You are on page 1of 7

00M-144

Cost Reduction Processes for Transfer Case Sprockets:


Part 1: Metallurgical Aspects
François Chagnon [1], Jeffrey A. Danaher [2], Edmond Ilia [3] and Steve Krise [3]

[1] Quebec Metal Powders LTD


[2] QMP America
[3] MascoTech Sintered Components

Copyright © 1998 Society of Automotive Engineers, Inc.

ABSTRACT Joules at NVG. Because this process involved many


steps, sinter hardening was looked at as an alternative to
Transfer case sprockets usually require quenching to reduce processing costs. Sinter hardening makes the
improve hardness and mechanical properties. This elimination of the quenching operation feasible because
additional process step can be avoided with sinter parts reach high apparent hardness during the post-
hardening. Indeed, sinter hardening allows the sintering cooling. Also, sinter hardening reduces
production of P/M parts with high strength and apparent thermal stresses and distortion which generally happen
hardness directly from sintering because the martensitic during heat treating. The sizing operation is therefore
transformation takes place during the cooling portion of not required since better dimensional tolerances can be
the sintering operation. Therefore, this process maintained. It is also worth noting that sinter hardened
eliminates the need for a post-sintering heat treatment parts cannot be sized because of the high hardness
with all the inherent related problems such as part reached after sintering. Finally, the cleaning operation
distortion, oil contamination and added processing to remove oil before shipping is eliminated together with
costs. Many low alloy steel powders have been the smoke generated during the tempering operation.
developed for sinter hardening applications. These
materials, combined with the availability of sintering The substantial weight of the transfer case sprocket,
furnaces equipped with enhanced cooling capacity, 1,300 g, offers an interesting challenge to meet the NVG
make sinter hardening particularly attractive for parts that requirements using the sinter hardening route. The base
are difficult to quench because of their size and shape. powder must show good compressibility and high
Moreover, the powder mix formulation and processing hardenability to reach the density and apparent hardness
conditions can be tailored to achieve a specific specifications. Part I of this case study reviews the
microstructure. metallurgical aspects involved in the sinter hardening
process. The second part of the study covers the
The objective of this paper is to review the metallurgical evaluation of various material formulations and
aspects involved in sinter hardening and to relate these processing conditions to successfully produce transfer
to the characteristics of the base powder, admixed case sprockets by sinter hardening.
additions and processing conditions in order to develop
appropriate mix formulations for the production of HARDENABILITY AND HARDNESS
transfer case sprockets.
Hardenability is the property which determines the depth
INTRODUCTION and distribution of hardness induced by quenching a
steel. Hardenability is affected by the chemical
The former process to manufacture the NVG transfer composition, austenitic grain size and structure of the
case sprockets by P/M consisted in compacting parts to steel before quenching [1]. Hardness is the resistance of
densities ranging from 6.8 to 7.2 g/cm³ from a FN-0205 steel to plastic deformation [1]. It is usually measured by
mix. These were sintered at 1120°C for 20 to 25 a hardness testing machine that makes an indentation
minutes in a nitrogen-based atmosphere, sized to meet into the surface of the steel. For P/M materials, the
dimensional tolerances and heat treated to reach an residual porosity affects the resistance to plastic
apparent hardness of 30 HRC minimum. Parts were de- deformation and the term apparent hardness represents
oiled and tempered before shipping to customer. The the combination of matrix hardness plus the effect of
case sprockets must survive an engine test of 800 porosity. As illustrated in Figure 1, the apparent

1
hardness increases linearly with density. The maximum HV
hardness is that of a fully dense, fully martensitic 1000 HRC

structure. In the reference study [2], the amount of 900 Effect of retained 64
martensite in the forged specimens was about 90%, and 800
austenite
61
that of the pressed and sintered ones was about 75%. 700 57
Martensitic Structure (quenched)

HARDNESS
This explains why the straight line does not intersect the
600 53
matrix hardness at full density.
500 47

400 41

300 31
Pearlitic Structure (air cooled)
65 Matrix Hardness
200 13
APPARENT HARDNESS, HRC

100 Spheroidized Carbide Structure


60

0.2 0.4 0.6 0.8 1.0 1.2


55 CARBON, %

50 Figure 2. Hardness as a function of carbon content


and microstructure [3].
45 40

40 75% Martensite
90% Martensite 35

APPARENT HARDNESS, HRC


35
6.8 7.0 7.2 7.4 7.6 7.8 30
DENSITY, g/cm³

Figure 1. Variation of apparent hardness with 25

density of a sinter hardened steel (ATOMET 4701+2%


Cu+0.8%C) [2]. 20

The maximum hardness in a steel is achieved in a fully 15


martensitic structure for any given carbon content. This
is well illustrated in Figure 2. The hardness of martensite
10
rapidly increases with the carbon content to reach 60 10 20 30 40 50 60 70 80 90 100
HRC at about 0.4%C. Beyond this carbon concentration, MARTENSITE, %
the rate of increase is significantly reduced up to about
0.80%C to reach 65 HRC and then levels off due to the
tendency to retain austenite in high carbon steels. For Figure 3. Variation of apparent hardness with the
pearlitic and spheroidized carbide structures, hardness amount of martensite in sinter hardened specimens
increases linearly with carbon content [3]. Therefore, in (ATOMET 4701, 1% Cu and 0.65% combined carbon
a quenched structure, when the concentration of softer at 6.8 g/cm³).
phases increases, i.e. less martensite, the hardness of
Carbon is a key element to achieve high hardness in
the material diminishes. This is illustrated in Figure 3 for
steels. However, carbon alone is not sufficient to
sinter hardened specimens made from ATOMET 4701
achieve a throughout martensitic structure because of a
with 1% copper and 0.65% combined carbon cooled at
lack of hardenability. Rapid quench rates are therefore
different rates, 0.8 to 14°C/s from 650 to 400°C. The
required to full harden medium carbon steels and these
apparent hardness increases linearly with the amount of
lead to shape distortion and cracking [1]. For P/M
martensite. At a green density of 6.8 g/cm, the
materials, this phenomena is amplified because of the
maximum apparent hardness that can be achieved with
presence of porosity which lowers heat transfer during
this material is about 39 HRC which corresponds to a
cooling due to the lower thermal conductivity of porous
martensite content of 100%. The only way to further
parts [4].
increase hardness is to raise the density.
Alloying elements are therefore added to plain carbon
steels to improve mechanical properties by increasing
the depth of hardening. This means that larger sections
can be produced with a throughout martensitic structure.
Also, a high hardenable steel requires a slower quench
rate which leads to a significant reduction of thermal
stresses and distortion. This is exactly the principle
behind sinter hardening. Alloying elements are added in
the liquid steel or admixed with the powder to improve
hardenability.
2
EFFECT OF ALLOYING ELEMENTS hardenability of steels while the effect of copper and
nickel is significantly lower. Nevertheless, nickel, in
Sinter hardening is defined as a process where the either admixed or alloyed conditions, and admixed
martensite transformation takes place during the cooling copper are the most utilized elements in P/M because
phase of the sintering cycle. This means that the alloy their oxides are easily reduced at conventional sintering
hardenability and/or the cooling rate from the sintering temperature. However, in the admixed condition, the
temperature must be high enough to make that reaction diffusion of nickel in iron is incomplete and leads to a
occurs. The martensite transformation is a diffusionless heterogeneous microstructure after sintering which is not
reaction [5], meaning that there is no change in suitable for many sinter hardening applications where
chemical composition but a sudden change in crystal uniform apparent hardness is required. This is the
structure when austenite transforms in martensite. The reason why fully low alloy steel powders are generally
face-centered cubic (f.c.c.) structure of austenite used for these applications. Figure 5 illustrates the
changes into a supersaturated solid solution of carbon microstructures of a FD-0408 (diffusion alloy powder with
trapped in a body-centered tetragonal (b.c.t) structure by 4% Ni, 1.5% Cu and 0.80%C) and a sinter hardened
a combination of shearing actions. This creates a powder with 2% copper and 0.80% carbon. The
distorted lattice and the degree of distortion increases heterogeneous structure of the diffusion alloy is evident
with the concentration of carbon. This distorted lattice with the presence of martensite, bainite, pearlite and
accounts for the high hardness of martensite. The both rich nickel and retained austenite phases. For the
martensite reaction is also athermal [5], meaning that it fully pre-alloyed FLC-4608 type material (FL-4600
proceeds only on cooling and stops if cooling is powder with 2% admixed copper and 0.85% carbon),
interrupted. the microstructure consisted of almost only martensite
with few areas of bainite.
Basically there are two different types of steel powders
for P/M applications. First, unalloyed iron powders can 5

be used in combination with admixed elements.


Mn
Graphite, copper and nickel are the most commonly
used elements in the P/M industry. Copper and nickel 4
MULTIPLYING FACTOR

can be also bonded to the steel powders by either Mo


binder or diffusion treatments. These treatments are
known to minimize segregation and improve Cr Ni
3
dimensional stability. The former requires the use of an
organic binder while the latter required a thermal
treatment to bond the metallic additives to the steel
powders. Admixed nickel alone does not sufficiently 2
improve hardenability to obtain a large amount of Cu
martensitic after sintering at conventional sintering
temperature because of its poor diffusion in iron. High 1
temperature sintering and long time at temperature are 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5
therefore required to promote diffusion [6,7,8]. The use ALLOYING ELEMENTS, %
of manganese, chromium and molybdenum under either
their elemental forms, ferro or master alloys combined Figure 4. Effect of alloying elements on
to high temperature sintering to get these elements in hardenability of steels [10,11].
solution makes sinter hardening feasible with unalloyed However, pre-alloying nickel in the iron matrix tends to
powders as base material [6,9]. reduce the compressibility of steel powders because this
element is a ferrite strengthener as seen in Figure 6.
The second type of steel powders used in P/M Copper is also known to be a strong ferrite strengthener.
applications are low alloy steel powders. Because the Elements that promote the strength of the ferrite will
alloying elements are fully dissolved in the iron matrix, a negatively affect the powder compressibility. It can also
homogenous microstructure can be achieved after be observed on Figures 4 and 6 that chromium and
sintering at conventional temperature i.e 1120°C. molybdenum could be valuable pre-alloying elements to
Graphite, copper or nickel can also be admixed to improve hardenability while maintaining good
increase strength. As for unalloyed steel powders, compressibility. However, during water atomization and
binder or diffusion treatments can be used to improve annealing, some elements like manganese and
dimensional control. The utilization of elements with low chromium can be oxidized and this can also negatively
coefficient of diffusion in iron like nickel or ferroalloys affect compressibility [12]. Therefore, the concentration
requires high temperature sintering to get homogenous of these elements are generally maintained below 0.6%
microstructure. to minimize their negative impact on compressibility [12].
Molybdenum is a very interesting element that promotes
Figure 4 illustrates the effect of various alloying elements hardenability without strongly affecting compressibility.
on the hardenability of steels. Manganese, molybdenum However, this element is expensive and significantly
and chromium are the most efficient elements to improve raises the cost of the part.
3
the sintering temperature. Figure 7 illustrates continuous
cooling transformation diagrams (CCT) of materials
having different hardenabilities. In order to reach a fully
martensitic structure for a given material, the cooling
rate must be fast enough to miss not only the pearlite
nose but also the bainite nose of the CCT curves.

CR1 >> CR4 Matl Hardenability


Matl 1 << Matl 4
CR1 CR4

Matl 1 Matl 4
Austenite Pearlite

TEMPERATURE
Austenite Bainite

a
Austenite Martensite

TRANSFORMATION TIME

Figure 7. Illustration of microstructures obtained for


different materials of different hardenability
submitted to various cooling rates.
P/M steels with heterogeneous microstructure due to
incomplete diffusion of admixed elements as seen I
Figure 5a, can be visualized as a combination of many
materials. Areas rich in alloying elements have greater
hardenability than poor ones and shift the CCT diagram
b to the right. As a result, for a given cooling rate, there is
Figure 5. Microstructure of FD-0408 (a) and FLC- a mixture of various constituents depending on the
4608 (b) sinter hardened materials. concentration in alloying elements in a specific area in
220 the part. When fully alloyed P/M steels are used as base
Si
materials, it is easier to determine the critical cooling
200 Mn
rate which will allow to reach the desired microstructure.
BRINELL HARDNESS NUMBER

180
A simple technique consists in recording the cooling rate
that is encountered by the part when cooling from the
160
Ni
sintering temperature and correlates it to the apparent
Mo hardness and percent of martensite in the part. It is
140
V worth noting that the sintering conditions (furnace load,
belt speed, sintering temperature, atmosphere
120 W
composition) and the section thickness and density of
100
Cr the parts will have a significant impact on cooling rate.
At cooling rates generally obtained in standard sintering
80 conditions and for materials exhibiting good hardenability
like FLC-0208, the pearlite nose is easily missed.
60
0 2 4 6 8 10 However, this is not the case for the bainitic nose (from
ALLOYING ELEMENT IN FERRITE, % 650 to 400°C) since most of the sintering furnaces are
not equipped with fast cool units which make the
Figure 6. Probable hardening effect of various reduction of the cooling rate in this critical temperature
elements as dissolved in ferrite [13]. range feasible. Materials with enhanced hardenability
PROCESSING SINTER HARDENABLE MATERIALS are therefore required to retard the bainitic
transformation. Figure 8 illustrates the effect of the
The main goal of using sinter hardenable materials is to weight of four inch diameter discs on apparent hardness
achieve almost fully martensite structure and therefore of two sinter hardened materials with different
maximum apparent hardness after sintering. It becomes hardenability [14]. For the 400 g specimens, both
therefore important to well understand the phase materials show similar apparent hardness. However as
transformation mechanisms involved when cooling from the weight of the specimens is raised to 800 g, ATOMET
4
4701 which has higher hardenability than FL-4600 600

powder, shows a lesser reduction in hardness.


500

50

TEMPERATURE, °C
ATOMET 4701+2% Cu+ 0.8%C 400
45 FLC4608
APPARENT HARDNESS, HRC

40 300

35 Ms
200
30
100
25
Mf

20
0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
15
PERCENT CARBON, %
10 Figure 9. Influence of carbon content on the
5 martensite range [5].
400 600 800 1000 1200 1400
35 50
Specimen weight, g
Retained Austenite
Figure 8. Effect of specimen weight on apparent Apparent Hardness

APPARENT HARDNESS, HRC


hardness of sinter hardened materials (green density 30

RETAINED AUSTENITE, %
of 6.8 g/cm³) [14].
40

It was previously mentioned that carbon content is the 25

key element to achieve high hardness. However, in high


carbon steels, it is easier to retain austenite at room 20
temperature. Raising the carbon content lowers both Ms 30
(temperature at which transformation of austenite to
martensite starts) and Mf (temperature at which 15

transformation ends) [5]. As illustrated in Figure 9, as


the carbon content exceeds 0.6%, austenite is not all 10 20
transformed into martensite at room temperature and the 0.65 0.80

range from Ms to Mf is enlarged with increasing carbon COMBINED CARBON, %


levels. Raising the concentration of alloying elements Figure 10. Effect of combined carbon concentration
also lowers Ms and increases the susceptibility of of percent of retained austenite in sinter hardened
retaining austenite in alloyed steels. Because sinter P/M steels (ATOMET 4701+2% Cu+C; 7.0 g/cm³) [15].
hardened P/M materials generally contain high combined
Figure 11 illustrates the effect of the tempering
carbon, they are susceptible to retain austenite. This is
temperature on apparent hardness, tensile properties
illustrated in Figure 10. Raising the combined carbon
and impact energy of sinter hardened materials
from 0.65% to 0.80% in this sinter hardened P/M steel
containing 0.65% and 0.80% combined carbon [15]. It is
increases the amount of retained austenite from 15% to
evident from this figure that maximum values of all
28% [15]. Because retained austenite is softer than
properties cannot be met at the same time and
martensite, the higher amount of retained austenite in
compromises are therefore required when designing a
the high carbon material probably limits the gain in
new part. The high carbon material exhibits the highest
apparent hardness to 4 HRC.
apparent hardness in the as-sintered condition and for
the various tempering temperatures. However, this
The transformation of austenite into martensite due to
material shows lower tensile and yield strengths than the
the change of the f.c.c. structure to b.c.t structure
0.65% C material in the as-sintered condition and for
creates a highly distorted lattice with volume expansion
tempering temperatures up to about 500°C. In the as-
which accounts for the high hardness of martensite.
sintered condition, both materials show comparable low
Therefore, a tempering treatment is generally carried out
impact energy values.
on sinter hardened parts to restore their mechanical
properties. The tempering temperature depends on
Therefore, for applications requiring high apparent
whether the strength, impact resistance or hardness
hardness and where mechanical properties are less
needs to be optimized.
critical, tempering can be avoided. However, for
applications requiring a good combination of hardness
and strength, tempering the 0.80%C material at only
150°C for 60 minutes is a good compromise with a loss
of only 2 HRC in hardness, from 41 to 39 HRC, but a
gain of more than 10% in tensile strength, from 817 to
910 MPa and 50% in impact energy from 12 to 17 joules.

5
Applications requiring high tensile strength and impact resistance.
energy require a lower carbon content i.e. 0.65%, and a
tempering treatment at 200°C. CONCLUSIONS
45
Sinter hardening makes the production of parts with high
0.80% C
apparent hardness feasible after sintering, eliminating
40
the need for a post-sintering heat treatment. The
APPARENT HARDNESS, HRC

following elements are key parameters to succeed with


35 sinter hardening:
0.65% C

30 1. Base powders must show sufficient hardenability in


order to produce martensite when P/M parts are
25
cooled from the sintering temperature. These
powders must also have good compressibility to
reach high green density during the compaction
20
step.
15
int
. 100 200 300 400 500 600 700 2. Because of the presence of porosity, P/M steels
-S
As
TEMPERING TEMPERATURE, °C always exhibit lower apparent hardness than the
1100
same material at full density. For a given martensite
content, apparent hardness of P/M steels increases
linearly with density.
1000 0.65% C Tensile Strength

3. At a given density, apparent hardness increases


STRENGTH, MPa

900
linearly with the martensite content.

4. To fully harden P/M parts, cooling rates from the


800
0.80% C No yield at 0.8%C
sintering temperature must be fast enough to avoid
at 400°C both the pearlite and bainite transformations.
Yield Strength
0.65% C
700
0.80% C
5. Proper adjustment of the carbon content is required
to reach the optimum combination of hardness and
600
.
strength.
int 100 200 300 400 500 600 700
-S
As
TEMPERING TEMPERATURE, °C
6. A good understanding of the application is required
22
to successfully design a sinter hardened part.
Specific part requirements must lead the choice of
20 0.80% C
the base powder and mix formulation as well as the
compaction and sintering parameters and the
IMPACT ENERGY, J

18 tempering conditions.

16 REFERENCES
0.65% C
14
1. Smith, W.F., “Structure And Properties Of Engineering
Alloys”, McGraw-Hill, New York, 1981, pp 114-161.
2. Chagnon F. and Trudel Y., “Effect Of Density On
12 Mechanical Properties Of Sinter Hardened P/M Materials”,
Advances in Powder Metallurgy & Particulate Materials,
Vol. 3 Metal Powder Industries Federation, Princeton, NJ,
10
-S
int
. 100 200 300 400 500 600 700 1998, pp 12-119 to 12-125.
As 3. Krauss G., “STEELS: Heat Treating And Processing
TEMPERING TEMPERATURE, °C
Principles”, American Society for Metals, Materials Parks,
Figure 11. Effect of tempering temperature and OH, 1990, pp145-179.
carbon content on apparent hardness, tensile 4. Ferguson, H., “The Heat Treatment Of P/M Steels-An
th
properties and impact energy of sinter hardened Overview”, Proceedings of the 16 ASM Heat Treating
materials (ATOMET 4701+2% Cu+C at 6.9 g/cm³) [15]. Society Conference & Exposition, 19-21 March 1996,
Cincinnati, OH, pp 319-322.
To maximize yield strength, a tempering treatment at 5. Avner, S.H., “Introduction To Physical Metallurgy”,
300°C is required. This is the temperature where McGraw-Hill, New York, 1974, pp 249-347.
retained austenite is almost completely transformed into 6. Danniger H., “Sintering Of Low Alloy Steels Prepared
From Elemental Powders”, Powder Metallurgy Science &
ferrite and carbides. However, at this temperature, sinter Technology-Vol.-4, July 1993, pp 22-36.
hardened materials are sensitive to temper 7. Kawase K., Morimoto K., Kohno T. and Yanagawa H.,
embrittlement which significantly deteriorates impact “High Temperature Sintering Of Low Alloy Steel Powders”,
6
SAE International Congress & Exhibition, Detroit February
26-29, 1996, SAE Technical Paper 960381.
8. Miura H., Baba T. and Honda T., “The Effect Of
Heterogeneous Structure On The Properties Of Sintered
Low Alloy Steels”, Advances in Powder Metallurgy &
Particulate Materials, Vol. 4 Metal Powder Industries
Federation, Princeton, NJ, 1996, pp 13-42 to 13-49.
9. Shivanath R., Jones P.K. and Lawcock R., “On The
Synergies Of High Temperature Sintering And Alloy
Development For High Endurance P/M Powertrain
Components”, Advances in Powder Metallurgy &
Particulate Materials, Vol. 4 Metal Powder Industries
Federation, Princeton, NJ, 1996, pp 13-427 to 13-437.
th
10. “The Making, Shaping And Treating Of Steel”, 9 edition,
United Steel Corporation, 1971.
11. Grossmann M.A. and Bain E.C., “Elements of
Hardenability”, American Society for Metals, Metals Park,
OH, 1952.
12. Trudel Y. Gagné and Racicot F., “Design Criteria For The
Manufacturing Of Low Alloy Steel Powders”, Advances in
Powder Metallurgy & Particulate Materials, Vol. 5 Metal
Powder Industries Federation, Princeton, NJ, 1991, pp
45-58.
13. Avner, S.H., “Introduction To Physical Metallurgy”,
McGraw-Hill, New York, 1974, pp 349-385.
14. Chagnon F. and Trudel Y., “Designing Low Alloy Steel
Powders For Sinter Hardening Applications”, Advances in
Powder Metallurgy & Particulate Materials, Vol. 4 Metal
Powder Industries Federation, Princeton, NJ, 1996, pp
13-211 to 13-220.
15. Chagnon F. and Gagné M., “Effect Of Tempering
Temperature On Mechanical Properties And
Microstructure Of Sinter Hardened Materials”, Advances
in Powder Metallurgy & Particulate Materials, Vol. 2 Metal
Powder Industries Federation, Princeton, NJ, 1999.

You might also like