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Journal of Materials Processing Technology 129 (2002) 354±358

Effect of die wall lubrication on warm compaction


powder metallurgy
Y.Y. Li*, T.L. Ngai, D.T. Zhang, Y. Long, W. Xia
Mechatronic Engineering Department, South China University of Technology, 510640 Guangzhou, PR China

Abstract

Die wall lubrication was applied on warm compaction powder metallurgy in the hope to reduce the concentration level of the admixed
lubricant, since lubricant is harmful to the mechanical properties of the sintered material. Iron-based samples were prepared by die wall
lubricated warm compaction at 135 and 175 8C, using polytetra¯uoroethylene (PTFE) emulsion as the die wall lubricant. Compacting
pressures of 700 and 550 MPa were used. An admixed lubricant concentration ranging from 0 to 0.6 wt.% was used in this study. The results
show that in addition to a decrease in ejection forces, the green density of the compacts increased linearly with the decrease in the admixed
lubricant content. The mechanical properties of the sintered compacts increase sharply when the admixed lubricant concentration was reduced
to 0.125 wt.% or less. No scoring was observed in all of the experiments.
# 2002 Elsevier Science B.V. All rights reserved.

Keywords: Warm compaction; Die wall lubrication; Powder metallurgy

1. Introduction overcome friction and avoid scoring. On the other hand, the
presence of lubricant may reduce the sintered density and
It is well known that increasing the density is the best way decrease the mechanical properties of the compact. Practi-
to increase the performance of powder metallurgy (P/M) cally no lubricant can burn off completely during sintering,
parts. Conventional P/M processing can produce iron-based leaving ashes inside the compact, thereby, hinder the diffu-
parts with a density of less than 7.1 g/cm3 (a relative density sion process during sintering. At the same time, gas pressure
of approximately 90%). Their mechanical properties are generated by the dissociation or evaporation of the lubricant
substantially less than those of their full density counterpart. during the pre-sintering or sintering stage may create more
Warm compaction is a low cost and simple process that can voids in the compact and reduce the compact's dimension
obtain high relative density P/M parts [1±3]. With minor stability. The vaporized lubricant is harmful to the quality of
modi®cation of the conventional equipment and an approxi- the sintered compacts and to the furnace. The admixed
mately 20% increase over the cost of conventional cold lubricant also reduces the ¯ow rate of powder and prolongs
compaction, a green compact density of 7.5 g/cm3 can be the compaction cycle time. Therefore, elimination of
obtained by single pressing. The only difference between admixed lubricant in metal powder blends has long been
warm compaction and conventional compaction is that the a dream for the P/M industry.
powder has to be treated with a special lubricant, after which Admixed lubricant is important when compacting metal
the powder is raised to the pre®xed temperature and pressed powders in a die, since it reduce inter-particle friction,
in the die, whilst maintaining the warm compaction tem- particle±die wall friction and ejection force. As pointed
perature. out by many workers [4,5], the most important role for
Industrialization of the technique matured in the mid- lubricant is to overcome die wall friction rather than inter-
1990s. The success of the warm compaction technique relied particle friction. Several researchers [6±10] have investi-
on the correct use of a special lubricant; however, it is well gated die wall lubrication as an alternative to admixed
known that there is a dilemma in using lubricant. Lubricants lubricant in metal powders and some effort has been made
are essential for the die compaction of metal powders to towards systems that can provide die wall lubrication. Ball
et al. [10] applied dry powder lubricant on the die wall using
*
Corresponding author. Tel./fax: ‡86-20-8711-2948. a tribostatic spray gun and this system was successfully
E-mail address: mehjli@scut.edu.cn (Y.Y. Li). marketed in 1996 [11]. The aim of the present work was to

0924-0136/02/$ ± see front matter # 2002 Elsevier Science B.V. All rights reserved.
PII: S 0 9 2 4 - 0 1 3 6 ( 0 2 ) 0 0 6 4 8 - 9
Y.Y. Li et al. / Journal of Materials Processing Technology 129 (2002) 354±358 355

Table 1 The results reported in this study are the average of at least
Composition of the mixed powders in wt.% three samples.
Sample Cu Ni Mo Si Mn Graphite Fe Lubricant

A 2.0 2.0 1.0 ± ± 1.0 Balance 0.0±0.6


B ± 2.0 0.4 0.45 0.6 0.4 Balance 0.5 3. Results
C 2.0 2.0 1.0 ± ± 1.0 Balance 0.6
Fig. 1 shows the relationship between the density of
sample A and the admixed lubricant concentration for both
die wall lubricated and non-die wall lubricated warm com-
study the effect of die wall lubrication on warm compaction paction using a compaction pressure of 700 MPa and a
P/M in hope of reducing the concentration level of admixed compaction temperature of 135 and 175 8C. In the admixed
lubricant. lubricant concentration range of 0±0.6 wt.%, both the green
and sintered densities increase linearly with decrease in
lubricant concentration for samples compacted at 135 and
2. Experimental work 175 8C with die wall lubrication. Compared with non-die
wall lubricated samples, the die wall lubricated samples
The chemical compositions of samples A±C is listed in have higher densities. The decrease in sintered density
Table 1. The powders were prepared by mixing Atomet 1001 compared to the green densities is almost constant and
atomized iron powder, which was produced by Quebec independent of the lubricant concentration.
Metal Powders, Canada, with other alloying elemental Figs. 2 and 3 show the tensile strength and elongation,
powders and a special lubricant. The particle size of the respectively, as function of the admixed lubricant concen-
iron powder was 147 mm. Carbonyl nickel with a size of tration for sintered and heat-treated sample A. Samples were
5 mm was used. The particle size of the other elemental prepared by die wall lubricated warm compaction using a
powders were 74 mm. The mixing time was 90 min. The compaction pressure of 700 MPa and a compaction tem-
admixed lubricant concentration used in this study ranged perature of 135 8C. Both the tensile strength and elongation
from 0 to 0.6 wt.%. of as-sintered and heat-treated samples show a steady
The pre-heated mix powders were pressed into standard increase as the admixed lubricant concentration is
tensile specimens (ISO 2740-1973) in a steel mold, which decreased, with a sharp increase when the lubricant con-
was heated to a temperature of 135 and 175  2 8C. Poly- centration reached 0.125 wt.%.
tetra¯uoroethylene (PTFE) emulsion was brushed on to the Table 2 lists experimental results for sample B, which was
die wall as the die wall lubricant. Compacting pressures of warm compacted at 175 8C using a pressure of 550 MPa.
700 and 550 MPa were used. Samples A and B were These results are consistent with those obtained for sample
degassed at 600 8C for 1.5 h in the pre-heating chamber A. Both the green density and mechanical properties
of a pusher type furnace protected by a reducing hydrogen± obtained by warm compaction with die wall lubrication
nitrogen atmosphere produced by an ammonia dissociator. have a higher values when compared with those obtained
Sintering was carried out at temperatures of 1200 and by warm compaction without die wall lubrication, except
1250 8C for 1.5 h in the sintering chamber, followed by for samples sintered at 1250 8C. For sample sintered at
holding at 850 8C in the cooling chamber for 1 h and 1250 8C, the densities and mechanical properties obtained
subsequent cooling to room temperature. A sintering tem- by die wall lubricated warm compaction are slightly lower
perature (TS) of 1200 8C was used for sample A, whilst for
sample B sintering temperatures of 1200 and 1250 8C were
used. The heat-treatment schedule for sample A was anneal-
ing at 823 8C for 30 min in N2, quenching in oil, then
annealing at 600 8C for 2 h followed by quenching in water.
The green density (rG), sintered density (rS), tensile
strength (rb) and elongation percentage (d) were measured.
Densities were measured by the water displacement method.
A computer controlled universal tensile testing machine was
used to measure the ultimate tensile strength and elongation.
Sample C was for ejection force measurement. It was
cylindrical in shape, of 20 mm in diameter and 20 mm
length. Samples were warm compacted at 175 8C using
pressures of 550 and 700 MPa. For comparison purposes,
samples compacted with and without die wall lubrication
were prepared. Ejection forces were read from a gauge Fig. 1. Relationship between density and lubricant concentration for
equipped provided on the hydraulic press. sample A warm compacted at 700 MPa.
356 Y.Y. Li et al. / Journal of Materials Processing Technology 129 (2002) 354±358

scoring was observed in all experiments, even for samples


containing no admixed lubricant.

4. Discussion

Friction between the compact and the die wall increases


the ejection force. If the admixed lubricant is too low in
content, it is not suf®cient to reduce the ejection force to an
acceptable level. If there is too much lubricant, the density
and mechanical properties of the sintered compact will be
reduced. Samples with two different compositions were
Fig. 2. Relationship between tensile strength and lubricant concentration prepared to examine the effect of die wall lubrication on
for sample A compacted at 135 8C and 700 MPa with die wall lubrication. warm compaction in the hope to reduce the lubricant content
in the powder. Sample A contains 1 wt.% of graphite and
sample B contains 0.4 wt.% of graphite. As is known,
Table 2 graphite is an effective solid lubricant; its concentration
Results on sample B warm compacted at 175 8C and 550 MPa in the powder compact will affect the frictional condition
Die wall TS (8C) rG rS sb d (%) during the compaction. Results obtained from samples A
lubrication (g/cm3) (g/cm3) (MPa) and B are shown in Figs. 1±3 and Table 2, showing that die
No ± 7.255 ± ± ± wall lubricated warm compaction can produce compacts
Yes ± 7.265 ± ± ± with higher density and better mechanical properties at all
No 1200 ± 7.299 464 4.2 compaction temperatures and admixed lubricant concentra-
Yes 1200 ± 7.303 495 4.6 tions used in this study. This result is expected, since PTFE
No 1250 ± 7.348 598 4.3
has a very low friction coef®cient and, as mentioned earlier,
Yes 1250 ± 7.340 575 4.4
the major friction problem is between the powder and the die
wall, PTFE on the die wall reduce a great portion of the
friction during compaction and thus increase the effective
or approximately the same when compared with those pressure on the powder. As shown in Fig. 1, the density of
obtained by warm compaction without die wall lubrication. warm compacted samples with die wall lubrication increases
The ejection force data in this study was read from the linearly with the decrease in admixed lubricant concentra-
gauge provided in the hydraulic press, but this gauge was not tion, no matter whether it was compacted at 135 or 175 8C.
suf®ciently accurate for quantitative analysis. All the data The presence of admixed lubricant occupied spaces in the
indicated that samples with die wall lubrication show lower compact at the expense of the relatively heavier metal
ejection forces. At a compaction pressure of 700 MPa the powders and unavoidably reduces the green density of the
ejection force for the die wall lubricated sample was compact. Inter-particle friction can be reduced by admixed
approximately 60% of that of the non-die wall lubricated lubricant and therefore is bene®cial to the densi®cation of
sample. At a compaction pressure of 550 MPa the ejection the powder compacts and provides compacts of better
force for the die wall lubricated sample was approximately quality. For sample contains no admixed lubricant, the
65% of that for the non-die wall lubricated sample. No inter-particle friction should reduce the green density to
some extent. The linearity in Fig. 1 did not show this
decrease in density at low internal lubricant concentration
level. The linearity indicated that the lubricant volume factor
is one of the dominant contributions to the increase in
density. The consistent decrease in densities after sintering
is independent of the admixed lubricant concentration. This
is a re¯ection of the lubricant easily ®nding its way to escape
from out of the compact through inter-connected voids. If
the lubricant is in excess, or of green density is high enough
that the compact contains a considerable amount of closed
pores, or if the heating rate is too fast, swelling of the
compact may occur as the vaporized lubricant tries to escape
from the part. The 0.6 wt.% of admixed lubricant used in this
study did not cause the swelling of the compact that due to
Fig. 3. Relationship between elongation and lubricant concentration for the rapid build up of gas pressure that is generated by the
sample A compacted at 135 8C and 700 MPa with die wall lubrication. vaporized lubricant. From Figs. 2 and 3, it can be seen that
Y.Y. Li et al. / Journal of Materials Processing Technology 129 (2002) 354±358 357

mechanical properties increase sharply when the admixed effective. There is no certainly PTFE adhering to the die wall.
lubricant concentration is reduced to 0.125 wt.% or less. The In the present case, PTFE emulsion was used, a ®lm of PTFE
better mechanical properties of warm compacted samples remaining to be seen on the die wall.
with die wall lubrication when compared with those without The present results indicated that under the experimental
die wall lubrication is mainly due to the increase in density condition used in this study, no matter at which compaction
and, for sample containing no admixed lubricant, to the pressure, compaction temperature, graphite and lubricant
clean inter-granular boundaries, whilst the better inter-diffu- contents in the powder, the die wall lubricated warm com-
sion during the sintering is also a factor contributing to high paction gives the highest green density and lowest ejection
mechanical properties. This became obvious from the elon- force. This study shows that the combination of die wall
gation data, since it is very sensitive to porosity. lubrication with warm compaction can effectively reduce the
Bene®ts, such as increase in green density and increase in admixed lubricant concentration to obtain compacts with
tensile strength, achieved by die wall lubricated warm better quality, without scoring, during compaction.
compaction, could be overwhelmed by the high temperature
sintering since high temperature sintering is an effective way
for high-density P/M material fabrication. As shown in 5. Conclusions
Table 2 the mechanical properties of sample B sintered at
1250 8C obtained by warm compaction with die wall lubri- In the lubricant concentration range from 0 to 0.6 wt.%
cation are slightly lower or approximately the same when both green and sintered densities increase linearly with
compared with those obtained by warm compaction without decrease in admixed lubricant concentration for samples
die wall lubrication. Although high temperature sintering is compacted at 135 and 175 8C with die wall lubrication.
a simple way for high-density parts fabrication, it is not Compared with non-die wall lubricated samples, the die wall
generally used because the dimensional stability of the parts lubricated samples have higher green densities. Both the
deteriorates rapidly as the sintering temperature increases. tensile strength and elongation of as-sintered and heat-
Further, the equipment cost and processing cost for high treated samples show a steady increase as the admixed
temperature sintering are much greater. Nevertheless, the lubricant concentration is decreased and there is a sharp
higher green density usually gives higher green strength, increase when the lubricant concentration reaches at
therefore higher green density is always preferred. 0.125 wt.%. The bene®ts, such as increase in density and
Degoix et al. [12] investigated the effect of lubrication increase in tensile strength, achieved by die wall lubricated
mode and compaction temperature on the properties of Fe± warm compaction could be neutralized by high temperature
2Ni±2Cu±0.85Mo±0.8C. Their result did not agree well with sintering, since high temperature sintering is an effective
the present result. They used 0.25 wt.% PTFE as lubricant in way for high-density P/M material fabrication.
three different ways: (1) dry admixed to the powder; (2) die Ejection force data indicated that samples with die wall
wall lubricated by PTFE±alcohol suspension without lubrication show lower ejection forces when compared with
admixed lubricant; (3) wet mixed using PTFE±alcohol sus- samples without die wall lubrication. No scoring was
pension. Samples were prepared by compacting the powders observed in all experiments, even for samples containing
with a pressure of 690 MPa at room temperature and at no admixed lubricant. The present results indicated that
150 8C. The green compacts were sintered at 1300 8C for under the experimental condition used in this study, no
50 min. It was found that the wet mixed lubricant gave the matter at which compaction pressure, compaction tempera-
worse results in density and strength, and the dry admixed ture, graphite and lubricant contents in the powder, die wall
lubricant gave the highest sintered density and strength, and lubricated warm compaction gives the highest green density
the lowest ejection forces, under their experimental condi- and lowest ejection force. It can be concluded that a com-
tions. Die wall lubricated warm compaction at 150 8C gave bination of die wall lubrication and warm compaction can
the highest green density but their sintering temperature was provide P/M products of higher density and better quality. It
1300 8C, which was high enough for a high value of densi- is a feasible way to produce high performance P/M parts to
®cation which overwhelmed the high green density obtained use a suitable die wall lubrication system.
by die wall lubricated warm compaction. The greatest contra-
diction between the present results and their results are in
respect of the ejection forces. They found that die wall Acknowledgements
lubricated warm compaction needed a greater ejection force,
their results showing that die wall lubricated warm compac- This work was supported by the National Natural Science
tion needed an ejection force of 40.1 kN instead of 34.8 kN Foundation of China (Key Project No. 50135020), the
for admixed lubrication, whereas the present data indicate that National Advanced Technology Research and Development
the ejection force for the die wall lubricated sample was Project (863 Project No. 2001AA337010), the Ministry of
approximately 60% of that for the non-die wall lubricated Education (Excellent Personnel for 21st Century Training
sample. The reason for this is that the way that they apply the Project (2000) No. 1) and the Natural Science Foundation of
die wall lubricant by using PTFE±alcohol suspension is not Guangdong Province (Research Group Project No. 003019).
358 Y.Y. Li et al. / Journal of Materials Processing Technology 129 (2002) 354±358

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