Results in Materials 17 (2023) 100374

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Results in Materials
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Influence of micro-alloying elements and deep cryogenic treatment on

microstructure and mechanical properties of S5 cold work shock resisting
tool steel
Mahmoud A. Essam a, Ahmed Y. Shash b, c, *, Mohamed Kamal El-Fawakhry d, Emad El-Kashif b,
Hassan Megahed b
a
Mechanical Engineering Department, Higher Technological Institute (HTI), 10th of Ramadan City, Egypt
b
Mechanical Design and Production Department, Faculty of Engineering, Cairo University, Cairo, Egypt
c
Faculty of Engineering and Materials Science, German University in Cairo, Cairo, Egypt
d
Steel and Ferroalloys Department, Central Metallurgical Research and Development Institute (CMRDI), Cairo, Egypt

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

Keywords: Shock resistance cold work tool steel (S5) has many applications such as blades for sheet cutting, manufacturing
Tool steel of chisel and hammers etc. This Steel has the ability to accommodate residual stresses without premature failure.
Cold work This work investigates the effect of carbide forming elements; V and Nb on the microstructure and mechanical
Shock resisting
properties of S5 tool steel. Three heats were prepared with different content of carbide forming elements via
Deep cryogenic treatment
Hardness
vacuum melting and the effect of heat treatment [hardening, tempering and deep cryogenic treatment (DCT) at -
Impact toughness 196 ◦ C] on the mechanical properties was investigated. Retained austenite for quenched samples were calculated
Retained austenite using X-ray diffraction method, also impact test was used to determine the toughness of all samples after different
Martensite heat treatment conditions. Microstructure observation showed that the basic structure for the tested samples are
tempered martensite for traditional S5 samples and fine tempered martensite for other micro alloyed samples.
Scanning electron microscope (SEM) was also used to ensure that the amount of retained austenite have been
eliminated or reduced due to deep cryogenic treatment. Hardness (HRC) after quenching process reached 51
HRC, further increase in hardness values has been obtained after DCT due to reduction of retained austenite. The
toughness results showed lower values for deep cryogenic treatment than conventional heat treatment samples;
this is mainly due to the reduction in retained austenite content.

1. Introduction
Tool steels have similar chemical composition as other types of
steels, but higher content of carbon and carbide forming elements [1–4].
The vast range of alloying elements are employed to provide the steel
with particular properties for optimum performance [1]. Hardness,
strength, wear resistance, and toughness are among these properties [2].
Tool steels are commonly employed in industrial product
manufacturing, making them vital in the field of production technology
[4].
Tool steel is used to make tools for cutting, molding, or otherwise
shaping a material into a part or component that is fitted to a specific
function [5]. As a result, tool steels has high degree of hardness and
endurance in order to withstand harsh service conditions [6]. They
range from plain carbon steels with up to 1.2% carbon and no sub­
stantial levels of alloying elements to highly alloyed steels with up to
50% alloying additives [7]. Although some carbon and low-alloy tool
steels have a wide range of carbon content, the carbon range in most
higher alloy tool steels is quite narrow [5]. Tool steels are classified
using a mixed categorization system based on their use, composition,
particular mechanical qualities, or heat treatment procedure [1].
Tool steels were classified into a small number of groups for ease of
comparison and evaluation, as well as to aid in the selection of steel for a
specific application [8]. Because tool steels have such a wide range of
compositions, categorizing them into one of the alloy steel categories
has never been straightforward [9]. Tool steels have strict limits on the
quantity of alloying elements allowed, and entire steel series are pred­
icated on carbon content variations [4].

* Corresponding author. Mechanical Design and Production Department, Faculty of Engineering, Cairo University, Cairo, Egypt.
E-mail addresses: ahmed.shash@cu.edu.eg, ahmed.shash@guc.edu.eg (A.Y. Shash).

https://doi.org/10.1016/j.rinma.2023.100374
Received 31 January 2023; Accepted 5 February 2023
Available online 9 February 2023
2590-048X/© 2023 Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
M.A. Essam et al.
Cold work tool steels are used to fabricate tools for cold work ap­
plications. High hardness (50–66 HRC), low impact toughness, high
wear resistance (less than 20 mg/min), and high compressive strength
are the mechanical qualities of cold work tool steels [10,11].
According to the AISI classification system, shock-resistant tool steels
are classified as group S steels [12]. Shock-resistant steels in group S
include S1, S2, S5, S6, and S7. The AISI type S tool steels have a lower
carbon content and a somewhat higher alloy content than the W steels
[13]. Type S steels are suited for shock and impact applications due to
their medium carbon content, which enhances toughness [5].
Shock-resistant tool steels have been developed to combine high
toughness and fracture resistance with high strength and wear resistance
under impact loading circumstances [14]. The high hardness is achieved
by limiting the carbon content and adding alloying elements. Because
shock-resistant tool steels contain more alloying elements than
water-hardening tool steels, their hardenability is also higher [6].
The chemical composition of tool steel has the largest impact on its
shearing performance. The alloying elements in tool steel such as
tungsten, chromium, molybdenum, and vanadium have the great effect
in determining the mechanical properties [12]. Alloying elements can be
split into two classes based on how they are distributed in steel [4].
1. Elements such as Ni, Si, Co, Al, Cu, and N that can’t form carbides in
steel.
2. Stable carbide-forming elements in steel, such as Cr, Mn, Mo, W, V,
Ti, Zr, and Nb
Vanadium was used as a scavenger to remove slag, impurities, and
nitrogen dissolved in the matrix, as well as a de-oxidant, during the
steelmaking process [15,16]. Vanadium was soon discovered to
generate exceptionally hard and thermally stable MC type carbides
(Where M denotes the carbide forming metal element such as V, Nb, Cr,
etc and C refer to carbide), which were usually isolated particles within
the matrix. These carbides increase abrasion resistance and provide
excellent cutting performance [16–19]. Because vanadium carbides are
only slightly soluble in the matrix, adding vanadium does not slow the
diffusional dissolution of austenite; instead, it elevates the Ms- and Mf
temperatures by binding carbon (forming carbides), enhancing hard­
enability. The addition of vanadium also refines the matrix’s grain
structure [19].
Molybdenum (Mo) is a carbide-forming element. It dissolves little in
cementite, but when the molybdenum percentage in steel reaches a
certain level, molybdenum carbides develop [19]. Molybdenum in­
creases the creep strength of low-alloy steels at elevated temperatures
and induces secondary hardening during the tempering of quenched
steels [19]. The inclusion of Mo results in fine-grained steels with
improved hardenability and fatigue strength [19]. Temper embrittle­
ment is delayed in alloy steels containing 0.20–0.40% Mo or V, but it
cannot be completely eliminated [20]. Molybdenum is utilized exten­
sively in high-alloy Cr ferritic stainless steels and Cr–Ni austenitic
stainless steels to boost corrosion resistance [20]. High Mo concentra­
tion reduces the susceptibility of stainless steel to pitting [21]. At high
temperatures, molybdenum has a very strong solid solution strength­
ening effect in austenitic alloys [21].
Niobium (Nb) and tantalum (Ta) are carbide and nitride formers that
are extremely strong. Small amounts of Nb can refine the grains and
generate fine nitrides or carbonitrides, boosting the yield strength of
steels [8]. Niobium is commonly utilized in micro alloying steels to
achieve high strength and toughness by using controlled rolling and
cooling techniques [22]. The yield strength of medium-carbon steel can
be increased by 150 MPa when adding 0.03% Nb to the austenite [22].
Niobium and Vanadium added Steels have better hardenability and
mechanical properties than Niobium and Vanadium free steels. In Cr–Ni
austenitic steels, niobium is used as a stabilizer to prevent intergranular
corrosion [23].
For simplicity of machining, tool steels are produced in the annealed
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Results in Materials 17 (2023) 100374
state [16]. Most tooling applications deem this annealed condition to be
excessively soft [16]. In order to achieve the requisite qualities, most
tooling applications require the steel to be hardened to an HRC hardness
of 45 or higher [12]. On the Rockwell “C" scale, annealed steel has a
hardness of less than 20 [12]. Depending on the type of steel used, the
steel is heat-treated and quenched after machining. The heat treatment
and quenching processes improve the material’s toughness and strength
[24].
To avoid decarburization, most steels must be protected from oxygen
exposure prior to the first step in the hardening process. During the
hardening process, decarburization is an undesirable loss of carbon [25].
During the hardening process, carbon in the steel is what gives it its
hardness [25]. Depending on how much carbon is lost during the
heating process, the steel will remain soft or will not attain its maximum
hardness. Steps must be taken to keep the tool from coming into contact
with oxygen [24].
The actual change in hardness happens during the austenizing pro­
cess. Austenizing is a phase transition in which the steel rearranges the
molecules into a desirable arrangement [7]. The steel matrix is enlarged,
allowing carbon and other components to embed in the matrix [24].
The steel is quenched when it is cooled to a temperature below its
critical temperature in a reasonably short period of time [19]. It must
move quickly enough through this range to trap carbon and other
components within the steel matrix [4]. The tool steel’s required qual­
ities, such as hardness and wear resistance, are provided by these trap­
ped or frozen elements [24].
Tempering is a process that involves heating previously hardened or
normalized steel to a temperature below the lower critical temperature
and cooling it at a controlled rate, mostly to improve ductility and
toughness but also to increase matrix grain size [24].
Cryogenic treatment of tool steels has been around for a long time,
but when compared to heat treatment, it is still in its infancy [26]. This
treatment was discovered to increase the performance of cutting tool
steels in the 1930s and 1940s [27].
Several researchers have concentrated their efforts on understanding
this mechanism and using cryogenics to improve the efficiency of tool
steels [28,29] Cryogenic treatment can increase the tool performance,
according to many researchers [30,31]. The most favorite spots of this
treatment was an increase in tool steel wear resistance [30]. This
approach has been used to improve wear resistance and dimensional
stability of components in the manufacturing lines of several industries,
such as aerospace, automotive, and electronics [32].
Cold treatment, which uses dry ice at temperatures as low as − 80 ◦ C,
and “deep cryogenic treatment,” which uses liquid nitrogen at − 196 ◦ C,
are the two types of low-temperature treatment [33].
Many small businesses have started offering cryogenic treatment to
extend the life of steel products like drills, cutters, gears, punch dies, and
tool bits in recent years [34]. The effect of cryogenic treatment can be
explained by the enhancement of fine carbide production in the
martensite phase [33,35], particularly nano-scale carbide [36]. How­
ever, its mechanism is unknown and deep cryogenic treatment’s low
adoption can be linked to a lack of understanding as well as a lack of
generally accepted deployment procedures [37].
Cutting performance usually refers to the tool’s life until it is
reground or until it wears out [11]. This performance has an economic
impact since it influences production costs. Mechanical qualities of tool
steel, such as sharpness, hardness, strength, toughness, and micro­
structure, can be used to assess cutting performance [3]. However, the
chemical composition and thermal treatment of the tool, which impact
the tool’s microstructure, influence these mechanical qualities [5].
In this work, the microstructure and mechanical properties were
analyzed. Optical microscope, XRD analysis, Hardenability test, Rock­
well hardness, and toughness test were conducted to investigate the
effect of micro alloying elements Nb and V on cold work (S5) shock
resisting tool steel.
M.A. Essam et al. Results in Materials 17 (2023) 100374

Table 1
Chemical composition of the investigated S5 cold work shock resisting tool steel.
Sample Name Chemical Composition %

C Si Mn Cr Mo P S Cu V Nb Fe

S5O 0.370 1.999 1.0 0.30 0.314 0.032 0.008 0.011 … … Balance
S5AO 0.370 2.268 1.0 0.253 0.169 0.026 0.006 0.011 0.251 … Balance
S5BO 0.480 2.164 1.0 0.384 0.223 0.024 0.003 0.011 … 0.013 Balance

2. Experimental procedure
Table 2
Heat treatment conditions for S5 samples.
2.1. Materials and its heat treatment
No. Heat Treatment Temperature Medium Time
(◦ C) (Hr.)
Cold work shock resisting tool steel (S5) samples were melted at
1 Annealing 780 Furnace 0.5 Central Metallurgical Research and Development Institute (CMRDI).
2 Hardening 880 Water 0.5
Three different samples (S5O, S5AO and S5BO) were produced by using
quench
3 Tempering 200 Air 0.5
induction furnace with a capacity 50 kg with the following chemical
4 Deep Cryogenic - 196 Liquid 5 composition as shown in Table 1.
Treatment (DCT) Nitrogen All samples were rolled to 5 mm thickness after casting and samples
(15 mm × 15mm x5mm) were cut from the rolled sheets. All samples

Fig. 1. Jominy –end quench test.

Fig. 2. Jominy –end quench hardenability test for S5 samples after austenitizing at 900 ◦ C

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M.A. Essam et al.
Fig. 3. Optical microscope of the specimens as annealed condition (A) S5O, (B) S5AO and (C) S5BO.
were annealed at 780 ◦ C for 30 min and keep it in furnace cooling to ease
the machining process.
All samples were austenitized at 880 ◦ C for 30 min, then quenched in
water. The tempering treatment was carried out at 200 ◦ C for 30 min
then air cooled to room temperature. Deep Cryogenic Treatment (DCT)
was used to figure out its effects on microstructure and mechanical
properties of S5 shock resisting tool steel. This type of treatment uses
liquid nitrogen as a treatment medium at – 196 ◦ C for soaking time 5 h,
Table 2 shows the heat treatment conditions.
2.2. Hardenability test
The Jominy end quench test was performed in accordance with
ASTM A255 to determine the hardenability of S5 cold work shock
resistant tool steel [38]. Three samples of cylindrical bar for each tested
steel were prepared with dimensions 25 mm in diameter and 100 mm in
length as shown in Fig. 1. Rockwel hardness test was recorded according
to scale C for each sample at 5 mm distance. When cooled from a high
temperature, the steel has the ability to convert partially or entirely from
austenite to some fraction of martensite at a particular depth below the
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Results in Materials 17 (2023) 100374
surface. Briefly, the hardenability describes the capacity of the steel to
harden in depth under a given set of conditions.
2.3. Microstructure observation
Microstructural examinations were carried out on tempered samples
by using scanning electron microscope. Standard metallographic
methods were used to prepare the samples. Samples were ground
manually and polished with diamond suspension with 1 μ m particle
size; then etched in 2% Nital solution.
X-ray diffraction (XRD) was conducted to measure volume fraction
and lattice parameter of retained austenite. The technical specifications
of X – ray diffractometer were cupper radiation with 2 theta ranging
between 35 and 95 ◦ and speed of scanning was 2 ◦ /min. The volume
fraction of retained austenite was measured by performing curve fitting
of the diffracted peaks on the plot of intensity as a function of 2θ. The
amount of retained austenite was calculated by comparing the inte­
grated intensities of the diffracted peaks of martensite and austenite
according to Cullity [39].
M.A. Essam et al. Results in Materials 17 (2023) 100374

Fig. 4. SEM of the specimens as tempered condition (A) S5O, (B) S5AO DCT + Tempering and (C) S5AO,(D)S5AO DCT + Tempering,(E)S5BO,(F)S5BODCT
+ Tempering.

2.4. Mechanical testing value is an average of four measurements.

Hardness measurements were carried out on specimens having
similar dimensions as those used for microscopy. A Zwick/Roell ZHR
hardness tester was used to assess Rockwell C hardness at room tem­
perature with diamond indenter at load 150 Kg. Each reported hardness
Impact toughness testing with V-notched was produced with di­
mensions 55 × 10 × 5 mm. The impact testing was carried out at room
temperature with average of three measurements.

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M.A. Essam et al. Results in Materials 17 (2023) 100374

Fig. 5. XRD pattern for samples after conventional treatment and DCT.

Table 3
XRD analysis.
Sample Name 2θ FWHM R.A % e D (nm) ρ
S5O Hardening 44.709020 0.164477 3.08 0.0348 52.22 9.3 × 10-4
S5AO Hardening 44.609020 0.164477 3.02 0.023516 52.22 6.2 × 10-4
S5BO Hardening 44.70902 0.158314 4.89 5.85* 10− 3 54.25 1.5 × 10-4
S5O Tempering 44.709560 0.198041 – 0.0348 43.37 1.12 × 10-3
S5AO Tempering 44.713730 0.223772 – 0.023516 38.38 8.5 × 10-4
S5BO Tempering 44.713730 0.226184 – 5.85* 10− 3 37.97 2.15 × 10-4

3. Results and discussions
3.1. Hardenability test
Most of the tool steel must undergo to a hardenability test to measure
its availability to transform into martensitic structure as shown in Fig. 2,
the micro alloying elements such as V and Nb have significant effect on
promoting the hardenability curve [15,40].
Sample S5AO, which contains vanadium, has the highest hardness
value of 65 HRC and the hardness rate remains nearly constant until the
length of 4.5 cm, at a hardness value of 63.13 HRC. Compared to sample
S5BO, which contains niobium as a carbide forming element, it has a
hardness value equal to 63 HRC, and the hardness rate is still approxi­
mately constant up to a length of 4.5 cm and a value of 60.1 HRC.
On the contrary, and as noted in the original sample S5O, there was a
sudden drop in the hardenability at a length of 1.5 cm, and the hardness
was recorded as 59 compared to the two previously mentioned samples
(S5AO and S5BO), which retained the hardness to a distance close to
50% of the length of the test sample.
The minimum hardness can be demonstrated as shown from Fig. 2
for sample S5O was recorded at the length 10 cm (end of Jominy test
bar) that equal 47.25 HRC due to slow cooling rate, but it can be noticed
that for this sample may be considered there are a deterioration in
hardness in comparison with the value of hardness at the tip of quenched
end that equal 63 HRC.
On the other hand, the minimum hardness values for samples S5AO
and S5BO at the end of Jominy test sample (length 10 cm) are 52.6 and
54.33 HRC respectively. It can be concluded that from Fig. 2, the sample
S5AO have higher hardenability followed by sample S5BO then S5O.
It is believed that, micro alloying elements such as V and Nb can
reduce the carbon content of the austenitic matrix and consequently rise
up martensite start temperature.
3.2. Microstructure analysis
The samples of S5 shock resistant tool steel were examined using an
optical microscope after they had been heat treated. Full annealing is
used in this research to establish the softest condition required in the
cold work shock resisting tool steel. In fact, the process of annealing
treatment is used to make enhancement for machinability process and to
produce a homogeneous microstructure.
The matrix of microstructure as shown in Fig. 3 composed of pearlite
and ferrite [7]. Surely, the existing of ferrite phase due to high per­
centage of silicon. By comparing microstructure for samples S5AO and
S5BO with S5O, it is obvious that the adding of micro alloying elements
for samples S5AO and S5BO (V and Nb) respectively, make the micro­
structure finer compared to sample S5O.
All samples underwent annealing before being austenitized at 900 ◦ C
for 30 min and quenched in water. To achieve the necessary mechanical
qualities and to enable the carbide particles to diffuse into the matrix,
the hardening process aims to create a fully martensitic structure.
Since the austenitizing procedure for S5 shock-resistant tool steel is
regarded as a crucial step, efforts had to be taken to avoid the decar­
burization phenomena, which is one of the issues with tool steel’s heat
treatment. However, one of the factors affecting the mechanical prop­
erties of cold work tool steel is the existence of residual austenite during
martensitic transformation.
In this investigation, the final step of the heat treatment procedures
(conventional treatment) involves tempering the specimens at 200 ◦ C
for 30 min while holding them there before cooling them in air. Using a

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M.A. Essam et al. Results in Materials 17 (2023) 100374

Fig. 6. SEM and EDAX, (A) S5AO tempering, (B) S5BO tempering + DCT, (C) EDX for sample S5AO tempering and (D) EDX for sample S5BO tempering + DCT.

Fig. 7. HRC measurements for traditional treatment and for DCT.

scanning electron microscope, Fig. 4 shows the microstructure following
the tempering treatment process. The fundamental goal of the tempering
process is to create a martensitic structure, but since this structure is
fragile and hard, tempering treatment is required.
In reality, the tempering process is carried out for two purposes: first,
to increase the heat of the martensitic structure and increase ductility;
and second, to attempt to reduce the percentage of retained austenite (R.
A). Because the residual austenite is in an unstable state, the tempering
heat treatment procedure can convert it into martensite.
Tempered martensite was formed for all three steels; however the V-
added steel (S5AO) exhibits the finest sub-lath structure when compared
to S5O and S5BO. Fig. 3 depicts the SEM microstructure of steels S5O,
S5AO, and S5BO under both as-tempered and DCT + tempering condi­
tions. In comparison to as tempered conditions for all steels, the DCT +
tempering condition leads to a smaller area fraction of residual austenite
and a larger area fraction of carbides.
After DCT + tempering, Nb-added steel (S5BO) exhibits the lowest
area fraction of preserved austenite and the highest area fraction of
carbides with uniform distribution.
The minimum retained austenite area fraction causes an increase in

7
M.A. Essam et al.
Fig. 8. Impact toughness test results for traditional treatment and for DCT.
the quenching residual stresses, which leads to the micro cracks seen in
Nb-added steel following DCT + tempering. Micro cracks might also
form as a result of carbides’ high area fraction. Rehan [39] noted the
finer microstructure that the V and Nb addition produced. As can be seen
in Fig. 4B, D, and F, the quantity of remaining austenite was reduced and
changed into martensite in the samples after DCT.
3.3. X-ray diffraction analysis
XRD peaks for samples at different treatment conditions are given in
Fig. 5. The main matrix for XRD pattern is martensite. According to
Fig. 5, it can be observed that a peak of retained austenite exists in
sample S5O hardening, by comparing this sample after tempering
treatment, it was found that it had vanished and this gives the impres­
sion that the percentage of retained austenite has decreased.
In general, by comparing XRD patterns after quenching and
tempering from Fig. 5, it can be noticed that, there is no difference in the
peaks, and this could be considered evidence that there is no decrease in
retained austenite and therefore the retained austenite percentage was
inferred using equation (1), since it is difficult to determine it by using
XRD analysis if the percentage less than 3% [41].
R.A. % = exp( − 1.1 ∗ 10 − 2(Ms – Tq)) (1)
Where,
R.A … Retained austenite, Ms … Martensite start temperature and Tq
… Quenching temperature.
As shown from Fig. 5 after DCT the diffraction peaks of retained
austenite where decreased as observed in crystal plane (022).
Table 3 shows the positions of the peaks (2θ), Full width half
maximum (FWHM), calculated retained austenite (R.A), lattice strain
parameter(e), average crystalline size(D) and density of dislocations (ρ).
As shown in the table, the FWHM have been obtained at approxi­
mately 44.7◦ , but there was a difference between the values of FWHM,
with sample S5BO having the highest value, followed by sample S5AO
with a value less than S5BO by 1.1%, and finally sample S5O with a
value less than S5BO by 12.44%.
It is possible to predict the fine grain size from values of FWHM. So, it
can be seen that the decrease in the values of FWHM means the grains
are not fine [42]. Based on this, it can be said that the higher values of
the FWHM as shown in the case of samples after tempering treatment
process, the smaller size of average crystalline size (D).
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Results in Materials 17 (2023) 100374
3.4. SEM and EDAX
To confirm that the addition of the elements V and Nb to the tool
steel helped create carbides, scanning electron microscopy (SEM) and
energy dispersive X-rays (EDX) were used. For sample S5AO, as illus­
trated in Fig. 6-A, there is some carbide and the primary microstructure
is tempered martensite. On the other hand, a heat treatment was used
using DCT, it was noticed that the basic microstructure of sampleS5BO is
tempered martensite, but the microstructure is more fine, and the
disappearance of retained austenite was also observed as explained in
Fig. 6-B.
Based on EDX analysis, it was confirmed that carbides were present
in samples S5AO and S5BO as a result of adding carbide forming ele­
ments such as vanadium and niobium as shown in Fig. 6-C and 6-D.
3.5. Hardness
The hardness (HRC) for conventional and deep cryogenic treatment
is shown in Fig. 7 (DCT). According to the accompanying figure, the
samples with quenching treatments have the highest (HRC) values. This
is a result of the steel going through a phase transformation during the
quenching process. The change in lattice structure from FCC to BCC or
the martensite phase is associated to an increase in HRC hardness levels.
However, a slight reduction in hardness was seen following the
tempering treatment procedure, which was brought about by a reduc­
tion in residual austenite, as shown in Fig. 7.
Whether after quenching or tempering, there is evidence of an
improvement in hardness after DCT. This can be explained by the fact
that applying DCT caused the retained austenite in the conventional
heat treatment case to convert into martensite [43].
3.6. Impact energy
The impact test was performed because the tool steel experiences a
dynamic load while the cutting blade is working. Fig. 8 displays the
findings of the tested samples plotted. Since there is a direct correlation
between the impact toughness value and the retained austenite, the
impact toughness can be thought of as providing an impression on the
quantity of retained austenite.
It was determined how DCT affected impact toughness absorption,
and it was discovered that for sample S5O, the toughness after cryogenic
treatment was 1.95 J/cm2, as opposed to 3.95 J/cm2 after conventional
quenching. However, as shown in Fig. 8, the results of the toughness test
M.A. Essam et al.
Fig. 9. (A) Surface texture (Abbott Firestone Curve), (B) Rose plot of intercept, (C) Mean surface roughness, and (D) Rose plot of slope for sample S5AO tempering.
after using DCT for sample S5AO were 7.05 J/cm2 and 12.4 J/cm2 for
traditional quenching. This suggested a drop in the value of the tough­
ness test after using DCT. In comparison to traditional quenching, the
hardness is decreased by around 50% for the sample S5BO on the same
behaviour. Following cryogenic treatment, a minor decrease in tough­
ness can be attributed to an increase in martensite content.
Fig. 8 also shows how tempering affects specimens that have un­
dergone both cryogenic and conventional treatments for toughness.
When subjected to classical tempering, the identical sample of S5O has a
toughness value of 7.55 J/cm2, but the sample following DCT has 5.4 J/
cm2. Sample S5AO’s toughness value after DCT is 8.75 J/cm2 lower than
the value after conventional tempering, which is 17.15 J/cm2. Accord­
ing to the same methodology, the hardness findings for the sample S5BO
were 4.3 J/cm2 after DCT and 6.3 J/cm2 after traditional tempering
treatment. In general, it was seen while comparing the samples after
DCT that the impact toughness values had decreased in comparison to
the conventional heat treatment. This is explained by the fact that the
amount of retained austenite was decreased and transitioned into
martensite [44].
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Results in Materials 17 (2023) 100374
3.7. Abbott Firestone Curve to determine surface texture
The Abbott Firestone curve is a useful tool for determining high
peaks, exploitation zones, and void ratios for shock-resistant tool steel
surfaces, especially when working with surfaces with high peaks,
exploitation zones, and void ratios [45,46]. The Abbott Firestone curve
can be used to see how a surface pattern’s peak and void heights are
distributed in reality. Figs. 9 and 10 demonstrate the mean surface
roughness, surface texture, rose plot of intercept, and rose plot of slope
for S5AO and S5BO DCT + tempering samples, respectively.
The surface texture of S5AO tempering and S5BO DCT + tempering is
shown in Figs. 9A and 10A, respectively. The predominant matrix for
sample S5AO is tempered martensite, with a percentage of 93%, while
the percentage of carbides was roughly 5% due to the addition of V as a
carbide producing element, and the remaining 2% can be projected for
residual austenite. On the other hand, as shown in Fig. 10A, the major
matrix was tempered martensite by a percentage of almost 100%, and no
voids for retained austenite were observed, indicating that the propor­
tion of retained austenite was reduced due to the use of DCT for sample
M.A. Essam et al.
Fig. 10. (A) Surface texture (Abbott Firestone Curve), (B) Rose plot of intercept, (C) Mean surface roughness, and (D) Rose plot of slope for sample S5BO DCT
+ tempering.
S5BO.
The distribution of the rose plot of intercept at different angles is
explained in Figs. 9B and 10B. Fig. 9B shows that the distribution for
sample S5AO tempering is homogenous about entire degrees, whereas
the distribution for sample S5BO DCT + tempering exhibits a little
disruption from 0 to 90◦ .
Low surface roughness, medium surface roughness, and finally high
surface roughness are depicted in Figs. 9C and 10C, respectively. Fig. 9D
depicts the distribution of the rose plot of slope for sample S5AO
tempering, which shows normal surface texture variations from 0 to
360◦ , but Fig. 10D depicts a minor distribution of fluctuations from 90 to
180◦ and in the range from 270 to 330◦ .
4. Conclusions
The effect of adding micro-alloying elements and deep cryogenic
treatment (DCT) at − 196 ◦ C for soaking time 5 h were studied for cold
10
Results in Materials 17 (2023) 100374
work S5 shock resisting tool steel. The following points were concluded:
• The microstructure of Samples after tempering treatment consists of
tempered martensite and 3% retained austenite.
• Average grain size for samples S5AO (0.25% vanadium) and S5BO
(0.013 niobium) have lower values 38.38 μm and 37.97 μm respec­
tively, compared with S5O (Nil V-Nil Nb) that has a value 43.37 μm.
This ensures the grain refinement effect of both V and Nb.
• It was observed that after tempering, the toughness test values were
lowered by 30–45% due to the transformation of retained austenite
to tempered martensite.
• DCT increases the carbides content, decreases the retained austenite
content and make the microstructure more homogeneous.
• The impact test results for samples after DCT have lower values
compared to conventional treatment, which is due to the retained
austenite reduction after DCT.
M.A. Essam et al.
Credit author statement
Mahmoud Essam: Conceptualization; Writing; Investigation; Meth­
odology; Validation. Ahmed Y. Shash: Supervision; Editing; Validation;
Investigation; Methodology. Mohamed El-Fawakhry: Supervision; Edit­
ing; Validation; Investigation; Methodology. Emad El-Kashif: Supervi­
sion; Editing; Validation; Investigation; Methodology. Hassan Megahed:
Supervision; Editing; Validation; Investigation; Methodology
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
References
[1] M.A. Rehan, Effect of Heat Treatment on Microstructure and Mechanical Properties
of a 5 wt.% Cr Cold Work Tool Steel, No. 28, 2019.
[2] G. Krauss, Steels: Processing, Structure, and Performance, Asm International, 2015.
[3] D.A. Fadare, T.G. Fadara, O.Y. Akanbi, Effect of Heat Treatment on Mechanical
Properties and Microstructure of NST 37-2 Steel, 2011.
[4] E. Elhachmi, Tool steels,” steel heat treat, Metall. Technol. (2006) 651–694,
https://doi.org/10.31399/asm.tb.spsp2.t54410621.
[5] Heat Treatment and Toughness Behavior of Tool Steels (D2 and H13) for Cutting
Blades.”.
[6] X. Zhao, T. Pan, Q. Wang, H. Su, C. Yang, Q. Yang, Effect of tempering temperature
on microstrueture and mechanical properties of steel containing Ni of 9, J. Iron
Steel Res. Int. 18 (5) (2011) 47–51.
[7] B. Sampson, Heat treatment,” Prof. Eng. 23 (7) (2010) 19–20, https://doi.org/
10.31399/asm.hb.v15.a0005230.
[8] G.E. Totten, Dieter, Steel Heat Treatment, 2006, pp. 1–12.
[9] A. Srinivasan, The Indian Institutes of Technology, Reclaiming Public Univ., 2022,
pp. 143–163, https://doi.org/10.4324/9781003229384-10.
[10] H. Berns, Comparison of wear resistant MMC and white cast iron, Wear 254 (1–2)
(2003) 47–54.
[11] A. Rehan, Microstructure and Mechanical Properties of a 5 wt.% Cr Cold Work Tool
Steel: Influence of Heat Treatment Procedure, University West, 2017.
[12] M. Algarni, Mechanical properties and microstructure characterization of AISI ‘D2’
and ‘O1’ coldwork tool steels, Metals 9 (11) (Nov. 2019), https://doi.org/10.3390/
met9111169.
[13] C. Faye, A Study of the Microstructural and Mechanical Properties of Novel Spring
Steels, 1998 [Online]. Available: http://shura.shu.ac.uk/19763/.
[14] T. Covered, S5 Tool Steel - Shock - Resisting Steel (UNS), 2012, pp. 3–5.
[15] R. Lagneborg, T. Siwecki, S. Zajac, B. Hutchinson, Role of vanadium in
microalloyed steels, Scand. J. Metall. 28 (5) (1999) 186–241.
[16] G.A. Roberts, R. Kennedy, G. Krauss, Tool Steels, ASM international, 1998.
[17] E. Pippel, J. Woltersdorf, G. Pöckl, G. Lichtenegger, Microstructure and
nanochemistry of carbide precipitates in high-speed steel S 6-5-2-5, Mater. Char.
43 (1) (1999) 41–55.
[18] G. Hoyle, High Speed Steels, 1988. Butterworths, Brgh. Green, Sevenoaks, Kent TN
15 8 PQ, 1988.
[19] C. Højerslev, Tool Steels, Risø National Laboratory, 2001.
[20] R.D. Cioffi, PhD Thesis: A Comparison Study on Depth of Decarburization and the
Role of Stable Carbide Forming Elements in 1075 Plain Carbon Steel and 440A
Stainless Steel, 2011, pp. 1–35.
11
Results in Materials 17 (2023) 100374
[21] P. Møller, Avanceret Teknologi, Tek. Forl., 1998.
[22] D.H. Stamatis, TQM engineering handbook, TQM Eng. Handb. (1997), https://doi.
org/10.1201/9781482269826.
[23] D.S. Sarma, Cold Work and Hot Work Tool Steels, 1994.
[24] J H, I. Flood, EFFECT OF TEMPERING TEMPERATURE ON THE MECHANICAL
PROPERTIES OF HARDENED 1.2842 TOOL STEEL, 2012, pp. 49–56. ЭконоМика
Региона, no. Kolisch 1996.
[25] D.A. Bales, A Study of Decarburization in SAE 1042 Steel: its Effect on Fatigue Life,
Tensile Properties, and Fatigue Fractography, 1977.
[26] S.S. Gill, J. Singh, R. Singh, H. Singh, Metallurgical principles of cryogenically
treated tool steels - a review on the current state of science, Int. J. Adv. Manuf.
Technol. 54 (1–4) (2011) 59–82, https://doi.org/10.1007/s00170-010-2935-5.
[27] C. Wilkins, Cryogenic Processing; the Big Chill, EDM Today, 1999, pp. 36–44.
[28] A. Akhbarizadeh, A. Shafyei, M.A. Golozar, Effects of cryogenic treatment on wear
behavior of D6 tool steel, Mater. Des. 30 (8) (2009) 3259–3264, https://doi.org/
10.1016/j.matdes.2008.11.016.
[29] K. Moore, D.N. Collins, Cryogenic treatment of three heat-treated tool steels, Key
Eng. Mater. 86 (1993) 47–54.
[30] A.N. Popandopulo, L.T. Zhukova, Transformations in high-speed steels during cold
treatment, Met. Sci. Heat Treat. 22 (10) (1980) 708–710.
[31] R. Singh, K. Singh, Enhancement of tool material machining characteristics with
cryogenic treatment: a Review, in: Proceedings of the 2010 International
Conference on Industrial Engineering and Operations Management Dhaka,
Bangladesh, 2010, pp. 9–10.
[32] D.M. Lal, S. Renganarayanan, A. Kalanidhi, Cryogenic treatment to augment wear
resistance of tool and die steels, Cryogenics 41 (3) (2001) 149–155.
[33] Y.M. Rhyim, S.H. Han, Y.S. Na, J.H. Lee, Effect of deep cryogenic treatment on
carbide precipitation and mechanical properties of tool steel, Solid State Phenom.
118 (2006) 9–14. https://dx.doi.org/10.4028/www.scientific.net/SSP.118.9.
[34] A. Pellizzari, M. Molinari, Deep cryogenic treatment of cold work tool steel, Proc.
6th Int. Tool. Conf. 1 (2002) 657–669.
[35] D.N. Collins, Deep cryogenic treatment of tool steels; a review, Heat Treat. Met. 2
(1996).
[36] F. Meng, K. Tagashira, H. Sohma, Wear resistance and microstructure of cryogenic
treated Fe-1. 4Cr-1C bearing steel, Scr. Metall. Mater. States) 31 (7) (1994).
[37] D.J. Kamody, Using deep cryogenics to advantage, Adv. Mater. Process. 154 (4)
(1998) 215–218.
[38] S. Hadi, E. Widiyono, W. Winarto, D.Z. Noor, EMS-45 tool steels hardenability
experiment using Jominy ASTM A255 test method, IPTEK J. Technol. Sci. 24 (1)
(2013), https://doi.org/10.12962/j20882033.v24i1.137.
[39] B.D. Cullity, Elemen of X-Ray Diffraction, Addison Wcsley Pusblishing Company,
USA, 1978, p. 531.
[40] N. Yamanaka, K. Kusaka, A. Tonooka, M. Hirayama, Effect of carbon and vanadium
on the properties of shock-resisting tool steel (ii), Tetsu-To-Hagane 42 (8) (1956)
648–652, https://doi.org/10.2355/tetsutohagane1955.42.8_648.
[41] M.K. El Fawkhry, A.M. Fathy, The effect of bad heat treatment technology on
failure mode of armor steel sheet under EN1522 ballistic test, Int. J. Mater.
Technol. Innov. 1 (1) (2021) 30–44.
[42] A. Kumar, Estimation of crystallite size, lattice strain and micro residual stresses by
FWHM method and impact of feed rates on residual stresses, IOP Conf. Ser. Mater.
Sci. Eng. 988 (1) (2020), https://doi.org/10.1088/1757-899X/988/1/012064.
[43] K. Amini, A. Akhbarizadeh, S. Javadpour, Effect of deep cryogenic treatment on the
formation of nano-sized carbides and the wear behavior of D2 tool steel, Int. J.
Miner. Metall. Mater. 19 (9) (2012) 795–799, https://doi.org/10.1007/s12613-
012-0630-2.
[44] D.N. Collins, J. Dormer, Deep cryogenic treatment of a D2 cold-work tool steel,
Heat Treat. Met. 24 (3) (1997) 71–74.
[45] R.N. Elshaer, M.K. El-Fawakhry, A.I.Z. Farahat, Behavior of carbon steel machine
elements in acidic environment: surface texture using Abbott Firestone curve,
Metallogr. Microstruct. Anal. 10 (5) (2021) 700–711, https://doi.org/10.1007/
s13632-021-00787-x.
[46] C. Georgescu, G.C. Cristea, C. Dima, L. Deleanu, Evaluating lubricating capacity of
vegetal oils using Abbott-Firestone curve, IOP Conf. Ser. Mater. Sci. Eng. 174 (1)
(2017), 12057.