International Journal of Adhesion & Adhesives 30 (2010) 595–601

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International Journal of Adhesion & Adhesives

journal homepage: www.elsevier.com/locate/ijadhadh

Influence on the strength and aging resistance of aluminium joints by laser

pre-treatment and surface modification
Rico Rechner a,n, Irene Jansen b, Eckhard Beyer a,b
a
Institute of Surface and Manufacturing Technology, George-Bähr-Str. 3c, 01069 Dresden, Germany
b
Fraunhofer Institute for Material and Beam Technology, Winterbergstr. 28, 01277 Dresden, Germany

a r t i c l e in fo abstract

Article history: This paper describes the pre-treatment of the wrought aluminium alloy AW 6016, which is mainly
Accepted 25 May 2010 employed in automotive car body manufacturing to reduce the weight. The major focus is on surface
Available online 9 June 2010 pre-treatment using laser to examine the influence of selected pre-treatment parameters on the
Keywords: strength and aging resistance of the bonded joint. The laser procedure presented is compared with
Epoxy/epoxides surface pre-treatments on the basis of the wet-chemical deposition of a TiZr oxide layer and
Aluminium and alloys atmospheric pressure plasma (AP-plasma) treatment. The pre-treated surfaces were characterised using
Surface treatment SEM–EDX, FTIR spectroscopy and XPS methods. Laser pre-treatment helped improve cleaning the
Laser surfaces and modify the oxide layer at the same time. The improvements resulted in better tensile shear
X-ray photoelectron spectroscopy
strength of the bonded joint before and after aging.
Fourier transform infrared spectroscopy
& 2010 Elsevier Ltd. All rights reserved.
Energy-dispersive X-ray spectroscopy

1. Introduction ensures corrosion protection of the aluminium in connection with

The surfaces of light metals consist of oxides and hydroxides;
the surface of magnesium consists also of carbonates [1]. Layers of
water and various contaminations (dirt, corrosion inhibitors and
lubricants) can be found. The creation of long-term stable
aluminium alloys requires surface pre-treatment to provide a
reproducible ground [2–6]. Long-term stable bonded joints are
mostly realised by wet-chemical processes, such as pickling,
anodising and formation of passive layers. Dry blasting processes
(e.g. sandblast coating, dry ice blasting) and atmospheric pressure
plasma treatment are increasingly employed [7–9]. In addition to
the expected cleaning effect, earlier experimentation had already
shown a magnesium deficiency at the surface of pre-treated
AlMg3 alloys [10–12]. Long-term tests showed that there is a
relation between the magnesium content and the aging behaviour
of adhesive aluminium bonds [13]. It is assumed that the reduced
magnesium content modifies the electrochemical potential of the
surface and thus improves corrosion resistance.
The EU Directive 2000/53/EC (End-of-Life Vehicles Regulation)
states that since 2007, the automobile industry must not use
hexavalent chromium compounds anymore [14]. For this reason
alternative pre-treatment methods without hexavalent chromium
are being developed. One of the alternatives is the large-area
deposition of TiZr conversion coatings in the rolling mill, which
n
Corresponding author. Tel.: +49 351 463 39639; fax: + 49 351 37755.
E-mail address: Rico.Rechner@iof.mw.tu-dresden.de (R. Rechner).
oil-based or dry lubricant layers. However, this limits the range of
suitable adhesives at the same time because the absorption or
displacement of the lubricant layers by the adhesive used must be
ensured. The best results for bonding on lubricant layers will be
obtained with hot-curing epoxy adhesives [15]. On the other
hand, the use of hot-curing adhesives is neither desirable nor
technically feasible for all applications. For example, the different
thermal expansion coefficients of the joining partners have to be
duly considered in the adhesive process of alloys or mixed
compounds to avoid internal stresses in the bondline. Another
essential parameter is the temperature resistance of the chosen
materials. The material-specific limit for fibre-reinforced compo-
sites (GRP, CFRP) is approximately 80–120 1C. This excludes the
use of hot-curing adhesives with a typical application tempera-
ture range of 150–180 1C. In these cases, systems of cold-curing
adhesives are more beneficial. The requirements made on the
pre-treatment of the surface of the joining parts are higher, as a
result. The tensile shear strength values for cold-curing adhesives
are low for bonding processes on corrosion inhibitor oils. For
bonding processes on dry lubricants no cold-curing adhesives are
known. It is therefore necessary to pre-treat the surface and
remove all lubricant layers.
Laser application can be an alternative for the dry pre-
treatment of aluminium surfaces [16–18] and other lightweight
materials (e.g. titanium, magnesium) [19,20]. With the selective
and reproducible method, all types of organic and inorganic
impurities can be removed on the surface. During laser pre-
treatment above the material-specific threshold value for the

0143-7496/$ - see front matter & 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijadhadh.2010.05.009
596 R. Rechner et al. / International Journal of Adhesion & Adhesives 30 (2010) 595–601
ablation of aluminium, the metal surface is subjected to short-
time melting and immediate cooling, which produces a dendritic
structure of the metal surface [21]. XPS testing of the aluminium
surface confirms the reduction of the magnesium content and the
carbohydrate compounds in the boundary layer [22]. All com-
mercial laser systems, ultraviolet to infrared, are suitable for laser
treatment [17,23,24]. For the parallel removal of organic layers
and inhomogeneous oxide layers Q-switched Nd:YAG lasers are
recommended. The optional beam guidance through flexible glass
fibres additionally offers the chance to combine pre-treatment
and automatic adhesive deposition [25,26].
In former investigations it was already proved that the laser
pre-treatment represents an effective procedure for the prepara-
tion of bonding surfaces. However, the interaction between laser
irradiation and material surface was analysed so far only
inadequately. This interaction will be analysed more closely in
this paper. First of all suitable laser parameters are selected for
the cleaning of oiled aluminium sheets and studied in terms of
their effect. Then the influence on the topography and chemical
composition of the aluminium surface is analysed. The concluding
tensile shear strength investigations show the effect of the laser
pre-treatment on the component strength of bonded aluminium
sheets (AW 6016). The procedure is directly compared with
conventional pre-treatment and atmospheric pressure plasma
pre-treatment. The tensile shear strength investigation is carried
out before and after various aging procedures.
2. Experimental
2.1. Pre-treatment techniques
In the laser tests, an Nd:YAG (l ¼1064 nm) laser of the type
CLA 050 manufactured by Clean-Lasersysteme GmbH was used. It
has a mean output power of 0–120 W (pulsed or cw) and a
continuous frequency range of 8–40 kHz. Owing to the short pulse
duration of few nanoseconds, a pulse maximum power of 120 kW
can be attained.
The laser power is coupled into a glass fibre immediately after
the resonator. The fibre ensures the quasi-lossless transmission of
the laser power even over long distances until it reaches the
workpiece [27]. At the place of processing, the laser beam is
decoupled from the fibre and projected onto the surface through a
2D scan head with built-in F-theta lens (f ¼100 mm). The range of
processing speeds is 0–4000 mm/s. The beam profile, after having
passed through the fibre, follows the continuous uniform
distribution that is also called top hat distribution. The beam
section is round and the beam size in the focus is 357 mm. The
pulse frequencies and thus the resulting laser intensities were
Table 1
Laser parameter (LP) for fibre-coupled laser processing.
Laser parameter (LP) 1 2
pulse intensity (W/m2) 1.73  1011
Table 2
Choice of materials.
Variant Type of material
A AW 6016
B AW 6016
varied on the specimen surface with full power and a fixed
average scan speed (Table 1).
For the sake of comparison, atmospheric pressure plasma
pre-treatment tests using an AP-plasma system by Plasmatreat
were conducted. A single nozzle was used for selective
pre-treatment. All tests were carried out for maximum system
output. The gas medium used was pressurised air and the specific
air flow rate (up to 2000 l/h) depends on the plasma nozzle. The
tests used different nozzle heads (standing, rotating) at varied
movement speeds (1–20 mm/min), nozzle–substrate distances
(3–10 mm) and pre-treatment widths (1–5 mm). Best results
could be achieved with a standing nozzle at a movement speed of
1 mm/min, a nozzle–substrate distance of 6 mm and a
pre-treatment width of 3 mm. These parameters were used for
the pre-treatment of the plasma specimen shown in Fig. 11.
2.2. Materials selection
The wrought aluminium alloy AW 6016 has been chosen for
experimentation (Table 2). The tensile shear specimens had the
dimensions (w  h  d) 100  25  1.6 mm3 and thus were in
accordance with ISO standard 4587. For reference bondings
(variant A), the TiZr coating Gardobonds X 4591 was applied to
the specimens, before the corrosion inhibitor oil Anticorit RP 4107
RV (by Fuchs) was deposited on top. The TiZr coating is not
applied on the specimens with laser and plasma pre-treatment,
the coating is replaced by the chosen laser or plasma process
(variant B).
2.3. Analytical techniques
XPS, FTIR spectroscopy and SEM–EDX methods were used to
characterise the surface.
XPS tests were conducted at a take-off angle of 451 using
non-monochromatized Al Ka radiation on a ESCA 5700 (Physical
Electronics). With a calibrated (SiO2/Ta2O5) sputtering rate the
surface was removed at about a rate of 1 nm/min using Ar ions to
be able to analyse deeper layers. For the final interpretation of the
measured values, the spectra were normalised to the contamina-
tion carbon peak at 285.0 eV. For the XPS analysis a specimen
(50  25  1.6 mm3) with small fields of about 10 mm2 for each
laser parameter and reference was prepared and measured
shortly after laser pre-treatment.
For the FTIR measurements, an IRspecXL (Fraunhofer IWS) at
grazing incidence (y ¼731) with p-polarised light in a wavenum-
ber range of 6000–500 cm  1 and for a fixed measuring dot size of
0.8 mm  1.5 mm was used. The spectra were recorded in
specular reflection mode with a DTGS-detector. An Au-mirror
was used for the reference signal.
3 4 5
2.10  1011 2.66  1011 3.48  1011 4.42  1011
Manufacturing method Surface properties/additives
Rolled TiZr+ anti-corrosion oil Anticorit RP 4107 LV
Rolled Anti-corrosion oil Anticorit RP 4107 LV
 R. Rechner et al. / International Journal of Adhesion & Adhesives 30 (2010) 595–601 597

A JSM 6400 with LaB6 cathode (by Jeol) was used for the 3. Results and discussion
SEM–EDX measurements. The images were made at an accelera-
tion voltage of 10 kV by scanning the surface with variable 3.1. Surface analysis
resolutions (3–500 mm). The secondary electron contrast (surface
topography) and the back scattered electron contrast (material Fig. 1 shows the results of an X-ray spectroscopy (XPS)
contrast) were used to image the sample surface. The element conducted with the aluminium alloy AW 6016. The normalised
composition was assessed using additional X-ray analysis for representation of the spectra between 0 and 1100 eV shows – on
selected magnifications (100:1, 500:1, 1000:1). the basis of the reference value – the modified composition of the
For the bonding tests, the hot-curing epoxy adhesive Betamate elements carbon, oxygen and aluminium after the laser pre-
1496 (Dow Automotive, lot no. 279844) a commonly used treatment. Table 3 gives a quantitative elemental analysis for the
adhesive in car body construction was chosen. The preheated investigated parameters. Carbon contamination decreases with
adhesive (50 1C) was applied with a spatula from both sides onto increasing laser intensity, while the measured oxygen content
the surfaces of the preheated samples (50 1C). Due to the increases. Only small amounts of aluminium can be detected on
unpredictable influence of spacers (e.g. in aging) the reproduci- the reference surface due to the heavy contamination. The related
bility of the bondline thickness was controlled by the amount of peaks for aluminium can be located on the laser pre-treated
the applied adhesive and a defined contact pressure using clamps. specimen surfaces. A change of intensity between the individual
The specimens were fixed after the joining process and then cured parameters cannot be measured. However, the quantitative
at 180 1C for 30 min. To ensure statistical reliability, a series of 5 elemental analysis shows an increase from 10.3% to 18.7%.
specimens was bonded for each parameter. Before the test cycle The additional layer removal by 5 nm through an Argon ion
was continued, all samples were conditioned at room tempera- sputtering process and the subsequent measurement (Fig. 2,
ture for 24 h and at 40 75% relative humidity. Table 4) of the exposed layers further show that the reference
Following ISO 9227, the specimens were subjected to aging in specimen surface is considerably contaminated by the deposited
the salt spray test for selected periods of time (1000 and 2000 h). corrosion inhibitor oil which in all probabilities immediately
A salt spray chamber of the type SC/KWT 450 (Weiss Umwelt- diffuses over the exposed area because of the low viscosity. The
technik GmbH) was used for the tests. The specimens were measured carbon content of the laser pre-treated specimens is
arranged in the chamber at an angle of 201 to the perpendicular. negligible. However, the presence of aluminium and oxygen on
After aging, the specimens were temporarily stored at room the specimen surface increases. The intensity detected remains
temperature and at 40 75% relative humidity for 24 h to ensure a nearly constant. Differences between the laser parameters cannot
comparable initial state without a full re-drying. be measured.
Before the lab aging process, some of the specimen series were The XPS results are confirmed by FTIR spectroscopy (Fourier
completely sealed in an electrophoretic deposition process (EPD) transform infrared spectroscopy) measurements. Fig. 3 shows the
to model the typical bonding and paintwork on bonded mid-infrared spectrum of 2700–3000 cm  1. The extent to which
components in the automobile industry. A dualscope MP40/probe
ED10 (Fischer) was used to determine the thickness of the
Table 3
deposited varnish layer in the eddy current mode and was found
Quantitative elemental analysis.
to be 24 mm.
The specimens were tested in a testing machine of the type Specimen Elements (at%)
Zwick/Roell Z050 to determine the tensile shear strength. The test
C O Al O/Al
speed was 10 mm/min. The load cell KAP-TC employed is suitable
for forces of up to 20 kN. The specimens were arranged Reference 84.1 12.1 1.3 9.1
symmetrically between the grips. The minimum distance LP1 52.8 28.8 10.3 2.8
between the grip and the nearest edge of the single lap joint LP2 43.0 34.0 14.3 2.4
was 50 mm according to ISO 4587. LP3 41.0 37.6 14.1 2.7
LP4 35.2 40.5 16.8 2.4
LP5 30.1 42.7 18.7 2.3

Fig. 1. XPS measurement of AW 6016. Fig. 2. XPS measurement of AW 6016 after sputtering of 5 nm.
598 R. Rechner et al. / International Journal of Adhesion & Adhesives 30 (2010) 595–601

Table 4
Quantitative elemental analysis after 5 nm argon sputtering.

Specimen Elements (at%)

C O Al O/Al

Reference 55.1 22.9 17.5 1.3

LP1 13.4 42.9 35.0 1.2
LP2 10.5 45.4 33.0 1.4
LP3 4.4 45.3 34.8 1.3
LP4 3.8 47.5 34.9 1.4
LP5 3.6 48.1 34.6 1.4

Fig. 3. FTIR spectrum of AW 6016.

the surface is contaminated with organic substances (such as oils

or fats) can be confirmed by the absorption of the measured signal
in the symmetric and asymmetric hydrocarbon compounds. The
changing reflection for increasing intensities in the range of
Fig. 4. Secondary electron (a) and back scattered electron (b) contrasts of AW
2850–2960 cm  1 reflects the cleaning effect of the laser pre- 6016 reference surface.
treatment. In the spectra recorded for parameters 4 and 5, the
characteristic CH bands are no longer discernible. The
contamination of the surface is almost completely removed.
The untreated aluminium surface is not only contaminated by
lubricants but also by other elements (e.g. Fe). Fig. 4 shows part of
the reference surface of the alloy AW 6016 in the secondary
electron and back scattered electron contrast of an SEM–EDX. The
secondary electron contrast displays not only the surface
morphology but also particles that appear even more clearly in
the back scattered electron contrast thanks to the light and dark
colouring, respectively.
An EDX measurement can be additionally performed to
ascertain the exact element composition (Fig. 5). The
spot-measurement on the highlighted particle seen in the
middle of the back scattered electron contrast detected a high
iron level in the composition of the largest particle. This is
presumably a metal filing rubbed off the cutting edge of the tool
during cutting. The smaller particles characterise accumulations
of organic contaminations.
After laser pre-treatment, the visible organic and inorganic
contaminations are completely removed from the surface. The Fig. 5. EDX analysis of the reference surface element composition.
secondary electron contrast also makes visible how the original
surface topography changed (Fig. 6), from which one may The cleaning effect of the laser pre-treatment (LP5) can be seen
conclude that these stem from near-surface partial melting also in the EDX mode as the modified element composition and
(Fig. 7). intensity (Fig. 8). The organic and inorganic contaminations on
 R. Rechner et al. / International Journal of Adhesion & Adhesives 30 (2010) 595–601 599

Fig. 6. Untreated and laser pre-treated (LP5) surface in secondary electron Fig. 8. EDX analysis of LP5 pre-treated surface.
contrast.

Fig. 9. Partial melting (LP5) in the high-resolution secondary electron contrast.

the surface are minimal. The base material can be clearly

Fig. 7. Secondary (a) and back scattered electron (b) contrasts after pre-treatment identified as a marked aluminium peak during the measurement
with LP5. on the cleaned surface.
600 R. Rechner et al. / International Journal of Adhesion & Adhesives 30 (2010) 595–601
Fig. 10. EDX analysis of area with partial melting.
Fig. 11. Tensile shear strength for AW 6016 bonded with Betamate 1496.
Fig. 12. Failure patterns.
The high-resolution secondary electron contrasts clearly reveal
the punctual meltings on the pre-treated aluminium surface
(Fig. 9).
The subsequent EDX test (Fig. 10) shows (oxygen peak) that
around the area of partial melting clearly more oxygen is
absorbed than in areas without surface changes. Thus, it is
evident that the laser changes the native aluminium oxide layer.
We expect that the short temperature entry through the laser
pulse cause a thermal oxidation. The analytical methods
employed can, however, not eventually identify the quantity
and quality of the resulting oxide layer.
3.2. Tensile shear strength
Fig. 11 shows the results of the subsequent bonding. The
drawn error bars represent the standard deviation of the tested
samples. The specimens produced were tested either immediately
after conditioning or after the aging procedure and subsequent
conditioning. The unaged specimens, which were subjected to
plasma and laser pre-treatment (LP5), displayed 14% and 20%
improvement of the tensile shear strength in the test, the exact
value depending on the pre-treatment process.
There is no evidence that the atmospheric pressure plasma
pre-treatment improved the strength of the EPD-passivated,
tensile shear specimens after 1000 and 2000 h of salt spray
testing, respectively. The strength values measured were approxi-
mately the same as those for the reference samples. On the other
hand, the EPD-passivated specimens showed better strength
values after laser pre-treatment and after salt spray aging. The
strength values obtained here were 26% and 15%, respectively,
above the measured reference values. The effect of both plasma
and laser pre-treatment was particularly obvious for specimens
without the protective EPD coating which had also been subjected
to lab aging in a salt spray chamber for 1000 h. While the
reference specimens had only a residual strength after aging,
AP-plasma and laser pre-treatment gave markedly higher values.
All unaged tensile shear specimens failed due to cohesive
failure of the adhesive (Fig. 12). After aging, adhesive failure
 R. Rechner et al. / International Journal of Adhesion & Adhesives 30 (2010) 595–601
started to prevail and increased depending on the duration and
the intensity of the aging process. The resistance to aging
depended on the chosen type of surface pre-treatment. Both
atmospheric pressure plasma pre-treatment and laser pre-treat-
ment demonstrated visible improvements. After 1000 h of salt
spray testing, the reference specimens showed adhesive failure on
one side over the entire bonding area. The bonded joints of the
plasma pre-treated specimens, however, displayed adhesive
failure alternating on both sides, and the laser pre-treated
samples showed adhesive failure only along the edges.
The related failure patterns thus confirmed the results of the
strength measurement.
The high-resolution secondary electron contrasts clearly reveal
the punctual meltings on the pre-treated aluminium surface
(Fig. 9).
4. Conclusions
This paper examines the laser pre-treatment of the wrought
aluminium alloy AW 6016 in comparison with the atmospheric
pressure plasma pre-treatment and the surface pre-treatment on the
basis of the wet-chemical deposition of a TiZr layer. First of all suitable
laser parameters were selected and tested. Afterwards, cleaning effect,
topography and chemical composition have been determined on the
pre-treated surfaces. Surface characterisation methods, such as XPS,
FTIR spectroscopy and SEM–EDX confirmed the influence of laser pre-
treatment on surface contaminations and the oxide layer.
An additional increase of the oxygen content at the aluminium
surface could be observed during the analyses. It is assumed that
the interaction with the material causes the formation of a
thermal oxide layer. The oxygen content grows with increase in
the laser intensity. The maximum values were achieved with the
most intensive laser parameter LP5. Simultaneously, the material
removal grows with increase in the laser intensity. Through the
laser pre-treatment a crater-similar structure forms by itself at
the surface. Compared to the geometrical surface of the
component the true surface is extended.
It is known that a diffusion of the adhesive into the porous
oxide layer improves the bonding strength. Furthermore, the
boundary layer between metal and adhesive is shifted into the
porous oxide layer. Both effects are used during the anodic
oxidising of aluminium to improve the bonding surface.
The influence of laser pre-treatment onto the thermal oxida-
tion layer and resulting bonding strength could not be definitively
clarified. The effects of oxide layer formation and surface
enlargement overlap through the simultaneous change of the
surface structure. Laser parameter LP5 shows the highest tensile
shear strength results but also a heavy structured surface. The
influence of the oxide layer onto the bonding strength must be
clarified in further investigations.
Cleaning and oxide deposition had a beneficial effect on the
strength and resistance of the tested adhesive bonds against the
corrosive attacks in the salt spray tests. The tensile shear strength
values obtained for unpassivated adhesive bonds after aging were
much higher than the values obtained for the wet-chemical
deposition of a TiZr oxide layer or the atmospheric pressure
plasma pre-treatment. The failure patterns confirm the improved
resistance to corrosive media on the basis of less adhesive failures
in the bondline of the laser-pre-treated tensile shear specimens.
The laser pre-treatment shows that the technique is suitable
for the reliable cleaning of oiled sheet metals. Considering the
tensile shear strength results with hot curing adhesives we expect
that the laser pre-treatment advantages for surface preparation
(e.g. lubricant removal) are in particular useful for bonding
processes with cold curing adhesives.
601
Acknowledgements
The research was financed by budgetary means of the Federal
Ministry of Economics and Technology (BMWi) through the
German Federation of Industrial Research Associations (AiF
no. 14780 BR) and supported by the Society for Chemical
Engineering and Biotechnology (DECHEMA). The authors would
like to thank for this support and for the helpful cooperation
between all participants in the project committee.
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