Euro PM2011: Sintered Steels: Fatigue and Durability

Manuscript refereed by Professor Herbert Danninger, Vienna University of Technology

Influence of Selected Alloying Elements on the Hardenability and

Fatigue Strength of Recently Developed Sinter-Hardening PM Steels

I. Rampin , M. Zanon ,S. Saccarola and F. Castro*

POMETON SpA, Maerne, Italy

* CEIT & TECNUN, San Sebastian, Spain

ABSTRACT
The final microstructure and consequently the performance in service of PM steels are strongly
dependent on chemical composition as well as on processing conditions. Furthermore, for sinterhardening grades the amount of martensite formed is also affected by the cooling rate used after
sintering. Consequently potentiating the performance of PM steels using a minimum of alloying
elements requires powders with adequate alloy design so to optimise chemical composition and
alloying method. This approach was applied for obtaining selected lean and recently developed PM
steels which exhibit an attractive hardenability and performance as compared to typical diffusion
bonded grades currently containing higher overall amounts of alloying elements. A deep investigation
was carried out on properties of these materials, with a special interest on fatigue strength. This
important characteristic property was investigated, through bend tests carried out with an R value of
0.1, comparing these materials with the common diffusion bonded grades.
INTRODUCTION
Due to price fluctuations of the raw materials as well as environmental issues, optimising the chemical
composition of PM steels is becoming a more stringent requirement in order to achieve the best
performance with a minimum of alloying elements. Alloy design based on a proper selection of alloying
elements combined with an adequate alloying method can also be aimed at obtaining more
economical processing for instance by sinter-hardening. The requirement of high performance
materials under dynamic loading in service makes fatigue resistance one of the most important
properties [1-4]. In the present work the mechanical properties of PM steels obtained from recently
developed Cr-containing powders [5-7] were studied with the main objective to evaluate fatigue
resistance. However, other mechanical characteristics such as UTS, elongation, impact energy and
hardness, obtained from the same batch of powders and sintered under identical conditions, are also
reported. Since 3-point bending fatigue is not a commonly used testing method a set of samples
prepared from other commercially available powders was used for comparison purposes. A
suggested explanation on the tests results is described.
EXPERIMENTAL PROCEDURE
PM steels used in this work were prepared from the newly developed chromium-containing Fe-based
ECOsint powder family. Table 1 shows the nominal chemical composition of the PM steels identified
as different alloys from A to D. As seen from the Table, and without considering graphite, the total
amount of alloying elements in these PM steels is between 2.6 and 4.2 in weight percent.
The fatigue properties for these PM steels were evaluated using 3- point bending fatigue testing with
bar shape (TRS) specimens (31.7x12.7x6.35 mm) applying MPIF Standard 41. ECOsint powders
were mixed with additional graphite and die pressed at 750 MPa reaching a density between 7.0 and
3
7.1g/cm . Sixty specimens per material were cold pressed in order to use 15 specimens for producing
each S-N curve. Specimens were sintered at 1120C and 1240C for 30 min followed by normal
(0.25C/s) or accelerated cooling (~1C/s). After sintering all the specimens were subjected to a stress
relief treatment at 200C for 1hr. Sintering and tempering were carried out using a 90N2-9H2-1CH4
atmosphere. Final densities were measured by the Archimedes principle on selected TRS specimens.

Euro PM2011: Sintered Steels: Fatigue and Durability

Table 1.- Chemical composition of the steels prepared using ECOsint powders.
Alloying elements
ALLOY A
ALLOY B
ALLOY C
ALLOY D
(wt %)
Cr
1.4
1.4
1.4
1.4
Ni
0.4
1
1
0.4
Mo
0.8
0.8
0.8
0.8
Cu
1
1
Graphite
Fe
Balance
Balance
Balance
Balance
Before testing all specimen corners were lightly polished in the longitudinal direction using emery
paper to eliminate asperities. The fatigue tests were performed at room temperature with a load factor
of R = 0.1 and calculations were carried out based on the following equations:

(1)
where, L represents length = 25.4 mm
b and h are respectively the width and thickness in [mm] for each specimen

R: 0.1
and

max

is the applied load [N]

Taking these values into account equation (1) may be re-written as:

34.29 *

max

b * h2

(2)

It is important to emphasize that due to the reduced number of specimens tested (15specimens per SN curve) the reported data should be taken with caution. Nevertheless, it must also be pointed out that
in all cases five run-outs were invariably imposed to determine the fatigue strength. The criterion fixed
7
for a run-out was a survival >10 cycles without fracture. Finally, some specimens were used for
preparing polished cross sections to be observed under the optical microscope and measure apparent
hardness.
RESULTS AND DISCUSSION
Figures 1 and 2 show the S-N curves corresponding to the PM steels while Figure 3 shows a
summary of the data including results obtained after high temperature sintering. For identification the
figures also show the sintering conditions and cooling rates used as well as the measured density and
carbon in solution prior to testing. As a nomenclature in the Figures, sintering temperatures of 1120
and 1240C are identified by LTS and HTS respectively, while cooling rates of 0.25 and 0.88C/s are
indicated as NC and RC.
It may be seen that Alloy A sintered at 1120C and cooled normally (0.25C/s) shows fatigue strength
of 340 MPa at the same time that increasing Ni (Alloy B) produces an increase of fatigue strength to
375MPa. Nevertheless, a drop in fatigue resistance is observed for Alloy D which seems to be
associated to adding Cu without increasing Ni.

Euro PM2011: Sintered Steels: Fatigue and Durability

Figure.1.- 3-point bending fatigue results for Alloys A, B, C, and D sintered at 1120C for 30min
followed by cooling at 0.25C/s and tempered at 200C for 1hr. Run-outs encircled.

Figure 2.- 3-point bending fatigue results for Alloys A, B, C, and D sintered at 1120C for 30min
followed by cooling at 0.88C/s and tempered at 200C for 1hr. Run-outs encircled.
As noticed in Figure 3, Alloy D gives the lowest fatigue strength of all material in this group
independently of the sintering temperature and cooling rate used. That additional Ni has a positive
effect on fatigue strength is supported by the response observed from other mechanical properties
obtained in this work. Table 2 includes data like UTS, elongation and fractures toughness. Clearly, an
increase in fatigue strength is produced as the Ni content is also increased. Alloy C which also
contains copper seems to benefit particularly from an accelerated cooling rate (Figure 2). In this case,
combining an accelerated cooling rate around 0.9C/s with conventional sintering temperature results
in fatigue strength of 440 MPa.

Euro PM2011: Sintered Steels: Fatigue and Durability

Figure.3: Fatigue results for Alloys A, B, C, and D after 3-point bending fatigue testing.
Table.2: Summary of mechanical properties for alloys A, B, C and D after different combinations of
sintering conditions and cooling rates.
Sintered
Fatigue
Impact
Apparent
Sintering
CR
Alloy
density
UTS
%E
strength
energy
hardness
conditions (C/s)
3
(g/cm )
(MPa)
(MPa)
(J)
(HV30)
A

7.07

708

1.58

350

12

173

7.09

787

1.60

375

15

196

7.1

772

1.44

340

12

230

7.05

759

1.62

320

14

248

7.16

867

2.44

360

24

196

7.19

844

2.05

380

25

234

7.18

905

2.22

355

22

230

7.14

926

1.99

330

22

286

7.08

848

1.20

355

15

230

7.09

1009

1.28

415

16

272

7.11

932

1.16

440

15

279

7.08

948

0.95

380

16

354

7.15

1105

1.20

370

20

254

7.21

1043

2.16

380

19

272

7.18

1098

1.60

370

20

318

7.13

1277

1.51

380

18

382

B
C

1120C30min

0.25

A
B
C

B
C

1240C30min

1120C30min

D
0.8-1

A
B
C
D

1240C30min

Figure 3 shows that high temperature sintering results in a slight increase in density for all the
3
specimens thus reaching an average value around 7.17g/cm . Fatigue results after HTS-NC show
nearly the same trend observed with LTS-NC since Ni seems to favour higher fatigue strength. It may

Euro PM2011: Sintered Steels: Fatigue and Durability

also be noticed that despite the increase in density HTS shows only a marginal changes of fatigue
properties. The fatigue results obtained after HTS followed by normal cooling are in the range of 350380MPa. A slight increase is also observed after accelerated cooling, however, such increase is not
as pronounced as that obtained after LTS. According to the data in Figure 3 nearly all values of fatigue
strength are found in a range from 340-390MPa, whereas Alloys B and C stand out after LTS followed
by accelerated cooling. This negligible influence of HTS is not well understood yet so that further
research is underway. On the other hand, as realized from Table 2, an important benefit is obtained
after HTS in terms of increased elongation and impact energy.

c
Figure 4: Optical micrographs of Alloy C
sintered for 30 min at (a) 1120C followed by
cooling at 0.25C/s, (b) 1120C and cooled at
0.88C/s, and (c) 1240C cooled at 0.25C/s.

This effect is expectedly less pronounced as the amount of alloying elements is increased since higher
hardness and mechanical strength are simultaneously obtained. The important influence exerted by
accelerated cooling after LTS is clearly associated with a noticeable increase in the amount of
martensite formed. This is illustrated for Alloy C in Figure 4. It may be realised that after cooling at
around 0.9C/s the specimen develops a nearly fully martensitic microstructure with only minor
amounts of bainite. The opposite is true after cooling at such a slow cooling rate as 0.25C/s.
Comparing the microstructures in Figures 4 and considering the properties reported in Table 2, it may
be realised that after HTS and normal cooling the material also develops a high amount of martensite
but reaches lower hardness and UTS values than those attained by combining 1120C with
accelerated cooling. It must also be pointed out that increasing the cooling rate after HTS, thus
obviously increasing the amount of martensite, produces higher hardness, UTS, elongation and
impact energy but, as mentioned before, a surprisingly lower fatigue resistance.
As mentioned before the fatigue results obtained for these alloys were compared against those
obtained under exactly the same fatigue testing conditions but using some well known commercially
available PM powders. The mechanical properties for these commercial alloys are included in Table 4.
For a comparative evaluation it may be realised that the fatigue resistance obtained for these newly
developed steels is higher or at least comparable to that of the commercially available alloys. The
higher amount of alloying elements contained in those PM steels does not seem to give extra benefits
as compared to those presented here. It may be pointed out that the hybrid with 1.5 % Mo (4%Ni)
reaches 363 MPa bending fatigue strength after HTS whereas the specimen from Alloy B reaches
380MPa fatigue strength after sintering at 1120C and followed by normal cooling. It is important to
emphasize that this latter PM steel only contains 1%Ni. The prealloyed Cr steel shows a benefit on

Euro PM2011: Sintered Steels: Fatigue and Durability

fatigue strength from HTS that the alloys presented here do not seem to exhibit. It is however
interesting to notice that Alloy C does not seem to require HTS since after 1120C followed by
accelerated cooling (< 1C/s) the PM steel develops 440 MPa fatigue strength.
Table.4: Mechanical properties, sintering parameters and fatigue results of well known commercial
steels after 3-point bending fatigue in the as-tempered condition.
Alloy
Sintered
Fatigue
Sinter
CR
%C
UTS
Material
content
density
%E
strength
T [C] [C/s]
[MPa]
3
(wt %)
(g/cm )
[MPa]
Prealloyed Cr-containing

3.5

1120

Prealloyed Cr-containing

3.5

1240

Hybrid with1.5 Mo

7.5

1240

0.45

0.41

7.03

1.08

799

395

0.38

7.17

1.99

922

429

0.59

7.23

2.5

1080

363

CONCLUSIONS
The developed powders allow obtaining high performance steels of the sinter-hardening type which
exhibit very attractive properties for highly demanding applications. It is demonstrated that the sinterhardening characteristics may be tuned at ease by selecting adequate combinations of chemical
composition, sintering temperature and cooling rate. Using an accelerated cooling rate <1C/s is
beneficial for obtaining high fatigue strength. Besides, the sinter-hardening response of some of these
steel grades allows obtaining components with high amounts of martensite at very conservative
cooling rates. Increased nickel contents helps achieving better mechanical properties, especially
fatigue strength. In contrast copper-additions produce an increase of UTS and hardness but cause a
drop of fatigue properties. Additionally, the evaluation of other commercially available grades using the
same fatigue test method proves that fatigue strength of ECOsint grades are comparable to other well
known commercial powders.
REFERENCES
1.- F. J. Esper and C. M. Sonsino, Fatigue design for PM components , Published by EPMA,
Shrewsbury, England, 1994.
2.- P. Beiss and M. Dalgic, Sructure property relationships in porous sintered steels, Materials
Chemistry and Physics, 2001, vol. 67, N 1-3, 37-42.
3.- P. Beiss, Functional relationships between fatigue data, Materials Science Forum, 2007, 534-536,
681-684.
4.- H. Danninger and B. Weiss, The influence of defect on high cycle fatigue of metallic materials, J.
of Mat. Processing Technol., 2003, vol 143-144, 179-184.
5.- S. Saccarola, S. Sainz, A. Karuppannagounder, F. Castro, Hardenability and mechanical
properties of novel sinterhardening PM steels, Adv. in Powder Met & Part Mater 10, 52 (2009).
6.- S. Saccarola, G. Bellin, S. Bueno, S. Sainz and F. Castro, Novel high performance and
dimensionally controlled PM steels for sinterhardening, Euro PM2009, Sintered Steels III,
Copenhagen, Denmark (2009).
7.- S. Saccarola, A. Karuppannagounder, S. Sainz and F. Castro, Developing novel Cr-Mo-Ni PM
steels, PM World Congress and Exhibition, (2010), Florence, Italy.