Sintering Furnace Cycle Influence on Sinter Hardened Part

Parameters
PM2TEC 2001
John McLelland, Owe Mårs, North American Höganäs, Inc. &
Thomas J. Jesberger, ABBOTT Furnace Co.

ABSTRACT:

It is well known that the cooling rate influences the final microstructure and therefore the properties of
sinter hardened steel parts. This investigation looked at the relationship between the sintering furnace
cycle (time, temperature and atmosphere) and cooling rate to part microstructure. The objective was to
identify how the above sintering variables influenced the development of martensite, hardness and
strength.

Tests were conducted varying the sintering cycle. The changes to the cycle were sintering time, sintering
temperature, atmosphere composition (specifically hydrogen concentration), and cooling rate. The final
microstructure was evaluated and correlated to the sintering cycle.

INTRODUCTION:

Sinter hardening has become a very attractive processing technique due to the resulting beneficial
mechanical properties and production advantages due to the elimination of some secondary operations.
Much knowledge about sinter hardening has been gained as more companies use this process to sinter
production parts. Cooling rate is one known factor that influences the as sintered microstructure and
ultimately, the properties of the part. However, there are other elements that can affect the outcome of the
final parts such as sintering time, temperature, and atmosphere composition. Recent work has been
conducted in this area to understand and to help quantify the positive aspects of sinter hardening.

The goals of this investigation are:

1. To relate the properties of 3 sinter hardenable materials with respect to variations in sintering
parameters (sintering time, cooling rate, and atmospheric composition).
2. To gain a quantitative representation of which sinter hardening parameters create the most impact
on the final properties of the materials.
3. To better understand the other factors that might influence sinter hardened parts.

PROCEDURE:

3 sinter hardenable materials were analyzed for this investigation:

1. Astaloy A + 2% Cu + 0.8% Graphite + 0.75% Acrawax C

2. D.DH-1 + 0.8% Graphite + 0.75% Acrawax C
3. Astaloy CrM + 0.4% Graphite + 0.75% Acrawax C

Note: materials above made up of following compositions

1. Pre-alloyed (2% Ni + 0.5% Mo)
2. Diffusion bonded (2% Cu + 1.5% Mo)
3. Pre-alloyed (3% Cr + 0.5% Mo)
Each material was pressed into transverse rupture strength bars (TRS) and tensile bars to 7.0 g/cm3.

The TRS and tensile bars were sintered on a six-inch laboratory designed furnace with a convection
cooling system. Four (4) temperature profiles were taken to document the cooling rates. It was assumed
that the cooling rates for the 30 minutes sintering time would be the same as those obtained for the 10
minutes. The only difference between these cooling rates was the longer holding time in the hot zone
from 10 minutes to 30 minutes as an index system was used with the same 6 inch per minute belt speed
for the remaining portion of the sintering cycle.

Sintering was performed varying the cooling fan speed from 0 Hz to 10 Hz, H2 % from 5% to 20%, and
sintering time in the hot zone from 10 minutes to 30 minutes. Thus, each material experienced 8 profiles
in the sintering furnace.

After sintering, TRS bars and tensile bars were annealed in air for 1 hour at 380 deg. F. Some TRS bars
were also left un-annealed.

Hardness was measured on the un-annealed and annealed TRS bars.

TRS was measured on the un-annealed and annealed TRS bars.

Tensile strength and elongation were measured on the annealed tensile bars.

As sintered bars were analyzed at each condition for combined carbon. The Cr based material was also
checked for O2 and N2 after sintering.

RESULTS:

Below is a table representing the time to cool in seconds for the temperature ranges indicated. The data is
presented from the fastest cooling rate (CR1) to the slowest cooling rate (CR4). Cooling rate 1 (CR1)
was for the condition 20% hydrogen and fan speed set to 10Hz. CR2 through CR4 are as indicated in the
table for their conditions. The values are cumulative; ie. time to cool from 1400 to 400 for CR1 is 162
seconds.

Table 1
20% H 5% H 20% H 5% H
10 Hz 10 Hz 0 Hz 0 Hz
Temp (F) CR1 CR2 CR3 CR4
1400-1300 18 18 18 21
1300-1200 33 36 33 39
1200-1100 48 48 48 60
1100-1000 57 60 63 78
1000-900 66 69 78 99
900-800 81 87 99 123
800-700 102 108 126 150
700-600 120 129 156 186
600-500 138 147 201 240
500-400 162 174 264 315
C/sec 3.4 3.2 2.1 1.8
F/min 370 345 227 190

Cooling Rates in degrees C per second and degrees F per minute

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A design of experiments (DOE) was conducted to see what were the major contributing factors [1].

From the DOE as well as the raw data, charts were created for each material to demonstrate the effect of
the sintering process variations.

Figures 1 and 2 demonstrate the data obtained for the Astaloy A + 2% Cu + 0.8% C mix.

Ast A + 2% Cu + 0.8% Graphite @ 5% H2

36.5 230
36 225
220
Hard., Ann. (HRC)

35.5

TRS, Ann. (kpsi)

215 Hard. 10 min.
35
210 Hard. 30 min.
34.5
205 TRS 10 min.
34 TRS 30 min.
200
33.5 195
33 190
32.5 185
0 2 4 6 8 10
Cooling Speed (Hz)

Figure 1

Ast A + 2% Cu + 0.8% Graphite @ 20% H2

35.5 225
224
35
223
Hard., Ann. (HRC)

TRS, Ann. (kpsi)

34.5 222
Hard. 10 min.
221
Hard. 30 min.
34 220
TRS 10 min.
219
33.5 TRS 30 min.
218

33 217
216
32.5 215
0 2 4 6 8 10
Cooling Speed (Hz)

Figure 2

It is seen in Figure 1 how the hardness increases slightly with cooling speed. It is difficult to draw
conclusions on any effects on TRS. Figure 2 shows much of the same trends.

Figures 3 and 4 represent the results of the D.DH-1 + 0.8% C mix.

D.DH-1 + 0.8% Graphite @ 5% H2

38 245
36
240
34
Hard., Ann. (HRC)

TRS, Ann. (kpsi)

235
32 Hard. 10 min.
30 230 Hard. 30 min.
28 225 TRS 10 min.
26 TRS 30 min.
220
24
215
22
20 210
0 2 4 6 8 10
Cooling Speed (Hz)

Figure 3

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 D.DH-1 + 0.8% Graphite @ 20% H2

40 250
35 245

Hard., Ann. (HRC)

30 240

TRS, Ann. (kpsi)

25 235 Hard. 10 min.
Hard. 30 min.
20 230
TRS 10 min.
15 225 TRS 30 min.
10 220
5 215
0 210
0 2 4 6 8 10
Cooling Speed (Hz)

Figure 4

Both Figures 3 and 4 demonstrate the increase of hardness with increasing cooling speed. TRS is affected
by the longer sintering time. The greater slope of the hardness curves in relation to increasing cooling
speed supports this. This is evidenced by the upward shift of the TRS curves with respect to increasing
sintering time.

Figures 5 and 6 show the data from the Astaloy CrM + 0.4% C mix.

Ast CrM + 0.4% Graphite @ 5% H2

29 260

27 250
Hard., Ann. (HRC)

TRS, Ann. (kpsi)

25
240 Hard. 10 min.
23 Hard. 30 min.
230
21 TRS 10 min.
220 TRS 30 min.
19

17 210

15 200
0 2 4 6 8 10
Cooling Speed (Hz)

Figure 5

Ast CrM + 0.4% Graphite @ 20% H2

29 260

27 250
Hard., Ann. (HRC)

TRS, Ann. (kpsi)

25
240 Hard. 10 min.
23 Hard. 30 min.
230
21 TRS 10 min.
220 TRS 30 min.
19

17 210

15 200
0 2 4 6 8 10
Cooling Speed (Hz)

Figure 6

Figures 5 and 6 both show how hardness increases with increasing cooling speed. TRS increases with
both sintering time and cooling speed.

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Total carbon after sintering was conducted on all materials as well as oxygen and nitrogen for the Astaloy
CrM grade to verify that the atmosphere was not causing any carburizing, de-carburizing, or oxidizing
conditions. The tests were encouraging as changes in carbon were little, only 0.1% less than the as-mixed
condition. Oxygen and nitrogen levels were extremely low.

Sintered densities were also measured for each of the materials. Astaloy A mix was 6.83 g/cc; D.DH-1
mix was 6.87 g/cc; and Astaloy CrM mix was 6.93 g/cc.

DISCUSSION:

Referencing Table 1 from above, several statements can be made regarding cooling rate. First is that
convection cooling is necessary to increase cooling rate. The next statement is that increasing the
hydrogen percent increases the cooling rate regardless of the fan speed.

Ast A Mix: Some trends have been seen based on the results. For the Astaloy A material, the hardness
slightly increased with the increase in the cooling fan speed. Any effects of any sintering process
variables on TRS were hard to decipher. It was difficult to show any type of contrast due to processing
effects with this material due to the high carbon content and presence of large amounts of martensite.
Due to the higher hardness and levels of martensite, the elongation and TRS as well as tensile strength
were lower for this material than both of the others.

It is also evidenced in Figure 1 how TRS decreases at the 30 minutes sintering time when the cooling rate
increases. More investigation will be required to examine this phenomenon, but the high levels of
martensite could in fact cause residual stresses thus decreasing ultimate tensile strength.

D.DH-1 Mix: The D.DH-1 material showed some interesting traits due to sintering process variations.
The hardness in the tempered state was nearly as high as the Astaloy A material. The cooling rate was the
driving force in the hardenability of this material. However, this was not the only finding.

Increased sintering time allows for better sintering necks. It also allows for the copper to diffuse better
into the matrix. Figure 7 shows poor copper diffusion at only 10 minutes sintering time. The copper is
still present in the bainitic regions.

Cu-rich bainite

Figure 7: D.DH-1 + 0.8% C (1% Nital/4% Picral)

Increasing sintering time from 10 to 30 minutes leads to higher strength due to better sintering necks and
copper diffusion. This results in higher TRS and tensile strength values. It was even noticed that even

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when the cooling rate decreased along with hardness as well as martensite content, the TRS and tensile
strength still increased for the D.DH-1 as long as the sintering time was increasing.

Ast CrM Mix: The Astaloy CrM material benefited from both the cooling rate and the sintering time.
Hardness as well as TRS were improved from the faster cooling rates and the sintering time yielded better
TRS and tensile strength. In this case, cooling rate increases the hardenability and strength of this
material. Increased sintering time allows for better sintering.

Table 2 below, shows the percent martensite with respect to sintering time and cooling rate for each
material. As mentioned previously, the Astaloy A material had very large amounts of martensite. All
materials benefited from the increase in sintering time at each cooling rate, cooling rate one (CR1) being
the fastest. D.DH-1 was the only material to have less martensite present with the increase in sintering
time for the two fastest cooling rates. The differences in amounts of martensite are minimal though.
Some differences in the part location in the sintering furnace could contribute to this. The Astaloy CrM
material shows the most contrast in martensitic content, but only 0.4% C was used in this grade.

TABLE 2: Percent Martensite

Matl. Ast A Ast A D.DH-1 D.DH-1 Ast CrM Ast CrM
Time 10 30 10 30 10 30
CR1 98 99 90 85 70 85
CR2 98 99 90 85 40 60
CR3 95 97 55 65 40 40
CR4 95 99 55 65 25 40

Below are some of the microstuctures seen representing the sintering process variable effects on the
materials and their properties.

Figures 8 and 9 represent the Astaloy mix tested at the CR3 and CR2 with 10 minutes sintering time,
respectively. 95% martensite/5% bainite (95M/5B) is present in Figure8, 98M/2B for Figure 9.

Figure 8: Ast A + 2% Cu +0.8% C (1% Nital/4% Picral)

95M/5B

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 Figure 9: Ast A + 2% Cu + 0.8% C (1% Nital/4% Picral)
99M/1B

Figures 10 and 11 show CR2 and CR4 for the D.DH-1 mix at 10 minutes and 30 minutes sintering,
respectively. These represent the decrease in hardness and martensite content, but increase in strength.

Figure 10: D.DH-1 + 0.8% C (1% Nital/4% Picral)

90M/10B

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 Figure 11: D.DH-1 + 0.8% C (1% Nital/4% Picral)
65M/35B

Figures 12 and 13 show the microstructures of the Ast CrM mix. CR1 and CR2 are shown respectively.
The only difference between the cooling rates here is the hydrogen content. Increasing the hydrogen for
5% to 20% changed the amount of martensite from 60% to 85% with the balance being bainite.

Figure 12: Ast CrM + 0.4% C (1% Nital/4% Picral)

85M/15B

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 Figure 13: Ast CrM +0.4% C (1% Nital/4% Picral)
60M/40B

CONCLUSIONS:

The above investigation revealed some findings. Hardness is primarily dependant on cooling rate.
Sintering time had its biggest effect on strength. Hydrogen improved the cooling rate after sintering.
Most importantly, the effect of process variables is entirely material dependant. The results of this
investigation support this.

The properties and structure of materials is also material dependant. Application details should be
addressed before choosing a sinter hardenable grade material. What properties are most desirable for the
application? So much emphasis is on hardness when sinter hardening is discussed. Not every application
requires the highest hardness. Once application details are discussed, then the correct sinter hardening
material and process parameters can be utilized.

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REFERENCES:

1. G. Box, W. Hunter and S. Hunter, Statistics for Experimenters, John Wiley & Sons, Inc., New York,
NY, 1978.

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