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Wear 318 (2014) 49–61

Contents lists available at ScienceDirect

Wear
journal homepage: www.elsevier.com/locate/wear

Alignment and wear debris effects between laser-patterned steel


surfaces under dry sliding conditions
Andreas Rosenkranz 1, Leander Reinert, Carsten Gachot n, Frank Mücklich
Saarland University, Department of Materials Science and Engineering, Campus, 66123 Saarbrücken, Germany

art ic l e i nf o a b s t r a c t

Article history: In this experimental study periodic line-like patterns with different periodicities (5, 9 and 18 mm) were
Received 12 March 2014 fabricated by laser-interference patterning on stainless steel samples (AISI-304) and on 100 Cr 6 steel
Received in revised form balls. Linearly reciprocating dry sliding tests with a ball-on-disk configuration were performed on
11 June 2014
patterned pairs and on patterned-substrate/unpatterned-ball pairs Alignment effects were studied by
Accepted 16 June 2014
Available online 20 June 2014
means of a newly developed positioning method, which ensures an optimal alignment. The number of
cycles was set to 200 and 20,000 to study the run-in and stability behaviour of the patterned surfaces, all
Keywords: of which exhibited a lower kinetic coefficient of friction than the unpatterned reference. Depending on
Laser processing the respective alignment, different friction and wear mechanisms can be distinguished. Differences in
Sliding wear
the real contact area, the possibility to store wear particles and the time needed to remove the native or
Surface topography
laser-induced oxide layer can be well correlated with the temporal evolution of the coefficient of friction.
Steel
& 2014 Elsevier B.V. All rights reserved.

1. Introduction higher COF when sliding parallel to the ridges [17], contradicting
Menezes et al. [18,19].
The idea of creating tailored surfaces with laser-based technol- Very recently, Yu et al. have published a manuscript studying
ogies has been around for many years. Numerous research articles the topographic dependence of friction on micro- and nano-
report the benefits of textured surfaces in biological and tribolo- grooved surfaces [20]. Dry sliding tests (ball radius R) on different
gical applications [1–4], particularly well described for lubricated line patterns made of 139 nm to 110 mm wide (width b) laser-
sliding contacts [5–9]. However, optimum design parameters such ablated grooves were performed parallel and perpendicular to the
as texture or pattern geometry, feature sizes and area densities are grooves. Assuming no wear, the influence of the contact area, the
still a matter of lively debate [6–8, 10]. stiction length, the energy barrier and the contact stiffness were
As far as dry friction between mating surfaces is concerned, discussed with respect to these two cases. For small ratios
most of the research has been focussed on single-sided pattern (b/R o10  3), the tribological behaviour is mainly influenced by
friction pairs and their ability to trap wear debris in order to avoid the stiction length which is different for the parallel or perpendi-
third body interactions or to reduce stiction in magnetic storage cular orientation [20].
disks [11–15]. Additionally, regarding double-sided pattern friction pairs, we
Borghi et al. observed a 10% decrease in the coefficient of published a paper which deals with interlocking laser-patterned
friction (COF) of nitrided steel surfaces due to embedded wear surfaces and the influence of the periodicity and surface chemistry
particles in laser-patterned dimples [16]. Moreover, Rapoport and on the tribological behaviour [21]. Interlocking surfaces could be
co-workers showed the enhanced storing capability of laser- particularly interesting for micro- and nano-positioning systems.
patterned steel surfaces for solid lubricants such as MoS2 [13]. In this work, we study the tribological effects of the sliding
Applications aside, looking at a simple line-patterned surface direction and the pattern alignment on single (patterned sub-
reveals another aspect of controversy. Several studies inconsis- strate) and double-sided pattern (substrate and ball) friction pairs
tently argue about the frictional response of perpendicular or and continue the previous work on interlocking contacts for 200
parallel sliding with respect to said patterns. He et al. observed a and 20,000 sliding cycles. In order to ensure a desired alignment
between the pairs, a new positioning method has been developed
and will be presented in detail within this article. For the texturing
n
process, interfering beams from a solid-state Nd:YAG laser guar-
Corresponding author. Tel.: þ 49 681 302 70554; fax: þ 49 681 302 70502.
antee homogeneous surface patterns with different interference
E-mail addresses: a.rosenkranz@mx.uni-saarland.de (A. Rosenkranz),
c.gachot@mx.uni-saarland.de (C. Gachot). geometries and lateral feature sizes on the micron scale in a
1
Tel.: þ49 681 302 70546; fax: þ49 681 302 70502. single laser shot covering several mm2 [22]. The topographic and

http://dx.doi.org/10.1016/j.wear.2014.06.016
0043-1648/& 2014 Elsevier B.V. All rights reserved.
50 A. Rosenkranz et al. / Wear 318 (2014) 49–61

microstructural changes are analysed by optical microscopy, white to 1 mm/s. The velocity profile is a sinusoidal function with a
light interferometry (WLI), scanning electron microscopy (SEM) maximum speed of 1 mm/s in the middle of the stroke. Based
and electron backscatter diffraction (EBSD). upon a mechanical equilibrium analysis of the used cantilever, the
load of 1 mN combined with the maximum velocity of 1 mm/s is
sufficient to achieve a vertical displacement of the cantilever of
2.5 mm. This is larger than the structural depth of the laser-
2. Experimental procedure textures and therefore it can be concluded that the chosen
parameters are appropriate to obtain interlocking. The number
Flat stainless steel substrates (20  20  1 mm3 AISI-304) with of cycles was adjusted to 200 (6 min measuring time) and 20000
a mirror-like surface finish (rms-roughness E30 nm) were laser- (6 h measuring time) cycles. A stiff cantilever acting as a friction-
patterned for subsequent tribological experiments with bearing less force transducer in both vertical and horizontal directions
steel balls (ø 3 mm AISI 52100) with a polished surface finish (rms- holds the 100Cr6 ball. The cantilever is loaded onto the substrate
roughnessE350 nm) as counterparts. Based upon the rms-values with a precise force using piezo actuation in order to accurately set
of the polished ball and substrate, the composite surface rough- up the normal load. During the experiment, the deflection of the
ness is around 351 nm. The chemical composition of the substrate elastic arms in the horizontal and vertical directions is measured
and ball are given in Table 1 as specified by the supplier. using optical fibre displacement sensors with high precision
Samples were patterned with a single 10 ns pulse from a pulsed and accuracy. The stiffness in both directions is known (normal
solid-state Nd:YAG laser (Spectra Physics, Quanta Ray PRO 290) stiffness ¼ 0.1536 ðmN=μmÞ, lateral stiffness ¼ 0.2094 ðmN=μmÞ).
under normal atmospheric conditions (room temperature and Accordingly, the normal and friction force can be easily calculated
atmospheric pressure). The primary laser beam is split into two based upon the stiffnesses and the corresponding deflections.
sub-beams which interfere on the sample surface resulting in a Through a feedback loop, the piezo actuation maintains the
sinusoidal line-like interference pattern [23,24]. The pattern normal load independent of any surface irregularities. Tempera-
wavelength, or period (P), defined as the distance between two ture and relative humidity were kept constant at 2072 1C
adjacent topographical peaks, is a characteristic quantity of the and 47 0.5%, respectively.
line pattern. P can be easily varied by changing the laser wave- In addition to the tribological reference measurements with an
length or the angle between the interfering beams [25]. Beam unpatterned pair, four different geometrical configurations were
splitters define the intensity of each beam and the laser fluence studied. The first two (Fig. 2a and b) concern single-sided pattern
was set to approximately 29 J/cm2 for all specimens in order to pairs: one with perpendicular sliding with respect to the pattern
achieve well-defined surface patterns. Due to the good absorption (perp), another, parallel (para). The two other configurations
characteristics of the materials used, the third harmonic, 355 nm, (Fig. 2c and d) concern double-sided pattern pairs with identical
was selected. P was thus set to 5, 9 or 18 mm. The experimental set- pattern periods and the sliding direction perpendicular to the ball
up for two-beam interference and the resulting surface pattern pattern: one with parallel pair patterns (01), the other perpendi-
(P ¼9) mm can be seen in Fig. 1. Further details concerning the laser cular (901). In this case, new patterned tribometer balls were used
patterning process and the experimental set-up as well as the in order to ensure reproducibility and avoid previous wear effects.
laser-matter interaction have been already published elsewhere In order to ensure statistically significant tribological results, 10
[24,25]. measurements were performed per period and configuration and
The tribological experiments were conducted on a Nanotrib- averaged, including one standard deviation.
ometer (CSM Instruments) using a ball-on-disk configuration in a For a precise alignment of the patterns for to the tribological
linearly reciprocating sliding mode with a stroke length of 0.6 mm testing, a cross was previously milled with a focused ion beam
and a normal force of 1 mN. Moreover, the sliding speed was set (FIB) in a dual beam workstation (FEI Strata DB 235).
The topography of the patterned surfaces was measured by a
Table 1
white light interferometer (Zygo New View 7300), equipped with a
Chemical composition of the used steel samples in weight % as specified by the
supplier. 3D imaging surface structure analyser. That of the original surfaces
and the wear tracks was observed by optical microscopy (light
Used steel specimens Fe Cr Ni Mn Si C Mo microscope Olympus BX 60) and scanning electron microscopy
(SEM) (FEI Strata DB 235). The composition was analysed by an
Stainless steel (AISI 304)—substrate 68.9 18 10 2 1 0.1 /
100Cr6 steel (AISI 52100)—tribometer ball 96.7 1.5 / 0.4 0.3 1 0.1
electron dispersive spectroscopy (EDS) system (EDAX) in the Strata
workstation. Crystallographic analysis was done with an electron

Fig. 1. Laser interference set-up including beam attenuator, lens, beam splitter and mirror. The primary beam of the nanosecond laser is split into two sub beams interfering
through a quadratic mask and thus transferring the interference pattern to the steel surface. The SEM micrograph shows a periodic line-like surface pattern with a pattern
period P of 9 mm.
A. Rosenkranz et al. / Wear 318 (2014) 49–61 51

Fig. 2. Four configurations of the tribometer ball and the substrate in order to illustrate dependencies. In the case of a patterned substrate and an unpatterned ball, ((a) and
(b)) indicate parallel and perpendicular alignments of the sliding direction with respect to said pattern. The 01 ((c) and 901 (d)) configurations indicate the angles between the
double-sided patterns of each pair. The latter slide both perpendicularly with respect to the ball pattern. The vector v denotes the sliding direction in the tribometer.

backscatter diffraction (EBSD) system (TSL OIM analysis) in uniformly distributed and largely homogeneous. Only in the case of
another SEM/FIB dual beam workstation (FEI Helios Nanolab). 18 mm, slight irregularities appear with a typical double-peak profile
The Kikuchi patterns are generated at an acceleration voltage of [26]. According to Table 2, the structural depth of the patterned balls
20 kV and recorded by means of a Hikari camera system with and substrates were measured by WLI and are comparable to each
about 250 frames per second. The results of the EBSD measure- other in the range of approximately 1 mm. Considering the different
ments are presented as inverse pole figure (IPF) maps. periods, it can be seen from Table 2 that the structural depths for the
patterned ball and substrate are nearly the same.

3. Results and discussion


3.3. Tribological behaviour vs. cycles
3.1. Positioning method
3.3.1. 200 Cycles
In order to obtain reliable and precise sample positioning, a 3.3.1.1. Parallel and perpendicular alignment. First, tribological
new method was developed. For the para and perp configurations, experiments with 200 sliding cycles were conducted in order to
a 500 mm  30 mm  0.3 mm alignment cross was FIB milled at an study the run-in behaviour of the patterned surfaces as well as the
unpatterned edge of the patterned samples. The cross is perfectly reference. This regime is important because it allows for a careful
aligned with respect to the line patterns. The digital cross of a analysis of the underlying friction and wear mechanisms [27–29].
portable digital microscope (Dino-Lite Digital Microscope pro), Linear reciprocating sliding tests with three different periods, namely
adapted to the nanotribometer, is aligned parallel to the edge of 5, 9 and 18 mm and two different configurations (parallel-para and
the tribometer translation stage. The digital cross and the FIB- perpendicular-perp) were examined. All tests were repeated under
milled alignment cross can thus be superimposed as shown in the same conditions 10 times to obtain a reliable data set.
Fig. 3. This procedure ensures that the sliding direction of the Fig. 6 shows the results of the reference measurement as well
translation stage is nearly perfectly aligned (accuracy below 0.11) as the para and perp configurations, with standard deviations.
parallelly or perpendicularly to the line structures. Every measuring point is calculated as the averaged value of one
For the 01 and 901 configurations, alignment is achieved using a forward and backward stroke excluding the static friction at the
50 mm thick acetyl cellulose replica foil which can be fully dissolved reversal points of the stroke length.
in acetone. After mounting the tribological pair in the nanotrib- According to Fig. 6a–c, it is clear that the polished reference
ometer, the acetyl cellulose foil was moistened with acetone from shows higher static and kinetic friction over the entire measure-
both sides. It is thus possible to reproduce the pair patterns on ment than the patterned samples, regardless of the alignment and
either side of the foil, due to its large thickness compared to the the period. Furthermore, the para configuration shows a higher
patterns (artificial surface roughness). The angle between the two COF than perp for all periods. This observation is consistent with
patterns can be determined, using a transmitted light microscope, other published experimental findings [10,17,20].
and corrected accordingly to 01 or 901 with a rotation table, adapted A closer look at the very first 10 sliding cycles reveals a drop in
to the nanotribometer for this purpose. The precision of the home- the COF of the patterned samples and an increase in the COF for
built rotation table is in the range of 70.51. This value arises from the reference. The latter can be explained by an increasing contact
the sum of the mean value and the standard deviation of 10 area due to plastic deformation of the substrate material [30]. This
approaches, checked by the light microscope. For interlocking seems to be reasonable because the hardness of the ball material
patterned surfaces (01-configuration), a misalignment below 41 is quadruples that of the steel substrate. Regarding the drop
still acceptable, above which the peak-valley mismatch, over half of observed in the para and perp measurements, similar observations
the smallest P (5 mm) at the edge of the pattern, would prevent were made by Blau et al. [31]. Within these studies, the initial drop
interlocking. In order to prove the accuracy of the positioning was correlated with the wear rate. Single sharp asperities must be
system, optical micrographs prior to and after the alignment are worn off before the tribological system can stabilise. A careful
given in Fig. 4, improving the misalignment down to  0.61. The analysis of the surface topography by means of WLI proved the
misalignment for the 901 configuration is the same range. existence of such asperities in the laser-patterned surfaces. The
skewness Rsk seems suitable for this analysis [21]. As can be seen
3.2. Topographic analysis of the laser-patterned substrates from Table 2, the polished reference has a negative skewness
which is typical for a good bearing capability [32]. In contrast,
Fig. 5 shows typical line patterns with different periods (5, 9 and the patterned samples have a positive skewness, characteristic
18 mm) on a stainless steel substrate imaged by SEM. The patterns are of sharp asperities. Therefore, it can be concluded that these
52 A. Rosenkranz et al. / Wear 318 (2014) 49–61

Fig. 3. The digital cross of the portable digital microscope is superimposed with the cross produced by FIB. Depending on the rotation angle, the sliding direction of the
nanotribometer can be perfectly aligned parallel (para configuration) or perpendicular (perp configuration) to the line-like structures.

Fig. 4. Light microscope images of the replica foils measured in transmission mode prior to (a) and after the correct alignment (b). In both images, the line pattern from the
bottom and the top side are clearly visible.

asperities are responsible for a higher wear rate, opposing higher the contact area of the patterned surfaces and therefore slightly
resistance to the sliding motion of the ball accompanied by a reduced [30,31].
higher friction force at the beginning of the measurement [31]. During the 200 cycles, there is a slight increase in the COF for
Once these asperities are worn off the COF is mainly dependent on all the patterned surfaces, which can be attributed to flattening of
A. Rosenkranz et al. / Wear 318 (2014) 49–61 53

Fig. 5. SEM-micrographs displaying laser-induced line patterns. By adjusting the angle of the interfering sub-beams, a pattern period of 5 mm (a), 9 mm (b) and 18 mm (c) was
achieved.

Table 2
Roughness parameters Ra and Rsk measured by WLI for the laser-patterned substrates with pattern periods 5, 9 and 18 mm compared to the unpatterned reference.
Furhermore the structural depth for the balls and the substrates as well as the resulting aspect ratio are given.

Sample Ra (mm) Rsk Structural depth ball (mm) Structural depth substrate (mm) Aspect ratio

Reference (mm) 0.05 (7 0.02)  0.61 ( 70.16) / / /


5 0.26 (7 0.01) 0.71 ( 70.04) 0.88 ( 7 0.33) 0.80 ( 70.16) 0.16
9 0.36 (7 0.01) 0.94 ( 70.11) 1.13 ( 7 0.17) 1.09 ( 70.15) 0.12
18 0.24 (7 0.01) 1.41 ( 70.07) 0.79 ( 7 0.27) 0.82 ( 70.28) 0.04

the topographical peaks and a consequent increase in the contact the grains during sliding. This reorientation favours a preferred
area. For both para and perp configurations, the magnitude of the sliding plane typically arranged parallel to the sliding direction
COF is much smaller compared to the polished reference, and can [31,34]. This preferred sliding plane has a lower shear strength
be explained by a smaller contact area. thus reducing the friction force and the COF [34,35].
As shown in Fig. 6, there is a strong effect of the sliding Furthermore, studying the wear tracks of both orientations can
direction on the frictional response. However, the influence of provide a deeper insight into the underlying wear mechanism.
the alignment is a matter of a controversial discussion in the Fig. 7 reveals the differences in the corresponding wear tracks,
literature [17–20,33]. delimited with a red rectangle, for the 5 mm period imaged by
In addition to topographic factors, microstructural effects may light microscopy (Fig. 7a and b) and SEM (Fig. 7c and d). Similar
also play an important role. In this context, several authors already results were found for the other periods. After 200 cycles, the perp
discussed dynamic recrystallisation leading to a reorientation of wear tracks show rather point-like contacts. However, in the para
54 A. Rosenkranz et al. / Wear 318 (2014) 49–61

Fig. 6. Temporal evolution of the COF for the reference measurements as well as for the para and perp configurations. ((a)–(c)) Display the results for the three pattern
periods 5, 9 and 18 mm, respectively.

configuration, a material displacement along the ridges of the components have to be taken into consideration when discussing
pattern can be observed which increases the contact area, as does the aforementioned friction results. Considering the deformation
the COF [30]. component, the line pattern leads to the maximum constraint in
From Fig. 6, it is also clear that the displayed error of the the perpendicular direction. For the parallel alignment, plastic
reference sample is much larger than for the patterned specimens, flow occurs along the topographic peaks causing a smaller con-
regardless of period and configuration. This fact can be explained straint in sliding direction. The argumentation based on the
by the interaction of wear particles in the contact zone. For the deformation component would favour a higher COF for the
reference, wear particles are strongly interacting in the contact perpendicular alignment [18]. However, considering the influence
zone, as they tend to continuously agglomerate and collapse, of the contact area seen in Fig. 7, it can be stated that the contact
resulting in an unstable evolution of the COF [36]. Furthermore, area is smaller in the perpendicular alignment due to point-like
if wear particles are not shifted away they increase the ploughing contacting spots. As a consequence, the parallel alignment should
component due to the absence of storage volumes to remove them have the higher COF which is in fact the case in our experiments.
from the contact zone. On the other hand, the patterned surfaces The work of Yu et al. also supports the tribological results
offer the possibility to store wear particles in the topographic demonstrating a higher friction for the parallel alignment. The b/R
valleys [36–38]. ratio for the tested periods is in a range from 1.6  10  3 to
The friction force consists of two main contributions: adhesion 6  10  3 which can be correlated with the range of thin and
and deformation (ploughing) during sliding. Therefore, the COF intermediate grooves. Following the argumentation of Yu et al., the
under dry conditions can be written as the sum of an adhesive stiction length in the parallel configuration is longer compared to
component ma and a deformation component md [39]. Due to the the discontinuous contact in the perpendicular case. Relating the
existence of wear particles, a third quantity, the deformation of the stiction length to adhesion leads to a higher friction in the case of
particles mdp, must be added to the model [40,41]. The adhesion the parallel alignment [20].
component is mainly influenced by the material combination and
the real contact area. The deformation component strongly
depends on the degree of plastic deformation which is directly 3.3.1.2. 01 and 901 Alignment. Note that, in this case, the friction
related to the hardness of the contacting surfaces [39]. All these pair patterns are double-sided, the sliding is perpendicular to the
A. Rosenkranz et al. / Wear 318 (2014) 49–61 55

Fig. 7. Light ((a) and (b)) and SEM micrographs ((c) and (d)) of the wear track (after cleaning) for the perp and para configurations are shown. In the case of perp, only
punctual contact regions are visible. For the para orientation, a material displacement in the sliding direction is evident. The results of the respective wear track are
exemplarily shown for a period of 5 mm. Similar results were found for the other two tested periods. (For interpretation of the references to color in this figure legend, the
reader is referred to the web version of this article.)

ball pattern and, to avoid confusion with the previous section, the just barely for 9 and 18 mm. The high initial COF for 01 can be traced
configuration notation, 01 and 901, describes the angle between back to a possible geometrical interlocking. Due to an optimal
pattern and counter pattern. alignment of the surfaces in this configuration (cf. positioning method),
Fig. 8 displays the temporal evolution of the COF for three the surfaces tend to interlock after setting up the normal load. The
periods (5, 9 and 18 mm) and two different configurations (01 and interlocked surfaces hinder the relative movement thus increasing
901). The displayed curves in Fig. 8 clearly demonstrate that the the COF [30]. During the first 10 sliding cycles, a sudden drop in the
kinetic COF of the laser-patterned surfaces is lower than the COF of COF can be observed regardless of period and configuration. This
the reference, regardless of configuration and period. Moreover, behaviour can be correlated with a gradual degradation of the surface
the kinetic COF of the reference sample is larger than that of the 01 patterns after some run-in [21]. After 25 cycles of sliding, the COF
configuration. Comparing the two alignments, the 901 configura- remains nearly constant displaying only a slight slope over the entire
tion demonstrates a lower COF. This trend is valid for all tested measuring time.
periods; however the effect seems to be more pronounced for An explanation for the lower COF observed in patterned pairs
5 and 9 mm. For the 18 mm period, the error bars overlap during the might be a reduction in the real contact area. It is well known that the
entire sliding time and the COF at 901 is only slightly lower real contact area can be reduced by introducing laser textured surfaces
compared to 01. A closer look at the curves in Fig. 8 reveals that [42]. Prodanov et al. performed numerical simulations which demon-
the laser patterning of both contacting surfaces leads not only to a strate the smaller contact area of a 901 orientation compared to a 01
reduction in the COF but also to a reduction in the magnitude of orientation [43]. However, those simulations do not include wear
the error bars. Periods of 9 mm show the smallest error bars. This phenomena such as plastic deformation or abrasive wear.
observation can be well correlated with the homogeneity of the In order to allow for additional insights into the observed
laser-patterned surfaces. Periods of 9 mm show the most homo- frictional behaviour, light and SEM micrographs of representative
geneous height distribution resulting in the most regular pattern. wear tracks on 9 mm patterns at 01 and 901 are displayed in Fig. 9.
Considering the temporal evolution of the coefficient of friction for Similar results were found for 5 and 18 mm and are not shown here
01 and 901, the same experimental trend can be observed. The initial due to a matter of space. For both alignments, a wear track is
COF is higher for 01 than for 901 the reference, for all periods, although clearly visible. The 01 wear track is more pronounced than the 901.
56 A. Rosenkranz et al. / Wear 318 (2014) 49–61

Fig. 8. The temporal evolution of the COF using a patterned tribometer ball and substrate vs. the alignment and period are demonstrated for 5, 9 and 18 mm, respectively. Due
to the partial overlap of the standard deviations ((a) and (c)), these regions are highlighted with a mixed colour. (For interpretation of the references to color in this figure
legend, the reader is referred to the web version of this article.)

This can be explained by the higher stress level induced in this No significant wear features were observed at 901 after the tribolo-
configuration. The light microscope and SEM images for 01 clearly gical measurements (Fig. 10). A slight reduction in height in the
indicate a material displacement from the topographic peaks to the middle of the ball is visible for 01 (marked by the arrows) indicating
valleys. It can be concluded that the line pattern is gradually degraded plastic deformation. The wear process predominantly takes place on
and destroyed, emphasizing the underlying principle of geometrical the patterned substrate, being the softer material.
interlocking. Possible wear mechanisms are plastic deformation and Laser treatment may influence the microstructure, in particular
abrasion, resulting in the formation of wear particles. Wear particles the grain sizes and orientation as well as the defect density, for
are shifted towards the topographical valleys due to the sliding example. This could lead to a change in mechanical properties
direction. Temperature and mechanical stress effects may cause the such as hardness which directly influences the frictional proper-
wear particles to be welded to the base material. ties. For that purpose, EBSD was used in order to study micro-
The plastic flow of the material leads to a second effect. It structural effects prior to and after laser patterning (Fig. 11). Based
increases the contact area at 01, further contributing to the higher upon this analysis, the mean grain size was calculated and the
COF. As can be seen in Fig. 9, the wear track of the substrate clearly results are given in Table 3. As can be seen in Fig. 11 and Table 3, no
indicates a ploughing component for 01. Adhesive wear does not considerable changes in the mean grain size could be detected
seem to be the main contribution in this case, because almost no when comparing the grain size of the reference with the laser
welded wear particles can be found in the contact area of the four- patterned surface. Furthermore, no preferential grain orientation
times-harder textured ball, as can be seen in Fig. 10. For the 901 for the laser patterned surface was detected.
orientation, a material displacement into the topographic valleys In two related previous studies, a correlative chemical and micro-
of the substrate is not visible. Only slight plastic deformation of structural analysis was published. The results should be briefly
the surface pattern can be seen. The underlying wear mechanism summarised because these findings are very helpful for further
seems to have a predominant adhesive component for 901. The discussion. Due to the very high heating and cooling rates of 1010 K/
abrasive wear component leads to higher friction than the adhe- s of the used laser system, it is known that transformation hardening
sive component, in good correlation with the experimental results may occur in steel [23,45–47]. However, X-ray diffraction demon-
in Fig. 9 [37,40,44]. strated the presence of the austenitic phase [21]. A detailed chemical
A detailed analysis of the patterned tribometer balls prior to and analysis performed by X-ray photoelectron spectroscopy (XPS) and
after the tribological experiments was performed by means of WLI. atom probe tomography demonstrated an increase in the oxide layer
A. Rosenkranz et al. / Wear 318 (2014) 49–61 57

Fig. 9. Comparison of the cleaned wear tracks measured by light and scanning electron microscopy for the 01 and 901 orientation for 9 mm period.

Fig. 10. Comparison of the laser-patterned tribometer balls prior to ((a) and (b)) and after the tribological measurements for the 01 ((c) and (d)) and 901 ((e) and (f))
configurations. Fig. 10 a, c and e are 3-D contour plots of the WLI, whereas parts (b), (d) and (f) correspond to intensity maps. Part (g) displays three cross-section plots for the
corresponding height profiles along the marked line in (a), (c) and (e).

thickness by a factor of 4. The corresponding oxide layer thickness of Finally, it should be mentioned that, despite the observed wear of
the reference was determined to be 3.6 nm, whereas the oxide layer the tribological pairs, the reduction in friction due to laser patterning
of the patterned surfaces was in the range of 15.4 nm measured by of both contacting surfaces persists over the entire measuring time
XPS [48]. and the surface patterns are still intact after 200 sliding cycles.
58 A. Rosenkranz et al. / Wear 318 (2014) 49–61

Fig. 11. EBSD orientation maps of the laser-patterned surfaces with different periods prior to the tribological testing with the corresponding standard orientation triangle.

Table 3
Calculated averaged mean grain size for the refer- [33,44]. Basically, the asperities are much sharper and therefore
ence sample and the laser patterned surfaces based wear is more severe due to higher edge stresses [21]. Furthermore,
upon the performed electron backscatter diffrac- the double-peak structure of the 18 mm pattern leads to a further
tion analysis. increase in the real contact area. An increased real contact area
reduces the contact pressure acting in the contact zone and
Sample Mean grain size (mm)
therefore the deformation component. Based on this comparison,
Reference 8.677 4.59 a laser-patterned substrate with 18 mm period was selected for the
5 mm 7.99 7 5.75 experiments with 20,000 sliding cycles.
9 6.917 4.84
Prior to tribological tests with patterned surfaces, unpatterned
18 5.65 7 3.81
reference experiments were carried out following the above men-
tioned experimental procedure for the smaller cycle numbers.
3.3.2. 20,000 Cycles Fig. 13 shows the temporal evolution of the COF for the unpat-
In order to analyse the stability of the laser-patterned surfaces, terned reference as well as patterned substrate in para and perp
tribological experiments with 20,000 cycles were conducted. The configurations. The initial COF of the reference is around 0.42 and
goal of these measurements is to study the influence of the plastic increases with time. After 7000 cycles the COF reaches a value of
deformation and the degradation of the oxide layers on the around 0.9. Afterwards, a sharp rise up to 1.4 is visible within the next
frictional properties. Fig. 12 compares the wear tracks of a 01 1500 sliding cycles. The initial friction coefficient for the para config-
configuration for the three tested pattern periods after 200 sliding uration is around 0.21 followed by an increase up to 0.6, reaching
cycles. The 18 mm pattern shows the lowest wear. An explanation finally steady state conditions (0.5). The perp configuration starts at
for this behaviour is the shape of the pattern profile and the around 0.18 and reaches the steady state regime after 17,500 cycles at
double-peak structure. It could already be shown by the authors in around 0.4. The difference in the initial COF is consistent with the
[21] that the periodicity has a strong influence on the shape of the results of the measurements with 200 sliding cycles.
laser-induced topography profiles. The smaller periods (5 mm) A comparison clearly points out the smaller COF of the
tend to have smaller real contact areas than larger periods patterned specimens over the entire 20,000 cycles. After having
A. Rosenkranz et al. / Wear 318 (2014) 49–61 59

Fig. 12. Comparison of the wear tracks measured by light microscopy for the 01 orientation for 5, 9 and 18 mm after 200 sliding cycles.

fatigue in the oxide layer. Fatigue leads to crack initiation and


propagation, parallel to the interface for subsurface cracks [51–53].
Due to the fracture of the oxide layer and the large plastic
deformation component introducing a large wear rate, wear
particles are generated [54]. These particles can be of oxidic nature
or a mixture of metal and oxide. Metallic wear particles can be
oxidised due to the stress level and elevated temperatures in the
contact zone. Therefore the wear particles typically increase the
abrasive component which can be explained by a higher hardness
compared to the base material due to the oxidic nature [55]. The
sharp increase in the COF of the reference sample can be traced
back to wear particle interactions that remain in the contact zone
with nowhere to go. Similar experimental observations were done
by Blau [49] and Hwang [36]. The reduction in the COF in the case
of the laser-patterned surfaces can be well explained by the
possibility to store the wear particles in the topographic valleys,
therefore reducing the ploughing component. The differences in
Fig. 13. COF versus sliding cycles up to 20.000. The substrate was line-patterned the para und perp configurations can be correlated with the
with an 18 mm period but not the tribometer ball. Two different relative alignments different real contact areas and stiction lengths as discussed
(para and perp) were tested. A comparison with the results of the reference
before. Furthermore, the possibility to store wear particles is
measurements is given.
reduced in the para configuration due to the sliding direction of
the ball along the ridges. The perpendicular movement of the ball
reached steady state (415,000 cycles) in perp, the COF is approxi- crossing the ridges leads to a more effective entrapment of the
mately one third of the reference’s. Furthermore, a similar reduc- wear particles and so favours a lower COF. The peak in the
tion can be found for para. A closer look at the temporal evolution temporal evolution of the reference sample can be explained by
reveals an increase in the COF in the first 5000 sliding cycles for a removal of the initial oxide layer causing a strong adhesion.
both alignments. The slope of this increase is comparable with the Finally, a preferred orientation is formed resulting in a slight
slope observed in the reference sample. decline of the COF.
Finally, it can be stated that the temporal evolution of the Fig. 14 shows the temporal evolution of the COF for two laser-
reference and para samples can be referred to the type b friction patterned specimens with 20.000 sliding cycles. First of all, it should
behaviour according to the classification of Blau [49]. The perp be mentioned that the COF of both alignments is lower than the COF
configuration demonstrates the same behaviour but to a lesser of the reference over the entire measuring time. The same conclu-
degree. A slow rise in the friction coefficient, which can be seen at sions with regard to the static and kinetic COFs of both alignments as
the beginning of the 20,000 sliding cycles in Fig. 13, can be in the case of 200 sliding cycles are valid. After 500 sliding cycles at
interpreted by a removal of an oxide layer combined with the 01, the COF reveals a sharp increase up to a value of around
generation of wear debris [36,50]. Due to the applied load and 0.6 followed by a slight decrease to 0.5. The COF of the 901
the contact of sharp asperities, the true contact pressure exceeds configuration shows an increase up to 0.7 with a deviating slope.
the elastic limit and induces plastic deformation. The linearly The faster increase in the COF of the 01 configuration can be
reciprocating sliding combined with the applied load causes traced back to enhanced wear phenomena taking place due to
60 A. Rosenkranz et al. / Wear 318 (2014) 49–61

shift for the first local maximum can be observed. The local maxi-
mum corresponds to a characteristic wavelength of 18.55 mm in
the spatial domain. This wavelength fits quite well to the period
induced by laser interference patterning. Despite 20,000 sliding
cycles, the worn surface clearly demonstrates periodic features
having an 18 mm period.

4. Conclusions

This study has two main parts: the development of a new


positioning method and tribological experiments for different patterns
and configurations composed of sliding directions and pattern align-
ments, for 200 and 20,000 sliding cycles under dry conditions.

1. A new positioning method was developed which allows for the


precise alignment of a line-like surface pattern with respect to the
sliding direction. For sliding tests with a patterned substrate and an
Fig. 14. The temporal evolution of the COF for laser-patterned tribometer ball and
unpatterned reference ball, this method was realised using an FIB-
substrate. Both surfaces were line-patterned with an 18 mm period. Two different
relative orientations 01 and 901 were tested. A comparison with the results of the milled alignment cross and a subsequent analysis by a portable
reference measurements is given. digital microscope. The positioning method for experiments with
patterned pairs was done using a replica foil combined with a
rotation table. This set-up allows for a precise alignment of two
line-like patterns with an accuracy of 0.51. In this context, an angle
deviation of less than 51 is necessary. Otherwise, the resulting
mismatch is larger than half of the smallest period (5 mm) which
prevents interlocking.
2. Sliding tests (200 cycles) were conducted for reference sam-
ples, patterned substrate versus tribometer ball (parallel and
perpendicular configuration with respect to the sliding direc-
tion) and patterned substrate versus patterned tribometer ball
(01 and 901 alignment between the patterns). All tested con-
figurations and alignments point out a lower kinetic coefficient
of friction than the unpatterned reference sample. Further-
more, the perp configuration shows a lower COF compared to
the para configuration. The investigation of the wear tracks
reveals a large difference in the real contact area that can be
well correlated with the frictional results. With regard to the
tribological testing of patterned pairs, the 901 alignment dis-
plays a lower coefficient of friction than at 01. Through a
Fig. 15. Fourier analysis of the as-patterned and worn surfaces prior to and after
the tribological testing procedure. The inset shows the wear track of the 18 mm detailed analysis of the respective wear tracks, friction and
period after 20.000 sliding cycles imaged by light microscopy. (For interpretation of wear mechanisms explaining the temporal evolution of the
the references to color in this figure legend, the reader is referred to the web friction behaviour could be determined.
version of this article.) 3. Tribological experiments with 20,000 sliding cycles were
performed in order to study the stability behaviour of the
higher contact stresses. An enhanced wear rate could also lead to a laser-patterned surfaces. Similar results with regard to the
faster generation of wear particles which can cause a higher reduction of the COF were found for 200 and 20,000 sliding
abrasive wear component. This can induce a faster removal of cycles. For the experiments with patterned substrate and
the oxide layer and lead to a larger amount of pure metal–metal smooth ball, the COF of the perp configuration is smaller
contact at lower cycle number. compared to the reference and the para configuration during
The smaller and constant slope observed in the first 10,000 the entire 20,000 cycles. The line-like patterns are only
sliding cycles at 901 can be correlated with the stress level. This partially worn after 20,000 sliding cycles. The temporal evolu-
causes a smaller amount of wear particles, reduces the plastic tion of the COF for two patterned surfaces also reveals a lower
component and leads to a slower oxide removal as well as wear coefficient for both alignments over the entire sliding time. For
particle generation. these experiments, the temporal evolution of the COF can be
Fig. 15 depicts the radial power spectra of the as-patterned and linked to different storage possibilities of the wear particles
worn surface after 20,000 sliding cycles at 01. The inset shows depending on the sliding direction. Furthermore, characteristic
the wear track imaged by light microscopy. The red and black rises of the COF could be explained by a removal of the oxide
rectangles mark the areas used for the Fourier analysis in order to layer and an increasing metal-metal contact.
obtain the respective radial power spectra. These plots show the
magnitude of various frequencies in the frequency domain and can
be used to prove the existence of periodic features. The first local
maximum in the radial power spectrum corresponds to the Acknowledgements
inverse of a characteristic wavelength of periodic features (pat-
terned period). As can be seen in Fig. 15, both radial power spectra The present work is supported by funding from the Deutsche
show the first local maximum at 0.0538 mm  1 and no position Forschungsgemeinschaft (DFG, project: MU 959/30-1) and SPP
A. Rosenkranz et al. / Wear 318 (2014) 49–61 61

1551. The EU funding for the project AME-Lab (European Regional [24] F. Mücklich, A. Lasagni, C. Daniel, Laser interference metallurgy-using inter-
Development Fund C/4-EFRE-13/2009/Br) is gratefully acknowl- ference as a tool for micro/nano structuring, Int. J. Mater. Res. 97 (2006)
1337–1344.
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state government of Saarland (INST 256/298-1 FUGG). Mr. C. Pauly, a new method for periodic surface microstructure design on multilayered
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