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EFFECT OF COPPER ALLOY ADDITION METHOD

ON THE DIMENSIONAL RESPONSE OF SINTERED FE-CU-C STEELS

Michael L. Marucci and Francis G. Hanejko


Hoeganaes Corporation
Cinnaminson, NJ 08077 - USA

Abstract

Fe-Cu-C is the most common alloy system used in press and sinter powder metallurgy. This system has
many advantages including excellent mechanical properties, sinterability, and competitive cost. However,
as end customers continue to require tighter dimensional control of finished parts this alloy is at a
disadvantage due to its inherent dimensional variability. Changing the method of copper addition influences
the dimensional stability of this system. This work studies the mechanical, dimensional, and microstructural
differences of sintered Fe-Cu-C steels with atomized copper, diffusion alloyed Fe-Cu, and chemically
bonded copper additions.

Introduction

Copper additions to iron powder were among the first additions to improve the strength of sintered steels.
Additions of graphite to Fe-Cu sintered steels are also desirable because the carbon promotes the
formation of a pearlitic microstructure, imparting additional strength and hardness to the steel.
Unfortunately, these admixed elements result in dimensional growth upon sintering which can result in
dimensional variation of the finished component. As dimensional precision requirements for PM
components continue to become more demanding, alternate alloying methods need to be considered to
reduce the inherent dimensional variation of Fe-Cu-C sintered steels.

Elemental copper is advantageous due to its melting point at 1083 C (1981 F), which promotes sintering
and enhances the strength of the steel. Despite the relatively low melting point of the copper, it does not
fully diffuse within the iron at conventional sintering times and temperatures. This results in a copper
gradient from the iron powder surface to the core. 1 Earlier work also has shown that the amount of carbon
present within a compact changes the rate at which copper alloys with the steel matrix due to the change
in the dihedrial angle of the molten phase. 2 Both effects result in dimensional growth after sintering. The
dimensional growth is dependent on the chemical composition of the compact and is particularly sensitive
at 2 w/o copper additions. 3 Unlike other PM material systems, FC-0208 type materials exhibit less
dimensional growth as the sintered carbon increases, as seen in figure 1. Utilizing a 1 w/o copper
addition reduces the sensitivity of sintered carbon on dimensional variation. However, at this reduced
copper addition level, the strength is below that of a standard FC-0208 material.

Figure 1: Dimensional change of Fe-Cu-C steels (chart from Lindsley, et-al, ref 3)

As a 2 w/o copper addition remains desirable for mechanical properties, every effort needs to be made to
reduce the local variation of copper and graphite within the compact. The current work examines the
effect of different copper addition methods on dimensional variation and also looks at the effects of
bonding the admixed ingredients. The use of ANCORBOND or Fe-20Cu Distaloy is of particular interest
because these methods limit the possibility of elemental powder segregation during premix handling,
which could induce the dimensional variation detailed in figure 1.

Experimental Procedure

Table I outlines the materials used for this study, all prepared as 225 kg (500 lb.) premixes. All materials
conform to FC-0208 4 . The base steel powder used was Hoeganaes Ancorsteel 1000B, which is an
unalloyed water atomized steel powder. All premixes were prepared with 0.80 w/o natural flake graphite.

Three different types of copper additions were investigated. The Standard Atomized is water atomized
copper powder having a D90 of 84 m and a D50 of 39 m. The Fine copper is a reduced copper
powder having a D90 of 17 m and a D50 of 10 m. FD-20Cu is steel powder that is diffusion alloyed
with 20 w/o copper powder. This alloy is produced by Hoeganaes. Figures 2-4 show SEM
photomicrographs of each type of copper evaluated. The photomicrographs clearly show the differences
in particle size and morphology.

Different lubricant systems were also evaluated. The standard premix used admixed EBS for the
lubricant. Hoeganaes ANCORBOND was also used in combination with the EBS to gauge the impact
of bonding the mix ingredients on dimensional stability.

Table I: Test alloy matrix

Designation Base Steel Copper Addition Graphite Lubricant Addition


(w/o) (w/o) (w/o)
Std Cu Mix Ancorsteel 1000B 2.0 Standard Cu 0.80 0.75 EBS Premix
Std Cu Bond Ancorsteel 1000B 2.0 Standard Cu 0.80 0.75 EBS ANCORBOND
Fine Cu Bond Ancorsteel 1000B 2.0 Fine Cu 0.80 0.75 EBS ANCORBOND
FD-20Cu Bond Ancorsteel 1000B 10.0 Fe-20Cu Distaloy 0.80 0.75 EBS ANCORBOND
Figure 2: SEM Photomicrograph
of the Standard Cu powder, water
atomized, 1000x original
magnification.

Figure 3: SEM Photomicrograph


of the Fine Cu powder, reduced,
1000x original magnification.

Figure 4: SEM Photomicrograph


of the FD-20Cu powder, water
atomized, 800x original
magnification.
All premixes in Table I were compacted at room temperature. Green density and green strength were
measured using the green strength samples (MPIF Std 15). Mechanical properties were determined using
Transverse Rupture (MPIF Std 41), dog bone tensile (MPIF Std 09), and un-notched Charpy Impact
(MPIF Std 40) samples, which were compacted from each mix over a range of compaction pressures.

Sintering was conducted in a continuous belt furnace at 1120 C (2050 F) in an atmosphere of 90 v/o N2
+ 10 v/o H2. The test samples remained at sintering temperature for approximately 15 minutes.
Conventional cooling was used. Selected samples were tested in the heat-treated condition. Heat-
treatment consisted of austenitizing at 871 C (1600 F) in an atmosphere of 25 v/o N2 + 75 v/o H2 and
quenching in agitated oil heated to 66 C (150 F). The quenched samples were subsequently tempered at
204 C (400 F) in 100 v/o N2 for 1 hour.

Results and Discussion

The compressibility of the test alloys is shown in figure 5. The chart shows that the different copper
addition types have a small effect on the compressibility. The densities achieved are within 0.04 g/cm3
over the test range. The fine copper resulted in a slightly higher green density, most likely due to the
better packing of the fine particles.

Compaction Pressure (tsi)


20 30 40 50 60
7.30

7.20
Green Density (g/cm3)

7.10

7.00

6.90 Std Cu Mix


Std Cu Bond
6.80 Fine Cu Bond
FD-20Cu Bond

6.70
275 413 551 688
Compaction Pressure (MPa)

Figure 5: Compressibility of test alloys.

The as-sintered and heat-treated mechanical properties of the test alloys are summarized in Tables II and
III. At a given sintered density, the mechanical properties are largely within experimental error when
comparing the different copper addition methods along with different mixing techniques. All properties
meet or exceed MPIF Standard 35 for FC-0208.
Table II: As-Sintered Mechanical Properties
Sintered at 1120 C (2050 F) 90 v/o N2 + 10 v/o H2

Compaction Sintered Transverse Ultimate Tensile Impact Apparent


Yield Strength Elongation
Pressure Density Rupture Strength Strength Energy Hardness
3 3
tsi MPa g/cm psi x 10 MPa psi x 103 MPa psi x 103 MPa % ft.lbf J HRA
2.0 w/o Std Cu Mix
30 414 6.75 134 924 55 376 66 453 1.3 8 11 45
40 552 6.97 157 1082 62 427 77 530 1.3 10 13 49
50 689 7.08 168 1160 64 442 80 552 1.5 12 17 50
2.0 w/o Std Cu Bond
30 414 6.75 132 911 55 377 65 450 1.2 7 10 45
40 552 6.95 154 1065 60 415 74 511 1.3 10 13 49
50 689 7.06 166 1144 63 433 79 543 1.3 12 17 51
2.0 w/o Fine Cu Bond
30 414 6.74 130 897 55 378 66 454 1.2 7 10 46
40 552 6.95 147 1012 62 430 76 524 1.4 9 12 50
50 689 7.04 151 1044 63 434 77 530 1.2 10 14 51
10.0 w/o FD-20Cu Bond
30 414 6.74 130 899 53 367 65 451 1.3 7 10 47
40 552 6.95 151 1041 63 432 77 530 1.4 10 13 50
50 689 7.06 162 1116 68 468 84 579 1.5 12 16 51

Table III: Heat-Treated Mechanical Properties


Sintered at 1120 C (2050 F) 90 v/o N2 + 10 v/o H2
Austentized at 871 C (1600 F), Tempered at 204 C (400 F)

Compaction Sintered Transverse Ultimate Tensile Impact Apparent


Yield Strength Elongation
Pressure Density Rupture Strength Strength Energy Hardness
3 3
tsi MPa g/cm psi x 10 MPa psi x 103 MPa psi x 103 MPa % ft.lbf J HRA
2.0 w/o Std Cu Mix
30 414 6.75 143 988 60 412 82 567 0.6 5 7 67
40 552 6.95 157 1079 67 464 94 647 0.6 7 9 71
50 689 7.05 170 1171 79 547 101 693 0.7 8 11 71
2.0 w/o Std Cu Bond
30 414 6.75 132 907 66 455 83 572 0.6 5 7 67
40 552 6.95 159 1096 77 533 98 673 0.6 6 9 69
50 689 7.05 174 1196 68 471 99 683 0.5 7 10 71
2.0 w/o Fine Cu Bond
30 414 6.75 135 931 69 474 88 605 0.6 6 8 67
40 552 6.94 166 1147 74 509 98 673 0.6 7 9 69
50 689 7.04 171 1177 86 591 100 689 0.5 8 11 71
10.0 w/o FD-20Cu Bond
30 414 6.75 134 924 60 411 80 550 0.5 5 7 67
40 552 6.95 168 1155 69 479 99 680 0.5 6 8 70
50 689 7.05 169 1164 73 504 101 697 0.5 8 11 71
10.0 w/o FD-20Cu - HD
30 414 6.83 73 504 25 173 45 313 0.2 3 4 69
40 552 7.05 82 568 23 162 46 316 0.2 3 5 71
50 689 7.16 92 632 29 198 56 384 0.2 3 4 73
60 827 7.21 90 621 29 197 60 415 0.2 3 5 74

Figure 6 shows the tensile strength of both the as-sintered and heat-treated condition for the bonded test
mixes. The copper addition type does not influence the ultimate tensile strength. The quench and temper
heat-treatment results in a 140 MPa (20,000 psi) increase in tensile strength over the range of densities
evaluated.
120 828
Std Cu Bond
Fine Cu Bond
110 FD-20Cu Bond 759
Std Cu Mix Heat-Treated

UTS (psi x 1000)


100 690

UTS (MPa)
90 621

80 552
As-Sintered
70 483

60 414

50 345
6.70 6.80 6.90 7.00 7.10 7.20
3
Sintered Density (g/cm )
Figure 6: Ultimate tensile strength comparison.

The as-sintered axial fatigue behavior of the different copper addition types is detailed in figure 7. The
fatigue response is very similar for all copper addition types. Both the standard Cu and the FD-20Cu had
a fatigue endurance limit (FEL) of 131 MPa (19.0 psi x 1000). The fine Cu version had a slightly lower
FEL of 124 MPa (18.0 psi x 1000). This indicates that all copper addition types would be acceptable for
use in the as-sintered state. Testing of heat-treated materials was not completed due to difficulty in
gripping the dog-bone type samples.

Figure 7: As-Sintered axial fatigue comparison (R = -1).


Apparent hardness is highlighted in figure 8. Again, the copper addition type does not impact the
hardness level achieved. Heat-treating results in a substantial increase in apparent hardness. For all
materials at 6.95 g/cm3, the hardness goes from 50 HRA (81 HRB) to 68 HRA (35 HRC).

80
75 Heat-Treated
Apparent Hardness (HRA)
70
65
60
55
As-Sintered
50
45
Std Cu Bond
40 Fine Cu Bond
FD-20Cu Bond
35
Std Cu Mix
30
6.70 6.80 6.90 7.00 7.10 7.20
3
Sintered Density (g/cm )
Figure 8: Apparent hardness comparison

Unlike the mechanical properties, the dimensional change is impacted by the copper addition technique.
Figure 9a shows the dimensional change in the as-sintered condition. For all materials, the dimensional
growth increases as density increases. Typically, dimensional change as close to 0.0% is desired for
dimensional stability. The standard copper and the FD-20Cu had similar values and the fine copper
addition produces the highest dimensional growth. It is hypothesized that the higher growth is caused by
larger number of Fe-Cu interfaces within the compact. Upon melting, the copper diffuses along the grain
boundaries causing swelling; the finer copper has more particles resulting in more interfaces and added
swelling. The higher growth caused by the fine copper makes this powder type an undesirable copper
addition method for the FC-0208 system.

a.) As-Sintered b.) Heat-Treated

0.70 0.70
Dimensional Change (%)

Dimensional Change (%)

0.60 0.60

0.50 0.50

0.40 0.40

0.30 0.30
Std Cu Mix
0.20 Std Cu Bond 0.20 Std Cu Mix
Std Cu Bond
Fine Cu Bond Fine Cu Bond
0.10 0.10
FD-20Cu Bond FD-20Cu Bond
0.00 0.00
6.70 6.80 6.90 7.00 7.10 7.20 6.70 6.80 6.90 7.00 7.10 7.20
3 3
Sintered Density (g/cm ) Sintered Density (g/cm )
Figure 9: As-sintered and heat-treated dimensional change.
Heat-treatment results in a similar trend in dimensional response (figure 9b), however, the final
dimensional growth is lower than in the as-sintered state. Typically, the transformation to a martensitic
microstructure results in a positive size change. However, additional shrinkage occurs during the
austenization/tempering of the steel, offsetting this effect. Again, the standard copper and the FD-20Cu
have the lowest dimensional growth.

Data from a separate study 5 show that when the carbon and copper content of the test alloys are moved
over a range of values, the dimensional change varies, as shown in figure 10. Unlike the behavior shown
in figure 1, the rate of change as a function of chemistry is almost the same for each alloying method and
carbon content, but the relative dimensional growth is similar to what is found in the present study. This
shows that the FD-20Cu could be used as an alternative to the standard Cu.

a.) 2.0 w/o Cu b.) 0.8 w/o Graphite


0.80 0.80
0.70 0.70
Dimensional Change (%)

Dimensional Change (%)


Std Cu Std Cu
Fine Cu Fine Cu
0.60 FD-20Cu 0.60 FD-20Cu

0.50 0.50
0.40 0.40
0.30 0.30
0.20 0.20
0.10 0.10
0.00 0.00
0.5 0.6 0.7 0.8 0.9 1.0 1.0 1.5 2.0 2.5 3.0
Graphite Addition (w/o) Cu Addition (w/o)
Figure 10: As-sintered dimensional change as a function of carbon and copper addition. All samples
compacted to 6.90 g/cm3.

The as-sintered and heat-treated microstructures for the standard Cu and FD-20Cu are compared in
figures 11 and 12. As expected, both copper addition types produced a pearlitic as-sintered
microstructure. The heat-treated microstructure consists of lath martensite with some areas of bainite.
The FD-20Cu sample has a larger amount of bainite; this is most likely due to incomplete diffusion of
copper in the iron particles. Moving from a pure copper particle to an Fe-Cu Distaloy has minimal effect
on the finished microstructure.
a.) b.)

Figure 11: Standard copper, a.) as-sintered and b.) heat-treated, 2% nital/4% picral etch

a.) b.)

Figure 12: FD-20Cu, a.) as-sintered and b.) heat-treated, 2% nital/4% picral etch

To determine the relative dimensional stability of the test materials a prototype spur gear was produced
and a measurement over wires (MOW) technique was used to determine dimensional variation. The
geometry of the prototype gear is shown in Figure 13. 500 samples per material were compacted with a
target density of 6.9 g/cm3 on a 140 t Dorst press. All samples were sintered/heat-treated under the same
conditions as listed above. MOW was conducted on 20 random gears from each test condition.

Major OD 1.10 in (28.3 mm)


Minor OD 0.85 in (21.6 mm)
Pitch Diameter 0.96 in (24.5 mm)
Pressure angle 20
ID 0.38 in (9.5 mm)
# Teeth 16
Module 1.66

Figure 13: Prototype gear produced to evaluate part-to-part consistency


Table IV summarizes the MOW results. The data show, as predicted above, that gears in the as-sintered
and heat-treated condition produced with fine Cu resulted in slightly larger dimensions. The scatter in the
dimensional measurements for all materials falls within a tight range. However, the bonded version with
the standard Cu results in a lower measured scatter than the premixed version. The standard Cu compared
to the FD-20Cu shows mixed results and indicate that the dimensional scatter is similar under these test
conditions. The fine Cu version resulted in the largest scatter of the group.

Table IV: Measurement Over Wires Evaluation As-Sintered

Std Cu Std Cu Fine Cu FD-20Cu


Premix Bond Bond Bond
As-Sintered
Average (mm) 30.70 30.69 30.72 30.69
Standard Deviation 0.021 0.015 0.024 0.019
Heat-Treated
Average (mm) 30.72 30.71 30.74 30.71
Standard Deviation 0.019 0.017 0.020 0.015

Conclusions

Different types of copper additions are viable in FC-0208 alloys. The resulting mechanical
properties in the as-sintered and heat-treated states are within measurement error for fine copper
and FD-20Cu addition when compared to the standard Cu.
The finished microstructure is minimally impacted by changing the copper addition type.
The use of fine Cu in this alloy induces higher dimensional growth than other copper addition
types. Standard Cu and FD-20Cu additions produce a similar dimensional response.
ANCORBOND processed premixes show a reduction in dimensional scatter when compared to a
standard premix
The use of bonded FD-20Cu in FC-0208 is equivalent to bonded Standard Cu under the
conditions evaluated. The use of FD-20Cu in place of standard Cu should be considered where
there the possibility of copper segregation due to powder handling exists.

References
1
T. Murphy and M. Baran, An Investigation into the effect of Copper and Graphite Additions to Sinter-
Hardening Steels, Advances in Powder Metallurgy & Particulate Materials 2004, Metal Powder
Industries Federation, Princeton, NJ, part 10, pp. 266-274
2
R. Lawcock and T. Davis, Effect of carbon on dimensional and microstructural characteristics of Fe-Cu
compacts during sintering, Powder Metallurgy, Vol. 33, No. 2, 1990, p 147-150, Elsevier
3
B. Lindsley, G. Fillari and T. Murphy, Effect of composition and cooling rate on physical properties
and microstructure of prealloyed P/M steels, Advances in Powder Metallurgy & Particulate Materials,
compiled by C. Ruas and T. A. Tomlin, Metal Powder Industries Federation, Princeton, NJ, 2005, part 10,
p. 10-353.
4
MPIF Standard 35, Material Standards for PM Structural Parts, 2009 ed. MPIF, Princeton, NJ - USA
5
B. Lindsley, 2009, Internal Hoeganaes Study on the effects of premix chemistry on dimensional change.