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Wear 258 (2005) 166–177

Abrasive wear of steam-treated sintered iron


W.M. da Silvaa , R. Binderb , J.D.B. de Melloa,∗
a Laboratório de Tribologia e Materiais, Faculdade de Engenharia Mecânica, Universidade Federal de Uberlândia, 38400-902 Uberlândia, MG, Brazil
b Empresa Brasileira de Compressores, 89219-100, Joinville, SC, Brazil

Received 22 December 2003


Available online 21 November 2004

Abstract

Steam oxidized sintered iron-based materials have been, and continue to be used for load bearing parts in sliding contacts. Although the
permanence of an oxide layer on the external surface is reported to be the main factor affecting tribological behaviour, in industrial practice
as well as in laboratory tests abrasive wear is reported to play an important role in the final stage of the process. The removal of the superficial
oxide layer, its fragmentation and transfer to the counter-body associated with metallic debris generation, induces the formation of hard
debris particles acting as abrasives on the tribological system. In this paper, abrasive wear of steam-treated sintered iron is analysed by
means of micro-abrasion tests. Sixteen specimens were produced from atomised iron powders (Ancor Steel 1000B Höganäs) of different
sizes (<65, 65–90, 90–125, >125 ␮m). They were compacted at four different pressures (300, 400, 500 and 600 MPa), sintered for 30 min at
1120 ◦ C and then subjected to continuous steam treatments at 540 ◦ C for 2 h. The micro-abrasion tests were conducted under constant load
and speed conditions while special emphasis was given to the nature of the abrasive; two exogenous (Al2 O3 and SiO2 ) and one endogenous
abrasive (Fe2 O3 ) were used. The results show that the abrasion resistance is strongly influenced by the processing parameters, the lowest wear
coefficients were obtained by using the highest compaction pressures and the smallest powder grade. The pore size is the main micro-structural
parameter affecting the abrasive resistance. For all abrasives, interrupted tests showed that the small pores are completely filled by abrasive
particles in the initial stage of the tests while the biggest ones remains open until the completion of the tests. Wear coefficients were strongly
influenced (up to 10 times) by the abrasive nature. Scanning electron microscopy analysis showed that the abrasive wear mechanisms were
determined by the abrasive particle features.
© 2004 Elsevier B.V. All rights reserved.

Keywords: Micro-abrasion; Sintered iron; Steam treatment

1. Introduction in the interconnected porosity is reported to provide an in-


crease in hardness; in mechanical properties as a whole, and
Steam oxidation is a frequently used surface treatment ap- in wear resistance in particular, a decrease in the friction co-
plied to sintered iron-based parts, mainly for low or medium efficient and an increase in corrosion resistance in moderately
density components (5.4–7.0 g/cm3 ) [1,2]. Initially this pro- aggressive environments [2,5]. Furthermore, steam oxidation
cess was used as an economic way to seal the network of inter- produces a blue/black layer, which enhances the aesthetic ap-
connected pores characteristic of sintered iron, thus making pearance of components. The main disadvantages of the pro-
the component impervious to liquid and gases. This treatment cess are the reduction in tensile strength, impact resistance
is claimed to improve the superficial properties of sintered and ductility.
materials [2–7]. Besides the closing of the interconnected Examples of components that are steam-treated are gears,
porosity, steam treatment is claimed to improve other prop- cams, chain pinions, compressor parts, bearings, pulleys, and
erties of sintered iron. The oxide formed on the surface and sprockets [4].
Molinari and Straffelini [1,8] studied the effect of slid-
∗ Corresponding author. Fax: +55 34 3239 4186. ing speed on the dry sliding behaviour of sintered and steam
E-mail address: ltm-demello@ufu.br (J.D.B. de Mello). oxidized iron, Fe–Cu (2%) and Fe–C (0.3%) alloys. They

0043-1648/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.wear.2004.09.042
W.M. da Silva et al. / Wear 258 (2005) 166–177 167

showed that the wear rate is low and independent of the chem- given to the nature of the abrasive; two exogenous (Al2 O3
ical composition of the specimens as long as the oxide layer and SiO2 ) and one endogenous abrasive (Fe2 O3 ) were used.
produced by the steam oxidation is able to carry out its lubri-
cating function between the sliding surfaces. After removal of
the oxide layer by adhesion, two different wear mechanisms 2. Experimental procedure
are active according to the sliding speed: a delamination wear
mechanism at low sliding speed and a delamination-oxidation Specimens were produced from Ancor Steel 1000B
mechanism at high sliding speed. In the latter case, the wear Höganäs atomised iron powder. The powder was sieved into
rate is lower, the influence of the mechanical properties of four different fractions (<65, 65–90, 90–125 and >125 ␮m)
the matrix is reduced, and the behaviour of pure iron tends to to provide four different powder grades (denoted 1–4, re-
be comparable with that of the alloyed materials. spectively). After mixing with 0.8 wt.% zinc stearate as a lu-
de Mello and Hutchings [9] studied the behaviour of sin- bricant, the powders were compacted at four different com-
tered and oxidized iron samples worn in reciprocating sliding paction pressures (300, 400, 500, 600 MPa) with a double
tests. They showed that during the wear tests fragmentation action automatic press in such a way that the surfaces to be
of the oxide layer occurs. Besides, greatly deformed metallic tested were in contact with the moving punch.
particles are produced from both the sample and the counter- The samples were designated as Axy where x is the com-
body. These particles become adherent to the worn surface, paction pressure (in MPa) divided by 100 and y the pow-
generating a compacted layer of iron and iron oxide. The der grade. For example: A34 denotes a sample pressed at
gradual and localized degradation of this layer is the main 300 MPa, with particle size >125 ␮m. The resulting com-
factor controlling the wear process. In the final stage of the pacts, 50 mm in length by 10 mm in width with height de-
oxide layer removing process, loose and hard oxide debris pending on compaction pressure and powder grade, were sin-
caused abrasive wear as well as localized fragmentation of tered in an industrial furnace. The sintering was conducted
the compacted layer. These authors [9,10] showed that the in a mildly reducing atmosphere (N2 + 10% H2 ) at a con-
abrasive wear mechanism is the main degradation agent in stant temperature of 1120 ◦ C for 25–30 min. After cooling to
the final stage of the process. room temperature the samples were steam-treated. The steam
Other authors [11–15] highlight the effect of the particles treatment was carried out at 540 ◦ C for 2 h in a continuous
presence on the global wear behaviour of oxidized sintered industrial furnace.
materials. However only two works, Amsallem et al. [16] and The micro-structure of the samples used in this work
Razavizadeh and Davies [17], consider a direct approach to was comprehensively characterized in a previous paper by
abrasive wear behaviour. de Mello et al. [6]. These authors studied both superficial
In this paper, the effect of processing parameters (com- and volumetric aspects of the micro-structure. The micro-
paction pressure and powder size) on abrasive wear of steam- structure is greatly dependent on the processing parameters
treated sintered iron is analysed by means of micro-abrasion (compaction pressure and powder grade). Thickness of oxide
tests. The micro-abrasion tests were conducted under con- layer is nearly constant (3.5–4 ␮m) and independent of the
stant load and speed conditions while special emphasis was processing conditions used. X-ray diffraction showed that the

Table 1
Micro-structural characteristics [6]
Sample CPa (MPa) PGb Porosity (%) Pore size (␮m) MFPc (␮m) Oxide content (%) HV (kgf mm−2 )
A31 300 1 42.7 ± 3.3 14.8 ± 2.8 19 ± 8 29 ± 2 152 ± 4
A32 300 2 39.8 ± 3.8 15.1 ± 4.3 22 ± 8 27 ± 2 105 ± 4
A33 300 3 37.4 ± 1.2 15.5 ± 4.9 25 ± 9 20 ± 1 87 ± 2
A34 300 4 33.1 ± 3.4 15.8 ± 5.2 32 ± 0 19 ± 1 76 ± 2
A41 400 1 36.8 ± 2.0 13.5 ± 2.6 23 ± 2 22 ± 2 141 ± 1
A42 400 2 32.4 ± 2.3 14.2 ± 3.8 29 ± 6 20 ± 1 131 ± 2
A43 400 3 29.9 ± 1.7 14.6 ± 4.1 34 ± 1 16 ± 1 103 ± 3
A44 400 4 26.6 ± 1.9 14.4 ± 4.2 39 ± 8 15 ± 2 93 ± 4
A51 500 1 29.5 ± 1.1 7.9 ± 2.2 25 ± 3 18 ± 1 124 ± 2
A52 500 2 26.6 ± 1.3 9.5 ± 2.9 32 ± 6 14 ± 2 115 ± 2
A53 500 3 22.8 ± 3.2 10.6 ± 3.5 35 ± 8 14 ± 1 105 ± 3
A54 500 4 21.7 ± 1.4 10.9 ± 3.7 39 ± 2 12 ± 1 92 ± 2
A61 600 1 25.5 ± 1.8 6.8 ± 1.8 19 ± 8 14 ± 2 116 ± 2
A62 600 2 24.1 ± 1.2 7.4 ± 2.1 27 ± 3 10 ± 1 105 ± 3
A63 600 3 20.6 ± 1.6 8.1 ± 2.7 31 ± 1 10 ± 1 102 ± 1
A64 600 4 18.9 ± 1.6 8.4 ± 3.1 36 ± 1 9±1 98 ± 1
a Compaction pressure.
b Powder grade.
c Mean free path between pores.
168 W.M. da Silva et al. / Wear 258 (2005) 166–177

oxide layer is composed of magnetite (Fe3 O4 ) and haematite


(Fe2 O3 ) [6]. Other micro-structural parameters are synthe-
sized in Table 1.
Abrasive wear tests were carried out in a ‘free ball’ micro-
abrasion tester [18,19]. In this method, a sphere of radius R is
rotated against a specimen in the presence of a slurry of fine
abrasive particles. The geometry of the wear scar is assumed
to reproduce the spherical geometry of the ball, and the wear
volume may then be calculated by using Eq. (1):

πb4
k= for b << R (1)
64RSN

where k is the ‘wear coefficient’ with units m3 (N m)−1 ; b the


surface chordal diameter of the crater, S the sliding distance
and N the normal load on the contact.
In this variant of the experimental apparatus, the ball is
driven by friction from a drive shaft against which it rests,
and in which the load applied to the sample is essentially
due to the weight of the ball. Hard martensitic steel bearing
balls (20 mm in diameter) were used as a counter-body in all
tests. They were ultrasonically cleaned before each test and
induced a normal load of 0.22 ± 0.01 N, monitored by a load
cell.
The drive shaft rotation was kept constant at 150 rpm,
which represent a relative velocity between ball and sample
surfaces about 0.11 m s−1 .
In order to determine the permanent wear regime, sequen-
tial tests at a range of test times (10, 20, 30, 40, 50, 60, 80, 100,
120, 180, 240, 300 and 360 s) were carried out on the speci-
men at the same location. Three sets of test were performed
for each abrasive-sample pair.
Abrasive slurries of alumina (Al2 O3 ), silica (SiO2 ) and
haematite (Fe3 O4 ) particles suspended in distilled water were
used, at a concentration of 75 g of abrasive per cubic centime-
tre of water. The slurries were agitated continuously through-
out each test to prevent the settling of the abrasive particles.
A peristaltic pump fed slurry on to the top of the ball at a rate
of approximately 3 drops per minute.
The granulometric distribution of the abrasive particles
was determined by laser granulometry while their morphol-
ogy was shown by scanning electron microscopy.
The worn samples were examined by optical microscopy,
scanning electron microscopy and laser interferometry. Fig. 1. Particle size distribution of the abrasive particles as determined by
laser interferometry. (a) Haematite (Fe2 O3 ); (b) silica (SiO2 ); (c) alumina
(Al2 O3 ).

3. Results and discussion tends to be spherical while the alumina particles are more
elongated and sharper.
The mean size of abrasives and their particle size distri- Fig. 2 presents a typical aspect of the craters produced by
butions as well as their morphology are shown in Fig. 1. The the tests. It is clear that the test conditions impose a spherical
haematite presents an asymmetric normal distribution and the wear scar geometry, validating the use of Eq. (1) to determine
smallest mean particle size. The mean particle size increases the wear coefficient by optically measuring the diameter of
for silica and alumina, which presents the biggest particle the imposed spherical crater.
size. The same statistical distribution is presented by the sil- The evolution of the wear coefficient with test time is il-
ica particles while the alumina particles present a bi-modal lustrated in Fig. 3. This figure shows the results presented
distribution. The shape of the silica and haematite particles by samples produced in the most extremes conditions of the
W.M. da Silva et al. / Wear 258 (2005) 166–177 169

Fig. 2. Typical aspect of the craters obtained by laser interferometry. Sample A61, alumina, 360 s. (a) 3D surface; (b) trace AA. The trace of the theoretical
profile of a perfectly smooth sphere, 10 mm in diameter, is shown for comparison.

processing parameters when abraded by silica. They are typ- in thickness) had already been penetrated when the steady
ical of all the tested conditions. Wear coefficients were ob- state wear regime was established, suggesting that the micro-
tained in three sets (Kt1, Kt2 and Kt3), of 13 tests each. The abrasive wear process is governed by the substrate behaviour
mean value (M) was calculated and is also shown in the fig- in close correlation with the tribological conditions act-
ure. The averaged crater depth (d) for each test time is also ing at the final stages of the wear process of this fam-
included. ily of materials as reported by de Mello and Hutchings
The wear coefficient increases in a random manner with [9].
the test time up to 80 s. After that time the dispersion de- Fig. 4 presents the effect of processing parameters on the
creases and the evolution of the wear coefficient becomes wear coefficient. For all abrasives, the smallest abrasive wear
roughly constant. For the low compaction pressure, samples coefficients were obtained by the combination of a high com-
A31 and A34, Fig. 3a and b, the initial transient is more accen- paction pressure with a fine powder grade. In general, for the
tuated and the wear coefficient is stable for test times above same powder grade, an increase in compaction pressure led to
180 s. For the high compaction pressure, samples A61 and a decrease in the wear coefficient. On the other hand, for the
A64, Fig. 3c and d, the stabilization of the wear coefficient is same compaction pressure an increase in powder size gave
reached after 100 s of test time. The permanent wear regime, rise to a slight decrease in the wear coefficient.
i.e. the stability of the wear coefficient was reached for all The effect of porosity on abrasive wear resistance is quite
tested conditions (sample/abrasive pair) after 180 s [20]. In complex as illustrated by Fig. 5. In general, for a fixed powder
this paper, all the analyses were done in the permanent wear grade, increasing porosity always caused an increase in the
regime. This regime is represented by an averaged wear co- wear coefficient. On the other hand, at constant compaction
efficient (K), obtained by the averaging of the results relative pressure, an increase of porosity produced a decrease in the
to the test times 180, 240, 300 and 360 s, e.g. this coefficient wear coefficient.
is representative of an average of 12 tests carried out in each Other micro-structural parameters like the mean free path
sample/abrasive condition [20]. between pores and the amount of oxide formed on the in-
The crater depth increases logarithmically with test time terconnected porosity showed a complex relationship with
until the permanent wear regime is reached. In this regime, abrasive wear resistance [20,21].
the evolution of the crater depth with time is linear. For all tri- It is also noticeable in Fig. 4 that the nature of the abra-
bological conditions, the superficial oxide layer (3.5–4.0 ␮m sive has a strong influence on the abrasive wear behaviour
170 W.M. da Silva et al. / Wear 258 (2005) 166–177

Fig. 3. Evolution of the wear coefficient and crater depth with test time.
Silica. (a) A31; (b) A34; (c) A61; (d) A64.
Fig. 4. Effect of processing parameters on wear coefficient. (a) Haematite;
(b) silica; (c) alumina.
of steam-treated sintered iron. The highest wear coefficients
were produced by alumina while abrasion by haematite pro-
duced the lowest wear coefficient. The general behaviour A34. For sample A61, wear coefficient decreases from alu-
can be more easily understood by analysing the influence mina to silica and then shows a slight decrease from silica to
of the nature of abrasive on the wear coefficient of the sam- haematite. On the other hand, sample A64 presents an approx-
ples produced when using the extreme processing parame- imately constant wear coefficient for silica and haematite.
ters, e.g. A31, A34, A61 and A64, Fig. 6. It can be seen in This fact suggests that the samples produced with small com-
Fig. 6 that the wear coefficient for sample A31 decreases in paction pressure (300 MPa) are more sensitive to the type
the following sequence: alumina, silica and haematite. Sim- of abrasive than the samples produced with higher com-
ilar behaviour is observed for the wear coefficient of sample paction pressure (600 MPa). In all the studied cases, an in-
W.M. da Silva et al. / Wear 258 (2005) 166–177 171

Fig. 5. Effect of porosity on wear coefficient. (a) Haematite; (b) silica; (c)
alumina.

crease in powder grade resulted in a small increase in the wear


coefficient.
As previously mentioned, the wear coefficient increases
as follow: haematite, silica and alumina. For the studied
tribo-systems, abrasive hardness and sample hardness ra-
tio (characterized as a volumetric property of the samples)
are very high, indicating that the abrasive process is the re-
sult of severe wear regime [22–24]. The relative hardness
(Habrasive /Hsample ) of the studied conditions decreases from

Fig. 7. Wear mechanisms. SEM. Centre of the crater. (a) Sample A64
abraded by alumina; (b) sample A61 abraded by silica; (c) sample A64
abraded by haematite.

Fig. 6. Wear coefficient as a function of the abrasive type.


172 W.M. da Silva et al. / Wear 258 (2005) 166–177

alumina (11.5–27) to silica (4.8–17) and then to haematite abrasive size the greater the wear of the samples. Besides,
(6.4–14). This decrease in severity correlates very well with the individual load per abrasive particle is one of the most
the wear coefficients presented by the studied samples e.g. important parameter controlling the wear mechanism acting
the higher the relative hardness (and as a consequence the on the micro-abrasion process [25].
severity of the abrasive process) the higher the wear co- Fig. 7 shows typical aspects of the abraded surfaces and il-
efficient. In addition, Fig. 2 shows that alumina particles lustrates the wear mechanism acting according to the nature
present a sharp, angular, elongated geometry while the sil- of the abrasive. When using alumina, the dominant mech-
ica and haematite grits are blunted and spheroidal in shape. anism was like that of a three-body process, in which the
It has been reported that particles with an angular shape abrasive particles roll between the two surfaces producing
cause higher wear than spherical particles [22] thus induc- a heavily deformed, multiply indented wear surface with no
ing an even more severe wear regime when using alumina evident directionality, Fig. 7a. On the other hand, a grooving
grits. wear mechanism similar to a two-body mechanism was found
The severity of the wear system is also related to the abra- to be dominant for silica and haematite. This process occurs
sive size: an increase in abrasive mean size decreases the in the micro-scale abrasion test when a significant proportion
number of particles present at the interface, thus promoting a of the particles slide without rolling at the specimen/ball in-
substantial increase on the force per abrasive particle. Fig. 2 terface, thus producing a series of fine parallel grooves in the
shows that alumina grits have the largest mean diameter, fol- specimen surface, Fig. 7b and c. Trezona et al. [25] suggested
lowed by silica and haematite, respectively. The greater the that the abrasive particles are embedded in the surface of the
ball bearing and act as fixed indenters.
In addition, the analysis of the wear mechanisms showed
that those produced by silica grits remarkably reproduced the

Fig. 8. Wear mechanisms. (a) Surface of sample A61 abraded by silica,


0.22 N, 0.11 m s−1 , 360 s. (b) Worn surface of a real component after 2000 Fig. 9. Influence of the hardness on wear coefficient. (a) Haematite; (b)
work hours. silica; (c) alumina.
W.M. da Silva et al. / Wear 258 (2005) 166–177 173

Fig. 10. Typical aspects of abraded surfaces. Test time 360 s. SEM. (a) A31 abraded by SiO2 ; (b) A34 abraded by SiO2 ; (c) A61 abraded by SiO2 ; (d) A64
abraded by SiO2 ; (e) A31 abraded by Fe2 O3 ; (f) A34 abraded by Fe2 O3 ; (g) A61 abraded by Fe2 O3 ; (h) A64 abraded by Fe2 O3 .

wear mechanisms acting on the real conditions experienced For the exogenous abrasives (Al2 O3 and SiO2 ), increas-
by steam-treated sintered iron components, Fig. 8. This sug- ing the hardness produces a decrease in the wear coefficient,
gests that the use of micro-abrasion tests using the same tri- which reaches a minimum, Fig. 9a and b. It can be noticed
bological conditions may constitute a powerful tool for the that the samples associated with hardness values lower than
optimisation of these components. the value corresponding to the minimum in the wear coef-
The correlation between hardness and abrasive wear is ficient were produced by using the larger powder grades (3
quite complex too, Fig. 9. and 4), while those associated with values above the min-
174 W.M. da Silva et al. / Wear 258 (2005) 166–177

imum were produced by using the smaller powder grades


(1 and 2).
For the endogenous abrasive (haematite), it is observed,
Fig. 9c, that the wear coefficient decreases with an increase
in hardness up to 106 kgf mm−2 . From this point, the wear
coefficient tends to be independent of the hardness and is as-
sociated with samples produced by using the smaller powder
grades (1 and 2). The relationship between hardness and pro-
cessing parameters is very complex as reported by de Mello
et al. [6]. These authors showed that decreasing powder size
always led to high hardness. Samples produced with smaller
powder size show a continuous decrease in hardness as the
compaction pressure increases, although for the large powder
size there is a slight increase to a constant value of ultimate
hardness. For the intermediate powder size a maximum hard-
ness is obtained as the compaction pressure increases. They
also reported that the resulting hardness of these samples is
the result of a compromise between the porosity and the oxide
content formed in the interconnected porosity.
Fig. 9 shows that the powder grade plays an important
role in the evolution of the wear coefficient with hardness
and suggests that a compromise between the hardness and
micro-structural features governs the micro-abrasive process.
Fig. 10 presents typical aspects of the abraded surfaces.
They correspond to the central part of the wear scar and to
samples produced in the most extreme conditions of process-
ing parameters e.g. samples A31, A34, A61 and A64 when
abraded by silica and haematite.
For all the studied conditions, the presence of open pores
on the abraded surface is clearly visible. For the specimens
produced by using the lowest compaction pressures, corre-
sponding to those presenting the biggest pore size, the quan-
tity of open pores is high; Fig. 10b, d, f and h. In addition,
they presented bigger open pores. The wear scar of the sam- Fig. 11. Effect of pore size on micro-abrasion wear coefficient. (a) Alumina;
ples abraded by alumina, although produced by a different (b) silica; (c) haematite.
wear mechanism (multiple indentation due to the rolling of
the abrasive particles on the interface) presented a similar cient is less sensitive to those parameters and is characterized
aspect concerning the open porosity existing in the abraded by its higher value.
surfaces. To study the mechanisms involved in the interactions of
The presence of open pores on the active surface is re- abrasive grits with pores, a subsidiary series of interrupted
ported to act as foci for the generation and trapping of wear tests was performed. These tests were interrupted at fixed
debris in sliding wear [9,14] suggesting that the open porosity, test times and the samples were slightly cleaned with a moist-
in particular the pore size, should play an important role on ened piece of cotton and then dried by an air stream. In the
the micro-abrasive behaviour of steam-treated sintered iron. sequence, the specimens were chemically attacked by a so-
The influence of the pore size on the wear coefficient is lution composed of 6.14 g of copper chloride (CuCl2 ), 3.86 g
presented in Fig. 11. of ammonium chloride (NH4 Cl) and 100 g of distilled water.
Abrasive wear coefficient was strongly affected by pore In these conditions, the solution is over saturated in aqueous
size. Fig. 11 shows that wear increases with pore size in all the CuCl2 (aq), which dissociates according to Eq. (2):
studied tribo-systems. This increase is more pronounced for CuCl2(aq) → Cu(aq) 2+ + 2Cl− (aq) (2)
pore size larger than 13 ␮m, corresponding to samples pro-
duced by using the smallest compaction pressures (300 and When this solution is applied, the iron present in the worn
400 MPa). It is also noticeable that the samples associated surface oxidizes according to Eq. (3) and the ion of copper
with the small powder, grade 4, presented a quite different may react with the free electrons according to Eq. (4) gen-
behaviour when abraded by haematite, Fig. 11c. Although a erating a solid copper layer, which is deposited on the worn
slight increase in wear coefficient is presented as pore size surface. This copper layer coats both the worn surface and
increases and compaction pressure decreases, the wear coeffi- the remaining abrasive grits allowing the analysis of their
W.M. da Silva et al. / Wear 258 (2005) 166–177 175

Fig. 12. Typical aspects of the interactions between abrasive particles and pores. SEM. (a) A34 abraded by Al2 O3 , test time 10 s. (b) A34 abraded by Al2 O3 ,
test time 240 s. (c) A64 abraded by Al2 O3 , test time 10 s. (d) A64 abraded by Al2 O3 , test time 240 s. (e) A34 abraded by Fe2 O3 , test time 30 s. (f) A34 abraded
by Fe2 O3 , test time 240 s. (g) A61 abraded by Fe2 O3 , test time 30 s. (h) A61 abraded by Fe2 O3 , test time 240 s.
176 W.M. da Silva et al. / Wear 258 (2005) 166–177

distributions in the surface itself as well as their interactions nism of pore closure, the micro-abrasive wear behaviour is
with the pores. After coating the samples with gold, they were governed by a compromise between hardness and pore size.
observed by scanning electron microscopy. Wear coefficient decreases with hardness up to a critical value
(roughly 110 kgf mm−2 ), Fig. 9. From this point, which corre-
Fe(s) → Fe(aq) 2+ + 2e− (E0 = 0.44 V) (3) sponds to a critical value in pore size, the hardness continues
to increase, the pore size also continues to increase, as shown
Cu(aq) 2+ + 2e− → Cu(s) (E0 = 0.34 V) (4)
by Figs. 9 and 10, and negatively affects the wear resistance.
Fe(s) + Cu(aq) 2+ → Fe(aq) 2+ + Cu(s) (E0 = 0.78 V) (5)

In the early stages of the micro-abrasive wear process of sam- 4. Conclusions


ples presenting small pore size, abrasive grits are trapped in
the pores starting the process of pore closure, Fig. 12c and g, 1. For all tribological conditions, the superficial oxide
while the larger pores, associated with the low compaction layer had already been penetrated when the steady state
pressure, remain open, Fig. 12a and e. As this family of sam- wear regime was established, suggesting that the micro-
ples is characterized by large pore size, even after reaching abrasive wear process is governed by the substrate be-
the permanent wear regime up to the completion of the test, haviour in close correlation with the tribological condi-
some pores remained open at the surface, Fig. 12b and f, tions acting at the final stages of the wear process of this
enhancing the wear severity and thus producing high wear family of materials;
coefficients. On the other hand, for the specimens present- 2. For all abrasives, the smallest abrasive wear coefficients
ing small pore size, the great majority of the pores are filled were obtained by the combination of a high compaction
with abrasive grits, Fig. 12d and h, thus reducing the wear pressure with a fine powder grade. In general, for the same
severity. powder grade, an increase in compaction pressure led to
The capacity of our proposed technique to “freeze” the a decrease in the wear coefficient. On the other hand, for
dynamic conditions acting during the micro-abrasion pro- the same compaction pressure, an increase in powder size
cess is quite remarkable, in particular its ability to show gave rise to a slight decrease in the wear coefficient;
the surface distribution of the abrasive grits. The distribu- 3. In general, for a fixed powder grade, porosity had a posi-
tion of the “frozen” abrasive grits on the surface, Fig. 12b, tive effect on the micro-abrasion wear coefficient. Increas-
d, f and h, surprisingly reproduces their expected position ing porosity always caused an increase in the wear coeffi-
during the abrasive process, in particular the line up of the cient. On the other hand, at constant compaction pressure,
grits when the particles are expected to slide on the inter- an increase of porosity produced a decrease in the wear
face, e.g., the two-body like process. Ongoing work is in coefficient;
course in order to further exploit this original feature of the 4. The nature of the abrasive had a strong influence on the
technique. abrasive wear behaviour. This was explained in terms
As reported in an early paper by de Mello et al. [6], the rela- of the severity of the abrasive process, which was anal-
tionship between processing parameters and micro-structural ysed according to relative hardness, abrasive grit size and
features is quite complex. Mainly at the lower compaction shape. The highest wear coefficients were produced by
pressure, pore size tends to increase slightly with powder alumina while abrasion by haematite produced the lowest
grade. In general, the pore size decreases as the compaction wear coefficient;
pressure increases. There is evidence of a critical pressure 5. The nature of the abrasive also controls the mechanism
leading to two different magnitudes of pore size. For the lower acting on the different tribo-systems. When using alu-
compaction pressure the pores are larger and little affected mina, the dominant wear mechanism was multiple inden-
by the powder grade. Increased compaction pressure causes tation. On the other hand, a grooving wear mechanism
a substantial reduction in pore size as well as a stronger influ- was found to be dominant for silica and haematite;
ence of powder grade on this parameter. Moreover, they re- 6. The proposed original methodology (based on the in situ
ported that for low-compaction pressures (300 and 400 MPa), deposition of a thin layer of copper on slightly cleaned
the pore size is almost independent of porosity and powder abraded surfaces) successfully allowed further under-
grade. However, for the higher compaction pressures (500 standing of the mechanisms involved in the interactions
and 600 MPa), an increase in porosity, which is normally of the abrasive grits with pores and the role played by the
associated with a reduction in powder grade, produces a de- pores on the wear behaviour;
crease in pore size. For the same powder size, the increasing 7. For all the abrasives studied, the micro-abrasive wear be-
porosity, which arose from reducing the compaction pressure, haviour was governed by a compromise between hardness
led to an increase which reached a constant value of pore size. and pore size. Wear coefficient decreases with hardness
They also noticed that this threshold in porosity increases as up to a critical value (roughly 110 kgf mm−2 ). From this
the compaction pressure increases. point, which corresponds to a critical value in pore size, the
In conclusion, for all the abrasives studied, although their hardness continues to increase, the pore size also contin-
particle size may affect, in a quantitative way the mecha- ues to increase and negatively affects the wear resistance.
W.M. da Silva et al. / Wear 258 (2005) 166–177 177

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