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Methodology to obtain the 1.7709 steel tempering diagram

Article · October 2017

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 Methodology to obtain the 1.7709 steel
tempering diagram.
S. Katsimardos1, D.G. Papageorgiou1,2, C. Medrea1, C. Stergiou1
1Dpt. of Mechanical Engineering, Piraeus University of Applied Sciences, 250 Thivon &
P. Ralli Ave. 12244 Egaleo-Athens, Greece
2Stassinopoulos-Uddeholm Steel Trading S.A., 20 Athinon Str. 18540 Piraeus, Greece

Tel: +40 2105381165, E-mail: stef.kats@hotmail.com, d.papageorgiou@uddeholm.gr,

stergiou@puas.gr, cmedrea@puas.gr

W. Nr 1.7709 is a special structural steel suitable for components resistant to high

temperatures. Under certain processing conditions it develops corrosion, heat, wear or
high-pressure resistance. Therefore, the specific material is selected for numerous
applications in the construction of ship, vehicle, airplane, guided missile and weapons,
pressure vessel, machine tools, and diverse mechanical components, usually supplied
after quenching and tempering. Tempering conditions depend on desired properties of
the finished products. Steel makers offer tempering diagrams where the hardness is
plotted as function of tempering temperature, for a nominal tempering time. Despite the
variety of applications, the tempering diagram of 1.7709 steel hasn’t been provided yet.
The aim of this paper is to establish a methodology that can be implemented for the plot
of the specific chart. Sufficient material was purchased, assuring identical chemical
composition of samples during experiment. Groups of ten specimens were subjected to
heat treatment sequence consisting of oil hardening and tempering at different
temperatures. Vickers hardness measurements were carried out and results were
statistically processed. Part of the tempering diagram was plotted and steel grade’s
resistance to tempering back was evaluated. Discussions regarding methodology were
presented and suggestions in order to assure diagram repeatability were provided. The
tempering diagram of steel is of great importance as it permits designers to acquire the
appropriate mechanical properties by choosing specific hardness value.

1. Introduction

W. Nr. 1.7709 is a high temperature, low alloy, structural steel suitable for working
temperatures up to 540°C [1, 2]. It belongs to the group of steels with specified high
temperature properties, described by the European standard BS EN 10269:2013 [3].
The steel can be found under equivalent grades as: 21CrMoV5-7 (DIN EN 10028-2,
DIN 17755), 20CDV5-07 (AFNOR), 25KH1MF (GOST). It is alloyed with chromium
(Cr), Molybdenum (Mo) and Vanadium (V). The presence of specific alloy elements
makes it corrosion resistant, heat resistant, wear resistant and high-pressure
resistant [4]. The material is mainly used in the steam industry (fasteners for high
temperature environments, manifolds and turbine parts), gas turbine industry
(turbofan discs) and in construction of apparatuses [1, 5]. Furthermore can be found
in a large number of applications in the field of ship, vehicle, airplane, guided missile,
weapons, railway, bridges, pressure vessel, machine tools, and mechanical
components with a bigger sectional size [6, 7]. Mostly, it is suitable in manufacturing
power generation turbine fasteners, boiler support rods, process plant fasteners,
mechanical gears, gear shaft, main axis, valve rods, mechanical parts, connecting
rods, screws, bolts, nuts, multi diameter shafts, pressure vessels, seamless pipes,
etc.
Steel makers recommend to be forged between 1100oC and 850oC, heat treated by
annealing between 650℃ and 730℃, stress relieved between 580oC and 650oC,
heated for hardening between 890 oC and 940 oC depending on cooling media (air or
oil), followed by tempering at temperatures depending on properties required
(usually between 680 oC and 720 oC). It has good weldability if suitable heat
treatment is applied after processing. Alloy structural steels are provided with higher
yield strength, tensile strength, fatigue strength, yield ratio, sufficient plasticity and
toughness. In order to cover ever-increasing requirements in material selection, an
adequate knowledge of the material properties as well as the working conditions
(pressure, temperature, dynamic operation conditions, corrosion level) are
mandatory. Commonly, the products manufactured of 1.7709 steel have high
strength at room and high temperatures, good creep resistance, high notch
tolerance, thermal expansion coefficients compatible with low alloy steel turbine
casing materials, lower design and operating risks, simplified design for bolting
configurations compared with other materials, proven performance in long-term
service. Particularly, its main mechanical properties could achieve: 700-850MPa
tensile strength (Rm), minimum 550MPa proof stress (R0,2), minimum 16%
longitudinal fracture elongation (ε), minimum 14 % tangential fracture elongation
(A5), 60% reduction in cross section on fracture (Z), minimum 31J of longitudinal
notch impact energy (KCV) at 20oC, minimum 24J tangential notch impact energy
(KCV) at 20oC, 275MPa fatigue resistance, 229HBW hardness after softening and
annealing (annealing to achieve carbides spheroidization) and 255HBW hardness
treated to improve shearability. Quenched in oil from 980°C and tempered at 690°C
will improve its properties. At ambient temperature can attributes 900MPa tensile
strength, 800MPa yield strength, and 150J/cm2 impact strength KCU, respectively.
Tested at 500°C retained high mechanical performances consisting of 700MPa, Rm,
650MPa, R0.2, and 110 J/cm2, KCU, and at 525°C 650MPa, Rm, 600MPa, R0.2, and
110 J/cm2 , KCU can be acquired [6].
The specific steel can be supplied in round, square and flat bars, plates and sheets,
tubes and pipes, rolled or forged, annealed or quenched and tempered [3,5].
Quenching and tempering are applied in order to increase steels toughness (Fig. 1).

Figure 1. TTT diagram showing continuous quenching and tempering of steels [8].
 Tempering is performed immediately after hardening, in order to reduce hardness.
The process consists of reheating the part to a temperature below the lower critical
point for a required period of time and then cooling it in air at room temperature.
Tempering conditions (temperature and time) are determined by the desired
mechanical properties of the finished product. Holding time of one or two hours at
tempering temperature is commonly used. Consequently, tempering temperature
has significant impact in mechanical properties of the finished products. Steel
makers and manufacturers give specific recommendations regarding the heat
treatment sequence. The tempering graphs provide significant information about the
heat treatment conditions that should be followed, for each material, in order to have
the anticipated results (Fig. 2). Tempering diagrams are one of the most important
tools in hardening practice. In fact, the hardness variation is plotted as function of
tempering temperature, for a predicted, nominal tempering time. The diagram is of
great practical value as it allows manufacturers to choose the tempering conditions
for predicted hardness (represents component’s mechanical behavior).

Figure 2. Tempering diagram of Sitherm 2344 steel [10].

Despite the wide range of application in hardened and tempered condition of 1.7709
steel, there is no tempering diagram provided. The purpose of this work was to
provide an experimental method that could be conducted in order to plot the
tempering chart of the specific steel.

2. EXPERIMENTAL DETAILS

The first objective was to purchase sufficient material, assuring identical chemical
composition of samples, during experiment. The material was mill certified according
to standards. Eight 8m long bars with 25.4mm diameter were delivered. Specimens
were accordingly prepared; firstly were machined to a final diameter of 23.0mm, and
then cut to samples of 25mm length. A special saw and a cutting machine type
“Struers Labotom – 3” were used. The specimens were properly marked for
identification. Their top and bottom flat surface were grinded using a “Presi Mecapol
P262” polishing machine using P220 abrasive paper. For statistical purposes,
groups of five (5) specimens were created using Minitab 17 randomization. Two
groups (ten specimens) were subjected to the same heat treatment sequence,
consisting of oil hardening under the same conditions and tempering at different
 temperatures for nominal time. Vickers hardness [10] and Rockwell hardness [11]
measurements were carried out. The results were statistically processed in
accordance to engineering practice [12]. Part of the tempering chart was plotted for
a low tempering temperature interval. Steel grade’s resistance to tempering back
was evaluated.

3. RESULTS AND DISCUSSIONS

The main aim of the research was to develop a methodology for the plot of the
specific tempering diagram. Practically, the tempering resistance of 1.7709 steel at
low temperatures, was thoroughly analysed. The success of the experiment could
have been affected from several factors. Setting up those factors properly in order to
eliminate any “external noise” from human errors is critical. A minor fluctuation on
material composition, of samples; within the standard limits, will affect their final
hardness. Consequently, a sufficient quantity of material was purchased from the
same manufacturer, with the additional requirement to be selected from the same
batch (the same casting process). In this way, it was assured that the derived
specimens will have the same chemical composition. The typical chemical
composition of the steel was provided by the certificate of the steelmaker (Table 1)
and was in compliance with Standards Specifications [13].

Table1. Chemical composition of 1.7709 steel (%)

Chemical
C Si Mn Ni P S Cr Mo V Al
Elements
Delivered
0.23 0.32 0.70 0.45 0.013 0.002 1.45 0.71 0.285 0.02
steel
Standard max max max. max max
0.17-0.25 0.4 - 0.8 1.2 - 1.5 0.55 - 0.8 0.2 - 0.35
specifications 0.4 0.6 0.03 0.03 0.03

Microstructure uniformity is another factor that could affect final hardness

measurements. Steel was delivered in bars of 25.4mm diameter. So in order to
eliminate possible dissimilarities induced during material processing (usually hot
rolling) or during transport and/or storage, the outer surface was removed by
machining the bars to 23.0mm diameter. A number of 170 specimens have been cut
to equal length of 25.0mm and numbered accordingly. The specimens were
randomised using Minitab 17; with the purpose of assuring real industrial conditions
as well as the actual hardness dispersion can be monitored.
Then, the hardening conditions were established. The suitability of quenching and
tempering sequence commonly depends on the steel grade and the predicted final
hardness. In order a representative tempering diagram to be plotted, it was essential
to determine the optimum quenching conditions. Using steelmaker’s specifications,
the nominal hardening conditions were selected; austenitizing at 960°C for 55
minutes and oil quenching. Full transformation of austenite to martensite can be
assured if uniform cooling in oil with a very fast cooling rate can be implemented.
The time interval for the quenching in oil was less than two seconds in every batch.
Two specimens from each group were randomly selected for HRC hardness
measurements, in order to validate the quenching process. The specimens were
tempered just after quenching as soon as the temperature reaches 500C. Each
batch was comprised of two groups of five pieces that were subjected to tempering
at different low temperatures; 180°C, 200°C, 225°C, 250°C and 275°C. All samples
were tempered for two hours (ten samples at each temperature) and then freely
 cooled in air at room temperature. Table 2 presents the specimens randomisation,
the groups treated and the tempering temperatures applied respectively.
Table 2. Randomization of the specimens using Minitab 17
(BOX) (BOX) (BOX) (BOX)
Tempering SAMPLES Tempering SAMPLES Tempering SAMPLES Tempering SAMPLES
Temperature Temperature Temperature Temperature

32 81 121 120
1 65 88 15
(1) (8) (12) (15)
93 165 5 76
200°C 250°C 180°C 275°C
40 56 115 116
31 167 143 159
52 133 29 4
148 150 49 30
(4) (10) (13) (16)
2 144 102 22
225°C 250°C 180°C 200°C
161 94 23 113
127 72 170 162
73 142 157
97 131 66
(6) (11) (14)
27 169 134
225°C 275°C 275°C
38 168 20
137 87 104

The specimens were thoroughly cleaned from the residuals of salt and polished with
abrasive paper P220 in accordance with standards. Vickers hardness
measurements (of 30 kP load) were carried out on the cross section of the samples.
Six imprints were marked on the top flat surface as shown in figure 3. The results
were statistically processed [12].

Figure 3. Samples cross section; schematics of hardness measurements points.

Table 3 shows the average value of the hardness measurements from all the
specimens of each temperature (60 values). Those results have been further
processed as to calculate the mean value and the standard deviation (S.D.) using
Minitab 17. As expected, there is no a significant decrease on the steel hardness.
By tempering the steel between 180oC and 275oC the diffusion rate is weak at low
temperature and the steel resists to tempering back. Furthermore, it was observed a
non-uniform distribution across the range of the results, in case of tempering at
 200°C and 225°C, respectively. It could be caused either by local non-
homogeneous chemical composition or either uneven microstructure. Although the
bars have the same alloy content, samples microstructure can vary enough affecting
the results. This could have been caused from impurities being penetrated during
the casting process.
Table 3. Average hardness variation in function tempering temperature
Tempering Initial Average
S.D.
temperature distribution HV30 value
180°C 352.09 – 474.25 401.82 29.27
200°C 347.70 – 578.80 435.47 59.39
225°C 356,26 – 618,28 430.23 42.77
250°C 365.76 – 474.75 389.31 16.16
275°C 365.76 – 503.20 402.27 28.72

Another factor is the transportation procedure as the material may experience local
strikes either during loading or unloading from the van or from human errors. As a
consequence, it is strongly suggested to repeat the sequence treatment of those
tempering temperatures, in order to obtain more uniform hardness values. The
other temperatures have a uniform distribution of the values.

Interval Plot of 180; 200; 225; 250; 275

95% CI for the Mean
440

430

420
Data

410

400

390

380
180 200 225 250 275

Individual standard deviations are used to calculate the intervals.

Figure 4. Tempering diagram of 1.7709 steel for low tempering temperature.

4. CONCLUSIONS

The main objective of the paper was to design and execute a methodology that can
be implemented for the plot of the tempering diagram of 1.7709 steel. For this
purpose material with the same chemical composition was purchased, specimens
were adequately processed and heat treatment sequence was designed. Two
groups of five samples were subjected to heat treatment sequence consisting of oil
hardening and tempering at low temperatures, between 180oC and 275oC. The
quenching process is critical to the acquired hardness of the specimens. The
specimens are tied together using cable wire in order to be quenched uniformly. Any
failure in hardening of the group will affect the reliability of the hardness
 measurements. Therefore, it is suggested to carefully select suitable wire and
thoroughly inspect the twisting mode of each group.
Vickers hardness measurements were carried out and results were statistically
processed. Part of the tempering diagram was plotted. High standard deviation
resulted for tempering at 200°C and 225°C. The procedure for those temperatures
has to be repeated so to determine more uniform hardness values. The main cause
for errors during the methodology or the heat treatment phase was human error
meaning that the methodology is reliable and fits for purpose for anyone willing to
continue populating the diagram using values at higher temperatures. The tempering
chart of steel is of great importance for the industry as it permits heat treatment
designers to choose the appropriate mechanical properties for a specific hardness
value.

Acknowledgments

The authors gratefully acknowledge N. Mastoridou from Ν. Bazigos S.A., for

supporting macrohardness HV30 measurements of the specimens.

References
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