crystals
Article
Mechanical Properties of Pack Carburized SCM 420 Steel
Processed Using Natural Shell Powders and Extended
Carburization Time
Ramli 1 , Chung-Chun Wu 1, * and Adel Shaaban 2






Citation: Ramli; Wu, C.-C.; Shaaban,
A. Mechanical Properties of Pack
Carburized SCM 420 Steel Processed
Using Natural Shell Powders and
Extended Carburization Time.
Crystals 2021, 11, 1136. https://
doi.org/10.3390/cryst11091136
Academic Editor: Cyril Cayron
Received: 12 July 2021
Accepted: 15 September 2021
Published: 18 September 2021
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
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iations.
Copyright: © 2021 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Crystals 2021, 11, 1136. https://doi.org/10.3390/cryst11091136
1 Mechanical Engineering Department, Southern Taiwan University of Science and Technology,
Tainan 71005, Taiwan; ramli.barmawi83@gmail.com
2 National Center for Radiation Research (NCRRT), Department of Radiation Engineering, Atomic Energy
Authority, Cairo 11765, Egypt; engadelsas@gmail.com
* Correspondence: wcc@stust.edu.tw
Abstract: The feasibility of using coconut shell powder (CSP) and dog conch shell powder (DCSP) as
carburizing media in the pack carburization of SCM 420 steel was investigated. The carbon content
and surface hardness of the carburized specimens prepared with different CSP:DCSP ratios and
carburizing durations were examined and compared. A CSP:DCSP ratio of 60%:40% and an extended
carburizing time of 12 h were found to increase the carbon content of the carburized specimens to
1.14 ± 0.007 wt%. Furthermore, the surface hardness was significantly improved to 961.3 ± 4.918 HV
following water quenching. Finally, the thickness of the carburized layer of the quenched specimens
increased by around 2.5 times as the carburizing duration was increased from 3 to 12 h.
Keywords: packed carburization; dog conch shell; carburizing time; activated carbon; hardness;
carbon content
1. Introduction
Low-to-medium-carbon steels, such as SCM 420, have excellent ductility and high
toughness, and are therefore used to manufacture many automobile components, such as
racks and gears, shafts, pinions, cams, rockers, axles, valves, and so on [1–4]. However, low-
carbon steels have low hardness and poor mechanical strength. Consequently, in real-world
applications, surface treatment is commonly applied to ensure that the components reach
the necessary performance standards. Traditional heat-treatment methods fail to yield a
significant improvement in the strength and hardness of low-carbon steel components.
Thus, induction hardening, cold-working, immersion hardening, and case carburizing are
generally preferred [5–7]. Among these methods, case carburizing is particularly effective
and is thus one of the most commonly used [8]. In the pack carburization process, the
components are packaged into a carbon powder box and heated at a temperature higher
than a certain critical value to prompt the diffusion of carbon atoms into the component
surface. The carburized component is then either left to cool naturally in the furnace,
or is removed from the furnace and quenched in water. The finished component has an
extremely high surface hardness while retaining the natural toughness and ductility of the
original material in the core [9,10]. Importantly, the material properties of the component
can be tuned by adjusting the time and temperature of the carburizing process [11–14].
Generally speaking, a longer carburizing time and a higher temperature result in a thicker
carbon diffusion layer and hence a greater surface hardness [15–18].
Many different materials can be used as the carbon source in the pack carburizing pro-
cess, including barium carbonate (BaCO3 ), sodium carbonate (NaCO3 ), and charcoal [19–25].
In addition, various shells and bones have been considered as the energizing source for
carburization. For example, Darmo et al. [26] performed the pack carburization of SS400
steel cylinders using teak wood charcoal and Pomacea Canalikulata Lamarck (PCL) shell
https://www.mdpi.com/journal/crystals
Crystals 2021, 11, 1136 2 of 17

powder as the carbon source and energizing medium, respectively. The results showed that
the addition of PCL shell power yielded an effective increase in the hardness of the SS400
components. Soenoko et al. [27] also used PCL shell powder to energize the carburization of
SS400 steel components and found that the fatigue strength of the final components could
be enhanced through tempering and then quenching the carburized parts in 30% NaCl
solution. Aramide et al. [28] found that the addition of pulverized bone as an energizer
improved both the impact resistance and the stiffness of carburized mild steel specimens.
Negara and Widiyarta [29] performed the pack carburization of low carbon steel using
goat bone charcoal (GBC) or bamboo charcoal (BC) as the carburizing medium. The results
showed that a significant improvement in the hardness, tensile strength, yield strength,
and elastic modulus could be obtained given an appropriate choice of carburizer (i.e., GBC
or BC). Miswanto et al. [30] significantly improved the carbon content of low-carbon steel
by utilizing a combination of cow bone and coconut shell charcoal as carburizing media.
The feasibility of using seafood shells as energizing sources for the packed carburiza-
tion process has received considerable attention in recent years. Seafood shells are generally
treated as garbage. Therefore, reusing them as an energizing source in the carburization
process has significant environmental benefits. In a previous study [31], the present group
showed that the addition of dog conch shell powder (DCSP) improved the carbon content
of SCM 420 from 0.221 wt% to 0.647 wt% given a carburizing temperature of 950 ◦ C and a
DCSP content of 40%. Moreover, the surface hardness increased from 165.61 ± 4.67 HV to
850.10 ± 4.84 HV following quenching. However, the study only considered a carburizing
duration of 3 h. Therefore, the present study investigated the elemental composition,
microhardness, microstructure, and carbon diffusion layer thickness of SCM 420 specimens
carburized using DCSP and coconut shell powder (CSP) for durations of 3, 6, and 12 h,
respectively. For each carburizing experiment, the carburizing temperature was fixed as
950 ◦ C and the DCSP content was set in the range of 10–50%. Following the carburization
process, the specimens were allowed to cool naturally in the furnace. Some of the samples
were then reheated to 950 ◦ C for 10 min and then quenched in water to investigate the
effect of the quenching process on the hardness of the samples.

2. Materials and Methods

The carburizing trials were performed using SCM 420 steel bars with a length and
diameter of 50 mm and 20 mm, respectively. The samples were placed in a low-carbon steel
carburizing box with dimensions of 240 × 120 × 80 mm3 (length × width × height) and a
thickness of 5 mm. The experiments were conducted using CSP:DCSP percentage ratios
of 100%:0%, 90%:10%, 80%:20%, 70%:30%, 60%:40% and 50%:50%, respectively. In each
experiment, the specified quantity of carburizing media (CSP and DCSP) was added to the
box and the box was then placed in an electric furnace and heated at 950 ◦ C for 3, 6, and
12 h. To prevent oxidation, nitrogen gas was circulated continuously through the furnace
during the entire carburization process. The specimens were allowed to cool naturally
to room temperature in the electric furnace after the carburizing process. To investigate
the effect of quenching on the microhardness of the carburized specimens, all carburized
specimens were re-heated at a temperature of 950 ◦ C for 10 min and then rapidly coo
in water.
The carburized and quenched samples were machined into test pieces and polished
with a motor-driven disk grinder and polisher to a certain surface roughness. Microhard-
ness measurements were carried out using a Vickers hardness testing machine (Wilson
Hardness, Tukon 1102, China) under a 1 kgf load. To ensure the reliability of the mea-
surement results, the hardness was measured five times (using a new sample each time)
for every experimental condition. The five measurement results were then averaged to
obtain a representative value for the sample. The chemical compositions of the carburizing
media were identified by Scanning Electron Microscopy (SEM) machine (Hitachi S-3000N,
Tokyo, Japan) with a detector energy dispersive spectroscopy (EDS) (X-maxN20, Horiba
Ltd., Tokyo, Japan). The activated carbon made of coconut shell powders (CSP) from
Crystals 2021, 11, 1136 3 of 17

the company was washed with distilled water repeatedly to remove the contaminants
and then dried in a furnace at 60 ◦ C overnight. Before being powdered, the dog conch
shell was immersed in a 10% H2SO4 solution for 6 h, then washed with distilled water
repeatedly and dried in an oven for 24 h at 60 ◦ C to remove any impurities. In addition, the
carbon content of the various SCM 420 carburized and quenched samples was analyzed
using glow discharge spectrometry (GDS) (Leco-GDS500A, Michigan, MI, USA). Before
performing GDS analysis, all samples were ground with 120-grit ZrO2 pape to smooth
out the surface and washed in alcohol, then dried with an air compressor to remove any
surface impurities. Again, to ensure the reliability of GDS analysis results, the carbon
content was measured three times per sample (five samples for each carburizing condition),
and was then averaged to find a representative value for each experimental condition. Fur-
thermore, the carbon content value distributed within the carburized layer of the quenched
specimen was also measured three times per depth carburizing layer of 100 µm. The phase
compositions of the carburizing media and treated specimens were examined by X-ray
diffractometry (XRD) (Bruker D2 Phaser, Karlsruhe, Germany) using a diffraction angle
range of 20–80◦ and CuKα radiation. Finally, the microstructures of the specimens were
observed by optical microscopy (Olympus BX51M, Tokyo, Japan).

3. Results and Discussion

3.1. Phase and Chemical Composition of Carburizing Media and Specimens
The EDS analysis results for the chemical composition of the CSP and DCSP used
as carburizing media in the pack carburizing experiments are shown in Figures 1 and 2.
Three different spectrum areas were detected to analyzed chemical compositions for each
carburizing medium. From Figure 1, the EDS analysis revealed that the carbon element
was present in a higher amount than Ca and O elements. This result indicated that CSP
particle is mainly made of carbon. Furthermore, referring to the EDS results presented in
Figure 2, it is seen that the 100% DCSP also consists of Ca, C, and O elements. However,
the amount of carbon element is lower than Ca and O. Figure 3 presents the XRD results
for the CSP and DCSP media. The XRD patterns reveal that the pure CSP (i.e., 100% CSP)
had an amorphous carbon (C) structure. This result is consistent with XRD patterns of
graphitic carbon for FeGC1100 non-catalyst sample [32], and also XRD results of activated
carbon from rubber fruit shell using KOH activation [33]. The pure DCSP (i.e., 100%
DCSP) had an orthorhombic aragonite (CaCO3 ) structure [34]. Notably, the orthorhombic
aragonite phase persisted even after mixing the DCSP with CSP in various quantities
(i.e., 90%:10%, 80%:20%, 70%:30%, 60%:40% and 50%:50%, respectively), as shown in
Figure 4 [31]. However, the peak position of the aragonite CaCO3 shifted slightly to the
right as the DCSP concentration increased.
Figure 5 shows the XRD analysis results for the original SCM 420 raw material and
the carburized samples prepared using a CSP:DCSP ratio of 60%:40% and carburizing du-
rations of 3, 6, and 12 h, respectively. (Note that for the carburized samples, XRD patterns
are presented for both the as carburized samples and the quenched samples.) As shown,
the original SCM 420 raw material had a high Fe-intensity peak and a body-centered cubic
(BCC) crystal structure. The carburized SCM 420 specimens consisted predominantly of
Fe and Fe3 C phases with a BCC and orthorhombic crystal structure, respectively. Finally,
the quantity of Fe3 C phase increased following the quenching process, particularly in
the specimens carburized for a longer duration. The presence of (Fe3 C) carbides on
the quenched specimens was pointed out by SEM/EDS observations, as illustrated in
Figures 6 and 7. From Figure 6, it can be clearly seen that some Fe3 C carbides existed in
the carburized and diffusion layers of the specimen. Figure 7 shows the EDS analysis
results of quenched specimens in different areas. Base on EDS results, some particles were
enriched in carbon elements, showing that these particles were Fe3 C carbides. This result
is consistent with the result of the XRD analysis depicted in Figure 5.
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Figure
Figure1.1.
Figure 1.EDS
EDSanalysis
EDS analysis results
analysis for CSP.
results for
results for CSP.
CSP.

Figure
Figure 2.
2. EDS
EDS analysis
analysis results
results for
for DCSP.
DCSP.
Figure 2. EDS analysis results for DCSP.
Crystals 2021, 11,
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(111)
(111)

(221)
(221)
(012)

(112)

(220)
(012)
(021)
Dog Conch Shell Powder (100% DCSP)

(112)

(220)
(200)
(021)

(130)
Dog Conch Shell Powder (100% DCSP)

(113)
(202)
(132)
(110)

(200)
(002)

(211)
(130)

(014)
(113)

(313)
(311)
(202)

(400)
(132)
(110)

(002)

(211)

(014)

(313)
(311)

(400)
(a.u)
(a.u)

(002)
(002)
Intensity
Intensity

(100)
(100)
(111)
(111)

Coconut Shell Powder (100% CSP)

(021)

(112)
(012)

Coconut Shell Powder (100% CSP)

(021)

(112)
(200)

(202)

(113)
(012)

(132)
(220)

(221)
(130)
Orthorhombic Aragonite CaCO3 JCPDS 71-2396

(211)
(200)

(202)
(110)

(113)
(002)

(132)
(220)

(221)
(130)

(014)

(400)
(311)

(313)
Orthorhombic Aragonite CaCO3 JCPDS 71-2396

(211)
(110)

(002)

(014)

(400)
(311)

(313)
Amorphous Carbon (C)
(002)

(100)
Amorphous Carbon (C)
(002)

(100)

20 30 40 50 60 70 80
20 30 40 50
2θ(deg.) 60 70 80
2θ(deg.)
Figure 3. XRD
Figure 3. XRD analysis
analysis results for pure
results for pure CSP
CSP and
and DCSP.
DCSP.
Figure 3. XRD analysis results for pure CSP and DCSP.
(111)
(020)

(021)
(110)

(111) (111)
(020)

(021)
(110)

(221)
(012)

(220)
(002)

(112)

(221)
(200)

(202)
(012) (012)

(220)

(132)
(113)
(002)

(112) (112)

90% CSP + 10% DCSP

(200)(200)

(311)
(111)

(202) (202)
(132) (132)

(113) (113)

90% CSP + 10% DCSP

(021)
(020)

(311)

(313)
(110)

(014)
(021)
(020)

(221)

(313)
(110)

(220)

(014)
(200)

(221)
(211)
(012)

(112)

(220) (220)

80% CSP + 20% DCSP

(202) (202)
(211) (211)
(111)

(113) (113)
(132) (132)

80% CSP + 20% (313)

DCSP
(111)
(021)
(a.u)

(020)
(110)

(313)
(221)
(012)
(021)

(112)
(a.u)

(020) (020)
(110)

(200)

(221) (221)
(012) (012)

(112) (112)

70% CSP + 30% DCSP

(220)

(202) (202)
(132) (132)
(200) (200)

(211)

(113) (113)
Intensity

(111) 70% CSP + 30%(313)

DCSP
Intensity

(111)
(021) (313)
(020)

(220)

(221) (221)
(112) (112)
(012) (012)

(021)
(220) (220)
(200) (200)

60% CSP + 40% DCSP

(202) (202)
(132) (132)
(113) (113)

(111)
60% CSP + 40% DCSP
(021)

(111)
(110)

(021)

(002)
(012)

(211)

(221) (221)
(112)

(220)
(110)

50% CSP + 50% DCSP

(200)

(202)
(002)

(113)
(211)

(132)

50% CSP + 50%(313)

(014) DCSP
(014) (313)
(021)

Orthorhombic Aragonite CaCO3

(012)

(221)
(112)
(021)

(200)

Orthorhombic Aragonite CaCO3

(132)
(012)

(202)

(113)
(111)

(112)

JCPDS 71-2396
(220)
(200)

(211)

(132)

(313)
(202)

(113)
(111)

(311)
(002)
(110)

(014)
(020)

JCPDS 71-2396
(220)
(211)

(313)
(311)
(002)
(110)

(014)
(020)

20 30 40 50 60 70 80
20 30 40 50 60 70 80
2θ(deg.)
2θ(deg.)
Figure 4. XRD analysis results for various CSP:DCSP ratios “Reprinted from [31] under the CC BY
Figure 4.
Figure 4. XRD
license”. XRDanalysis
analysisresults
resultsfor
forvarious
variousCSP:DCSP
CSP:DCSPratios “Reprinted
ratios from
“Reprinted [31][31]
from under the the
under CC CC
BY
license”.
BY license”.
Figure 5 shows the XRD analysis results for the original SCM 420 raw material and
Figure 5 shows
the carburized samplestheprepared
XRD analysis
usingresults for theratio
a CSP:DCSP original SCM 420
of 60%:40% raw
and material and
carburizing du-
the carburized samples prepared using a CSP:DCSP ratio of 60%:40% and carburizing
rations of 3, 6, and 12 h, respectively. (Note that for the carburized samples, XRD patterns du-
rations of 3, 6, and 12 h, respectively. (Note that for the carburized samples,
are presented for both the as carburized samples and the quenched samples.) As shown,XRD patterns
are original
the presented SCMfor 420
both thematerial
raw as carburized samples
had a high and the peak
Fe-intensity quenched
and a samples.) As shown,
body-centered cubic
the original SCM 420 raw material had a high Fe-intensity peak and a body-centered
(BCC) crystal structure. The carburized SCM 420 specimens consisted predominantly cubic
of
(BCC) crystal structure. The carburized SCM 420 specimens consisted predominantly
Fe and Fe3C phases with a BCC and orthorhombic crystal structure, respectively. Finally, of
Fe and Fe 3C phases with a BCC and orthorhombic crystal structure, respectively. Finally,
the quantity of Fe3C phase increased following the quenching process, particularly in the
the quantitycarburized
specimens of Fe3C phasefor increased following the
a longer duration. Thequenching
presence process,
of (Fe3C)particularly
carbides onin the
the
specimens carburized for a longer duration. The presence of (Fe3C) carbides on the
 quenched specimens was pointed out by SEM/EDS observations, as illustrated in Figure
quenched
6; Figure specimens
7. From was pointed
Figure out by
6, it can be SEM/EDS observations,
clearly seen that some as
Feillustrated in Figure
3C carbides existed in the
6;carburized
Figure 7. and
Fromdiffusion
Figure 6,layers
it can of
be the
clearly seen that some Fe3C carbides existed in the
specimen. Figure 7 shows the EDS analysis results
carburized and diffusion layers of the specimen. Figure 7 shows the EDS analysis results
of quenched specimens in different areas. Base on EDS results, some particles were en-
Crystals 2021, 11, 1136 of quenched specimens in different areas. Base on EDS results, some particles were en-6 of 17
riched in carbon elements, showing that these particles were Fe3C carbides. This result is
riched in carbon elements, showing that these particles were Fe3C carbides. This result is
consistent with the result of the XRD analysis depicted in Figure 5.
consistent with the result of the XRD analysis depicted in Figure 5.

Fe
Fe

(a) Before carburizing (raw material)

(a) Before carburizing (raw material)
Fe Fe

(b)carburizing
(b) After After carburizing for 3 hours
for 3 hours
Fe3C
Fe3C Fe Fe
(c)carburizing
(c) After After carburizing for 6 hours
for 6 hours
Fe Fe
Fe3C Fe3C
Intensity (a.u)
(a.u)

(d) After
(d)carburizing for 12 hours
After carburizing for 12 hours
Fe Fe3C Fe3C
Fe

(e) Carburizing for 3 hours

for 3 and quenching by waterby water
Intensity

(e) Carburizing hours and quenching

Fe3C
Fe3C Fe Fe3Fe
C Fe C
3
(f) Carburizing for 6 hours
(f) Carburizing for 6 and quenching
hours by waterby water
and quenching
Fe3C Fe Fe3Fe Fe3C
C Fe
Fe3C 3C Fe3C

(g) Carburizing for 12 hours and quenching by water

(g) Carburizing for 12 hours
C FeandC quenching by water
Fe3C C Fe3C Fe Fe3Fe Fe33C Fe3C
Fe3C C Fe3C

(110)

(200)
BCC Fe JCPDS 06-0696

(110)

(200)
BCC Fe JCPDS 06-0696

(006)
Carbon (C) JCPDS 50-1083

(006)
Carbon (C) JCPDS 50-1083
Orthorhombic Fe3C

(222)
(200)

Orthorhombic Fe3C

(240)

(232)
(123)
(222)
JCPDS 65-2412
(200)

(240)

(232)
(123)
JCPDS 65-2412

20 30 40 50 60 70 80
20 30 40 50 60 70 80
2θ(deg.)
2θ(deg.)
Figure
Figure 5.
5. XRD
XRDanalysis
analysisresults
resultsforfor
original SCM
original SCM420420
rawraw
material andand
material carburized and and
carburized quenched
quenched
Figure
SCM
SCM 4205.
420 XRD analysis
specimens
specimenspreparedresults
prepared with
with fora original
a CSP:DCSP
CSP:DCSP SCM
ratio 420
of
ratio ofraw material
60%:40% andand
60%:40% and carburized
carburizing and
durations
carburizing of quenched
durations3, 6,
of 3, 6,
SCM
and 12 420
h. specimens prepared with a CSP:DCSP ratio of 60%:40% and carburizing durations of 3, 6,
and 12 h.
and 12 h.

Figure 6. The SEM micrograph of quenched specimens carburized using a CSP:DCSP ratio of
60%:40% and a carburizing time of 12 h.
Figure6.6. The
Figure The SEM
SEM micrograph
micrograph of of quenched
quenched specimens
specimens carburized
carburized using
using aaCSP:DCSP
CSP:DCSPratio
ratioofof
60%:40%and
60%:40% andaacarburizing
carburizingtime
timeofof12
12h.h.
Crystals 2021, 11, 1136 7 of 17
Crystals 2021, 11, x FOR PEER REVIEW 7 of 18

Figure 7.
Figure 7. EDS
EDS analysis
analysis result
result on
on the
the different
different areas
areas of
of quenched
quenched specimens
specimens carburized
carburized with
with aa CSP:DCSP
CSP:DCSP ratio
ratio of
of 60%:40%
60%:40%
and a carburizing time of 12 h.
and a carburizing time of 12 h.

Table
Table 1 1 shows
shows the
the lattice
lattice constant
constant values
values ofof various
various phases
phases for
for different
different carburizing
carburizing
media
media concentrations shown in Figures 3 and 4. For each concentration, a gapgap
concentrations shown in Figure 3; Figure 4. For each concentration, a existed
existed be-
between the standard and calculated values of the lattice constants. Moreover,
tween the standard and calculated values of the lattice constants. Moreover, the magnitude the magni-
tude
of theofgapthevaried
gap varied with
with the the CSP/DCSP
CSP/DCSP ratio.inspection,
ratio. From From inspection,
the minimalthe minimal
gap occurredgap oc-
for
curred for the
the sample withsample with a ratio
a CSP:DCSP CSP:DCSP ratio ofwhich
of 60%:40%, 60%:40%, which
indicates thatindicates that the
the aragonite arago-
(Ca-CO 3)
nite (Ca-CO
phases 3) phases
for this for CSP:DCSP
particular this particular
ratioCSP:DCSP
were moreratio were
stable thanmore
thosestable thanCSP:DCSP
for other those for
other CSP:DCSPTable
concentrations. concentrations.
2 shows theTable 2 shows
standard and the standard
calculated and constant
lattice calculatedvalues
latticeofcon-
the
stant values of the SCM 420 base material, carburized specimens,
SCM 420 base material, carburized specimens, and quenched specimens shown in Figure 5. and quenched speci-
mens shown
Generally in Figure
speaking, 5. Generally
a good agreement speaking, a goodbetween
was observed agreement was observed
the standard between
and calculated
the standard
lattice constant andvalues
calculated lattice
in every constant
case. Hence,values in every
it is inferred case.
that all Hence, it is inferred
of the phases formed that
in
theofvarious
all specimens
the phases formedwere relatively
in the variousstable.
specimens were relatively stable.
Crystals 2021, 11, 1136 8 of 17

Table 1. Lattice constants of various phases for different carburizing media concentrations.

Relative Concentration of Standard

JCPDS Lattice Constant Calculated Values (Å)
Carburizing Media Values (Å)
a 4.961 4.946
100% DCSP b 7.970 7.884
c 5.739 5.717
a 4.961 4.998
CSP:DCSP ratio of 90%:10% b 7.970 7.937
c 5.739 5.430
a 4.961 4.972
Orthorhombic b 7.970 7.921
CSP:DCSP ratio of 80%:20%
Aragonite (CaCO3 ) c 5.739 5.917
JCPDS 71-2396
a 4.961 4.967
CSP:DCSP ratio of 70%:30% b 7.970 7.909
c 5.739 5.704
a 4.961 4.960
CSP:DCSP ratio of 60%:40% b 7.970 7.981
c 5.739 5.765
a 4.961 4.951
CSP:DCSP ratio of 50%:50% b 7.970 7.897
c 5.739 5.382

Table 2. Lattice constants of various phases in original SCM 420 steel; carburized samples with a CSP:DCSP ratio of 60%:40%
and carburizing durations of 3, 6 and 12 h, respectively; and quenched specimens.

Specimen JCPDS Lattice Constant Standard Values (Å) Calculated Values (Å)
Body centered cubic Iron, syn
Original SCM 420 raw material a=b=c 2.886 2.870
(Fe) JCPDS 6-696
Body centered cubic Iron, syn
a=b=c 2.886 2.865
(Fe) JCPDS 6-696
SCM 420 carburized specimens with
40% DCSP for 3 h a 5.089 5.029
Orthorhombic Iron carbide b 6.743 6.601
(Fe3 C) JCPDS 65-2412 c 4.523 4.564
Body centered cubic Iron, syn
a=b=c 2.886 2.870
(Fe) JCPDS 6-696
SCM 420 carburized specimens with
40% DCSP for 6 h a 5.089 5.044
Orthorhombic Iron carbide b 6.743 6.684
(Fe3 C) JCPDS 65-2412 c 4.523 4.526
Body centered cubic Iron, syn
a=b=c 2.886 2.874
(Fe) JCPDS 6-696
SCM 420 carburized specimens with
40% DCSP for 12 h a 5.089 5.043
Orthorhombic Iron carbide b 6.743 6.670
(Fe3 C) JCPDS 65-2412 c 4.523 4.526
Body centered cubic Iron, syn
a=b=c 2.886 2.848
(Fe) JCPDS 6-696
SCM 420 carburized specimens with
40% DCSP for 3 h after quenching a 5.089 5.076
Orthorhombic Iron carbide b 6.743 6.712
(Fe3 C) JCPDS 65-2412 c 4.523 4.501
Body centered cubic Iron, syn
a=b=c 2.886 2.887
(Fe) JCPDS 6-696
SCM 420 carburized specimens with
40% DCSP for 6 h after quenching a 5.089 5.112
Orthorhombic Iron carbide b 6.743 6.921
(Fe3 C) JCPDS 65-2412 c 4.523 4.557
Body centered cubic Iron, syn
a=b=c 2.886 2.848
(Fe) JCPDS 6-696
SCM 420 carburized specimens with a 2.522 2.497
Carbon (C) JCPDS 50-1083 c 12.35 12.201
40% DCSP for 12 h after quenching
a 5.089 5.061
Orthorhombic Iron carbide b 6.743 6.654
(Fe3 C) JCPDS 65-2412 c 4.523 4.526
Crystals 2021, 11, 1136 9 of 17

Table 3 shows the average grain size of the SCM 420 raw material; carburized SCM
420 samples with a CSP:DCSP ratio of 60%:40% and carburizing durations of 3, 6, and 12 h,
respectively; and quenched SCM 420 samples. Note that the grain size was determined
directly from the FWHM data of the corresponding XRD patterns shown in Figure 5. It is
seen that the original SCM 420 material had an average grain size of 14.54 ± 0.09 µm, while
the carburized samples processed for 3, 6 and 12 h had average grain sizes of 12.71 ± 0.11,
10.18 ± 0.13 and 6.57 ± 0.07 µm, respectively. After quenching, the average grain size
reduced further to 7.76 ± 0.10, 5.97 ± 0.09, and 5.72 ± 0.12 µm, respectively. Overall, the
results show that the carburizing and quenching processes both led to a grain refinement
effect. Furthermore, a significant reduction in the grain size also occurred as the carburizing
duration increased.

Table 3. The average grain size of original SCM 420 raw material; carburized samples with a CSP:DCSP ratio of 60%:40%
and carburizing durations of 3, 6, and 12 h, respectively; and quenched samples.

Specimen Average Grain Size D (µm)

Original SCM 420 raw material 14.54 ± 0.09
SCM 420 carburized specimens with 40% DCSP for 3 h 12.71 ± 0.11
SCM 420 carburized specimens with 40% DCSP for 6 h 10.18 ± 0.13
SCM 420 carburized specimens with 40% DCSP for 12 h 6.57 ± 0.07
SCM 420 carburized specimens with 40% DCSP for 3 h after quenching 7.76 ± 0.10
SCM 420 carburized specimens with 40% DCSP for 6 h after quenching 5.97 ± 0.09
SCM 420 carburized specimens with 40% DCSP for 12 h after quenching 5.72 ± 0.12

Table 4 shows the chemical composition of the original SCM 420 material. It is seen
that the sample had a carbon content of 0.221 wt% [31]. Figure 8 shows the carbon contents
of the carburized samples prepared with various CSP:DCSP ratios and carburizing dura-
tions. For each carburizing time, the samples prepared using only CSP as the carburizing
medium exhibited the lowest carbon content. By contrast, the samples prepared with
a CSP:DCSP ratio of 60%:40% exhibited the highest carbon content, irrespective of the
carburizing duration applied. In general, the results presented in Figure 8 show that as the
stability of the CaCO3 phase increased, its effectiveness as an energizer also increased (see
Table 1). The results additionally show that for all values of the CSP:DCSP ratio, the carbon
content increased with an increasing carburizing time. The maximum carbon content
(1.14 ± 0.007 wt%) was that obtained in the SCM 420 sample treated with a CSP:DCSP
ratio of 60%:40% and a carburizing duration of 12 h. It is noted that this value is approxi-
mately 1.76 times higher than that obtained in a previous study (0.647 ± 0.008 wt%) with a
lower carburizing time of just 3 h [31]. Moreover, it is also around 1.46 times higher than
that obtained in another previous study (0.78 wt%) using 30% PCL shell powder and a
carburizing time of 7 h [26].

Table 4. Chemical composition of original SCM 420 raw material. “Reprinted from [31] under the CC BY license”.

Specimen C Si Mn P S Cr Ni Mo Cu Fe
Raw material of
0.221 0.248 0.641 0.012 0.013 0.947 0.048 0.140 0.063 Bal.
SCM 420 Steel
 Table 4. Chemical composition of original SCM 420 raw material. “Reprinted from [31] under the
CC BY license”.

Specimen C Si Mn P S Cr Ni Mo Cu Fe
Raw
Crystals 2021, 11, 1136material
of 10 of 17
0.221 0.248 0.641 0.012 0.013 0.947 0.048 0.140 0.063 Bal.
SCM 420 Steel

1.2
1.14
3 Hours
6 Hours
1.0 12 Hours
0.896 0.906
0.879
Carbon content (wt %)

0.8 0.761
0.791

0.687 0.693
0.673
0.647
0.61
0.6
0.536
0.512 0.502
0.485
0.457
0.437
0.414
0.4

0.2

0.0
100% CSP + 90% CSP + 80% CSP + 70% CSP + 60% CSP + 50% CSP +
0% DCSP 10% DCSP 20% DCSP 30% DCSP 40% DCSP 50% DCSP
Various concentrated compounds
Figure 8. The average carbon content of SCM 420 steel specimens with various CSP:DCSP ratios and carburizing durations.
Figure 8. The average carbon content of SCM 420 steel specimens with various CSP:DCSP ratios and
carburizing durations.
3.2. Surface Hardness of Carburized and Quenched SCM 420 Specimens

3.2. Surface Hardness ofFigure 9 presents

Carburized the surfaceSCM
and Quenched hardness values of the SCM 420 carburized samples
420 Specimens
prepared with various CSP:DCSP concentrations and carburizing durations of 3, 6, and
Figure 9 presents the surfaceFigure
12 h, respectively. hardness values
10 shows theofequivalent
the SCMresults
420 carburized samples
for the samples reheated to a
prepared with various CSP:DCSP
temperature ◦
of 950 concentrations andthen
C for 10 min and carburizing
quencheddurations
in water. of
For3,both
6, and
types of the
12 h, respectively. Figure (i.e.,
specimen 10 shows the equivalent
carburized results
and quenched), for the samples
the hardness increasedreheated to aconcentra-
as the DCSP
temperature of 950tion
°Cincreased
for 10 minfrom 10–40%.
and However, the
then quenched hardness
in water. Forreduced as the
both types ofDCSP concentration
the spec-
was further
imen (i.e., carburized increased tothe
and quenched), 50%. Moreover,
hardness the hardness
increased as thealso increased
DCSP with an increasing
concentration
carburizing time. For the non-quenched samples, the maximum hardness was around
604.9 ± 4.674 HV (CSP:DCSP ratio: 60%:40%; carburizing time: 12 h). It is approximately
1.72 times higher than that obtained in a previous study (352.70 ± 4.96 HV) with a lower
carburizing time of 3 h [31]. This result related to the quantity of pearlite on the microstruc-
ture of SCM 420 steel-carburized specimen attained with a carburizing time of 12 h is
more than that obtained with carburizing times of 6 and 3 h, respectively, as illustrated
in Figure 11. Comparing the results presented in Figure 9; Figure 10, it is seen that the
quenching process resulted in a significant improvement in the hardness of all the samples.
For example, the surface hardness of the optimal sample in Figure 9 (CSP:DCSP ratio:
60%:40%; carburizing time: 12 h) increased from 604.9 ± 4.674 HV in the as-carburized
condition to 961.3 ± 4.918 HV in the quenched condition.

Crystals 2021, 11, 1136
ture of SCM 420 steel-carburized specimen attained with a carburizing time of 12 h is more
than that obtained with carburizing times of 6 and 3 h, respectively, as illustrated in Figure
11. Comparing the results presented in Figure 9; Figure 10, it is seen that the quenching
process resulted in a significant improvement in the hardness of all the samples. For ex-
ample, the surface hardness of the optimal sample in Figure 9 (CSP:DCSP ratio: 60%:40%; 11 of 17
carburizing time: 12 h) increased from 604.9 ± 4.674 HV in the as-carburized condition to
961.3 ± 4.918 HV in the quenched condition.

650
3 Hours
600 6 Hours
12 Hours
550

Vickers hardness (HV) 500

450

400

350

300

250

200
100% CSP 90% CSP + 80% CSP + 70% CSP + 60% CSP + 50% CSP +
10% DCSP 20% DCSP 30% DCSP 40% DCSP 50% DCSP
Various concentrated compounds
Figure
Figure9.9.Surface
Crystals 2021, 11, x FOR PEER REVIEW Surfacehardness
hardnessofofSCM
SCM420
420steel-carburized
steel-carburizedspecimens
specimensprepared
preparedwith
withvarious
variousCSP:DCSP
CSP:DCSP
12 of 18
ratios
ratiosand
andcarburizing
carburizingtimes.
times.

1000
3 Hours
6 Hours
950
12 Hours
900
Vickers hardness (HV)

850

800

750

700

650

600

100% CSP 90% CSP + 80% CSP + 70% CSP + 60% CSP + 50% CSP +
10% DCSP 20% DCSP 30% DCSP 40% DCSP 50% DCSP
Various concentrated compounds
Figure 10. Surface
Surface hardness of quenched SCM 420 steel specimens prepared with various CSP:DCSP
CSP:DCSP
ratios and carburizing times.
ratios and carburizing times.
 600

100% CSP 90% CSP + 80% CSP + 70% CSP + 60% CSP + 50% CSP +
10% DCSP 20% DCSP 30% DCSP 40% DCSP 50% DCSP
Various concentrated compounds
Crystals 2021, 11, 1136 12 of 17
Figure 10. Surface hardness of quenched SCM 420 steel specimens prepared with various CSP:DCSP
ratios and carburizing times.

(a)

(b) (c)

Figure 11. Microstructures

Microstructures of SCM 420 carburized specimens prepared
carburized specimens preparedwithwithaa CSP/DCSP
CSP/DCSP ratio of 60%:40% and carburizing
times of:
times of: (a)
(a) 33 h
h “Reprinted from [31]
“Reprinted from [31] under
under the
the CC
CC BY
BY license”,
license”, (b)
(b) 66 h,
h, and
and (c)
(c) 12
12 h.
h.

3.3. Microhardness Profiles of Carburized and Quenched SCM 420 Specimens

Figure 12 shows the microhardness profiles of the quenched SCM 420 specimens
prepared with various CSP:DCSP ratios and a carburizing duration of 3 h. For all of the
samples, the hardness gradually decreased with an increasing distance from the surface and
began to stabilize at a depth of approximately 1300 µm. For a longer carburizing time of 6 h,
the diffusion layer thickness increased to 2300 µm, as shown in Figure 13. Moreover, for
the maximum carburizing time of 12 h, the diffusion layer thickness increased significantly
to 3300 µm, as shown in Figure 14. In other words, the diffusion layer thickness increased
by around 2.5 times as the carburizing duration increased from 3 h to 12 h.
Figure 15 shows the carbon content distribution within the diffusion layer of the
quenched specimen prepared with a CSP:DCSP ratio of 60%:40% and carburizing times of
6 and 12 h. For a carburizing time of 6 h, the maximum carbon content of 0.906 ± 0.008 wt%
in the surface gradually reduced with an increasing depth and approached a constant value
of approximately 0.224 ± 0.006 wt% at a depth of 2300 µm. After extending the carburizing
time to 12 h, the carbon content gradually decreased from 1.14 ± 0.007 wt% at the surface
to 0.225 ± 0.006 wt% at a distance of 3300 µm toward the center. In general, the results
confirmed that the carburizing time has a critical effect on the carburized layer thickness
of pack-carburized SCM 420 steel. Figure 16a–c present OM images of the quenched
specimens prepared with a CSP:DCSP ratio of 60%:40% and carburizing times of 3, 6, and
12 h, respectively. Again, the results confirmed that the depth of the carburized layer
increases with an increasing carburizing time. In order to compare the wear resistance of
the samples, pin-on-disk wear tests were performed with a load of 20 N and a distance of
200 m. Figure 17 shows that the weight loss value for SCM 420 original raw material (i.e.,
 3.3. Microhardness Profiles of Carburized and Quenched SCM 420 Specimens
Figure 12 shows the microhardness profiles of the quenched SCM 420 specimens
prepared with various CSP:DCSP ratios and a carburizing duration of 3 h. For all of the
Crystals 2021, 11, 1136
samples, the hardness gradually decreased with an increasing distance from the surface 13 of 17
and began to stabilize at a depth of approximately 1300 µm. For a longer carburizing time
of 6 h, the diffusion layer thickness increased to 2300 µm, as shown in Figure 13.
Moreover, for the maximum carburizing time of 12 h, the diffusion layer thickness
non-carburized) of 2.8 mg. The quenched specimen prepared with a CSP:DCSP ratio of
increased significantly to 3300 µm, as shown in Figure 14. In other words, the diffusion
60%:40% and a carburizing time of2.512times
layer thickness increased by around h obtained a weight loss
as the carburizing valueincreased
duration of 1.1 mg. This result
from
indicates that
3 h to 12 h. the wear resistance of SCM 420 steel increases after the carburization process.

CSP:DCSP ratio of 100% : 0% for 3 hours at temperature of 950 ⁰C

CSP:DCSP ratio of 90% : 10% for 3 hours at temperature of 950 ⁰C
900
CSP:DCSP ratio of 80% : 20% for 3 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 70% : 30% for 3 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 60% : 40% for 3 hours at temperature of 950 ⁰C
800 CSP:DCSP ratio of 50% : 50% for 3 hours at temperature of 950 ⁰C
Microhardness (HV)

700

600

500

400
0 300 600 900 1200 1500
Depth of carburizing layer (µm)
Crystals 2021, 11, x FOR PEER REVIEW
Figure 12.
Figure 12. Microhardness
Microhardness profiles
profiles of
of SCM
SCM420
420quenched
quenchedspecimens
specimensprepared
preparedwith
withvarious 14 of 18
variousCSP:DCSP
CSP:DCSP concentrations and a carburizing duration of 3 h. “Reprinted from [31] under the CC
concentrations and a carburizing duration of 3 h. “Reprinted from [31] under the CC BY license”.BY
license”.

CSP:DCSP ratio of 100% : 0% for 6 hours at temperature of 950 ⁰C

1000
CSP:DCSP ratio of 90% : 10% for 6 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 80% : 20% for 6 hours at temperature of 950 ⁰C
900 CSP:DCSP ratio of 70% : 30% for 6 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 60% : 40% for 6 hours at temperature of 950 ⁰C
Microhardness (HV)

CSP:DCSP ratio of 50% : 50% for 6 hours at temperature of 950 ⁰C

800

700

600

500

400
0 500 1000 1500 2000 2500
Depth of carburizing layer (µm)
Figure 13. Microhardness
Figure 13. Microhardness profiles
profiles of SCM
of SCM 420 quenched
420 quenched specimens
specimens preparedprepared with
with various various
CSP:DCSP
CSP:DCSP concentrations and a carburizing duration
concentrations and a carburizing duration of 6 h. of 6 h.

CSP:DCSP ratio of 100% : 0% for 12 hours at temperature of 950 ⁰C

1000 CSP:DCSP ratio of 90% : 10% for 12 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 80% : 20% for 12 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 70% : 30% for 12 hours at temperature of 950 ⁰C
 500

400
0 500 1000 1500 2000 2500
Crystals 2021, 11, 1136 Depth of carburizing layer (µm) 14 of 17
Figure 13. Microhardness profiles of SCM 420 quenched specimens prepared with various
CSP:DCSP concentrations and a carburizing duration of 6 h.

CSP:DCSP ratio of 100% : 0% for 12 hours at temperature of 950 ⁰C

1000 CSP:DCSP ratio of 90% : 10% for 12 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 80% : 20% for 12 hours at temperature of 950 ⁰C
CSP:DCSP ratio of 70% : 30% for 12 hours at temperature of 950 ⁰C
900
CSP:DCSP ratio of 60% : 40% for 12 hours at temperature of 950 ⁰C
Microhardness (HV) CSP:DCSP ratio of 50% : 50% for 12 hours at temperature of 950 ⁰C
Crystals 2021, 11, x FOR PEER REVIEW 800 15 of 18

700
value of approximately 0.224 ± 0.006 wt% at a depth of 2300 µm. After extending the
carburizing time to 12 h, the carbon content gradually decreased from 1.14 ± 0.007 wt% at
the surface to 0.225 ± 0.006 wt% at a distance of 3300 µm toward the center. In general, the
600
results confirmed that the carburizing time has a critical effect on the carburized layer
thickness of pack-carburized SCM 420 steel. Figure 16a–c present OM images of the
quenched
500 specimens prepared with a CSP:DCSP ratio of 60%:40% and carburizing times
of 3, 6, and 12 h, respectively. Again, the results confirmed that the depth of the carburized
layer increases with an increasing carburizing time. In order to compare the wear
resistance
400 of the samples, pin-on-disk wear tests were performed with a load of 20 N and
a distance 0 of 200500
m. Figure 17 shows
1000 1500that 2000
the weight
2500loss value
3000 for SCM
3500 420 original raw
material (i.e., non-carburized) of 2.8 mg. layer
Depth of carburizing The quenched
(µm) specimen prepared with a
CSP:DCSP ratio of 60%:40% and a carburizing time of 12 h obtained a weight loss value
Figure
Figure 14. Microhardness profiles
14. Microhardness profiles of
of SCM 420
SCM 420quenched
quenchedspecimens
specimensprepared
preparedwith
withvarious
variousCSP:DCSP
of 1.1 mg. This result indicates that the wear resistance of SCM 420 steel increases after
CSP:DCSP concentrations and a carburizing duration of 12 h.
concentrations
the carburizationandprocess.
a carburizing duration of 12 h.
Figure 15 shows the carbon content distribution within the diffusion layer of the
1.2 specimen prepared with a CSP:DCSP ratio of 60%:40% and carburizing times
quenched
of 6 and 12 h. For a carburizing
CSP:DCSP time
ratio of 60%:40%
6 h, the maximum
for 12 hourscarbon content of
at temperature of950
0.906
⁰C ± 0.008
wt% in the surface gradually reduced
CSP:DCSP with
ratio of an increasing
60%:40% depth
for 6 hours and approached
at temperature a constant
of 950 ⁰C
1.0
Carbon content (wt %)

0.8

0.6

0.4

0.2

0.0
0 500 1000 1500 2000 2500 3000 3500
Depth of carburizing layer (µm)
Figure Carbon content
Figure 15. Carbon contentdistribution
distributionwithin
withinthethe carburized
carburized layer
layer of aof a quenched
quenched specimen
specimen prepared
prepared with a CSP:DCSP
with a CSP:DCSP ratio of 60%:40%
ratio of 60%:40% and carburizing
and carburizing durations
durations of 12
of 6 and 6 and
h. 12 h.
Crystals 2021, 11, 1136 15 of 17
Crystals 2021, 11, x FOR PEER REVIEW 16 of 18

(a)

(a)

(b) (b)
(c) (c)

Figure 16. Microstructures of 16.

diffusion
Figure
Figure layersofindiffusion
16. Microstructures
Microstructures SCMof420 quenched
diffusion
layers in SCM 420specimens
layers prepared
in SCMspecimens
quenched 420 withspecimens
quenched
prepared awith
CSP/DCSP ratio
ratio of
prepared
a CSP/DCSP with
of a
60%:40% and carburizing60%:40%
times and(a)
of: carburizing
3 h, (b)times
6 h, of:
and (a)(c)
3 h,12
(b)h.
6 h, and (c) 12 h.
CSP/DCSP ratio of 60%:40% and carburizing times of: (a) 3 h, (b) 6 h, and (c) 12 h.
3.0
3.0

2.5

2.5
2.0
Weight loss (mg)

2.0
1.5
Weight loss (mg)

1.5 1.0

0.5
1.0

0.0
Non-carburized Quenched specimen Quenched specimen Quenched specimen
0.5 specimen for carburizing time for carburizing time for carburizing time
of 3 hours of 6 hours of 12 hours

0.0 Figure 17. The wear test results of SCM 420 original raw material and quenched specimen
carburized
Non-carburized with CSP:DCSP
Quenched specimen ratio of 60%:40%.
Quenched specimen Quenched specimen

specimen for carburizing time for carburizing time for carburizing time
of 3 hours of 6 hours of 12 hours

Figure 17.The
Figure 17. Thewear
weartesttest
results of SCM
results of 420
SCM original raw material
420 original raw and quenched
material and specimen
quenchedcarburized
specimen
with CSP:DCSP ratio of 60%:40%.
carburized with CSP:DCSP ratio of 60%:40%.
4. Conclusions
This study investigated the viability of dog conch shell powder (DCSP) and coconut
shell powder (CSP) as carburizing media for the pack carburization of SCM 420 steel at a
temperature of 950 ◦ C. The investigation considered both as-carburized and as-quenched
samples and focused particularly on the effects of the CSP:DCSP ratio (100%:0%, 90%:10%,
Crystals 2021, 11, 1136 16 of 17

80%:20%, 70%:30%, 60%:40%, and 50%:50%) and carburizing time (3, 6, and 12 h) on the
microstructure, carbon content, and microhardness of the samples. The results showed
that the optimum carburizing performance, i.e., the highest carbon content and surface
hardness, was achieved using a CSP:DCSP ratio of 60%:40%, and was associated with
increased stability of the CaCO3 phase. It was also shown that the carbon content and
surface hardness increased with an increasing carburizing time. For the as-carburized
samples, the maximum carbon content was around 1.14 ± 0.007 wt%, while the maximum
surface hardness was 604.9 ± 4.674 HV. However, the quenching process increased the
maximum surface hardness to around 961.3 ± 4.918 HV and resulted in the formation of a
carburized layer with a thickness of around 1300 µm given a carburizing time of 3 h. The
thickness of the carburized layer increased by around 2.5 times as the carburizing time was
increased to 12 h. Additionally, the wear property of SCM 420 steel-carburized specimens
was promoted, as the wear resistance of SCM 420 steel increased after carburization. Future
studies will examine the wear resistance, impact strength, and fatigue resistance of SCM
420 carburized specimens in detail to complete the mechanical properties characterization.

Author Contributions: Conceptualization, R. and C.-C.W.; methodology, R. and C.-C.W.; software,

R. and A.S.; formal analysis, R. and C.-C.W.; investigation, R. and C.-C.W.; data curation, R., C.-C.W.
and A.S.; writing—original draft preparation, R., and A.S.; writing—review and editing, R., C.-C.W.
and A.S.; visualization, R. and C.-C.W. All authors have read and agreed to the published version of
the manuscript.
Funding: This research was funded by the Ministry of Science and Technology, Taiwan R.O.C., under
grant No. MOST 110-2622-E-218-002.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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