metals

Article
Effect of Carbon Content on the Properties of
Iron-Based Powder Metallurgical Parts Produced by
the Surface Rolling Process
Yan Zhao 1,2 , Di Chen 3,4 , Dekai Li 3,4 , Jingguang Peng 1,2,3,4, * and Biao Yan 1,2, *
1 School of Materials Science and Engineering, Tongji University, Shanghai 201804, China;
zhaoyan@tongji.edu.cn
2 Shanghai Key Laboratory for R&D and Application of Metallic Functional Materials, Shanghai 201804, China
3 Shanghai Automotive Powder Metallurgy Co. Ltd., Shanghai 201908, China; chendi1201@126.com (D.C.);
lidekaimilan@163.com (D.L.)
4 Shanghai Powder Metallurgy Automobile Material Engineering Research Center, Shanghai 201908, China
* Correspondence: jingguangp@shautopm.com.cn (J.P.); 1433110@tongji.edu.cn (B.Y.);
Tel.: +86-159-2124-5327 (J.P.); +86-21-6958-2007 (B.Y.)

Received: 8 November 2017; Accepted: 24 January 2018; Published: 26 January 2018

Abstract: In recent years, the rolling densification process has become increasingly widely used to
strengthen powder metallurgy parts. The original composition of the rolled powder metallurgy blank
has a significant effect on the rolling densification technology. The present work investigated the
effects of different carbon contents (0 wt. %, 0.2 wt. %, 0.45 wt. %, and 0.8 wt. %) on the rolling
densification. The selection of the raw materials in the surface rolling densification process was
analyzed based on the pore condition, structure, hardness, and friction performance of the materials.
The results show that the 0.8 wt. % carbon content of the surface rolling material can effectively
improve the properties of iron-based powder metallurgy parts. The samples with 0.8 wt. % carbon
have the highest surface hardness (340 HV0.1 ) and the lowest surface friction coefficient (0.35). Even if
the dense layer depth is 1.13 mm, which is thinner than other samples with low carbon content, it
also meets the requirements for powder metallurgy parts such as gears used in the auto industry.

Keywords: powder metallurgy; rolling; surface densification; carbon content

1. Introduction
Powder metallurgy (PM) parts have become increasingly widely used in the auto industry [1,2].
Compared with forging, the advantages of the PM process are that it is suitable for complexly shaped
parts, the raw material utilization rate is high, and the production cost is reduced [3,4]. However,
the inherent porosity in traditional single pressed and sintered products is one of the major factors
causing reduction in the mechanical properties of PM parts [5,6]. Although new advances in powder
metallurgy such as hot isostatic pressing (HIP), selective laser melting (SLM), and high-velocity
compaction technology are used to manufacture high-performance components with homogeneous
high density, the facilities required for these processes are more specialized and the production costs
are higher compared with those of the surface rolling process [6–8]. Therefore, in order to expand
the application field of PM parts, surface densification is a cost-effective and highly precise method
enabling the surface of parts to be densified, while still keeping the internal porous state. Surface
densification can greatly enhance the mechanical properties and surface properties of PM parts while
retaining the advantages of powder metallurgy; specifically, maintaining the light weight and damping
capacity of PM parts [6–10].
Rolling densification belongs to the secondary processing process in the PM industry [11]. In the
rolling process, the dense layer is obtained by plastic deformation on the surface of the sintered

Metals 2018, 8, 91; doi:10.3390/met8020091 www.mdpi.com/journal/metals

Metals 2018, 8, 91 2 of 11

blank [12]. This surface densification process takes only 8–15 s for each blank; therefore, the efficiency
is significantly higher than other densification methods [13].
The original powder chemical composition affects the structure and mechanical properties of the
sintered blanks and then has an impact on the effect of surface rolling. Because the original powder
composition is complex, the roles of different elements will be mutually influenced. Consequently,
this work studied the effect of single element carbon on surface rolling densification. Carbon exists in
steel mainly in the form of cementite and graphite. The ductility of carbon steel decreases rapidly with
an increasing proportion of cementite and graphite. It is noteworthy that the orientation of carbide
lamellae leads to the anisotropic mechanical properties in the materials, and the rolling process will
result in a highly controllable change in the direction of the carbide lamellae [12,14]. Meanwhile, the
finer carbide lamellae can be beneficial for wear resistance. Consequently, the effects of carbon content
are a priority research area for surface rolling in this work.
The carbon content added to the sintered steel was generally between 0.2 wt. % and 1.0 wt. %
in the previous published literature, and the form was graphite. However, the previous literature
mostly focused on comparing the properties of rolling parts with those of wrought parts as well as
researching rolling process parameters such as rolling speed and rolling pressure. For the material
used in the surface rolling process, the previous literature indicated that the rolling process requires
a soft material with sufficient core hardness in order to allow the densification of the surface region
while macro deformation is prevented [15]. However, there is no specific experiment or research to
support this assumption and define an appropriate carbon content in surface rolling sintered materials.
Therefore, this paper investigates the influence of the gradient of carbon content on the densification
of surface rolling in order to provide evidence for the selection of surface rolling PM materials. In PM
sintered steel, there is a threshold value of 1.0 wt. % for the carbon content. When the carbon content is
higher than 1.0 wt. % the tensile strength of the parts will decrease, and sintering deformation is more
likely to occur in the material. In addition, the alloying elements will also be segregated, leading to a
reduction in the cutting performance and plastic properties of the material. Therefore, in this paper, a
range of 0~0.8 wt. % carbon was chosen to investigate the effect of carbon content on the performance
of surface densification. Results obtained from this work will enrich the basic knowledge of PM surface
rolling technology and provide a reference for the selection of surface densification materials.

2. Materials and Methods

2.1. Preparation of PM Components

The raw material of the surface-densified samples was Höganäs powder. The steel powder was
pre-alloyed powder with 0.85 wt. % Mo mixed with 1.40 wt. % Cu and different contents of graphite
(0 C, 0.2 C, 0.45 C, and 0.8 C) in the Star-mix way. Table 1 below shows the chemical composition of
the PM materials, which have the same content of Cu and Mo and only differ in the carbon content.
The element Cu is used for improving the strength of the PM parts. The element Mo is used for
enhancing the hardenability of PM parts, as they undergo a high-frequency quenching process after
rolling. The size of these powders is about 150 µm. According to our production experience, the parts
with 1.0 wt. % carbon content are susceptible to cracking after sintering as a great amount of cementite
is generated in them. So, the values of carbon content up to 1.0 wt. % were not studied in this research.

Table 1. Chemical composition (mass %) of powder metallurgy (PM) material.

Specimen Astaloy85Mo Graphite Cu

0C - 1.4
0.2 C 0.2 1.4
Bal.
0.45 C 0.45 1.4
0.8 C 0.8 1.4
Metals 2018, 8, 91 3 of 11

TheMetals
blanks were
2018, 8, x FORpressed
PEER REVIEWon a mechanical press under a pressure of 650~700 MPa. The sintering
3 of 11
process was performed via a single normal-temperature sintering (1393 K × 30 min) route in a
The blanks were pressed on a mechanical press under a pressure of 650~700 MPa. The sintering
continuous furnace under an ammonia dissolving atmosphere. Ammonia dissolving is used as a
process was
Metals 2018, performed
8, x FOR via a single normal-temperature sintering (1393 K × 30 min) route3 in
PEER REVIEW a
of 11
protective atmosphere to protect the parts from oxidation during the sintering process. It does not
continuous furnace under an ammonia dissolving atmosphere. Ammonia dissolving is used as a
have any chemical
The blanks
protective reaction
atmosphere towith
were pressed on
protectthe
atheparts.
mechanical The
parts from carbon
press underpotential
oxidation aduring
pressurethewas
of controlled
650~700
sintering MPa. The
process. by the notprotective
It sintering
does
ammonia dissolving
process
have anywaschemicalatmosphere
performed aso
via with
reaction that
single the carbon content
normal-temperature
the parts. The carbon of thewas
sintering
potential blank
(1393 was
K maintained
× 30
controlled min)
by the route at
in the
protective a same
level as continuous
ammonia
the original furnace
ones. under
dissolving All ofan theammonia
atmosphere so that
part dissolving
the carbon
densities atmosphere.
content
were the Ammonia
wellofcontrolled
blank wasby dissolving
maintainedisatused
compacting. the as sintering,
same
After a
protective
level as the atmosphere
original to
ones. protect
All of thethe parts
part from
densities oxidation
were well during
controlled thebysintering
the densities of green parts with each of the different carbon contents were measured based on the process.
compacting. AfterIt does not
sintering,
have any chemical
the densities of greenreaction witheach
parts with the parts.
of the The carbon
different potential
carbon was were
contents controlled
measuredby the protective
based 3 .on the
Archimedes drainage method, with the values fluctuating between 7.08 and 7.12 g/cm The average
ammonia
Archimedes dissolving
drainageatmosphere
method, with so that the carbon
the values contentbetween
fluctuating of the blank was 7.12
7.08 and maintained
g/cm at the
3. The same
average
densitylevel
of the sintered samples was then calculated 3
as the
density of original
the ones.samples
sintered All of the
waspart densities
then were at
calculated about
well 7.10g/cm
controlled
at about 7.10 g/cm
by . Sample
compacting.
3. Sample Afterphotographs
sintering,
photographs are are
shown in theFigure
showndensities1, and
in Figure the
of green
1, dimensions
parts
and the with
dimensions areofouter
each diameter
theouter
are different (OD)
carbon
diameter = =2525mm,
contents
(OD) wereinner
mm, diameter
measured
inner based
diameter (ID)
(ID)on=the= 15 mm,
15
thickness = 8thickness
mm. drainage
Archimedes
mm, = 8 mm.method, with the values fluctuating between 7.08 and 7.12 g/cm3. The average
density of the sintered samples was then calculated at about 7.10 g/cm3. Sample photographs are
shown in Figure 1, and the dimensions are outer diameter (OD) = 25 mm, inner diameter (ID) = 15
mm, thickness = 8 mm.

Figure 1. Photographs of samples and the cutting after rolling.

Figure 1. Photographs of samples and the cutting after rolling.
2.2. Surface Rolling Apparatus and Methods
2.2. Surface Rolling Apparatus and1.Methods
Figure Photographs of samples and the cutting after rolling.
The rolling densification process was carried out on a FLEX M20 HCN rolling machine from
The Escofier,
rollingChalon-sur-Saône,
densification process France, as shown
was in Figure
carried out2.onDuring
a FLEXthe rolling
M20 HCN process, two roller
rolling dies from
machine
2.2. Surface Rolling Apparatus and Methods
Escofier,were spinning in the same
Chalon-sur-Saône, direction
France, and at the
as shown insame
Figurespeed. Throughthe
2. During moving
rollingboth of the roller
process, twodies
roller dies
with The rolling
pressure ondensification
the components, processthewas carried
surface areaout
wasondensified.
a FLEX M20 HCNthe
During rolling machine
process, from
the rolling
were spinning in the same direction and at the same speed. Through moving both of the roller dies
Escofier,
speed was Chalon-sur-Saône,
30 r/min and the France,
feeding as shown
speed in Figure
of the 2. During
roller dies was 0.6themm/s.
rolling process,
After two roller
reaching dies
the preset
with pressure
were
distance,onthe
the
spinning components,
in
rollerthe same
dies stopped the
thesurface
direction andat
feed area
at0.8
themm was
sameand densified.
speed. Through
kept the During forthe
moving
distance process,
both
1 s. of the
These the rolling
roller
parameters of speed
dies
was 30 r/min
with andprocess
the rolling theonfeeding
pressure the
have speed
components,
been of the
studied the roller
insurface dies
area was
our previous was 0.6 mm/s.
densified.
research After
During
[16], and reaching
the
it was the
process,
found that thepreset
with thesedistance,
rolling
the roller dieswas
speed stopped
parameters 30
wer/minthe
can andfeed
producetheat 0.8parts
feeding
PM mm andofakept
speed
with thedense-layer
the roller
surface distance
dies was for
0.6 1 s. These
mm/s.
deeper 0.3parameters
After
than reaching
mm andthe of the rolling
preset
a density
process distance,
higher the7.5
than
have been roller
g/cm
studied dies instopped
3. This meets
our the
thefeed
previous at 0.8 mm use
performance
research and kept theitdistance
requirements.
[16], and was found for 1 that
s. These
withparameters of
these parameters
the rolling process have been studied in our previous research [16], and it was found that with these
we can produce PM parts with a surface dense-layer deeper than 0.3 mm and a density higher than
parameters we can produce PM parts with a surface dense-layer deeper than 0.3 mm and a density
3 . This meets
7.5 g/cm the performance use requirements.
higher than 7.5 g/cm3. This meets the performance use requirements.

Figure 2. Schematic view of the experimental apparatus.

Figure 2. Schematic view of the experimental apparatus.

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Metals 2018, 8, x FOR PEER REVIEW 4 of 11

In
In the
the present
present work,
work, thethe pores
pores in
in the
the material
material were
were observed
observed by by aa metallographic
metallographic microscope
microscope
(Olympus,
(Olympus, bx51, Tokyo, Japan), and the depth and distribution of the dense layer
bx51, Tokyo, Japan), and the depth and distribution of the dense layer were
were analyzed
analyzed byby
image processing software. The hardness distribution on the cross-section of
image processing software. The hardness distribution on the cross-section of the sample was the sample was measured
by a microby
measured Vickers
a microhardness
Vickerstester (DHV-1000
hardness Shanghai, Shanghai,
tester (DHV-1000 Shanghai, Shanghai,
China) with a testwith
China) loadaof 0.98
test N
load
and an indentation of 10 s. Each hardness point on the distribution figure is the average
of 0.98 N and an indentation of 10 s. Each hardness point on the distribution figure is the average hardness value
of five different
hardness value indentations at the
of five different same distance
indentations from
at the the surface.
same distanceThefromroughness detector
the surface. (Mitutoyo,
The roughness
SJ-410, Kawasaki, Japan) detected the roughness level of the sample surface after
detector (Mitutoyo, SJ-410, Kawasaki, Japan) detected the roughness level of the sample surface rolling. The structure
after
and morphology of the samples were examined by SEM (Cam Scan, Apollo300,
rolling. The structure and morphology of the samples were examined by SEM (Cam Scan, Apollo300, Cambridge, UK).
The deformation and frictional properties of the microspheres were tested by nano-scratch
Cambridge, UK). The deformation and frictional properties of the microspheres were tested by nano- experiments
(CSM,
scratchNST, Peseux, Switzerland).
experiments (CSM, NST, Peseux, Switzerland).
3. Results
3. Results
3.1. Surface-Densified Layer Properties
3.1. Surface-Densified Layer Properties
The porosity distribution on the cross-section in the surface layer is shown in Figure 3. It can be
seen The
that porosity distribution
as the carbon contenton the cross-section
increases, the overallinlevel
the surface layerinisthe
of porosity shown in Figure
densified layer3.increases.
It can be
seen that as the carbon content increases, the overall level of porosity in the densified
It is obvious that the porosity of 0 C is the lowest of all the specimens. The porosity of 0 C fluctuateslayer increases.
It is than
less obvious
2% inthat the porosity
a large of 0 Cmm
region (0–1.2 is the
from lowest of all theTherefore,
the surface). specimens. theThe porosity
dense of 0 C(defined
layer depth fluctuates
as
less than 2% in a large region (0–1.2 mm from the surface). Therefore, the dense layer
porosity <3.84% [13]) of the 0 C samples is the thickest in this work. The porosity of 0.2 C is obviously depth (defined
as porosity
higher <3.84%
overall than [13]) of0the
that of C in0 the
C samples is the and
surface layer, thickest
it hasinsome
this work. The porosity
fluctuations after 0.7ofmm 0.2 with
C is
obviously higher overall than that of 0 C in the surface layer, and it has some
a mostly upward trend. The porosity distributions of 0.45 C and 0.8 C show large fluctuations and fluctuations after 0.7
mm with a mostly upward trend. The porosity distributions of 0.45 C and 0.8
instability in the dense layer region. The porosity declines first and then rises from the surface to the C show large
fluctuations
center in the and
0.45 instability
C and 0.8 Cinsamples.
the dense layer region. The porosity declines first and then rises from
the surface to the center in the 0.45 C and 0.8 C samples.

Figure 3. Porosity distribution on the cross-section in the surface layer.

layer.

In this
In this work,
work, the
the variation
variation of
of carbon
carbon content
content hashas little
little effect
effect on
on the
the theoretical
theoretical full
full density
density ofof the
the
PM material.
PM material. Therefore, the theoretical
Therefore, the theoretical full
full densities
densities are
are around
around 7.87.8 g/cm
g/cm 3 in
3
in 00 C,
C, 0.2
0.2 C,
C, 0.45 C, and
0.45 C, and
0.8 C specimens. The densification effect is obtained when the surface density is larger
0.8 C specimens. The densification effect is obtained when the surface density is larger than 7.5 g/cm3,, than 7.5 g/cm 3

i.e., the
i.e., the porosity
porosity is
is less
less than
than 3.84%.
3.84%. Figure
Figure 44 shows
shows thethe depth
depth ofof the
the densified layer of
densified layer of all
all samples, and
samples, and
indicates that
indicates that the
the densified
densified layer
layer depth
depth ofof 00 C
C is
is 22 mm,
mm, which
which isis the
the thickest.
thickest. AsAs the
the carbon
carbon content
content
increases, the depths of 0.2 C, 0.45 C, and 0.8 C are 1.36 mm, 1.32 mm, and 1.13
increases, the depths of 0.2 C, 0.45 C, and 0.8 C are 1.36 mm, 1.32 mm, and 1.13 mm, respectively.mm, respectively.
Metals 2018, 8, 91 5 of 11
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Figure4.4. Comparison
Figure Comparison of
ofdepth
depthof
ofthe
thedensified
densifiedlayer.
layer.
Figure 4. Comparison of depth of the densified layer.
3.2. Micro-HardnessAnalysis
3.2. Analysis
3.2. Micro-Hardness
Micro-Hardness Analysis
Figure 5 shows the
Figure the microhardness distributions
distributions on the the cross-section in in the surface
surface layer with
with
Figure 55 shows
shows the microhardness
microhardness distributions on on the cross-section
cross-section in the the surface layer
layer with
different
different carbon contents. The hardness values at a distance of 8 mm from the surface can represent
different carbon
carboncontents.
contents.The Thehardness
hardnessvalues
valuesatat a distance
a distance of of
8 mm8 mm fromfromthethe
surface cancan
surface represent the
represent
the hardness
hardness level level
of the ofmatrix
the matrix
of the of the specimens.
specimens. In In Figure
Figure 5, it is 5, it is shown
shown that the that the hardness
hardness of the of the
matrix
the hardness level of the matrix of the specimens. In Figure 5, it is shown that the hardness of the
matrix increases
increases with thewithwith the increase
increase of the carbonof the carbon At content. At the same time, the of hardness of the
matrix increases the increase of thecontent.
carbon content. the same At thetime,samethe time,
hardness the densified
the hardness of the
densified
areas of 0 Careas
and ofof 0 C
0.20CCare and 0.2 C are nearly the same, indicating that the same rolling condition can
densified areas andnearly
0.2 C the aresame,
nearlyindicating
the same,that the same
indicating rolling
that the samecondition
rollingcan increase can
condition the
increase the
hardness hardness
of the densified of the
layer densified
in 0 C and layer in 0 C and
obtain obtain the same level of with
densification with 0.2
increase the hardness of the densified layer in 0 Ctheandsame
obtain leveltheofsame
densification 0.2 C. When
level of densification with the
0.2
C. When
carbon the
content carbon content
of the content of the
samplesofincreases samples
to 0.45 increases
wt. % and to 0.45
0.8 wt.wt. % and 0.8 wt. %, it shows higher
C. When the carbon the samples increases to 0.45 wt.%,% itandshows higher
0.8 wt. %, ithardness in the
shows higher
hardness in thebecause
densified densified layer because the hardness of the matrix has reached a higher level. The
hardness layer
in the densified thelayer
hardness of the
because thematrix has reached
hardness of the matrixa higher haslevel. The highest
reached a higherhardness is
level. The
highest
340 HV0.1hardness is 340
in the densified HV 0.1 in the densified layer of 0.8 C.
highest hardness is 340 HVlayer of 0.8 C.
0.1 in the densified layer of 0.8 C.

Figure 5.
5. Micro-hardness
Micro-hardness distributions
distributions onthe
the cross-sectionin
in thesurface
surface layer.
Figure
Figure 5. Micro-hardness distributions on
on the cross-section
cross-section in the
the surface layer.
layer.
3.3. RoughnessAnalysis
3.3. Analysis
3.3. Roughness
Roughness Analysis
Sven Bengtssonet
Sven et al.showed
showed thatthe the surface
surface roughness
roughness ofsurface-densified
surface-densified partsisisbetter
better than
Sven Bengtsson
Bengtsson et al. al. showed thatthat the surface roughness of of surface-densified parts
parts is better than
than
that
that of shaved parts [17]. Figure 6 shows the comparison of tooth flank roughness in 0 C, 0.2 C, 0.45
that of
of shaved
shaved parts
parts[17].
[17].Figure
Figure66shows
showsthethecomparison
comparisonofoftooth
toothflank
flankroughness
roughness in in
0 C, 0.20.2
0 C, C, C,
0.45 C,
0.45
C, and
and 0.8 C0.8 C specimens.
specimens. It canItbe
can be that
seen seenthe
that the roughness
roughness levels levels
of 0.45 Cofand
0.450.8
CC and 0.8 0.5
reach C reach
µm, 0.5 μm,
which is
C, and 0.8 C specimens. It can be seen that the roughness levels of 0.45 C and 0.8 C reach 0.5 μm,
which
only is
half only half
that of that
thethat of
0 Cofand the 0 C and 0.2 C samples.
which is only half the0.2
0 CCand
samples.
0.2 C samples.
Metals 2018, 8, 91 6 of 11
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Figure 6.
Figure 6. Comparison
Comparison of
of tooth
tooth flank
flank roughness
roughness in
in materials
materials with
with different
differentcarbon
carboncontent.
content.
Figure 6. Comparison of tooth flank roughness in materials with different carbon content.
3.4. Metallographs
3.4. Metallographs and and SEM
SEM Analysis
Analysis
3.4. Metallographs and SEM Analysis
Figure 77 shows
Figure shows the the metallographs
metallographs of of the
the densified
densified layer
layer ofof the
thespecimens.
specimens. Figure
Figure 88 shows
shows thethe
SEM Figure
images 7 shows
of the the metallographs
densified layer of the of the densified
specimens. From layer of
Figure the
7a, specimens.
it can
SEM images of the densified layer of the specimens. From Figure 7a, it can be seen that the structure be Figure
seen that 8
the shows the
structure
SEM
of Cimages
of 00 C fullyofferrite.
isis fully the densified
ferrite. The black
The layer
black of the
region
region isspecimens.
is the pores
the From
pores left
left Figure
copper7a,
by copper
by it can during
melting
melting be seensintering,
during that the structure
sintering, and the
and the
of 0 C
reasonfor
reason is fully
for the ferrite.
the formation
formationofThe black
of darker region
darker areas is
areas in the
in the pores
the ferrite left by
ferrite grains
grains iscopper
is the melting
the solid during
solid solution
solution of sintering,
of copper. and
copper. Comparing
Comparing the
reason
between for the
Figureformation
7b–d, it of
is darker
noted areas
that in the
lamellar ferrite grains
pearlite is
appearsthe solid
in the
between Figure 7b–d, it is noted that lamellar pearlite appears in the material with the increasesolution
materialof copper.
with the Comparing
increase ofof
between
carbon Figure
content. 7b–d,
The it is
structure noted
of that
0.2 C lamellar
and 0.45 pearlite
C is appears
ferrite + in
pearlite the
and material
the
carbon content. The structure of 0.2 C and 0.45 C is ferrite + pearlite and the structure of 0.8 C is with
structure the
of increase
0.8 C is of
fully
carbon
pearlite.
fully content. The structure of 0.2 C and 0.45 C is ferrite + pearlite and the structure of 0.8 C is fully
pearlite.
pearlite.

Figure 7. Metallographs of the densified layer in specimens of (a) 0 C; (b) 0.2 C; (c) 0.45 C; and
Figure 7.Metallographs
(d) 0.8 7.
Figure C. Metallographsofof
thethe
densified layer
densified in specimens
layer of (a)of
in specimens 0 C;
(a)(b)
0 0.2
C; C;
(b)(c)
0.20.45
C; C;
(c)and
0.45(d)C;0.8and
C.
(d) 0.8 C.
There is
There is no
no carbide
carbide in
in the
the 00CCspecimens
specimens in inFigure
Figure8a.
8a. When
When the
the carbon
carbon content
content increases,
increases, the
the
There is
proportion of
proportion no carbide in the 0 C specimens
of pearlite gradually increases,
increases, as in
as shownFigure
shownin 8a. When
inFigures the carbon content
8b–d. Comparing Figures
Figure 8b–d. increases, the
8b–d,itit can
Figure 8b–d, can
proportion
be observedofthat
be observed pearlite
that the gradually
the carbide
carbide layerincreases,
layer is finer
is as
finer in shown
inthe in Figures
thespecimens
specimens 8b–d.
with
with Comparing
higher
higher FiguresThe
carboncontent.
carbon content. 8b–d,
The it can
carbide
carbide
be observed
lamella that the
has been carbide
formed layer
with is finer directional
a regular in the specimens with higher
arrangement and carbon content. The
the interlamellar carbide
spacing is
lamella has been
approximately 500formed
nm on with
averagea regular
in Figure directional
8d. arrangement and the interlamellar spacing is
approximately 500 nm on average in Figure 8d.
Metals 2018, 8, 91 7 of 11

lamella has been formed with a regular directional arrangement and the interlamellar spacing is
Metals 2018, 8, x FOR
approximately PEER
500 nmREVIEW
on average in Figure 8d. 7 of 11

As can be seen from the SEM images of these four dense layers, the pores are compressed and
As can be seen from the SEM images of these four dense layers, the pores are compressed and
closed under the rolling process, forming tiny elongated holes and/or triangular holes. The 0.2 C
closed under the rolling process, forming tiny elongated holes and/or triangular holes. The 0.2 C
sample has the most apparent boundaries between pearlite and ferrite. The microstructures of 0 C and
sample has the most apparent boundaries between pearlite and ferrite. The microstructures of 0 C
0.8 C are uniform compared with those of 0.2 C and 0.45 C.
and 0.8 C are uniform compared with those of 0.2 C and 0.45 C.

Figure 8.8. SEM

Figure SEMimages
imagesofof
thethe
densified layer
densified in specimens
layer of (a)of
in specimens 0 C;
(a)(b)
0 0.2 C; (c)
C; (b) 0.20.45
C; C;
(c)and
0.45(d)C;0.8and
C.
(d) 0.8 C.
3.5. Friction Performance Analysis
3.5. Friction Performance Analysis
In order to investigate the effect of carbon content on the wear resistance of the PM materials,
we useIn order to investigate
nano-scratch the effect
experiments of carbon content
to characterize on the wear
the densified layerresistance
area of 0 of C, the
0.45PM materials,
C, and 0.8 C
we use nano-scratch
specimens. The tests experiments
use constantto characterize
loading mode the anddensified
the scratchlayer
loadarea of mN.
is 10 0 C, The
0.45 radius
C, andof 0.8the
C
specimens.
diamond The
ball tiptests use The
is 2 µm. constant
scratchloading
speed is mode and the scratch
0.6 mm/min. load length
The scratch is 10 mN.
is 0.5The
mm.radius of the
The scratch
diamond
process canball
be tip is 2 μm.
divided intoThe scratch
three stages.speed
In theis first
0.6 mm/min.
stage, theThe scratch
sample length is 0.5 under
is pre-scratched mm. The scratch
a scanning
process
load canmN.
of 0.5 be The
divided intomorphology
surface three stages. of In
thethe first stage,
samples can bethe sampleafter
obtained is pre-scratched
pre-scratching. under
In thea
scanning
second loadthe
stage, of 0.5 mN. The
constant surface
scratch loadmorphology of the through
is used to scratch samplesthecansurface
be obtained
of theafter pre-scratching.
samples and obtain
In the
the second force–displacement
transverse stage, the constant curve.scratchAccording
load is used to scratch
to this through
curve, the the surface
relationship of the
between samples
friction and
and obtain the
displacement cantransverse
be calculated.force–displacement
In the final stage,curve. According
the instrument usesto the
thisscanning
curve, the
loadrelationship
to measure
between
the change friction and depth
of residual displacement can be calculated. In the final stage, the instrument uses the
with displacement.
scanning
Figureload to measure
9 shows the change
the variation of residual depth
of penetration depthwithwithdisplacement.
scratch length in different specimens.
With Figure 9 shows
the increase the variation
of carbon content, ofthe
penetration depth with depth
average penetration scratchinlength in different
the densified layerspecimens.
decreases,
With the increase of carbon content, the average penetration depth in the
indicating that the addition of carbon improves the hardness of the material, and the deformation densified layer decreases,
indicatingability
resistance that the addition of
is enhanced. carbon improves
Therefore, the hardness
the wear resistance of the material,
is improved. and the deformation
The penetration depth curve
resistance
in ability isthan
0 C is smoother enhanced.
others, Therefore,
and the peaks the wear
in theresistance is improved.
curves of 0.45 C and 0.8The penetration
C represent the depth
pores
curve in
which 0 C ison
formed smoother than others,
the cross-section and
of the the peaks in the curves of 0.45 C and 0.8 C represent the
materials.
pores which formed on the cross-section of the materials.
Metals 2018, 8, 91 8 of 11
Metals 2018, 8, x FOR PEER REVIEW 8 of 11
Metals 2018, 8, x FOR PEER REVIEW 8 of 11

Figure 9. Variation of penetration depth with scratch

Figure 9. scratch length.
length.
Figure 9. Variation of penetration depth with scratch length.
Figure 10 shows variation of the friction coefficient with scratch length in different specimens.
Figure 10 shows variation of the friction coefficient with scratch length in different specimens.
The Figure
friction10 coefficient in 0 C of
shows variation shows
the the declining trend from the surface todifferent
the center. On the
The friction coefficient in 0 C shows thefriction
decliningcoefficient
trend from with
thescratch
surfacelength
to the incenter. On thespecimens.
contrary,
contrary,
Thefriction the friction
frictioncoefficient coefficient
coefficientofin0.45 of
0 CCshows0.45 C falls
the and first
declining and then
trend rises
from thestarting
surfacefrom 0.25
to the mm,
center.while
On the
the falls first then rises starting from 0.25 mm, while the friction
friction coefficient
contrary, the of coefficient
friction 0.8 C showsofan entirely
0.45 C fallsrising
first trend
and in the
then densified
rises starting layer.
from It can
0.25 be seen
mm, whilefrom
coefficient of 0.8 C shows an entirely rising trend in the densified layer. It can be seen from Figurethe
10
Figure
friction 10 that the
coefficient overall
of 0.8 C level
showsof the
an friction
entirely coefficient
rising trend of
inthe
the sample density
densified layer. zone
It decreases
can be seen with
from
that the overall level of the friction coefficient of the sample density zone decreases with the increase
the increase
Figure of the
10 content.
that carbon content.
overall levelThe average
of the value of the friction coefficient of 0.8 zone
C reaches 0.4, which
of carbon The average value offriction coefficient
the friction of the
coefficient of sample density
0.8 C reaches 0.4, whichdecreases with
is the lowest
is the
the lowestof
increase ofcarbon
all the content.
specimens,
The and that of
average 0.45of
value C the
andfriction
0 C is more than 0.5
coefficient of andC0.6,
0.8 respectively.
reaches 0.4, which
of all the specimens, and that of 0.45 C and 0 C is more than 0.5 and 0.6, respectively.
is the lowest of all the specimens, and that of 0.45 C and 0 C is more than 0.5 and 0.6, respectively.

Figure 10. Variation of friction coefficient with scratch length.

Figure 10. Variation of friction coefficient with scratch
scratch length.
length.
4. Discussion
4. Discussion
Pores are affected by both hydrostatic pressure and shear stress in the rolling densification
process. Pores
Pores are are not only
affected by compressed by hydrostatic
both hydrostatic pressure pressure,
and shearbut also in
stress easily
the elongated and closed
rolling densification
by shearPores
process. deformation. Thecompressed
are not only maximum shear stress appears
by hydrostatic on but
pressure, the also
sub-surface rather than
easily elongated and on the
closed
by shear deformation. The maximum shear stress appears on the sub-surface rather than on the
Metals 2018, 8, 91 9 of 11

4. Discussion
Pores are affected by both hydrostatic pressure and shear stress in the rolling densification
process. Pores are not only compressed by hydrostatic pressure, but also easily elongated and closed
by shear deformation. The maximum shear stress appears on the sub-surface rather than on the
surface [9]. Therefore, the initial plastic deformation happens in the sub-surface area. Due to the
overall small deformation resistance of the 0 C and 0.2 C samples, both the sub-surface and the
outermost surface have severe plastic deformation during the rolling process. However, under the
same rolling conditions, the deformable sub-surface in the 0.45 C and 0.8 C samples is preferentially
densified, while the outermost surface does not reach the same densification as the sub-surface after
rolling. This indicates that the increase of carbon content will worsen the effect of rolling compaction
on density. The distribution of the density in the dense area is more unstable and non-uniform with a
high carbon content.
In the published work from Bengtsson, the depth of the densified layer in samples with 0.25 wt. %
carbon content is 1.3 mm [15], and is at the same level as the depth in this work. When the carbon
content increases in the samples, the material microstructure changes (from ferrite to pearlite), resulting
in the effect of rolling treatment. Therefore, the yield strength rises and the deformation resistance
ability is enhanced. In the same rolling condition, specimens with different materials will show
different densification behaviors.
The hardness fluctuation in the dense layer is related to the densification state of the samples.
The highest hardness of 0.8 C occurred at about 0.6 mm from the surface, where the porosity is at a low
state. In 0.45 C, hardness and density have the same trend of fluctuations. In 0 C and 0.2 C, hardness at
a distance of 0.4–0.5 mm from the surface has a slight increase, and at the same time there is a decrease
in porosity at this position. The reason for this phenomenon is that the existence of internal pores in
the material leads to increasing indentation deformation and then decreasing hardness. In addition,
the hardness changing rates in the densified layer decline with the increase of the carbon content.
This means that the same rolling process is highly efficient in samples with low carbon content.
In Bengtsson’s work, the roughness of the rolled gears with 0.3 wt. % carbon content is Ra1.13,
which is lower than that of the shaved reference gear [17] but significantly higher than that of the
0.45 C and 0.8 C samples. Therefore, the rolling process provides a good surface condition for the part
and can even be used as the final step in part machining. Furthermore, a high carbon content can lead
to better surface roughness.
The friction coefficient of the rolled material with a high carbon content is lower, which is mainly
due to the increase of the carbide lubrication. This indicates that the addition of carbon improves the
friction performance of the densified layer in PM parts and is conducive to extending the service life of
parts in actual working situations. The surface-densified layer, with relatively high hardness, could
hinder crack initiation and propagation on and under the surface and enhance the wear properties of
the PM material [6].
It has to be pointed out that the roughness should have been obtained via scratch results, but the
data obtained from the scratch test in this work gives the penetration depth and transverse force but
does not include the roughness. This will be improved in future research.
In future research, the friction and wear behaviors of the surface-densified material need to be
further studied via sliding wear tests. We can then investigate the effect of the carbon content on the
wear resistance of the surface-densified PM material through wear rate, the morphologies of the worn
surface, and the chemical composition of the wear debris. As a result, the wear mechanism could then
be researched.
Furthermore, residual stress is an important property generated by the rolling process, which
controls fatigue and the corrosion performance of materials. We would like to conduct residual
compressive stress measurements using an X-ray stress analyzer on the surface of rolling samples in
future research. This will indicate the performance of different carbon content materials after rolling.
Metals 2018, 8, 91 10 of 11

5. Conclusions
The influence of carbon content on the surface rolling performance of PM materials was
investigated. The results reveal that the porosity, hardness, roughness, and friction performance
of surface rolled parts have different trends with different carbon contents.
For the samples with 0 wt. % carbon content, an excellent and stable porosity distribution in a
2-mm-thick dense layer region was observed; however, the hardness at the surface was the lowest
(due to the lower hardness of the ferrite itself, even if the sample has high densification) and the wear
resistance and friction performance of 0 C performed worst in this work.
As the carbon content increases, the porosity distribution has a fluctuation in the region above
0.7 mm from the surface and the dense layer depth shows a decline in the 0.2 C samples. However, the
hardness value of 0.2 C is similar to that of 0 C because of the rising porosity. For the 0.45 C samples,
the porosity is slightly higher than that of 0.2 C, and therefore the maximum hardness of 0.45 C—about
280 HV0.1 —is about 20% higher than the maximum hardness of 0.2 C—about 230 HV0.1 —in the surface
region. Meanwhile, the roughness, wear resistance, and friction performance were also improved.
When the carbon content is 0.8 wt. %, the hardness reaches 340 HV0.1 while the roughness is close
to Ra0.5 and the friction coefficient is the lowest, about 0.35 approaching the surface. The microstructure
is uniform fine pearlite lamellae in 0.8 C. However, the depth of the densified layer is 1.13 mm, which
is thinner than the others, and meets the requirements for powder metallurgy parts such as gears used
in the auto industry.
Taking into account the application of surface-densified parts and the results obtained
from this work, high carbon content provides high strength and good performance in surface
rolling densification.

Acknowledgments: This work was funded by the “Morning Star” project supported by the Science and
Technological Commission of Shanghai. Contribution and encouragement to this work from Wei Lu is greatly
appreciated and acknowledged.
Author Contributions: Biao Yan and Jingguang Peng conceived and designed the experiments; Yan Zhao, Di Chen,
and Dekai Li performed the experiments; Yan Zhao analyzed the data; Yan Zhao and Jingguang Peng wrote the
paper; Biao Yan revised the manuscript. All authors discussed and approved the final manuscript.
Conflicts of Interest: The authors declare no conflict of interest.

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