Materials and Design 55 (2014) 758–763

Contents lists available at ScienceDirect

Materials and Design

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

Technical Report

Ultra-high cycle fatigue behaviour of warm compaction Fe–Cu–Ni–Mo–C

sintered material
Yu-Heng Lu, Zhi-Yu Xiao ⇑, Lei Hu, Fei Luo, Yuan-Biao Wu, Dong-Hui Ni
School of Mechanical and Automotive Engineering, South China University of Technology, Guangzhou 510641, China

a r t i c l e i n f o a b s t r a c t

Article history: The present work studied the ultra-high cycle fatigue behaviours of Fe–2Cu–2Ni–1Mo–1C sintered steels.
Received 3 May 2013 The partially pre-alloyed material was fabricated by die-wall lubricated warm compaction; its mechan-
Accepted 16 October 2013 ical properties, such as hardness and tensile strength, were measured. In addition, axial ultrasonic fatigue
Available online 26 October 2013
testing specimens were designed using the finite element method. The results indicated that fatigue fail-
ure appeared after more than 107 stress-cycles and that a fatigue limit existed. The fatigue strengths were
392, 249 and 159 MPa for the corresponding conditions of 105, 107 and 109 cycles, respectively. The fati-
gue crack sources were located at non-metallic inclusions or voids near the surface under high cycle con-
ditions but move to the internal sites under ultra-high cycle conditions. With an increase in the number
fatigue cycles the stress intensity range factor gradually reduced.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction material. In addition, fatigue resistance has always been a crucial

Powder metallurgy (PM) is an attractive technique for the prep-
aration of materials with outstanding properties. PM is a common
and economical method to produce complex shaped metal parts
with high quality and high precision. In recent years, some re-
search institutes have paid much attention to develop high density
and high performance PM materials [1–3]. Among them, warm
compaction technology is a new economical way to manufacture
high performance Fe-based sintered parts [4–6]. For the majority
of machine parts under cyclic loads, fatigue fracture is the main
failure mode, and the fracture usually occurs suddenly, thereby
resulting in a catastrophic accident. The fatigue characteristics of
the iron based PM materials is usually lower when compared with
its cast and forged counter parts [7], due to the presence of pores in
the materials, which reduce the effective bearing area [8]. In recent
years, some research institutes have studied the high cycle fatigue
behaviour of sintered material. Sulowski [9,10] observed that the
fatigue fracture of pre-alloyed sintered steel subjected to cyclic
loading exhibited typical fatigue striations. Guo [11] argued that
the fatigue crack source was located on large pores near the surface
by studying the high-cycle fatigue behaviour of high-density sin-
tered molybdenum steel. Carabaja [12] found that in the fatigue
behaviours (<107 cycles) of sintered steel, the internal porosity
plays a key role in the material life; fatigue cracks initiate from
non-metallic inclusions. Danninger [13] studied that the fatigue
properties of Fe–Mo–C sintered materials. He argued that the low-
er the critical defect size, the higher the basic performance of the
⇑ Corresponding author. Tel.: +86 20 87110099; fax: +86 20 87112111.
E-mail address: zhyxiao@scut.edu.cn (Z.-Y. Xiao).
design parameter in powder metallurgy parts, such as gears, con-
necting rods and transmission parts. The service life for these parts
exceeds 108 cycles. To ensure high reliability of Fe-base powder
metallurgy materials, it is of great importance to make high den-
sity materials that have high fatigue properties, especially under
ultra-high cycles [14].
In this paper, high-performance Fe–2Cu–2Ni–1Mo–1C material
was prepared by die-wall lubricated warm compaction and its ax-
ial ultrasonic fatigue behaviour was studied under 105–109 ultra-
high cycles.
2. Experimental details
The partially pre-alloyed powders were prepared by mixing
water atomised iron powder (<147 lm) with an alloyed powder
of 2% Cu (<74 lm), 2% Ni (3–5 lm) and 1% Mo (<74 lm) in mass%.
The pre-alloyed powders were first diffused at 830 °C, and then
ground into particulate form with an average particle size of
147 lm. In total, 1% carbon was added as fine particle natural
graphite (<74 lm). Extra 0.1% zinc stearate (<74 lm) was admixed
as a lubricant. The partially pre-alloyed powder, lubricant and
graphite were then blended in a V-type mixer. The ethanol suspen-
sion of zinc stearate was brushed on to the die wall as a lubricant
for warm compaction. The pre-heated powders were compacted in
a steel mould at 120 °C. The pressure was 700 MPa. The green den-
sity of Fe–2Cu–2Ni–1Mo–1C was in the range of 7.3–7.4 g cm3.
Sintering was conducted in a hydrogen–nitrogen atmosphere at
800 °C for 30 min, and then the samples were sintered at 1120 °C
for 60 min. When the temperature dropped to 700 °C, the samples
were rapidly cooled to room temperature. The sintered density of

0261-3069/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2013.10.049
 Y.-H. Lu et al. / Materials and Design 55 (2014) 758–763
the samples is approximately 7.3 g cm3. The tensile strength and
surface hardness were measured according to GB/T 228.1 [15] and
GB/T 231.1 [16].
Cylindrical axial fatigue specimens were machined from the
sintered blanks. Ultra-high cycle axial fatigue testing was per-
formed in the ultrasonic resonance system operating at 20 kHz
with zero mean stress (R = 1). The experiments were conducted
at room temperature. The longitudinal vibration equation of a
one-dimensional elastic rod is described by Eq. (1).
2
d UðxÞ S0 ðxÞ dUðxÞ 2
2
þ þ k UðxÞ ¼ 0
dx SðxÞ dx
where U is the longitudinal vibration displacement, pSffiffiffiffiffiffiffiffiffiffi
is theffi cross-
sectional area, k is the material constant, k ¼ 2pf q=Ed , where f
is the system vibration frequency, q is the density of the sample,
and Ed is the dynamic elastic modulus of the material.
According to the stress and strain curve, the elastic modulus of
Fe–2Cu–2Ni–1Mo–1C is 144 GPa. There are some experiential
relationships between the elastic modulus and the porosity [17].
Sometimes, it is difficult to know the precise location of the mate-
rial fracture. The middle part of the cylindrical rod was designed
to be the transition arc, as shown in Fig. 1. The solution of the
longitudinal vibration equation could be obtained by calculating
Eq. (2).
(
UðxÞ ¼ A0 cos½kðL  xÞ L1 6 jxj 6 L
sinhðbxÞ
UðxÞ ¼ A0 /ðL1 ; L2 Þ coshðaxÞ jxj 6 L1
where A0 is the displacement of the top of specimen (x = 0). Using
the known data of R1, R2, R0 and L1, the resonant length L2 is deter-
mined by Eq. (3).
  
1 1 b formed in the range of 106–107 cycles. This behaviour is different
L2 ¼ arctan  a tanhðaL1 Þ
k k tanhðbL1 Þ
Based on the system vibration frequency, the density of mate-
rial, the dynamic elastic modulus and the known sizes, the reso-
nant length L2 is equal to 16 mm. The dynamic analysis program
of the ANSYS FEM software was used to check the vibration modes
and the intrinsic resonance frequency. The boundary conditions
are R1 = 1.5 mm, R2 = 5 mm, R0 = 30 mm, L1 = 14 mm, and
L2 = 16 mm. The calculated resonance frequency is equal to
19.96 kHz, which is the required frequency for the ultrasonic fati-
gue tests. The axial tension and compression fatigue specimen
were designed and adjusted by the finite element method, as
shown in Fig. 1. Then, ANSYS was used to analyse the stress field
distribution and vertical displacement distribution of modal vibra-
tion in the same boundary conditions, which is shown in Fig. 2.
Fig. 1. Schematic of the axial tension and the compression fatigue sample.
759
During the vibration process, alternating loads were performed
periodically to produce stress and strain; the stress is the largest
at the centre of the sample. In this research, samples for micro-
structural analysis were etched with 3% Nital solution. The micro-
structure and pore size were imaged by a LEICA DMI 5000 M
optical microscope. Scanning electron microscopy (SEM) was used
to investigate the fractographic features.
3. Results and discussion
ð1Þ There are three major phases in the warm compaction of Fe–
2Cu–2Ni–1Mo–1C sintered material, bainite, pearlite and residual
austenite, as shown in Fig. 3. The tensile strength of the material
is 814 MPa, with an elongation of 7.8% and a surface hardness of
285 HB.
The ultra-high cycle (105–109 cycles) axial fatigue behaviour of
the material is shown in Fig. 4. The data can be fit with the Basquin
equation [18]:
ra ¼ r0f ð2Nf Þb ð4Þ
where r0f is the fatigue factor, b is the fatigue index or Basquin index
and Nf is the number of cycles. The corresponding equation for the
S–N curve of a warm compaction sample is:
ra ¼ 1279:7  ð2Nf Þ0:097 ð5Þ
ð2Þ
The S–N fitting curve of the fatigue test data exhibits a contin-
uous downward trend. The fatigue limit strength continuously re-
duces with an increasing number of cycles. The fatigue failure
occurs even after 107 cycles. There is no traditional horizontal zone
ð3Þ
from the curve tendency of high cycle fatigue behaviour (only
tested for less than 107 cycles) [3]. Fatigue strengths are 392,
312, 249, 199 and 159 MPa for the corresponding conditions of
105, 106, 107, 108 and 109 cycles, respectively. There are two test
points near the range of 109 cycles, the fatigue strength at 109 ul-
tra-high cycles is less than the strengths after 105 and 107 cycles.
Therefore, it can be concluded that if a part is designed based on
the fatigue strength at 107 cycles, it may be quite dangerous if
the working time corresponds to more than 107 cycles.
An SEM fractograph of the fatigue fracture under ±400 MPa and
3.74  104 cycles is shown in Fig. 5. The fatigue cracks initiate at a
group of pores or non-metallic inclusions (defects) near the sur-
face. There are some smooth facets in the crack source area. The
crack growth area is not obvious, and fatigue striations cannot be
found. This behaviour is different than the behaviour observed in
all of the sintered specimens after a low-frequency (50 Hz) fatigue
test, for which striations were observed [19]. This lack of striations
for the ultra-high cycle test may be because the ultrasonic fre-
quency is high and the test time is less than 2 s, resulting in the
occurrence of instantaneous fracture, thereby preventing striations
from forming. A large number of dimples appeared on the sintered
bridges, as shown in Fig. 6, indicating that plastic deformation oc-
curred in the local fracture zone. Cleavage facets, at pearlitic parti-
cle’s located near pores, are also identified.
The crack growth area is relatively rough under a high stress
load (±350 MPa); the combination of ductile and cleavage facets,
as well as some ultrasonic fatigue striation was observed. Some
dimples can be seen in the fast fracture area. These characteristics
are similar to the fracture surfaces after high cycle fatigue tests (R
ratio of 1 and a frequency of 30 Hz) [20]. With an increase in the
number of fatigue cycles, more cleavage facets appeared in the
fracture, which are located near fatigue striations, as shown in
Fig. 7; the distance between striations become gradually narrow,
760 Y.-H. Lu et al. / Materials and Design 55 (2014) 758–763

Fig. 2. (a) Axial tensile stress distribution specimen; (b) axial displacement distribution.

Fig. 3. Microstructures of the sintered sample.

Fig. 5. Fracture fractography (±400 MPa, 3.74  104 cycles).

Fig. 4. S–N curves of the samples obtained from the ultrasonic fatigue tests.

Fig. 6. Fast fracture area (±400 MPa, 3.74  104 cycles).

and the length of each striation step links to the degree of crack
growth in each cycle.
The fractograph of fatigue fracture under ±200 MPa and
1.29  107cycles is shown in Fig. 8. The crack source is located at
the pores in the internal sites, because a dark zone appears. This
behaviour is different from the fatigue crack initiated near the sur-
face for the low frequency fatigue test [12]. The pores size reaches
40 lm. The local micro-cracks only appeared around voids in the
material with martensite (Fig. 9). Because the fatigue crack growth
 Y.-H. Lu et al. / Materials and Design 55 (2014) 758–763
Fig. 7. Crack growth area (±350 MPa, 4.01  105 cycles).
Fig. 8. Fracture source area (±200 MPa, 1.29  107 cycles).
Fig. 9. Microcracks around a void.
stage accounts for the part life of the material, the ability of mar-
tensite within hard and brittle to prevent crack growth is weak
when the PM material is at ultrasound resonance. In addition,
compared with the high stress tests, the number of cleavage facets
increases, the fatigue striation increases and the stripe is smaller.
The fractograph of fatigue fracture under ±150 MPa and
1.01  109 cycles is shown in Figs. 10 and 11. The crack originated
in the internal sites of material. Both typical dimples and cleavage
761
Fig. 10. Fast fracture area (±150 MPa, 1.01  109 cycles).
Fig. 11. Crack growth area (±150 MPa, 1.01  109 cycles).
facets appeared on the fast fracture area (Fig. 10). Fatigue growth
area exhibit a smooth plane, on which some small unevenly dis-
tributed fatigue striations are observed, as shown in Fig. 11. With
stress decreasing, the fatigue source area of ultra-high cycle grad-
ually moves to the internal sites. This behaviour indicates that
internal defects play a key role in the ultrasonic fatigue strength.
The fractographs of Figs. 5–11 show that the crack source of
ultrasonic fatigue (20 kHz) crack fractures of the low and high cy-
cles have different features. The crack source area is usually located
at the inclusions or voids near the surface for low cycles, but it
moves to the internal sites for high cycles. This behaviour is differ-
ent to that of the crack source area in the low frequency fatigue test
[11,12]. The shape and distribution of the pores as well as the
microstructure and the size of inclusions are the main factors of fa-
tigue fracture. Typical morphology, such as dimples, cleavage facets
and fatigue striations, appeared on the fracture surface. Under lar-
ger stress, the fracture surface has no obvious fatigue striations; a
large number of dimples and fewer cleavage facets appeared. With
a gradual reduction of the loading stress, the proportion of dimples
decreased, the number of cleavage facets increased, and fatigue stri-
ations appeared. In addition, the fast fracture area is relatively
smooth; it is related to the ultrasonic vibration force. The largest
stress area is located in the middle of the specimen.
Schematics of the ultrasonic fracture source are shown in
Fig. 12. Fig. 12(a) indicates that the inclusions or voids near the
surface are the key to fracturing when the number of cycles is less
762 Y.-H. Lu et al. / Materials and Design 55 (2014) 758–763

Fig. 12. Schematics of the ultrasonic fatigue fracture crack source: (a) less than 107 cycles and (b) more than 107 cycles.

Fig. 13. Histogram of the defect sizes.

Fig. 14. Stress intensity range factor of defect for different numbers of cycles.
7
than 10 . The dark zone is the stable crack growth area, which is
surrounded by the crack rapid expansion zone. The dark zone lies
The stress intensity range factor of the defect zone gradually re-
between the crack initiation zone and the growth zone. Fig. 12(b)
duced with increasing fatigue cycles, as shown in Fig. 14. The de-
shows the fracture characteristics when the number of cycles is
fect occurrence probability in the interior of the powder
more than 107. The crack source is located at the internal sites.
metallurgy material is identical with that on the surface. The crack
Some possible reasons for the crack initiation are [21] (1) fatigue
source of the material is located near the surface, regardless of the
crack initiates from the interface of the substrate and the flaws,
number of cycles, based on Eq. (6). However, the relaxation effect
and then extends to the edge of the dark zone; (2) a micro-crack
of the PM material occurs in ultrasonic vibration, especially in
is initiated from the interface of the substrate and the flaws. At
the ultra-high cycles range, resulting in the reduction of the surface
the same time, the internal damage processes occurs in the dark
residual stress [24]. As a result, the impact of the surface stress on
zone, crack tips merge together and to form dark zone in the exten-
the surface defects will be reduced. Thus, the stress intensity range
sion of process; (3) each micro-crack appears simultaneously in the
factor of a surface defect is less than that of an interior defect in the
dark zone, and then the defects merge together to becomes long
ultra-high cycles range. The cracks can be initiated in the interior
cracks.
of the material more easily.
The ultrasound fatigue defect size in a fracture was measured in
nearly 20 samples, as shown by the histogram in Fig. 13. There is
4. Conclusions
no obvious relationship between the defect sizes and the fatigue
cycles. The measured average size statistics is 64.3 lm, with a min-
Fe–2Cu–2Ni–1Mo–1C powder metallurgy sintered steel was
imum size of 25 lm and the maximum size of 106 lm.
made by die-wall lubricated warm compaction. Under 105–109 ul-
In the fatigue crack source area, the stress intensity range factor
tra-high cycles, the main results of the axial ultrasonic fatigue
in the defect zone can be estimated by Eq. (6) [22].
behaviour are as follows:
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
pffiffiffiffiffiffiffiffi
DK i ¼ C r p ðAi Þ ð6Þ (1) The fatigue behaviour of high density Fe–2Cu–2Ni–1Mo–1C
where i is the defect; r is the fatigue stress; C is the position coef- sintered material was studied using the ultrasonic axial
ficient, with C being equal to 0.50 in the interior of material and C tension–compression fatigue test method. Fatigue fracture
being equal to 0.65 at the surface [23]; Ai is the projected area of appeared at more than 107 stress-cycles and the condi-
defect in the fracture. tional fatigue limit of the material occurred. The fatigue
 Y.-H. Lu et al. / Materials and Design 55 (2014) 758–763
strengths are 392, 312, 249, 199 and 159 MPa for the cor-
responding conditions of 105, 106, 107, 108 and 109 cycles,
respectively.
(2) Dimples, cleavage facets and fatigue striations appeared on
the fracture surface. The proportion of dimples decreased,
the number of cleavage facets increased and the fatigue stri-
ation appeared with the gradual reduction of the loading
stress.
(3) For high cycle tests, the ultrasonic fatigue crack source is
located at the inclusions or voids near the surface of the
material, while for ultra-high cycle tests, the ultrasonic fati-
gue crack source is located in the interior of the material.
The shape, distribution, microstructure and sizes of defects
are the primary factors that influence the fatigue fracture.
There is no obvious relationship between the defect size
and the fatigue cycles. In addition, the stress intensity range
factor of defects reduced with the gradual increase of the
number of fatigue cycles.
Acknowledgments
This work was financially supported by the National Natural
Science Foundation of China (No. 51274103) and NCET, China
(No. NCET-05-0739)
References
[1] Huang BY, Yi JH. Current development of modern powder metallurgy materials
and technologies. Shanghai Met 2007;29(3):1–3.
[2] Chawla N, Deng X. Microstructure and mechanical behavior of porous sintered
steels. Mater Sci Eng A 2005;390:98–112.
[3] Williams JJ, Deng X, Chawla N. Effect of residual surface stress on the fatigue
behavior of a low-alloy powder metallurgy steel. Int J Fatigue 2007;29(9–
11):1978–84.
[4] Xiao ZY, Zhou L, et al. Study on bending ultrasonic fatigue behavior of sinter-
hardened Fe–2Cu–2Ni–1Mo–1c materials prepared by warm compaction.
Materials Science Forum; 638–642.
763
[5] Xiao ZY, Ke MY. Die wall lubricated warm compacting and sintering behaviors
of pre-mixed Fe–Ni–Cu–Mo–C powders. J Mater Proc Technol
2009;209(3):4527–30.
[6] Shanmugasundaram D, Chandramouli R. Tensile and impact behaviour of
sinter-forged Cr, Ni and Mo alloyed powder metallurgy steels. Mater Des
2009;30(9):3444–9.
[7] Kanazawa K, Nishijima S. Fatigue fracture of low alloy steel at ultra-long cycle
regime under elevated temperature conditions. J Sco Mater Sci
1997;46(12):1396–401.
[8] Rahman MM, Ariffin AK, et al. Powder material parameters establishment
through warm forming route. Mater Des 2011;32(1):264–71.
[9] Sulowski M. Dilatometric investigation of Fe–Mn–Cr–Mo PM steels with
different carbon concentrations. Powder Metall Prog 2008;2(8):151–5.
[10] Sulowski M. Nitrogen as an alternative sintering atmosphere for sintering
atmosphere for production of PM parts. Arch Metall Mater
2005;540(4):827–31.
[11] Guo RJ, St-Laurent S, et al. Dynamic properties of sintered molybdenum steels.
Powder Metall Technol(in China) 2003;21(6):338–46. 238.
[12] Carabajar S, Verdu C, et al. Fatigue behaviour of a nickel alloyed sintered
steel[J]. Mater Sci Eng 1998;A257:225–34.
[13] Danninger H. Ultra high cycle fatigue properties of sintered steels. Powder
Metall Prog 2001;1:19–40.
[14] Abdoos H, Khorsand H, et al. Fatigue behavior of diffusion bonded powder
metallurgy steel with heterogeneous microstructure. Mater Des
2009;30(4):1026–31.
[15] GB/T 228.1-2010. Metallic materials-Tensile testing Part 1: Method of test at
room temperature. National standard of the people’s Republic of China.
Peking: China Standard Press; 2010.
[16] GB/T 231.1-2009. Metallic materials-Brinell hardness test Part 1: Test method.
National standard of the people’s Republic of China. Peking: China Standard
Press; 2009.
[17] Huang PY. Powder metallurgy principle. Peking: Metallurgical Industry Press;
2004.
[18] Suresh S. Fatigue of Materials. Cambridge: Cambridge University Press; 2003.
[19] Sudhakar KV. Fatigue behavior of a high density powder metallurgy steel. Int J
Fatigue 2000;22:729–34.
[20] Chawla N, Murphy TF. Axial fatigue behavior of binder-treated versus diffusion
alloyed powder metallurgy steels. Mater Sci Eng 2001;A308:180–8.
[21] Zhou CE, Hong YS. Experimental investigation on very-high-cycle fatigue of
GCr15 steel. Conference Proceedings of Twelfth National Fatigue and
Fracture(in China). 2004; p. 157–160.
[22] Murakami Y. Metal fatigue: effects of small defects and nonmetallic inclusions.
Amsterdam & Boston. 2002:17.
[23] Zhang YJ, Hui HJ. Effect of grain size on ultra-high-cycle fatigue properties of
42CrMoVNb steel. Acta Metall Sin 2009;45(7):880–6.
[24] Zhang JW, Lu LT. Analysis on fatigue property of microshot peened medium
carbon steel. Acta Metall Sin 2009;45(11):1378–83.