Fig. 7). Places of hydrogen accumulation accompanied by formation of corrosion pits;
are mostly the non-metallic inclusions, grain boundary areas and x the surface layer of band-arranged corrosion products located
martensite lamellas near sheet surface (Figs. 4-6). Recombination accordingly to the deformation direction has many cracks
of atomic hydrogen to the molecular state provides a pressure especially in surroundings of corrosion pits;
increase in formed H2 bubbles and creation of hydrogen cracks, x a higher mass decrement of 24.5Mn-3.5Si-1.5Al-Nb-Ti steel is
especially close to martensite plates of high hardness (Fig. 6) [15]. probably a result of the lower aluminum content compared to
The mass decrement in both steels is comparable (Table 4). 26Mn-3Si-3Al-Nb-Ti steel;
It concerns both non-deformed and cold deformed specimens. x identified craters are combined effect of various corrosion
It indicates, that martensite plates do not have any meaningful damages in high-manganese austenitic steels. Hydrogen
impact on the corrosion progress. This is probably due to the fact, impact is an additional effect accompanying general corrosion
that martensite H and D' are diffusionless products of austenite and corrosion pits forming. Its influence is enhanced by
transformation and have the same chemical composition like the numerous corrosion pits, sulfide non-metallic inclusions and
steel matrix. An acceleration of the corrosion progress occurs in martensite plates of high hardness.
steels with some ferrite fraction (with different chemical
composition than Jphase), formed during strain-aging of samples
which were previously plastically deformed [14]. Therefore, the References
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Corrosion behaviour of plastically deformed high-Mn austenitic steels 235

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