Transactions of the IMF

The International Journal of Surface Engineering and Coatings

ISSN: 0020-2967 (Print) 1745-9192 (Online) Journal homepage: http://www.tandfonline.com/loi/ytim20

Sulphuric acid anodising of EN AC-46500 cast

aluminium alloy

B Gastón-García, E García-Lecina, M Díaz-Fuentes, J A Díez & C Müller

To cite this article: B Gastón-García, E García-Lecina, M Díaz-Fuentes, J A Díez & C Müller (2011)
Sulphuric acid anodising of EN AC-46500 cast aluminium alloy, Transactions of the IMF, 89:6,
312-319

To link to this article: http://dx.doi.org/10.1179/174591911X13167804921037

Published online: 12 Nov 2013.

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 Sulphuric acid anodising of EN AC-46500 cast
aluminium alloy
B. Gastón-Garcı́a1, E. Garcı́a-Lecina*1, M. Dı́az-Fuentes1, J. A. Dı́ez1 and
C. Müller2
In this study, the anodising behaviour of commercial EN AC-46500 cast aluminium alloy in
sulphuric acid electrolyte was investigated in order to determine the optimal experimental
conditions. The results showed that the high content and variety of alloying elements disrupted
the classical porous morphology and changed the typical V–t curves of the high purity aluminium
anodising. The effects of electrolyte concentration, bath temperature, current density and
anodising time on the characteristics of the anodic layers obtained were studied, and it was
observed that the increase in any of these parameters produced a decrease in the mechanical
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properties of the layers. The best results were obtained by anodising at 5 vol.-%H2SO4, at
5?0 A dm22 during 30 min at 0uC. The application of a polishing pretreatment improved the film
appearance and did not modify the mechanical properties of the film, but considerably
decreased the film thickness.
Keywords: Aluminium, Anodising, Intermetallic particles, EN AC-46500

Introduction in the case of high purity aluminium, the anodising

process is easily performed and aesthetic, functional and
Aluminium has been widely used in industry for high ordered porous AAOL can be obtained,7–9 com-
decades. Its low density, high strength to weight ratio mercial aluminium alloys contain intermetallic particles,
and its corrosion resistance make aluminium and its elements in solid solution and, in some cases, impurities
alloys the material of choice for many applications in that negatively influence the general anodising response.10
the aircraft, aerospace, automotive, architectural and The final result is AAOL with cracks, voids and regions of
packaging industry, among others. Aluminium alloys different compositions which determine the aesthetic,
can be divided into two main categories, namely casting physical and mechanical characteristics of the anodic
alloys and wrought alloys. Although y85% of alumi- oxide film formed.11–16
nium is used for wrought products as foils, extrusions In this sense, it is known that it is difficult to obtain
and rolled plates, the industrial interest in cast alumi- appropriate AAOL on cast aluminium alloys, mainly
nium alloys is gradually increasing due to its low cost owing to low composition homogeneity, high porosity
and excellent fluidity, which allow the low cost produc- and presence of large concentration of alloying
tion of complex components with high size. However, elements such as silicon and copper which are in the
their poor tribological properties and low corrosion form of intermetallic compounds and are added to the
resistance notably reduce their application. matrix in order to increase the fluidity of the molten
In general, tribological and corrosion properties of metal and the resistance of the material.17–20 Thus,
aluminium and its alloys can be improved by anodising. although comparative studies of the anodising beha-
This electrochemical technique increases the thickness of viour of some cast alloys with Al and AlSi type alloys
the natural oxide layer, converting the surface of the are well documented,21–25 a systematic study is still
aluminium alloy into a ceramic coating (Al2O3) with necessary in order to overcome the anodising limita-
improved hardness, wear and corrosion resistance.1,2 The tions, determine the optimal anodising conditions and
characteristics of the anodic alumina oxide layer (AAOL) obtain good quality anodising films on different cast
formed depend not only on the anodising conditions, i.e. alloys of industrial interest. That is the case of EN AC-
composition of electrolyte, current density, voltage, 46500 die cast aluminium alloy, one of the most
temperature, etc.,3–6 but also on the chemical composi- popular die cast alloys used in the production of com-
tion and metallurgical history of the alloy. Thus, although ponents with complicated shapes that require strength
including air brake castings, gear cases and air cooled
1
heads. This alloy contains relatively large concentra-
Surface Finishing Department, CIDETEC-ik4, Pu Miramón 196, E-20009
San Sebastián, Spain tions of alloying elements that exceed the solid
2
ELECTRODEP, Departament de Quı́mica Fı́sica, Facultat de Quı́mica, solubility in aluminium, forming second phase particles
Universitat de Barcelona, C/Martı́ i Franquès 1, E- 08028 Barcelona, Spain during solidification. In the present paper, the effect of
*Corresponding author, email [email protected] different experimental parameters on anodising of

ß 2011 Institute of Metal Finishing

Published by Maney on behalf of the Institute
Received 31 March 2011; accepted 26 July 2011
312 DOI 10.1179/174591911X13167804921037 Transactions of the Institute of Metal Finishing 2011 VOL 89 NO 6
 Gastón-Garcı́a et al. Sulphuric acid anodising of EN AC-46500 cast aluminium alloy

commercial EN AC-46500 cast aluminium alloy in Fischer, Hünenberg, Switzerland) in cross-sections of

sulphuric acid electrolyte is reported. The growth and the samples, using a final load of 15 mN and a load
morphological characterisation of the oxide layers application time of 10 s. This load was selected to avoid
obtained are discussed, and microhardness and wear the influence of the substrate or the resin in the
resistance have been assessed and compared with those microhardness measurements of the layers obtained in
of the substrate. Moreover, the effect of a mechanical different anodising conditions. Vickers hardness was
pretreatment on the anodic film obtained has also been obtained by averaging 10 measurements on each sample.
analysed. Results from this work may assist in selecting Wear tests were performed using a ball on disc tribometer
the most appropriate experimental conditions for the (THT; CSM Instruments, Peseux, Switzerland) at room
development of high quality anodic oxide layers on this temperature. A 100Cr6 steel ball with a diameter of 6 mm
cast alloy that would made possible the implementation was used as the counterface material. The wear tests were
of aluminium in areas where it was not considered conducted under a normal load of 5 N, with a rotation
possible hitherto. diameter of 6 mm, at a sliding distance of 465 m and a
sliding speed of 4 cm s21. After testing, a section profile of
Experimental the wear tracks on the oxide layer was performed by a
contact profilometer (TALYSURF INTRA 50MM; Taylor
Flat shaped industrial pieces of cast aluminium alloy EN Hobson, Leicester, UK). From this information, maximum
AC-46500 provided by an aluminium die cast manu- depth penetration and wear section area were determined.
facturer were used in the present work [chemical The volumetric wear factor of the different oxide layers K
composition (wt-%): Al, 83?55; Si, 11?01; Cu, 2?28; Zn, was calculated using the following equation
1?22; Fe, 0?887; Mg, 0?511; Mn, 0?200; Pb, 0?0959; Ni,
0?0736; Ti, 0?0468; Cr, 0?0322; Sn, 0?0256; other,0?07]. K~2p rA=Nd (1)
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An active area of 13?5 cm2 was considered for the

experiments and the rest of the sample was protected where r is the rotation radius (mm), A is the wear section
with commercial resin. Before anodising, samples were area (mm2), N is the normal load applied and d is the sliding
distance (m).
submitted to a pretreatment process in order to prepare
the surface for the anodising process: soaking in an
alkaline cleaner at 45–50uC for 10 min, and desmutting Results and discussion
in an acid solution at room temperature for 10 min.
Samples were thoroughly rinsed in deionised water after Microstructure of cast alloy
each step. In some cases, aluminium samples were The microstructure of the EN AC-46500 aluminium
submitted to a mechanical pretreatment before the alloy was characterised by OM and SEM–EDS. In the
anodising process. optical micrograph in Fig. 1a, intermetallic particles and
The anodising process was performed in a sulphuric microvoids originating during the casting process can be
acid electrolyte at 5 and 15 vol.-% concentrations. A two distinguished from the aluminium alloy matrix. From a
electrode thermostated cell of 10 L with a cylindrical morphological point of view, the intermetallic particles
stainless steel cathode and agitation by air was used. observed in this alloy could be classified into two main
Aluminium samples were anodised under galvanostatic groups: particles with polyhedrical shape with sizes in
conditions, varying the current density between 1?0 and the range of 10–25 mm, and particles with an acicular
8?0 A dm22. The current was applied by a direct current geometry having sizes up to 25 mm. The EDS analyses
power supply (SM300-5; Delta Elektronika, Zierikzee, carried out in both types of particles showed that the
The Netherlands) and the evolution of the voltage polyhedrical shape particles were composed of Al–Fe–
during anodising was measured and transferred to Si–Mn–Cr; whereas, the particles with acicular shape
a computer by a multimeter (HP34401A; Agilent contained Al and Cu (inset, Fig. 1a). A detailed obser-
Technologies, Santa Clara, CA, USA). The temperature vation by SEM–EDS of the matrix of this aluminium
of the electrolyte was maintained constant by a alloy (Fig. 1b) also revealed the presence of granular a-
cryostatic bath (F12-MC; Julabo, Seelbach, Germany) Al phase surrounded by Si phase platelets formed in the
at three different values, i.e. 25, 0 and 20uC. Anodising interdendritic regions as part of the Al–Si binary
time was varied from 30 up to 120 min. Finally, samples eutectics.26
were thoroughly rinsed in deionised water and air dried.
Microstructural and morphological characterisations Voltage–time evolution during formation of
of the substrate and the oxide layers were performed anodic oxide layer on cast alloy
by optical microscopy (OM; EPIPHOT 200; Nikon, In order to study the effect of different experimental
New York, USA) and scanning electron microscopy parameters on the film growth, voltage–time (V–t)
(SEM; JSM 5500 LV; JEOL, Tokyo, Japan). To avoid responses were recorded during anodising experiments
charging, the samples were covered with a thin gold (Fig. 2).
layer, applied by a sputter coater (SCD 005; Bal-Tec, Figure 2a shows the V–t transients for anodising
Pfäffikon, Switzerland). Energy dispersive X-ray spec- processes at different current densities in a 15 vol.-
troscopy (EDS; INCA ENERGY SERIE 200; Oxford %H2SO4 electrolyte. In general, it was observed that
Instruments, Oxfordshire, UK) was used for qualitative there was an increase in the potential with time during
elemental chemical analysis. The thickness of the anodic the first minute of the experiment until attaining a
oxide layers was determined by OM analysis of the oxide relatively constant value. The final voltage increased
cross-sections. The data represent the average and with current density from 55 V at 1?0 A dm22 to almost
standard deviation of 30 readings for each sample. 80 V at 5?0 A dm22. In the case of 8?0 A dm22, a slight
Hardness of different layers was measured by a decrease in the final voltage was observed, probably
microhardness tester (FISCHERSCOPE HM2000; related to low quality films produced by heating effects

Transactions of the Institute of Metal Finishing 2011 VOL 89 NO 6 313

 Gastón-Garcı́a et al. Sulphuric acid anodising of EN AC-46500 cast aluminium alloy

1 Images (OM and SEM) of cross-sectional EN AC-46500 cast aluminium alloy. a Low magnification image of sample
microstructure. Inset shows EDS spectrum of intermetallic particles: (1) Al–Fe–Si–Mn–Cr particles; (2) Al–Cu particles
(small Au peaks are due to metallic gold that was sputter coated on aluminium alloy). b Detail of areas with different
morphologies in aluminium alloy matrix. Inset shows EDS spectrum from two marked zones

(Joule effect) generated under high current anodising steady state was accompanied by voltage fluctuations
conditions. In all the cases studied, the final voltage (55– indicative of cracking and reanodising processes pro-
80 V) was considerably higher than that obtained for voked by high level of stresses in the layer.28,29 When
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pure aluminium anodising (20–25 V), as a consequence analysing the curves at the initial stage of anodic
of a higher resistivity of the oxide or the substrate/ oxidation (i.e. first 2 min), three different regions (I, II
oxide interface probably due to the presence of oxygen and III) were detected before the onset of steady state
gas filled voids which hinder the ions transport voltage (region IV) (Fig. 2b). Thus, at the beginning of
processes.21,27 Moreover, in most of the cases, the the anodising process and regardless of the current

a, b effect of current density: 15 vol.-%H2SO4 electrolyte at 0uC and 1?0, 3?0, 5?0 and 8?0 A dm22 (marked with letters a,
b, c and d respectively); c effect of electrolyte concentration: 15 and 5 vol.-%H2SO4 electrolytes (marked with letters a
and b respectively) at 0uC and 5?0 A dm22; d effect of temperature and anodising time: 15 vol.-%H2SO4 electrolyte at 20,
0 and 25uC (marked with letters a, b and c respectively), at 5?0 A dm22 for 120 min
2 Voltage–time curves registered during galvanostatic anodising of EN AC-46500 cast aluminium alloy under different
conditions

314 Transactions of the Institute of Metal Finishing 2011 VOL 89 NO 6

 Gastón-Garcı́a et al. Sulphuric acid anodising of EN AC-46500 cast aluminium alloy

a at 3?0 A dm22 (homogeneous surface); b at 8?0 A dm22 (powdery surface)

3 Images (SEM) of top view of anodic alumina layers formed on EN AC-46500 aluminium alloy after anodising in 5
vol.-%H2SO4 electrolyte at 25uC for 120 min

density, there was a slope change y7 V (transition I–II) an homogeneously aesthetic dark grey colour and only
associated with the presence of an air formed film on the few, very thin cracks were visible on its surface (Fig. 3a).
surface of the alloy.27 The time period during which this However, when higher current densities, temperatures and
transition potential was stable decreased with the anodising times were applied, the anodic oxide layers showed
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increase in current density. Subsequently, the curve a brown pale tonality that in some cases was rough and
was characterised by a linear increase in voltage with powdery and could be easily detached from the substrate. The
time limited by another slope change (transition II–III), surface of these samples showed the presence of numerous
which may be related to pore nucleation. The rate of wide cracks (Fig. 3b), linked to the deterioration of the layer
voltage increase with time was enhanced by increasing properties by thermally enhanced (field assisted and chemical)
the anodising current density. Moreover, while the exact severe oxide dissolution. These results are in agreement with
transition II–III potential depended on the experimental V–t transients recorded (Fig. 2a), where it was observed that
current density, it occurred at voltages similar to those the final voltage corresponding to 8?0 A dm22 was slightly
of pure aluminium (25–35 V). Beyond that point, lower than that corresponding to 5?0 A dm22.
instead of observing a voltage decline to the steady The SEM observation of the cross-sections of the
stage value (general behaviour of pure aluminium), an anodic oxide layers revealed an undulating aluminium/
increase in voltage with time at a progressively reducing oxide interface (Fig. 4a) under all experimental condi-
rate until achieving a steady stage voltage was observed tions, attributed to the different oxidation reactivities of
(region III). the aluminium matrix in comparison with the inter-
As it has been described, anodising of EN AC-46500 metallic particles.11–16,23 In addition, the anodic layers
results in a different V–t response from that observed for presented considerable porosity and cracks. Most of
pure aluminium anodising, probably due to secondary them were likely to have come from acicular particles
processes that take place during the formation of the dissolution (principally formed by Cu and Al) taking
alumina film, such as anodic oxidation of intermetallic
place during the anodising process, because no such
particles, oxygen evolution, cracking and reanodising
precipitates were found within the anodic layer. This
processes.21
result is consistent with the considerations of other
Moreover, the analysis of different experimental
authors who declared that particles with similar
conditions showed that the voltage profiles also pre-
chemical composition (Cu2Al) tended to be anodic
sented different features as a function of the electrolyte
relative to the aluminium matrix.14,30 Apart from this,
concentration (Fig. 2c) and temperature (Fig. 2d). Thus,
previous studies showed that oxidation of copper was
it was observed that the transition voltages correspond-
also associated with the generation of oxygen within the
ing to the transitions from II to III regions of the V–t
curves increased with the decreases in electrolyte anodic film and the proliferation of oxygen bubbles
concentration and temperature. Moreover, the final with high pressure.31–34 These bubbles may grow and
voltage decreased with the increases in electrolyte coalesce and the contained gas may be released by the
concentration and temperature. rupture of the oxide film. Moreover, the stress
generated during the growth of the anodic oxide films
Morphology, microstructure and thickness of may also contribute to the cracking of the film.35 The
anodic oxide layers consequence of such processes is the development of
In an effort to correlate the differences among the anodic layers of bad quality.
voltage response with the properties of the films, the On the other hand, polyhedrical particles (Al–Fe–Si–
morphology, structure and thickness of the AAOL were Mn–Cr) did not prevent or hinder the growth of the
analysed. anodic film but seemed to remain partly oxidised after
anodic oxidation. In this sense, the highlighted area in
Morphology and structure Fig. 4a shows the evolution of one of these intermetallic
The surface appearance of the EN AC-46500 anodised particles subjected to the anodising process. The
samples varied according to the anodising conditions. composition of both regions of the particle was
Under suitable experimental conditions (e.g. 5 vol.-%H2SO4, determined by EDS (Fig. 4b). The analysis of the upper
25uC, 3?0 A dm22 and 120 min), the anodised film showed part (1) showed the presence of oxygen and sulphur

Transactions of the Institute of Metal Finishing 2011 VOL 89 NO 6 315

 Gastón-Garcı́a et al. Sulphuric acid anodising of EN AC-46500 cast aluminium alloy

4 a SEM image of cross-sectional anodic alumina layer formed on EN AC-46500 aluminium alloy after anodising in
15 vol.-%H2SO4 electrolyte at 0uC and 5?0 A dm22 for 30 min. Highlighted area corresponds to partially anodised Al–
Fe–Si–Mn–Cr particle. b EDS spectrum from different regions marked in a (small Au peak is due to metallic gold that
was sputter coated on anodic alumina layer to reduce electrical charging during SEM measurements)

coming from the sulphuric acid electrolyte used for the Thickness
anodising process.3 Moreover, the constituent elements The way in which the anodising parameters affect the
of the polyhedrical particles were also detected (Al, Fe,
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thickness of the anodic films is shown in Fig. 5. In this

Si, Mn and Cr). The differences in the peak intensities sense, as expected, for the same temperature and
of the oxidised part (1) when compared with that of the anodising time, the mean thickness of the oxide layers
residual particle (2) suggests a Si enrichment and an increased with current density (Fig. 5a), as the effect of
impoverishment of the rest of the alloying elements. increasing the current density is to speed up the rate of
Similar results have been obtained for other aluminium growth. On the other hand, no differences were observed
alloys.12,16,23 among the average thickness values of anodic films
As was previously mentioned, two regions were obtained from the two different electrolyte concentra-
determined in the aluminium matrix, one more silicon tions studied. This would indicate that the efficiency of
enriched than the other. After the anodising process, the the anodising process, from the electrochemical point of
difference between the morphologies of both regions was view, was similar in both electrolytes.
more accentuated, as can be observed in Fig. 4a. The The progress of thickness with time and temperature
EDS analysis showed that the rougher areas (3) effect is shown in Fig. 5b. The results showed that the
presented higher silicon content than the smoother ones thickness of the layer increased with anodising time,
(4). According to previous results,23,36 the presence although this rise was enhanced when operating
of these silicon particles may cause changes in the temperature was lower. In fact, at a current density of
distribution of the current in favour of less resistive 5?0 A dm22 and an anodising time of 120 min, it was
adjacent aluminium matrix. Consequently, the oxide possible to obtain films with thicknesses superior to
grows around the particle which remains trapped in the 100 mm at 25 or 0uC, while no more than 60 mm were
anodic layer. Anodic oxidation of silicon particles seems obtained at 20uC. The results indicate that there is a
also to occur, although only partially and at a reduced balance between oxide film formation and its redissolu-
rate compared with the adjacent aluminium matrix. tion in the sulphuric acid electrolyte, and that this

a effect of electrolyte concentration and current density (at 0uC for 30 min); b effect of temperature and anodising time
(in 15 vol.-%H2SO4 electrolyte at 5?0 A dm22)
5 Thickness of anodic alumina layers formed on EN AC-46500 aluminium alloy after anodising under different conditions

316 Transactions of the Institute of Metal Finishing 2011 VOL 89 NO 6

 Gastón-Garcı́a et al. Sulphuric acid anodising of EN AC-46500 cast aluminium alloy

a effect of electrolyte concentration and current density (at 0uC for 30 min); b effect of temperature and anodising time
(in 15 vol.-%H2SO4 electrolyte at 5?0 A dm22)
6 Vickers microhardness of anodic alumina layers formed on EN AC-46500 aluminium alloy after anodising under differ-
ent conditions

controls the upper limit of thickness which can be vol.-%H2SO4 (Fig. 7), and, because of this, presented
produced under any particular operating conditions.37 higher microhardness values. The data also showed a
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small reduction in mean microhardness values as the

Mechanical properties of anodic oxide layers: current density increased, especially at 8?0 A dm22, in
microhardness and wear resistance agreement with morphology results previously described
Microhardness and wear resistance are intimately (Fig. 3b).
associated with the rate of growth and the solvent On the other hand, the effect of electrolyte tempera-
action of the electrolyte, which not only determine the ture and anodising time on the microhardness of the
thickness of the coating but also its porosity, its anodic layers obtained was also studied (Fig. 6b).
mechanical properties and its chemical composition. Similar results were obtained on anodising at 25 and
0uC, with higher microhardness values than those
Microhardness obtained at 20uC. This behaviour is in agreement with
Vickers microhardness values measured in the middle of the literature38 where it is described that anodising
the cross-sectional anodic films and their corresponding processes performed at temperatures near 0uC are
standard deviations are shown in Fig. 6. The results characterised by thicker oxide layers with lower porosity
showed that under the anodising conditions studied, and better microhardness values than those formed in
the microhardness values of the anodic oxide layers processes carried out at 18–22uC. The results also
obtained were superior to that of the aluminium showed that microhardness decreases when long anodis-
substrate (140¡10 HV0?0015). ing times were applied. Thus, there is a critical time for
However, some differences were observed as a func- each anodising condition and, exceeding it, the anodic
tion of the operating conditions. Thus, a slight decrease film growth can be slowed down or stopped and
in mean microhardness values with the increase in chemical attack from the electrolyte may damage its
the electrolyte concentration was observed (Fig. 6a). integrity.
This effect could be explained as a result of the differences In all the cases, the rather high relative standard
in the quality of the layers. Thus, anodic films obtained deviations of the hardness measurements reflect the
at 5 vol.-%H2SO4 were more compact and with less compositional and structural heterogeneity and non-
cracks, pores and defects than those obtained at 15 uniformity of the anodic oxide films.

a 5 vol.-%; b 15 vol.-%
7 Images (SEM) of cross-sectional anodic alumina layers formed on EN AC-46500 aluminium alloy after anodising in sul-
phuric acid electrolytes of different concentrations at 0uC and 5?0 A dm22 for 30 min

Transactions of the Institute of Metal Finishing 2011 VOL 89 NO 6 317

 Gastón-Garcı́a et al. Sulphuric acid anodising of EN AC-46500 cast aluminium alloy

9 Images (SEM) of top view of anodic alumina layer

formed on mechanical polished EN AC-46500 alumi-
nium alloy after anodising in 5 vol.-%H2SO4 electrolyte
a without mechanical pretreatment; b with previous
mechanical polishing at 0uC and 5?0 A dm22 for 30 min
8 Voltage–time curves registered during galvanostatic ano-
dising of EN AC-46500 cast aluminium alloy in 5 vol.- Polished samples were submitted to the chemical
%H2SO4 electrolyte at 0uC and 5?0 A dm22 for 30 min pretreatment and the anodising process. V–t transients
obtained during anodising of these surfaces (Fig. 8) showed
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Wear resistance that polishing had an effect on the voltage evolution. Thus,
in comparison with non-polished surfaces, no changes on
Wear resistance of anodic layers formed under different
the voltage corresponding to region I were observed, as
experimental conditions was evaluated using a ball on
mechanical treatment does not modify the composition of
disc tribometer (Table 1). The results showed that at
the surface, and because of this, the effect of the air formed
5?0 A dm22 anodising current density, wear resistance
oxide film. However, a slight enhancement of the maximum
was improved with decreasing H2SO4 concentration,
corresponding to the breakdown of the barrier layer
temperature and anodising time. In all the cases, except
(y37 V) (region II) was observed, suggesting a more
at the highest anodising time studied (90 min), the wear
resistive behaviour associated with a higher thickness and/or
resistance was better than that of the substrate, which
compactness of the barrier layer.
indicates that the poor wear characteristics of EN AC-
The pretreatment of the aluminium surface also
46500 cast alloy can be improved by anodising under
influenced the morphology and structure of the resulting
certain experimental conditions.
AAOL. Thus, it can be seen (Fig. 9) that after me-
On the other hand, the results showed that, in
chanical pretreatment, more compact films with some
general, the wear rate of the films changed following the
3D structures were obtained. No cracks were detected
same tendency as the microhardness measurements.
and the roughness of the surface was lower than that of
However, in some cases, samples with similar micro-
non-polished samples (Table 2). However, polishing had
hardness values lead to different wear resistance re-
a negative effect on the efficiency of the process and
sponses. This could be attributed to the fact that the
films with ,50% of the thickness were obtained,
microhardness measurements were performed at micro-
indicating that current losses due to other processes,
scopic scale and therefore only local regions of the
such as oxide dissolution and/or oxygen evolution, were
anodic layer were evaluated. On the contrary, the
higher on the polished surfaces, probably due to changes
determination of wear resistance involves a bigger test
in the structure, thickness and reactivity of the barrier
area and as a result, the wear resistance values are
and porous alumina layer. Moreover, instead of what
mostly dependent on the presence of defects such as
was expected, compactness of the film did not lead to a
porous and cracks.
significant improvement in the film hardness and wear
resistance.
Mechanical pretreatment effect
In order to improve the quality of the anodic oxide
layers obtained, aluminium samples were submitted to a
Conclusions
mechanical polishing to a mirror-like finish before Sulphuric acid anodising of EN AC-46500 cast alloy
the chemical pretreatment. By the application of this was studied in order to determine the optimal experi-
polishing, the surface roughness Ra of the samples was mental conditions. The high content and variety of
reduced from 0?68¡0?02 mm (without polishing) to alloying elements were responsible for disrupting the
0?05¡0?01 mm (after mirror-like finish). classical porous morphology and changing the typical

Table 1 Thickness, microhardness and wear rate of several anodised samples

Operating conditions Thickness/mm Microhardness/HV K/61026 mm3 N21 m21

EN AC-46500 substrate … 140¡10 446¡20

5 vol.-%H2SO4, 0uC, 5.0 A dm22, 30 min 36.7¡3.2 370¡92 9¡2
15 vol.-%H2SO4, 0uC, 5.0 A dm22, 30 min 39.1¡3.3 319¡71 65¡13
15 vol.% H2SO4, 0uC, 5.0 A dm22, 90 min 90.5¡4.5 218¡52 587¡23
15 vol.-%H2SO4, 20uC, 5.0 A dm22, 30 min 30.5¡3.4 227¡44 95¡19

318 Transactions of the Institute of Metal Finishing 2011 VOL 89 NO 6

 Gastón-Garcı́a et al. Sulphuric acid anodising of EN AC-46500 cast aluminium alloy

Table 2 Thickness, microhardness and roughness of 9. L. Zaraska, G. D. Sulka, J. Szeremeta and M. Jaskula: Electrochim.
anodised samples after different pretreatments Acta, 2010, 55, 4377–4386.
(5 vol.-%H2SO4, 0uC, 5?0 A dm22, 30 min) 10. H. Habazaki, K. Shimizu, P. Skeldon, G. E. Thompson, G. C.
Wood and X. Zhou: Trans. Inst. Met. Finish., 1997, 75, 18–23.
Pretreatment Thickness/mm Microhardness/HV Roughness/mm 11. X. Zhou, H. Habazaki, K. Shimizu, P. Skeldon, G. E. Thompson
and G. C. Wood: Corros. Sci., 1996, 38, 1563–1577.
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