Effect of high temperature tempering on the mechanical properties and microstructure

of the modified 410 martensitic stainless steel

Efendi Mabruri, Rahmat Ramadhan Pasaribu, Moh. Tri Sugandi, and Sunardi

Citation: AIP Conference Proceedings 1964, 020032 (2018); doi: 10.1063/1.5038314

View online: https://doi.org/10.1063/1.5038314
View Table of Contents: http://aip.scitation.org/toc/apc/1964/1
Published by the American Institute of Physics
 Effect of High Temperature Tempering on The Mechanical
Properties and Microstructure of The Modified 410
Martensitic Stainless Steel
Efendi Mabruri1,a), Rahmat Ramadhan Pasaribu2), Moh. Tri Sugandi2), Sunardi2)

1)
Research Center for Metallurgy and Materials, Indonesian Institute of Sciences (LIPI), Kawasan Puspiptek Gd.
470 Serpong, Tangerang Selatan, Indonesia
2)
Mechanical Engineering Department, Faculty of Engineering, University of Sultan Ageung Tirtayasa, Jl. Jenderal
Sudirman Km 03 Cilegon, Indonesia
a)
Corresponding author: effe004@lipi.go.id

Abstract. This paper reports the influence of high tempering temperature and holding time on the mechanical properties and
microstructure of the recently modified 410 martensitic stainless steel. The modified steel was prepared by induction melting
followed by hot forging, quenching and tempering. The hardness and tensile strength of the steels decreased with increasing
tempering temperature from 600 to 700 C and with increasing holding time from 1 to 6 h. Based on microstructural images, it
was observed the coarsening of lath martensite and of the metal carbides as well. However, a relatively high hardness and
strength were still exibited by this steel after tempering at a such high temperature of 600-700 C. The partition of Mo into the
carbides identified by EDS analysis may correlate with this situation.

INTRODUCTION

The martensitic stainless steels type 403/410 which is widely used for blade materials have been continuously
modified aiming to increase the service life of the steam turbine blades [1-6]. The modified steel is expected to have
higher resistance to environmentally assisted cracking due to severe conditions of the services of high stress and
corrosive environment [7-10]. Improving mechanical properties and corrosion resistance of the 13Cr type
martensitic stainless steels can be accomplished by chemical composition modification and heat treatment.
Recently, the modified 410 martensitic stainless steels have been developed with improved properties compared to
standard 410 martensitic stainless steels s [11-14]. The combination of Ni and Mo incorporated in the modified
steels in similar higher content (3 wt.%) is suggested to increase pitting resistance and toughness as well [11,14].
The heat treatment of the martensitic stainless steels is an important process to obtain the mechanical and
corrosion properties suitable for the technical requirements of the specific application. The proper practices of
quenching and tempering should be performed ensuring the suitable microstructure of the steels. Air cooling or oil
quenching this type steels from austenite phase results in microstructure consists of mainly hard and brittle
martensite, small amount of retained austenite, and may some carbides exist [15-16]. Subsequent tempering process
reduces hardness and increases ductility and toughness. High temperature tempering should be subjected to the
steels for steam turbine blade application to ensure stable microstructure during the services and maintaining
mechanical properties at an acceptable level. A suitable temperature and time of the tempering process should be
applied to achieve the desired properties that meet the technical requirements of the turbine blade materials. For this
reason, the investigation of high temperature tempering applied to the recently modified steel has been conducted.
This paper reports the influence of high tempering temperature and time on the mechanical properties and
microstructure of the steel.

Proceedings of the International Seminar on Metallurgy and Materials (ISMM2017)

AIP Conf. Proc. 1964, 020032-1–020032-6; https://doi.org/10.1063/1.5038314
Published by AIP Publishing. 978-0-7354-1669-7/$30.00

020032-1
 MATERIALS AND METHODS

The steel ingots were fabricated in an electric induction melting furnace and the chemical composition of the
steel is shown in Table 1 according to Optical Emission Spectrometer (OES) analysis. The ingots with dimension of
5 x 5 x 10 cm were forged at a high temperature of 1200 C several times until the dimension of the ingots decreased
to about 2 x 6 x 21 cm (about 50% reduction). The forged steels were machined to prepare the specimens. The steel
specimens were austenitized at temperatures of 1050 C for 1 h followed by oil quenching. The subsequent
tempering of the quenched steel specimens was performed at various temperatures of 600, 650 and 700 C for varied
time of 1, 3 and 6 h followed by air cooling. The heat treated steel specimens were surface ground to remove
oxidation scales. The hardness (HRC/Hardness of Rockwell C) of the steel samples was measured by diamond
indenter of 120 with indentation load and time of 15 Kgf and 3s, respectively. The tensile properties of the steels
were tested on the sub size specimens of ¼ in wide (ASTM 370) by using universal testing machine (Tinius Olsen)
until the specimen broke. The samples for microstructural observation were prepared by grinding with SiC abrasive
paper and polishing with alumina until 0.3 micron particle size. Etching of polished specimens was performed by
using Kalling reagent. The microstructure was observed and analyzed by optical microscope and JEOL Analytical
Scanning Electron Microscope (SEM)/Energy Dispersive Spectrocopy (EDS).

TABLE 1. Chemical composition of the modified 410 martensitic stainless steels prepared in this work (wt.%).
Steel C S P Mn Si Cr Mo Ni Fe

410-Mod. 0.10 0.005 0.02 0.61 0.24 12.73 2.52 2.93 Bal.

RESULTS AND DISCUSSION

The hardness of the modified 410 martensitic stainless steels as a function of high tempering temperature for
various holding time is presented in Fig.1. The marker indicates the hardness values from the measurement, while
the linier dot line indicates the trend line of the hardness values at respective time of tempering. The hardness of the
steels linearly decreases with increasing tempering temperature from 600 to 700 C for all holding times. The
hardness tends to decrease as well with increasing holding time from 1 to 6 h. The hardness values of the steels
range from 51 HRC for tempering at 600 C for 1 h to 41 HRC for tempering at 700 C for 6 h. These results
suggested that the modified steel can maintain high hardness at relatively high tempering temperature for relatively
long holding time. As a comparison, H. Sharifi et al [17] reported the hardness of DIN 1.4021 martensitic stainless
steel (equivalent to 410 martensitic stainless steels) went down to below 30 HRC at tempering temperature 700 C
for holding time 5 h. While, similar lower hardness ( 23 HRC) of the 410 martensitic stainless steel tempered at
temperature 650 C for holding time 1 h was reported by G. Chakraborty et al [18]. The higher hardness of the
modified 410 martensitic stainless steels compared to 410 martensitic stainless steels at relatively high tempering
temperature may correlate with the incorporation of Mo and Ni in the modified steel.
Figure 2 shows the tensile strength, yield strength and elongation of the modified 410 martensitic stainless steel
after tempering at various high temperatures and holding time. The tensile strength and yield strength of the
modified steels have a similar trend, their values decrease as temperature or holding time of tempering increases,
respectively. While, the elongation of the modified steel tend to increase with increasing temperature for holding
time 3 and 6 h, while it slightly decreases for holding time 1 h. The holding time at tempering temperature 700 C is
observed to have a little effect to the tensile strength of the modified steels. The tensile properties range from tensile
strength 1100 MPa and elongation 9% for tempering temperature/time of 600 C/1h to tensile strength 896 MPa and
elongation 13% for tempering temperature/time of 700 C/6h. Other researcher reported lower tensile strength of
858 MPa but with larger elongation 24% for the equivalent 410 martensitic stainless steels tempered at similar
temperature 700 C for shorter holding time 5 h [17]. Meanwhile, comparable results of strength and elongation at
tempering temperature 650 C also reported for 410 martensitic stainless steels with lower content Ni and Mo than
those for the modified steel in this work [6]. The comparable tensile properties of the 410 martensitic stainless steels
reported by the reseacher [6] even with lower Ni and Mo content than the modified steel in this work may be due to
the larger carbon content of the former of about 2 times (0.195 compared to 0.1 wt.%). As it is well known that the
mechanical strength of the steels increases with increasing of carbon content.

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 To investigate the correlation between mechanical properties and the phases contained in the modified steel in
high temperature tempered condition, the microstructure was observed for three steel samples tempered at 600 C
for 1 h, at 700 C for 1 h and at 700 C for 6 h, respectively. The optical microscope images for the microstructure of
the three steel samples are displayed in Fig.3. The microstructure of the three steels is observed consisting of lath
martensite, delta ferrite and carbides. The retained austenite may present within the area between the laths of
martensite. The lath martensite seems to increase in size with increasing tempering temperature from 600 (Fig. 3.a)
to 700 C (Fig.3.b) and with increasing holding time from 1 h (Fig.3.b) to 6 h (Fig.3.c) at 700 C. The delta ferrite in
the microstructure is characterized by island-like shape, with some of them are elongated as in the steel tempered at
600 C for 1 h (Fig. 3.a). At higher temperature and longer holding time, the delta ferrite changes to irregular shape
(Fig.3.c). It can be observed that the delta ferrite exists in a quite large fraction (qualitatively) of the microstructure.
This may be due to relatively high content of ferrite stabilizing element Mo (3 wt.%) added in the modified steel.
The addition of almost similar content of Ni in the modified steel does not eliminate the delta ferrite. The formation
of delta ferrite also reported by other researchers in the martensitic stainless steel containing 1 wt.% Mo and even in
steel with relatively lower content of Mo [19-20].

FIGURE 1. The hardness of the modified 410 martensitic stainless steel as a function of high tempering temperature for various
holding time.

(a) (b) (c)

FIGURE 2. (a) Tensile strength (b) yield strength and (c) elongation of the modified 410 martensitic stainless steel tempered at
various high temperatures and holding time.

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 (a) (b) (c)

FIGURE 3. Optical microscope images showing the microstructure of the modified 410 martensitic stainless steel tempered (a)
at 600 C for 1 h (b) at 700 C for 1h and (c) at 700C for 6 h.

(a) (b) (c)

FIGURE 4. SEM images showing the microstructure of the modified 410 martensitic stainless steel tempered (a) at 600 C for 1
h (b) at 700 C for 1h and (c) at 700 C for 6 h.

(a) (b) (c)

FIGURE 5. EDS spectrum for carbides in the modified 410 martensitic stainless steel tempered (a) at 600 C for 1 h (b) at 700
C for 1h and (c) at 700 C for 6 h.

In order to clearly observe the carbides in the modified steel, the SEM and EDS are used and the results are
presented in Fig. 4 and 5, respectively. The carbides are characterized by small white particles with the sizes
qualitatively increase with increasing tempering temperature and time as well. The EDS analysis of the carbides
(Fig. 5) shows dominantly Fe and Cr peaks with the composition of the carbides are similar among the three steels
samples, i.e. (Fe,Cr,Ni,Mo)23C6. The formation of stable carbide M23C6 in the high temperature tempering observed

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in this work agrees with the results reported by other researchers [4]. It is interesting to note that the peak intensity
of Mo in the EDS spectrum increases with increasing tempering temperature and holding time. The concentration of
Mo in the carbides increases from 0.99 wt.% in the steel tempered at 600 C for 1 h to 4.24 wt.% in the steel
tempered at 700 C for 6 h.
It is well known that tempering of martensitic stainless steel is conducted to facilitate relaxation of as-quenched
hard martensite and promotes precipitation of carbides. These processes are strongly related to diffusion of the
elements which is temperature and time dependance. At high temperature, the relaxation of the martensite may take
faster, the carbides transforms to stable M23C6 and coarsening of the structures may occurs, decreasing the hardness
of the steel to a low value. The decreasing of mechanical properties of the modified 410 martensitic stainless steels
with increasing of tempering temperature from 600 to 700 C and holding time from 1 to 6 h may correlate with
increasing size of lath martensite and coarsening of the carbides observed in this work. However, a relatively high
hardness and strength exibited by this steel after tempering at a such high temperature (600-700 C) and long
holding time may indicate additional structure strengthening. The partition of Mo into the carbides as well as in the
martensite as identified by EDS analysis may be responsible this strengthening. Other researchers investigated the
effect of Mo on the properties of high Mn steel and they reported that the sample containing Mo showed a higher
strength and ductility (elongation) compared with the sample containing no Mo [21].

CONCLUSION
The influence of high tempering temperature and holding time on the mechanical properties and microstructure
of the recently modified 410 martensitic stainless steel has been investigated. The hardness and tensile strength of
the steels decreased with increasing tempering temperature from 600 to 700 C and with increasing holding time
from 1 to 6 h. The hardness values of the steels ranged from 51 HRC for tempering at 600 C for 1 h to 41 HRC for
tempering at 700 C for 6 h. The tensile properties ranged from tensile strength 1100 MPa and elongation 9% for
tempering temperature/time of 600C/1h to tensile strength 896 MPa and elongation 13% for tempering
temperature/time of 700 C/6h. Based on microstructural images, increasing size of lath martensite and coarsening
of the carbides were observed. The concentration of Mo in the carbides increased from 0.99 wt.% in the steel
tempered at 600 C for 1 h to 4.24 wt.% in the steel tempered at 700 C for 6 h. The partition of Mo into the carbides
may be responsible for the modified steel maintaining the mechanical properties at a high temperature of 600-700
C.

ACKNOWLEDGEMENT

This work is a part of the research on the development of high temperature materials for power plants. The authors
thank to Indonesian Institute of Sciences (LIPI) for supporting this research through The Program of Excelence.

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