You are on page 1of 12

International Journal of Pressure Vessels and Piping 202 (2023) 104915

Contents lists available at ScienceDirect

International Journal of Pressure Vessels and Piping


journal homepage: www.elsevier.com/locate/ijpvp

Effects of various double-quenching treatments on the microstructure and


corrosion properties of D2 tool steel
Monireh Ahmadi a, Omid Mirzaee a, Maboobeh Azadi a, *, Hootan Biukani b
a
Faculty of Materials and Metallurgical Engineering, Semnan University, Semnan, P, .O. Box: 35131-19111, Iran
b
Department of Ceramics, Materials and Energy Research Center, Karaj, P, .O. Box: 35131-19111, Iran

A R T I C L E I N F O A B S T R A C T

Keywords: The purpose of this paper is to study the effects of the various double-quenching treatments on the microstructure
D2 tool steel and corrosion properties of D2 tool steel. The percentage and the size of carbides and the phase types were
Double-quenching parameters that affected the properties of various specimens. Both optical and field emission scanning electron
Corrosion behavior
microscopy were used to study the specimen microstructure. Moreover, the Tafel polarization, electrochemical
0.6 M NaCl Solution
Microstructure
impedance spectroscopy, and weight loss tests were evaluated to investigate the corrosion behavior. The ob­
tained results showed that the martensite and tempered martensite phases exhibited the highest and lowest
corrosion rates in 0.6 M NaCl solution, respectively. A Higher percentage of (Cr, Fe)7C3 carbides with a higher
size also caused an increase in the corrosion resistance up to 91.2%. The lowest corrosion rate after 96 h was also
related to tempered specimens.

1. Introduction complex carbide in 0.3% NaCl solution. They reported that such coating
increased the corrosion resistance of the utilized tool steel. Egert et al.
D2 tool steel is a high carbon and chromium alloy steel that has [10] studied the properties of D2 Tool steel after cryo-treatment. The
excellent wear resistance based on the large volumes of carbides. It is obtained results showed that this treatment did not change the average
widely used in cold work applications requiring high wear resistance measured properties. Das et al. [11,12] investigated the microstructure
and compression strength. Therefore, it can be used in various tools such and the hardness of AISI D2 tool steel under sub-zero treatments. They
as pipes, punches, slitting cutters, forming die, spinning tools, blanking studied the effect of the time of cryogenic processing on the wear
dies, piercing, and shear blades [1–3]. However, there are many efforts properties of steel. In addition, they found that deep cryogenic treatment
to apply various heat treatments and other surface treatments to of D2 steel decrease the content of retained austenite [13,14] and caused
improve mechanical and chemical properties of this steel [4–7]. In the the refinement of carbide precipitates [15]. Moreover, Amini et al. [16]
following paragraph, some of these investigations are reviewed. found that the deep cryogenic treatment eliminated the retained
Diaz-Guillen et al. [1] studied the electrochemical property of austenite phases and precipitated the nano-sized carbides in the D2 tool
plasma-nitrided AISI D2 tool steel surfaces in a chloride ion-rich solu­ steel. Voglar et al. [17] studied the influence of the deep cryogenic
tion. Steels were quenched and tempered at 200 ◦ C. Their results showed treatment on the corrosion characteristics of various high-speed sheets
that the plasma treatment was an effective parameter for a reduction in of steel. It was reported that when the heat treatment caused the ho­
corrosion rate. Erdogan et al. [6] investigated the corrosion behavior of mogeneous distribution of precipitated carbides in the matrix, an in­
the borided cold work tool steel in a 4% M HCl acid solution. They crease in corrosion resistivity for treated specimens would be observed.
showed that the cryogenic treatment was beneficial to increase corro­ Consequently, although the mechanical and wear resistance of D2
sion resistance. Chen et al. [8] studied the corrosion property of tool steel is high, corrosive operation environments and severe operating
TiN-coated AISI D2 steel in 5% NaCl solution and 20% H3PO3 solution. conditions affect the lifetime of this type of steel. Therefore, in the
Their results demonstrate that the corrosion rate of coated specimens present paper, various double-quenching heat treatments were done on
decreased compared to AISI D2 steel as substrates. Castillejo et al. [9] D2 tool steel to establish the optimal heat treatment conditions. Then,
investigated the corrosion behavior of AISI D2 steel coated by Nb–Cr the corrosion properties of heat-treated specimens have investigated

* Corresponding author.
E-mail address: m.azadi@semnan.ac.ir (M. Azadi).

https://doi.org/10.1016/j.ijpvp.2023.104915
Received 31 December 2022; Received in revised form 1 February 2023; Accepted 6 February 2023
Available online 14 February 2023
0308-0161/© 2023 Elsevier Ltd. All rights reserved.
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Table 1
Details of the chemical composition of utilized material (D2 tool steel) in % wt.
C Cr V Mo Si Ni Mn Cu Co W Al Fe

1.48 11.50 0.85 0.82 0.35 0.32 0.23 0.12 0.07 0.06 0.02 Bal.

all heat-treated specimens contained preheating at 700 ◦ C for 10 min


Table 2
and then heating at 1030 ◦ C for 40 min. Such a treatment was also re­
Details of heat treatments (step 2) and the broadcast microstructure for various
ported in other research [18]. In addition, details of heat treatment (step
specimens based on the TTT diagram [19].
2) for all specimens are reported in Table 2. Besides, the broadcast
Specimens Heat treatment (Step 2) Broadcast microstructure microstructure for various specimens is also reported based on the TTT
name
diagram [19]. It was notable that the temperature for martensite for­
M − 12 m Oil quenching at 250 ◦ C for 12 min Tempered martensite + mation was about 200 ◦ C.
and air quenching, heating at 500 ◦ C Carbide
For representing better details of various heat treatments, the sche­
for 60 min, and air quenching
M-M-12 m Oil quenching at 150 ◦ C for 12 min Martensite + Low matic of the heat treatment procedure for all specimens is shown in
and air quenching retained austenite + Fig. 1. It was notable that the dimension of specimens that were heat-
Carbide treated for all tests was 25 × 5 mm (diameter × height). After the
T-500 Oil quenching at 25 ◦ C, heating at Tempered martensite + heat treatment, all samples were ground up to 2000 grit and polished
500 ◦ C for 60 min, and air quenching Carbide
A-120 m Oil quenching at 250 ◦ C for 120 min Bainite + Carbide +
using alumina suspension. Specimens were etched by an etchant that
and air quenching Martensite contained 10 mL nitric acid and 90 mL ethanol (10% Nital solution).
A-270 m Oil quenching at 250 ◦ C for 270 min Bainite + Carbide Both optical microscopy (OM-Olympus) and field emission scanning
and air quenching electron microscopy (FESEM-Mira TESCAN) were used for microstruc­
tural evaluations. An Image J software was also utilized to analyze the
carbide content and size through OM images. In addition, the FESEM
through Tafel polarization, electrochemical impedance spectroscopy,
device was equipped with energy-dispersive X-ray spectroscopy (EDS).
and weight loss tests in 0.6 M NaCl solution. Such a solution contained
The EDS was carried out at a voltage of 20 kV.
3.5% wt NaCl as a simulated seawater based on ASTM D1141–98. It was
X-ray diffraction (XRD-Bruker D8) analysis was also performed to
notable that enhancing the corrosion resistance of D2 tool steel in a
detect present phases in various specimens. An emitting monochromatic
chloride ion-rich solution like in marine solution was a challenge for
radiation Kα of copper was used. The range of scanned angle (2θ) was 10
various industries since this steel exhibits medium chromium content
to 90◦ with a step of 0.02◦ .
that gives it mild corrosion-resisting properties in free chloride ions.
Electrochemical tests were performed in a chloride ion-rich medium
Moreover, microstructure and phase detection of specimens were stud­
(0.6 M NaCl solution) by using the potentiodynamic polarization tech­
ied by optical microscopy, field emission scanning electron microscopy,
nique. The test sample acted as a working electrode (with an area of 1
and X-ray diffraction, respectively. Finally, the relation of carbide
cm2) based on ASTM G5. A calomel electrode was utilized as a reference,
properties with the corrosion resistance of this alloy was investigated in
and a platinum sheet as a counter electrode. The test temperature was
detail.
about 25 ◦ C. Specimens were immersed in the corrosive solution for 30
min to reach the stable potential. In Tafel polarization tests, the voltage
2. Materials and experiments
scan rate was 1 mV/s. The applied DC voltage was about ±250 mV
around the open circuit potential (OCP). For electrochemical impedance
The utilized steel as a substrate in this paper was D2 tool steel.
spectroscopy (EIS) tests, the range of frequency was from 100 kHz to
Table 1 shows details of the chemical composition of this steel. This
0.01 Hz by applying an AC voltage of ±10 mV around the OCP.
report was based on optical emission spectrometry measurements.
For weight loss tests to measure the corrosion rate, specimens were
Various double-quenching heat treatments were performed through
immersed in 0.6 M NaCl solution for 1–96 h at 25 ◦ C. Specimens were
austenitizing and aging processes. The austenitizing process (step 1) for
weighed before and after the immersion time. Then, the weight loss was

Fig. 1. Schematics of heat treatment procedure for all specimens.

2
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 2. OM images of specimens etched in 10% Nital solution, containing (a) B, (b) M-12 m, (c) M-M-12 m, (d) T-500 (e) A-120 m, and (f) A-270 m

reported to show the effect of a long time on the corrosion properties of also reported in other studies [2,20,21]. The chromium carbides were
specimens. It was notable that Tafel polarization and EIS methods as shown in white-colored areas and they were distributed in grain and
electrochemical methods and the weight loss test as a chemical method grain boundaries of the α-ferrite phase. However, grain boundaries were
were utilized for measuring the corrosion properties of D2 tool steel. not seen obviously. The black-colored area would be attributed to
non-metallics such as the sulfur phase.
For heat-treated specimens, black-colored spots also appeared in the
2.1. Microstructure evaluations OM images, which were most likely non-metallic inclusions. Similar
behavior was also reported in other research [17].
2.1.1. OM images The microstructure of both specimens T-500 and M-12 m contained
Fig. 2 shows OM images of all specimens. The microstructure of the the tempered martensite as a matrix and (Cr, Fe)7C3 carbides. However,
blank specimen (B) without any heat treatment contained α-ferrite the content of retained austenite and carbides phase could be changed
(α-Fe) and (Fe, Cr)7C3 carbides. The coarse carbides with a size of 40 μm for these specimens. A similar microstructure for the tempered
were distributed in a ferrite matrix. However, the mean size of small martensite phase was also found in other research [22,23].
carbides was about 2 μm. A similar microstructure for D2 tool steel was

3
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Table 3 For specimen M-M-12 m, the chromium carbides were distributed in


The mean carbide size and percentage for specimens. the martensite matrix. However, for better details of the martensite
Specimens name Mean carbide size (μm) Carbide content (%) phase, images with a higher magnification (higher than 1000×) would
be needed [18]. The microstructure of both specimens A-120 m and
B 15.1 ± 2.0 39.2 ± 2.5
M − 12 m 20.2 ± 2.0 31.0 ± 2.5 A-270 m included the bainite phase and carbides. In addition, specimen
M-M-12 m 10.1 ± 2.0 19.4 ± 2.5 A-120 m contained some martensite phase. Notably, since the matrix of
T-500 25.9 ± 2.0 35.6 ± 2.5 specimens was not obvious through OM images, the phase of matrix
A-120 m 15.3 ± 2.0 24.4 ± 2.5 were based on the data in Table 2 and similar references.
A-270 m 20.5 ± 2.0 36.3 ± 2.5
For more details, the percentage and the size of carbides were
measured through Image J software and reported in Table 3. The highest
and lowest percentage of carbides was related to specimens B and M-M-
12, respectively. The highest and lowest values of carbide content were

Fig. 3. FESEM images of specimens that were etched in 10% Nital solution, containing (a) B, (b) M-12 m, (c) M-M-12 m, (d) T-500 (e) A-120 m, and (f) A-270 m

4
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 4. EDS results of from the surface of specimens containing; (a) B, (b) M-M-12 m, and (c) A-270 m

39.2 and 19.4%, respectively. It was reported that the D2 tool steel had martensite phase. Similar behavior was also found in other research [10,
carbides more than 25% [24]. In addition, it was found that the carbide 17]. Specimens A-120 m and A-270 m also showed a microstructure
content would be increased after the cryogenic treatment [16]. The containing the bainite phase and carbides. Notably, other techniques,
highest and lowest size of carbides was attributed to specimens T-500 such as transmission electron microscopy (TEM) could show obvious
and M-M-12, respectively. Totally, changes in the percentage and the images in higher magnification to present various matrixes. Such
size of carbides would affect the properties of specimens. Consequently, investigation would be done in future studies.
it was reported that the size, amount, and distribution of the primary
carbides with the chemical composition of M7C3 were affected by the
type of heat treatment, the time, and the temperature of austenitizing 2.2. EDS results
step [11,12,15].
Fig. 4 shows the EDS results of various specimens including, B, M-M-
2.1.2. FESEM images 12 m, and A-270 m. The place of EDS analysis was specified on the
The microstructure of samples was also examined through FESEM related FESEM images in Fig. 3. It could be concluded that the carbides
images to get more details. Fig. 4 shows FESEM images of various were chromium carbides. The chromium percentage for specimen M-M-
specimens. All specimens contained a non-dissolved carbide phase 12 m was lower than others. This result was consistent with the results
observed in the black-colored areas. In addition, there was some small reported in Table 3. In addition, molybdenum and chromium percent­
white-colored area that was related to the inclusions. Although, it was ages for the specimen without treatment were also the highest among
notable that for specimen M-M-12 m, the light-colored area would be others. Moreover, similar EDS results for D2 tool steel without treatment
attributed to the retained austenite phase and the matrix was the were also found in other research [25].
Fig. 5 displays the EDS mapping results of various heat-treated

5
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 5. EDS mapping results of Cr, C, and Mo elements for three specimens; including (a) M-12 m, (b) T-500, and (c) A-120 m

specimens including, M-12 m, T-500, and A-120 m. It was found that the of (420), (202), (421), (402), (440), (203), (603) and (705) [13,15,26].
precipitates in the matrix were chromium carbides. Based on Fig. 5 (b), It was found that the martensite phase (PDF 00-076-0747) exhibited
the carbide content for specimen T-500 was the highest among others. peaks at various planes containing (110), (200), (211), (220), and (310)
This observation was consistent with the results reported in Table 3. The [14,21,27]. However, the three main planes were (110), (200), and
molybdenum element was dissolved in the iron matrix homogeneously (211), as shown in Fig. 6 (c). The martensite phase showed the highest
since the crystal structure for this element was body-centered cubic peak at 44.7◦ at the plane of (110) [10,16].
(BCC). Moreover, it could be reacted to carbon and form carbides when The ferrite phase (PDF 00-006–0696 and PDF 00-034-0396) could be
the amount of it was high [13]. detected in degrees of 44.3, 64.1, and 82.1◦ [1].
For both specimens M-12 m and T-500, three small peaks were found
in the range of 42 to 48◦ . These peaks were also related to the M3C
2.3. XRD carbides. The chemical composition of these carbides was Fe3C (PDF 01-
089-2005) [16,28]. Their planes were (201), (211), and (221). These
Since the matrix of specimens in the presented images was not carbides would be formed in the heating process during the tempering
obvious, XRD was used to detect phases in each specimen. Fig. 3 shows process. For specimen M-M-12 m, small peaks were also attributed to the
XRD patterns for all samples. All specimens contained chromium carbide retained austenite phase. A similar XRD pattern was also found for the
(Fe, Cr)7C3 (PDF 00-036-1482)with an orthorhombic crystal structure. A retained austenite phase in other research [8].
similar result was also reported in other research [2,5,11,20]. It was
notable that the M7C3 phase (M = Fe, Cr, V, Mo) showed peaks at planes

6
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 6. XRD partterns for all specimens, containing, (a) B, (b) M-12 m, (c) M-M-12 m, (d) T-500, (e) A-120 m, and, (f) A-270 m

2.4. Electrochemical tests values over the immersion time decreased it could be indicated that the
passive film on the substrate surface was not formed [29].
2.4.1. Tafel polarization Plots of Tafel polarization test results for specimens are depicted in
Fig. 7 shows the plot of OCP versus the immersion time in 0.6 M NaCl Fig. 8. In addition, Table 4 summarizes the data extracted from Tafel
solution for two specimens. This plot demonstrates that the OCP reached polarization measurements. The range of corrosion potential (Ecorr) for
a fixed value after 15 min immersion in the corrosive solution. In all specimens was about − 560 to − 640 mV. Thus, changes in the value
addition, the passive film in open circuit condition was not formed in of Ecorr were insignificant for all heat-treated specimens. The Ecorr and
0.6 M NaCl solution for these specimens. It was found that when the OPC corrosion current density (Icorr) for the specimen without any heat

7
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 7. The plot of OCP versus the immersion time in 0.6 M NaCl solution.

Fig. 8. Plots of Tafel polarization test results for specimens in 0.6 M Fig. 9. Plots of (a) Bode and (b) phase angle (EIS tests results) for specimens in
NaCl solution. 0.6 M NaCl solution.

concluded that the martensite phase showed the highest corrosion rate
Table 4
Measurements of Tafel polarization data for specimens in 0.6 M NaCl solution.
with respect to other phases such as bainite, tempered martensite, and
ferrite phases. It was found that the martensite phase was unstable and
Specimens βc (mV/ βa (mV/ Ecorr Icorr (μA/ %R
exhibited higher energy compared to other phases. Thus, this phase
name decade) decade) (mV) cm2)
needed lower energy for corrosion reactions [30]. Moreover, the size
B − 104.2 103.3 − 560.3 23.94 – and the content of carbide phases affected the corrosion rate of speci­
M − 12 m − 91.1 170.8 − 619.8 1.800 − 92.5
M-M-12 m − 65.8 151.3 − 577.4 84.120 +71.5
mens. Specimens with a lower size and a lower percentage of carbides
T-500 − 84.6 56.1 − 640.3 0.002 − 99.9 exhibited a higher corrosion rate. Therefore, the highest corrosion rate
A-120 m − 35.1 122.2 − 576.4 29.917 +19.9 with a value of 84.120 μA/cm2 was related to specimen M-M-12 m with
A-270 m − 109.6 99.1 − 597.2 0.005 − 99.8 the lowest carbide size (10.1 μm) and the lowest carbide content
(19.4%). However, the lowest corrosion rate was attributed to specimen
treatment were about − 560.3 mV and 23.94 μA/cm2, respectively. It T-500 with a value of 0.002 μA/cm2. This specimen contained tempered
was reported the Ecorr and Icorr in 5% NaCl solution were about − 866 mV martensite as the main phase with the highest carbide size (25.9 μm). It
and 64.55 μA/cm2 for D2 tool steel [8]. In addition, it was found that the was found that carbide precipitates as a ceramic phase showed a lower
Ecorr and Icorr in 3% NaCl solution were about − 807 mV and 1.19 μA/cm2 tendency for dissolution compared to other phases in specimens [4,29,
[5]. Notably, the R values in Table 4 show the difference in the corrosion 31]. In this situation, by the formation of higher content of carbides, the
rate of heat-treated specimens compared to the corrosion rate of the activity of the metallic matrix would be decreased for anodic dissolution
specimen without any treatment. Corrosion rates for specimens M − 12 and the corrosion rate would be reduced. Table 4 shows that changes in
m, T-500, and A-270 m were reduced to higher than 92% compared to the anodic Tafel slopes (βa) were more than in the cathodic Tafel slopes
the blank specimen. However, an increase in the Icorr value for speci­ (βc). This demonstrated that the anodic reaction was affected signifi­
mens M-M-12 m and A-120 m has happened. Based on changes in the cantly compared to the cathodic reaction. The cathodic reaction was
microstructure, such behavior was observed. Totally, it could be oxygen reduction (O2+ H2O+ 4e− = 4OH− ). The metal dissolution was
also the anodic reaction. Moreover, the passivation region did not also

8
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 10. Suggested electrical circuit for EIS data for all specimens. Fig. 11. Plots of weight loss versus the immersion time for all specimens in 0.6
M NaCl solution.

Table 5
Measurements of EIS data for all specimens in 0.6 M NaCl solution. Table 6
Specimens name Rs (Ω cm2) CPEdl (F/cm2) n Rp (Ωcm2) %R Extracted data from Plots of weight loss versus the immersion.

B 22.37 1.19 × 10-4 0.82 1024 – Specimens name Linear equation R2 %R after 96 h
M-12 m 28.69 2.99 × 10-5 0.89 1933 +47.0 B ΔW = 8 E-05t + 0.0016 0.95 –
M-M-12 m 20.21 3.19 × 10-3 0.79 151 − 85.1 M-12 m ΔW = 7 E-05t + 0.0012 0.94 − 13.8
T-500 43.21 4.01 × 10-9 0.98 11,595 +91.2 M-M-12 m ΔW = 9 E-05t + 0.002 0.96 +14.7
A-120 m 25.39 6.63 × 10-4 0.72 1003 − 2.1 T-500 ΔW = 3E-05 t + 0.0011 0.87 − 55.2
A-270 m 43.32 2.01 × 10-8 0.96 10,756 +90.4 A-120 m ΔW = 8E-05 t + 0.0015 0.94 +2.2
A-270 m ΔW = 5 E-05t + 0.0012 0.94 − 32.2

observed for this corrosive solution at this applied potential for this
alloy. Such an observation was also found in other investigations [4,8]. blank specimen was about 47–91%. Moreover, the highest resistance
was attributed to the tempered martensite matrix. By heating the
2.4.2. EIS martensite matrix as an unstable phase, it decomposed to stable phases
Fig. 9 shows the EIS test results for all specimens in 0.6 M NaCl so­ including ferrite and carbides. In this situation, the activation energy for
lution. These plots contained Bode and phase angle curves. The Bode the corrosion reaction increased [32]. Consequently, the corrosion
plots showed that the impedance value for the blank specimen without resistance would be also increased. Notably, both specimens M − 12 m
any treatment was about 1 kΩ at 0.01 Hz. However, the increase in the and T-500 exhibited a similar matrix of tempered martensite. However,
impedance for specimens T-500 and A-270 m was significant with a the higher percentage and size of carbides in specimen T-500 resulted in
value of 10 kΩ. Moreover, the impedance of specimen M-M-12 m was higher corrosion resistance. For specimens T-500, A-270 m, and M-12 m
about 0.1 kΩ at the frequency of 0.01 Hz. Therefore, the lowest with high polarization resistance, values of CPEdl were the lowest. It was
impedance was related to specimen M-M-12 m with the martensite phase found that the lower value of CPEdl could show that the thickness of the
and the lower size of carbides. Based on the phase angle plots, the lowest double layer increased and the area of the exposed surface decreased
phase angle values observed at the frequency range of 1–10 Hz for most [33]. When the area of the surface was low, it could be concluded that
specimens. However, for two specimens (T-500 and A-270 m) with high the anodic dissolution or corrosion reactions at the surface would be
impedance, the lowest phase angle values occurred at the frequency reduced. Since the roughness of the surface decreased for specimens
range of 1–10 kHz. The lowest phase angle value was about 85◦ and was with a lower corrosion rate [33,34]. Thus, in this situation, values of n
attributed to specimen T-500. were highest for specimens T-500, A-270 m, and M-12 m. Totally,
The equivalent circuit (EC) proposed for EIS results is shown in changes in the microstructure caused the corrosion resistance of various
Fig. 10. Moreover, measurements of EIS data are presented in Table 5. specimens. When the martensite phase was present and the percentage
The EC for all specimens contained a solution resistance (Rs) connected and size of carbides were low, the corrosion resistance would be
in series with two parallel elements; a constant phase element (CPEdl) reduced. Consequently, the corrosion resistance of specimen M-M-12 m
that related to the double layer with an exponent n and a polarization was the lowest among others.
resistance (Rp). A similar electrical circuit was also suggested in other
research [5]. It was notable that the R values in Table 5 showed the 2.4.3. Weight loss
difference in the corrosion resistance of heat-treated specimens Fig.11 shows plots of weight loss versus various immersion times
compared to the corrosion resistance of the specimen without any during 96 h for all specimens in 0.6 M NaCl solution at 25 ◦ C. In addi­
treatment. tion, Table 6 reports details of parameters extracted from these plots. As
Based on data reported in Table 5, the values of Rs for all specimens shown in Fig. 9, the weight loss for all specimens increased continuously
were about 20–43 Ω cm2, and changes in this resistance were insignif­ with the increase of immersion time based on increases in the corrosion
icant. The highest and the lowest values of Rp were related to specimens reaction. This event displayed that the passive layer was not formed
T-500 and M-M-12 m, respectively. This result was consistence with the continuously on the metal surface.
Tafel polarization test results. The increased range in the polarization In good agreement with Tafel polarization and EIS test results, the
resistance for specimens M-12 m, A-270 m, and T-500 compared to the highest and the lowest weight loss was related to specimens M-M-12 m

9
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 12. FESEM images of corroded surface for specimens after 72 h in 0.6 M NaCl solution containing (a) B, (b) M-12 m, (c) M-M-12 m, (d) T-500 (e) A-120 m, and (f)
A-270 m

and T-500, respectively. The slope of weight loss plots versus the im­ exhibiting lower carbide content and size.
mersion time could show the corrosion rate of specimens. In this situa­ It was notable that the R2 indicated the value of the correlation co­
tion, the highest and the lowest corrosion rate corresponded to efficient [35]. The values of R2 in Table 6 showed that the weight loss
specimens M-M-12 m and T-500. It was notable that the value of %R was behavior versus the immersion time could be considered linear. The
the changes in the corrosion rates of heat-treated specimens compared to linear behavior of weight loss versus the immersion time was also re­
the corrosion rate of the blank specimen after 96 h. The highest reduc­ ported in the other research [6,36,37].
tion in the corrosion rate after 96 h was related to specimen T-500. The
value of %R for this specimen was 55.2. The increase in the corrosion 2.4.4. FESEM image of corroded surfaces
rate of heat-treated specimens compared to the blank specimen was also Fig. 12 shows the FESEM images of corroded surfaces for various
attributed to specimens M-M-12 m and A-120 m. This could be related to specimens after 72 h. Most specimens were corroded generally. For the

10
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

Fig. 13. EDS results of corroded surfaces for two specimens after 72 h in 0.6 M NaCl solution containing (a) B, and (b) T-500.

blank specimen, there were many cracks plus the corrosion products on effective parameters to enhance the corrosion resistance of D2 tool
corroded surfaces. Severe corrosion attacks were also seen for two steel.
specimens of M-M-12 m and A-120 m. On the surface of these specimens,
there were pores and many discontinuities. However, the lowest attack Credit author statement
resulting from the corrosion reaction was related to specimen T-500
with a low depth of cracks. Monireh Ahmadi: Methodology, Data curation, Investigation; Visu­
For more details, the EDS results of the corroded surface for two alization. Omid mirzaee: Supervision; Methodology; Conceptualization.
specimens (B and T-500) after 72 h immersion in 0.6 M NaCl solution are Mahboobeh Azadi: Supervision; Writing – original draft. Hootan Biu­
shown in Fig. 13. The oxygen content for the blank specimen was higher kani: Methodology; Visualization.
than specimen T-500. This could indicate the lower corrosion products
at the surface of this specimen, as shown in Fig. 12(a). Moreover, the Declaration of competing interest
chromium content was also high for the blank specimen. The high
percentage of other elements such as V and Si at the corroded metal The authors declare that they have no known competing financial
surface could be attributed to the formation of other oxides such as interests or personal relationships that could have appeared to influence
vanadium oxides and silica. Na and Cl ions were also related to the the work reported in this paper.
corrosive environment.
Data availability
3. Conclusion
Data will be made available on request.
In this research, the effects of various double-quenching processes on
the microstructure and corrosion properties of D2 tool steel were per­ References
formed. These various double-quenching treatments resulted in chang­
ing the size and amount of carbides in addition to the matrix phase that [1] J.C. Diaz-Guillen, J.A. Diaz-Guillen, E.E. Granda-Gutierrez, M.R. Diaz-Guillen, M.
A. Gonzalez-Albarran, Electrochemical corrosion performance of AISI D2 tool steel
changed the corrosion behavior of D2 tool steel in 0.6 M NaCl solution. surface hardened by pulsed plasma nitriding, Int. J. Electrochem. Sci. 8 (2013)
The obtained results could be summarized as follows. 973–982.
[2] M.N. Mohammed, M.Z. Omar, S. Al-Zubaidi, K.S. Alhawari, M.A. Abdelgnei,
Microstructure and mechanical properties of thixowelded AISI D2 Tool Steel,
• The Tafel polarization measurements showed that corrosion rates Metals 8 (2018) 316.
would be decreased up to 99.9% when the matrix phase of specimens [3] M.N. Mohammed, M.Z. Omar, J. Syarif1, Z. Sajuri, M.S. Salleh, K.S. Alhawari,
was tempered martensite. In addition, the carbide size and amount A Study of microstructure properties of AISI D2 tool steel in partial re-melting
method, Appl. Mech. Mater. 699 (2015) 76–80.
played an effective role in the corrosion rates of D2 tool steel. [4] M. Azadi, M. Ferdosi, H. Shahin, The effect of different heat treatment procedures
• EIS results displayed that specimens with a higher content of car­ on duplex stainless steel microstructures and electrochemical properties, Iranian
bides and a higher size of carbides showed an increase (up to 91.2%) Journal of Materials Science and Engineering 17 (1) (2020) 91–101.
[5] F. Castillejo, J. Jairo Olaya, J. Edgar Alfonso, Wear and corrosion resistance of
in the corrosion resistance of heated-D2 tool steel in 0.6 M NaCl
chromium–vanadium carbide coatings produced via thermo-reactive deposition,
solution. Coatings 9 (2019) 215.
• During 96 h, the immersion test results showed that tempering heat [6] M. Erdogan1, I. Gunes, Corrosion behavior and microstructure of borided tool
treatment at 500 ◦ C was an effective process to lower the corrosion steel, Materia 20 (2) (2015) 523–539.
[7] L. Tang, C. Gao, J. Huang, H. Zhang, W. Chang, Dry sliding friction and wear
rate of D2 tool steel. However, the modified martempering process behavior of hardened AISI D2 tool steel with different hardness levels, Tribol. Int.
increased the corrosion rate of such steel. This could be attributed to 66 (2013) 165–173.
the small size of carbides. [8] B.F. Chen, W.L. Pan, G.P. Yu, J. Hwang, J.H. Huang, On the corrosion behavior of
TiN-coated AISI D2 steel, Surf. Coating. Technol. 111 (1999) 16–21.
• This study suggested that to choose the proper heat treatment, in
addition to the phase of the matrix, the carbide properties were

11
M. Ahmadi et al. International Journal of Pressure Vessels and Piping 202 (2023) 104915

[9] F.E. Castillejo, J.J. Olaya, J.M. Arroyo-Osorio, Nb–Cr complex carbide coatings on [26] N. Du, H. Liu, Y. Cao, P. Fu, C. Sun, H. Liu, D. Li, Formation mechanism of MC and
AISI D2 steel produced by the TRD process, J. Braz. Soc. Mech. Sci. Eng. 37 (2015) M2C primary carbides in as-cast M50 bearing steel, Mater. Char. 174 (2021),
87–92. 111011.
[10] G.K. Egert, T.D. Burleigh, Improved reproducibility of D2 Tool steel after cryo- [27] S. Hesamodin, H. Talebi, M. Ghasemi-Nanesa, H. Jahazi, Melkonyan, In situ study
treatment at -78◦ C (dry ice), Materials and Corrosion Engineering Management 1 of phase transformations during non-isothermal tempering of bainitic and
(1) (2020) 21–24. martensitic microstructures, Metals 7 (2017) 346.
[11] D. Das, A.K. Dutt, K.K. Ray, Sub-zero treatments of AISI D2 steel: Part I. [28] M. Azadi, A. Mirani Pazuki, M.J. Olya, The effect of new double solution heat
microstructure and hardness, Mater. Sci. Eng. 527 (2010) 2182–2193. treatment on the high manganese Hadfield steel properties, Metallography,
[12] D. Das, A.K. Dutt, K.K. Ray, Optimization of the duration of cryogenic processing to Microstructure, and Analysis 7 (5) (2017) 618–626.
maximize wear resistance of AISI D2 steel, Cryogenics 49 (2009) 176–184. [29] M. Arab, M. Azadi, O. Mirzaee, Effects of manufacturing parameters on the
[13] D. Das, A.K. Dutta, V. Toppo, K.K. Ray, Effect of deep cryogenic treatment on the corrosion behavior of Al–B4C nanocomposites, Mater. Chem. Phys. 253 (2020),
carbide precipitation and tribological behavior of D2 Steel, Mater. Manuf. Process. 123259.
22 (2007) 474–480. [30] J.R.J. Marcuci, E.C. de Souza, C.C. Camilo, P.L.D. Lorenzo, J.M.D. de Almeida
[14] D. Das, A.K. Dutta, K.K. Ray, Influence of varied cryotreatment on the wear Rollo, Corrosion and microstructural characterization of martensitic stainless steels
behavior of AISI D2 steel, Wear 266 (2009) 297–309. submitted to industrial thermal processes for use in surgical tools, Research on
[15] D. Das, A.K. Dutta, K.K. Ray, On the refinement of carbide precipitates by Biomedical Engineering 30 (3) (2014) 257–264.
cryotreatment in AISI D2 steel, Phil. Mag. 89 (1) (2009) 55–76. [31] F.E. Castillejo, D.M. Marulanda, J.J. Olay, J.E. Alfonso, Wear, and corrosion
[16] K. Amini, A. Akhbarizadeh, S. Javadpour, Effect of deep cryogenic treatment on the resistance of niobium–chromium carbide coatings on AISI D2 produced through
formation of nano-sized carbides and the wear behavior of D2 tool steel, TRD, Surf. Coating. Technol. 254 (2014) 104–111.
International Journal of Minerals, Metallurgy and Materials 19 (9) (2012) 795. [32] S. Herbirowo, D. Aryanto, A.L. Indharto, I. Saefuloh, B. Adjiantoro, Effects of
[17] J. Voglar, Z. Novak, P. Jovicevi-Klug, B. Podgornik, T. Kosec, Effect of deep martempering heat treatment on corrosion rate in 1.5Ni laterite steel, Mater. Sci.
cryogenic treatment on corrosion properties of various high-speed steels, Metals 11 Eng. 578 (2019), 012064.
(2021) 14. [33] M. Azadi, M. Ferdosi Heragh, M.A. Bidi, Electrochemical characterizations of
[18] High-Carbon, High-Chromium Cold Work Tool Steels (D Series) In: Heat treatment epoxy coatings embedded by modified calcium carbonate particles, Progress in
guide (2nd ed edition) 674–690. Color, Colorants and Coating 13 (4) (2020) 213–222.
[19] N. Pillai, R. Karthikeyan, Prediction of ttt curves of cold working tool steels using [34] M.A. Bidi, M. Azadi, M. Rassouli, An enhancement on corrosion resistance of low
support vector machine model, Mater. Sci. Eng. 346 (2018), 012067. carbon steel by a novel bio-inhibitor (leech extract) in the H2SO4 solution, Surface.
[20] N. Yasavol, H. Jafari, Microstructure, mechanical and corrosion properties of Interfac. 24 (2021), 101159.
friction stir-processed AISI D2 tool steel, J. Mater. Eng. Perform. 24 (2015) [35] S. Safarloo, F. Loghman, M. Azadi, M. Azadi, Optimal design experiment of ageing
2151–2157. time and temperature in Inconel-713C superalloy based on hardness objective,
[21] D. Das, A.K. Dutta, K.K. Ray, Correlation of microstructure with wear behaviour of Trans. Indian Inst. Met. 71 (7) (2018) 1563–1572.
deep cryogenically treated AISI D2 steel, Wear 267 (2009) 1371–1380. [36] H. Mobtaker, M. Azadi, N. Hassani, M. Neek-Amal, M. Rassouli, M.A. Bidi, The
[22] D. Nikolov, M. Nikolova1, Research on the optimum temperature regime for inhibition performance of quinoa seed on corrosion behavior of carbon steel in the
vacuum oxy-nitrocarburizing of AISI D2 steel, Mater. Sci. 3 (2015) 60–63. HCl solution; theoretical and experimental evaluations, J. Mol. Liq. 335 (2021),
[23] H. Kim, J.Y. Kang, D. Son, T.H. Lee, K.M. Cho, Evolution of carbides in cold-work 116183.
tool steels, Mater. Char. 107 (2015) 376–385. [37] M.A. Hamidzadeh, M. Meratian, M. Mohammadi Zahrani, A study on the
[24] D. Viale, J. Beguinot, F. Chenou, G. Baron, Optimizing microstructure for high microstructure and mechanical properties of AISI D2 tool steel modified by
toughness cold-work tool steels, Mater. Sci. 3 (2006) 300–320. niobium, Mater. Sci. Eng., A 556 (2012) 758–766.
[25] M.N. Mohammed, M.Z. Omar, M.S. Salleh, K.S. Alhawari, Study on thixojoining
process using partial remelting method, Adv. Mater. Sci. Eng. 2013 (2013),
251472.

12

You might also like