International Journal of Adhesion & Adhesives 23 (2003) 6979

Dry ice blasting as pretreatment of aluminum surfaces

to improve the adhesive strength of aluminum
bonding joints
F. Elbinga,*, N. Anagrehb, L. Dorna, E. Uhlmanna
a

Institute for Machine Tools and Factory Management, Technical University Berlin, Pascalstr. 8-9, Berlin 10587, Germany
b
Materials and Metallurgical Engineering Department, Al-Balqa Applied University of Al-Salt, Jordan
Accepted 3 December 2002

Abstract
The manifold application possibilities of dry ice blasting were presented several times already. This contribution summarizes the
results of an experimental study on the pretreatment of bonding surfaces for aluminum components. Alongside the removal of
disturbing lms of lubricants, impurities, and oxides, aluminum surfaces are pretreated chemically and mechanically so as to
increase the adhesive strength signicantly. The increase of the adhesive strength by up to 99% for epoxy and 27% for polyurethane
glues elucidate the suitability for automobile, airplane, and railway vehicle manufacture.
r 2003 Elsevier Science Ltd. All rights reserved.
Keywords: A. Epoxy; A. Polyurethane; B. Aluminum; B. Surface modication; SIP; Dry ice blasting

1. Introduction
To guarantee the optimal adhesive strength of glues as
well as the long-term endurance of the adhesive
bonding, grease lms, preservative oils, and impurities
deposited on aluminum surfaces must be removed.
Moreover, the oxide lms on the aluminum surface must
be stable, and must have sufcient adhesive strength to
the base material. In the automobile industry and in
railway vehicle manufacturing, aqueous and solventbased cleaners as well as chemical and mechanical
pretreatment methods have been used so far. The
disadvantage of these methods is that the cleaning and
blasting agents as well as caustics applied must be either
disposed of in a cost-intensive way or recycled.
Furthermore, the chemicals, solvents, and aqueous
cleaners used are hazardous to the health of the staff
and the environment. Due to dust development,
compressed air blasting with solid blasting agents may
also endanger the health of the staff. Further disadvantages of this method are the residues of the blasting
*Corresponding author. Tel.: +49-30-314-23349; fax: +49-30-31425895.
E-mail address: elbing@iwf.tu-berlin.de (F. Elbing).

agents on the surface, which can only be removed by

means of an additional degreasing. In the case of
chemical etching, surfaces have to be rinsed with water
and dried subsequently.
The disadvantages listed above do not apply to dry ice
blasting, which is considered an environment-friendly
method. Moreover, dry ice blasting is a mild pretreatment method, since the dry ice pellets are relatively
soft in contrast to corundum and duroplast, thus
causing only slight damage to the surface and the fringe
area.
This contribution reports on the surface pretreatment
of aluminum components by dry ice blasting as well as a
process optimization for the enhancement of the
adhesive strength of industrial epoxy and polyurethane
glues on aluminum surfaces. The pretreated aluminum
surfaces will be examined in terms of structure, roughness, and chemical composition under variation of the
most important pretreatment parameters and compared
with other pretreatment methods. The adhesive strength
of the bonded aluminum components is determined
according to EN 1465 with single-lap shear tension tests.
For the investigation of the fracture behavior, the
structure and the chemical composition of the fracture
surface are analyzed.

0143-7496/03/$ - see front matter r 2003 Elsevier Science Ltd. All rights reserved.
doi:10.1016/S0143-7496(02)00083-0

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

70

Nomenclature
a
Al
C
c
Ca
Cl
d
EDX
EP 1
EP 2
F
Fe
IPS
lu.
Mg

workpiece distance, mm
aluminum
carbon
chemical concentration, %
calcium
chlorine
glue lm thickness, mm
energy dispersive X-ray microanalysis
two-component epoxy glue Araldite 2011
two-component epoxy glue Permabond E 32
shear tension testing force, N
iron
ice pellet size, mm
overlapping length, mm
magnesium

2. Present state of knowledge

Considerable enhancement of the adhesive strength of
glues on aluminum surfaces can be achieved by
compressed air blasting with solid blasting agents such
as corundum and duroplast [1,2]. However, this method
is time-consuming since the surfaces must be cleaned
before and after blasting. The aim of the degreasing of
surfaces before blasting is to avoid the fast contamination of the blasting agent and to increase the efciency
of blasting, whereas the subsequent cleaning serves for
the complete removal of blasting agent residues that
may reduce the adhesive strength. The results of longterm tests on adhesive joints under extreme conditions,
such as increased air humidity, have shown that the
long-term endurance achieved still falls short of the
requirements of the automobile and railway vehicles
manufacturing [3]. Furthermore, the developing waste
products of solvents and aqueous cleaners may pose
hazard to the environment and to people, thus generating additional costs. The blasting agent used must be
recycled too, which leads to increased pretreatment
costs.
After the optimization of pretreatment parameters
and attuning them to the glues and adherents, the
pretreatment of aluminum surfaces with chemical
methods provokes a signicant improvement of the
adhesive strength as well as a sufcient long-term
endurance [3,4]. The impact on the environment through
noxious emissions, a possible contamination of the
ground water, the health hazard to the staff as well as
the cost- and time-consuming pretreatment fall short of
the industrial requirements of the automobile and
railway vehicles manufacturing.
Environment-friendly pretreatment methods include
the treatment with excimer laser [5], CO2-laser [6,7],

Mn
O
Pt
PU
Ra
RzDIN
S
s
SEM
Si
SIP
t
Ti
v

manganese
oxygen
prole depth, mm
two-component polyurethane glue Tivopur
1667
arithmetical mean deviation of the prole, mm
mean roughness, mm
sulfur
standard deviation, mm
scanning electron microscope
silicon
cleaning and bonding agent, SIP (self indicating pretreatment)
material thickness, mm
titanium
feed speed, m/min

electric arc treatment [8] and cyroblasting [9]. The

pretreatment with excimer laser provides an excellent
long-term endurance, which is partly better than the
results of the chemical and electro-chemical methods [5].
The CO2-laser treatment of aluminum surfaces leads to
a considerable increase of the adhesive strength in the
case of thermosetting single-component epoxy glues
[6,7]. After the bombardment of the surfaces with
carbon-dioxide snow (cryoblasting), the adhesive
strength is similar to the one after the pretreatment of
aluminum surfaces with solid blasting agents and
primary coat [9]. The bonding improvements and longterm endurance achieved on aluminum surfaces treated
with electric arc correspond to the results of the
chemical pretreatment and the blasting with solid
blasting agents [8].
A further eco-friendly method is dry ice blasting, so
far used for de-coating of metals and plastics [10],
cleaning pipelines [11], removing old silicon gaskets
from crankcases [12] as well as for cleaning machines
and plant. First feasibility studies are available in terms
of the pretreatment of aluminum, steel, and plastic
surfaces with the aim to increase the adhesive strength of
glues on these surfaces [13].

3. Dry ice blasting

The mechanism of dry ice blasting is based on a
thermal, a mechanical, and an expansive effect. The
thermal effect is caused by the impact of the dry ice
pellets of a temperature of
78.51C, which make the
surface cool down. This leads to a loss of elasticity as
well as to embrittlement and to the shrinkage of the
adherent impurity and oxide layers under the development of cracks. These layers detach from the base

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

material after exceeding the adhesive energy. This is due

to the different thermal expansion coefcients of the
impurity and oxide layers and the base material. The
layers partially chip off and are removed by the kinetic
energy of the dry ice pellets and the compressed air
stream. The abrupt volume increase by a factor of 800
during the sublimation of the dry ice pellets supports the
process [14]. The dry ice pellets are of a hardness of
23 Mohs. This classication corresponds to the hardness of calcium sulfate (2 Mohs) and calcium carbonate
(3 Mohs), respectively. Due to the small hardness
compared with other blasting agents such as corundum
and duroplast, the process parameters of different
materials to be cleaned can be chosen in a way that no
surface and fringe area damages occur to the component
[15].
Solid dry ice pellets are used as blasting agent, which
sublimate in the moment of the impact on the surface.
The production basis of the blasting agent is liquid
carbon dioxide, which is a byproduct of ammonia
production, oil and gas renery, and ethanol production
as well as a volcanic natural product [16]. Dry ice snow
develops in the course of the relief of the carbon dioxide
to a pressure of 1 bar at the temperature of
78.51C. In
a pelletizer, this snow is pressed through a mold with the
help of a hydraulically driven plunger. The results are
cylindrical dry ice pellets of a diameter of 3 mm and a
length of 515 mm [17].

4. Experimental set-up and conditions

The experimental equipment used at the Technical
University Berlin comprises a compressed air supplier
and treatment system, a blasting machine, an enclosed
machining space, a 6-axis industrial robot for the

guidance of the jet nozzle, a machining table for the

clamping of the aluminum samples, and an air extraction system with a particle lter (Fig. 1). The compressed air supply of the company Kaeser
Kompressoren GmbH consists of a DSB 170 stationary
single-stage screw compressor, an equalizing vessel with
a volume of 0.5 m3, an Eco-Drain 13 steam trap and an
FX lter element for the segregation of micro-particles
and water. The blasting plant Tornado Jet of the
company Green Tech GmbH & Co.KG, Hofolding,
transports the blasting agent according to the pressure
principle. A laval nozzle with an outlet diameter of
14 mm was used to accelerate the dry ice pellets. The
pellets are stored in a storage tank and are injected into
the compressed air stream by a metering disc. By means
of the laval nozzle, the dry ice pellets are accelerated
with the compressed air stream at a jet pressure of
312 bar and a volume stream of maximum 15 m3/min.
Fig. 2 shows the relevant parameters for the pretreatment of the bonding surface. The most important
settings of dry ice blasting are the jet angle, feed speed,
the working distance between jet nozzle and aluminum
surface, jet pressure, and the mass ow of the dry ice.
Further important parameters are properties of the dry
ice pellets, such as density, hardness, shape, geometrical
measurements, surface nish, carbon dioxide content,
and age.
In the framework of the present technological
investigation, the feed speed v and the diameter of the
dry ice pellets, the so called ice pellet size (IPS) were
varied. The IPS can be 0.5 mm, and 0.1 mm in case of
applying a scrambler in the blasting plant. The jet angle
was kept constantly at 901 since the kinetic energy and
the jet momentum rise with increasing jet angle from 701
to 901 [14]. An optimal working distance of 150 mm was
dened for the laval nozzle and was not varied during

21

8
7

13

20

17

12

71

15
16

PI

19

6
10

18

14

5
3
4

compressing unit
1
2
3
4
5
6
7

air filter
screw compressor
oil trap
oil cooler
oil filter
pressure controler
air cooler

11

purification unit
8
9
10
11
12
13
14

dosing unit

adsorption dryer
refrigerating dryer
surge tank
steam trap
micro filter
dry ice tank
dosing disk

blasting unit
15
16
17
18
19
20
21

dry ice tank

mass flow controler
blasting hose
jet nozzle
6-axis robot
particle filter
exhaust ventilator

Fig. 1. Schematic depiction of the experimental equipment for the pretreatment with dry ice blasting.

72

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

plant parameters
- process principle
- blasting hose
(length, diameter,
roughness, posture)
- jet nozzle
(geometry, roughness,
material)
- pellet storage and
dosage

pellet parameters

setting parameters

material parameters

density
hardness
shape
geometry
surface finish
carbon dioxide content
age

jet angle
feed speed
working distance
jet pressure
dry ice mass flow
jet flow conditions
air humidity
air temperature

material type
coating
impurities
coating thickness
geometry
density
hardness
temperature

process parameters
- impact force
- blasting time
- cleaning / removal rate

- workpiece temperature
- carbon dioxide concentration
- sound level

tecnical and economic parameters

tecnical parameters
- accuracy (shape, dimension) - fringe zone impact
- rest impurities
- surface topography
- surface roughness
- chemical composition

economic parameters
- manufacturing cost
- quantities
- disposal cost

Fig. 2. Relevant parameters for the pretreatment of bonding surfaces with dry ice blasting.

the investigations, since the number of impinging dry ice

particles decreases with a working distance bigger than
150 mm [10]. This would considerably reduce the
efciency of the removal of greases, preservative oils,
and impurities. The possible maximum dry ice mass ow
of 100 kg/h and a jet pressure of 6 bar were set on the
plant.

5. Test materials
A 1 mm thick aluminum sheet of AlMg4,5Mn0,4
(Table 1) was used as metallic joint partner as used in
automotive engineering for body construction. The
glues were chosen under consideration of the requirements often placed in the automobile industry such as
cold setting, high strength, and deformability as well as
high temperature and aging resistance. Therefore, the
cold setting two-component epoxy glues Araldite 2011
(EP 1) and Permabond E 32 (EP 2) as well as the twocomponent polyurethane glue Tivopur 1667 (PU) were
used for the gluing of the aluminum sheets (Table 2).
According to the manufacturers instructions, both glues
are suited for gluing different materials such as plastic,
metal and ceramics and are applied in a wide range in
the industry.
In the state as received, the aluminum sheets were
covered with rolling oil and grimes, which provide a
poor adhesive basis for glues. The surfaces were
therefore pretreated with dry ice blasting to increase
the adhesive strength. As pretreatment parameters, feed
speed v and IPS were varied. Subsequently, the
pretreated aluminum surfaces were dried with hot air.
Preliminary investigations have shown that aluminum
samples are deformed during the dry ice blasting due to

the jet pressure and the cooling. This irregular deformation of the aluminum sheets results in an irregular glue
lm thickness which, above all in the case of epoxy
glues, leads to a signicant decline of the adhesive
strength. To guarantee a homogeneous pretreatment,
the aluminum samples were clamped at both sides on the
machining table leaving blank the surface to be blasted.
The aluminum surface of ca. 5 mm covered on the side
to be glued was cut off with guillotine shears after the
pretreatment. In some tests, the blasted aluminum
samples were additionally pretreated with SIP (self
indicating pretreatment), a cleaning and bonding agent
of the company Permabond. SIP contains three components (A,B,C) in a mixing ratio of 2:1:9. Component A
has a viscosity of 1.5 mPa s and consists of methanol
(1y5%) and ethanol (more than 50%). Component B
has a viscosity of 3.0 mPa s and consists of more than
50% Gamma-Glycidoxypropyltrimethoxysilan and less
than 0.5% methanol. Component C has a viscosity of
1.0 mPa s, the chemical composition is not specied. SIP
provoked a degreasing of the surfaces and an increase of
the adhesive strength between the base material and the
glue. After the application of SIP to the aluminum
surfaces, the samples were air-dried for a few minutes
and nally wiped with a sponge. This guaranteed a thin
lm of SIP.
The two-component glues EP 1, EP 2 and PU were
mixed manually. To avoid air pockets, the twocomponent epoxy glues were degassed for a few minutes
under vacuum and then applied to the aluminum sheets.
To maintain a uniform glue lm thickness of 0.08 mm,
copper wires of this diameter were inserted in the glue
joint and a special device of compression weights for the
xing of the aluminum samples after joining was
applied.

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

73

Table 1
Technical data and SEM images of the surface of the metallic joint partners
Material

Aluminum forgeable alloy

Manufacturer
Trade name
Chemical formula
Material thickness
Arithmetical mean deviation of the prole
Mean roughness
Prole depth
Chemical composition of the surface

VAW aluminium-Norsk Hydro

VAW 63/44
AlMg4,5Mn0,4
t 1 mm
Ra =0.4670.02 mm
RzDIN =2.3670.3 mm
Pt =3.2270.46 mm
cAl =85.75%, cMg =8.86%, cO =3.35%, cC =2.04%

Surface topography

Table 2
Technical data of the glues
Adhesive basis

Two-component epoxy resin

Brief description
Manufacturer
Trade name
Resin
Hardener
Mixing ration
Pot conditions
Processing
Hardening conditions

EP 1
Ciba
Araldite 2011
2011A
2011B
100:80 (m%)
85 min, 301C
Manual
30 min, 801C

The adhesive strength was determined by means of a

single-lap shear tension test according to EN 1465. The
samples were pulled with a test speed of 5 mm/min in
standard climate. 5 samples were investigated in each
test series from which the arithmetic mean adhesive
strength was calculated. For the investigation of the
topographic structure of the pretreated aluminum surface and the fracture surfaces, a DSM 950 electron
microscope (SEM) of the Zeiss company, Jena, was
used. An EDX-analysis was carried out to detect the
chemical composition of the aluminum surfaces before
and after dry ice blasting as well as of the fracture
surfaces. Furthermore, the surface roughness parameters Ra ; RzDIN and Pt were dened with a Hommel
tester 2000, a surface measuring system using a
digital gauge H009 TKL300/5. Hereby, 8 measurements
were carried out per sample according to EN ISO
4287, 4288, 3274 and 11562. The arithmetic average
of the single measurements was calculated and
standard deviations were dened to detect the surface
parameters.

6. Test results
Compared with the state as received, dry ice blasting
causes a slight change in surface topography. However,
a smoothing of the groove structure occurred with
decreasing feed speed independently of the IPS. Fig. 3

Two-component polyurethane resin

EP 2
Permabond
Permabond E 32
E 32 A
E 32 B
100:100 (vol%)
120 min, 201C
Manual
45 min, 601C

PU
Tivoli
Tivopur 1667
Tivopur 1667
Tivopur 1600/07
100:30 (m%)
14 min, 201C
Manual
48 h, 201C+3 h, 1001C

shows SEM images of the surfaces in a 500-fold

magnication, Fig. 4 in a 1000-fold magnication. The
groove structure is a consequence of the rolling process
during the production of the aluminum sheets. Furrows
occurred at some places after dry ice blasting, which
have no form structure. With decreasing feed speed and
smaller IPS, the furrows spread unevenly on the surface
are getting more pronounced. Oxide, lubricant, and
impurity lms of differing thermal expansion coefcients are deposited on the aluminum surface. The
aluminum samples were cooled down during dry ice
blasting. As a result, the different lms shrunk to
different extends and broke. Due to the high kinetic
energy of the dry ice pellets, impurity and lubricant lms
were removed rst, then the oxide lms below and part
of the base material. The impurity and the lubricant
lms have lower bond energies to the base material than
the oxide layers. Machining the aluminum samples with
a higher feed speed leads to less cooling and thus to a
smaller thermal inuence on the lms. The removal of
the layers through the kinetic energy therefore takes
place unevenly on the entire surface, causing the grainlike structure. This structure is more pronounced in the
case of an IPS of 0.5 mm than with an IPS of 0.1 mm. In
the case of high speed feed, the SEM images show spots
on the surface, which may have a negative effect on the
adhesive strength.
The roughness measurement (Table 3) shows that dry
ice blasting has only small inuence on the parameters

74

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

Fig. 3. SEM images (500-fold magnication) of the aluminum surfaces dependent on the pretreatment method.

Fig. 4. SEM images (1000-fold magnication) of the aluminum surfaces dependent on the pretreatment method.

of surface roughness. No signicant changes in surface

roughness could be stated in comparison with the state
as received. The same applies to degreasing with ethanol

in the ultrasonic bath. The aluminum surfaces pretreated with SIP have a slightly higher surface roughness
than the samples treated with dry ice blasting. In

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

75

Table 3
Arithmetical mean deviation of the prole, mean roughness and prole depth of aluminum surfaces with different pretreatment
Type of pretreatment

Ra 7s (mm)

RzDIN 7s (mm)

Pt 7s (mm)

Condition as delivered
Ultrasonic, degreased with ethanol
Degreased with SIP
Dry ice blasting, v 0:1 m/min, IPS=0.5 mm
Dry ice blasting, v 0:5 m/min, IPS=0.5 mm
Dry ice blasting, v 1:0 m/min, IPS=0.5 mm
Dry ice blasting, v 0:5 m/min, IPS=0.1 mm
Dry ice blasting, v 1:0 m/min, IPS=0.1 mm
Compressed air blasting with corundum
Compressed air blasting with duroplast

0.4670.02
0.4770.01
0.6070.02
0.4370.15
0.4270.11
0.4170.11
0.4370.07
0.4670.10
0.8970.05
1.3670.23

2.3670.33
2.3970.27
2.7470.19
2.3770.75
2.4070.40
2.2870.47
2.7770.46
2.6070.28
8.2370.88
12.9471.82

3.2270.46
3.5571.08
3.4970.41
3.2671.17
3.3871.10
3.3471.25
3.8170.94
3.5070.33
11.9671.64
18.4873.83

Table 4
Chemical composition of aluminum surfaces with different pretreatment
Type of pretreatment

Condition as delivered
Degreased with SIP
Dry ice blasting, v 0:1 m/min, IPS=0.5 mm
Dry ice blasting, v 0:5 m/min, IPS=0.5 mm
Dry ice blasting, v 1:0 m/min, IPS=0.5 mm
Dry ice blasting, v 0:1 m/min, IPS=0.1 mm
Dry ice blasting, v 0:5 m/min, IPS=0.1 mm
Dry ice blasting, v 1:0 m/min, IPS=0.1 mm
Compressed air blasting with corundum
Compressed air blasting with duroplast

Concentration of the elements (counts of roentgen quanta) (%)

C

Mg

Al

Mn

Fe

Si

2.04
1.33
0.50
0.53
0.60
0.89
0.56
0.53
0.73

3.35
1.43
0.95
1.06
1.05
1.24
0.97
0.98
5.25
1.14

8.86
6.85
7.06
6.79
7.15
7.14
7.02
6.68
4.00
4.43

85.75
89.69
91.43
91.54
91.12
90.66
91.38
91.73
88.47
91.93

0.05
0.04
0.04
0.05
0.05
0.04
0.04
0.05
0.31

0.03
0.02
0.03
0.03
0.02
0.03
0.04
0.13
0.54

0.61

contrast, signicantly higher surface roughness occurs

after blasting with corundum and duroplast.
The EDX-analysis for the determination of the
chemical composition shows that only the elements
aluminum (85.75%) and magnesium (8.86%) as well as
oxygen (3.35%) and carbon (2.04%) could be detected
on the aluminum surface as received (Table 4). The
aluminum concentration rises to over 90% through dry
ice blasting and the concentration of the elements
magnesium, oxygen, and carbon declines to differing
amounts. The concentration of carbon is reduced to less
than 1%, of oxygen to ca. 1%, and of magnesium to ca.
7%. Additionally, the elements iron and manganese
were detected in small amounts. No signicant inuence
of the feed speed and the IPS on the chemical
composition can be stated during dry ice blasting. Thus,
it can be derived that dry ice blasting provokes a strong
reduction of the lubricant, magnesium-oxide, and
aluminum-oxide layers. Very similar elements were
detected on aluminum surfaces degreased with SIP, the
concentrations of oxygen and carbon however, were
higher than in the case of surfaces treated with dry ice
blasting. Furthermore, also silicon was detected on
aluminum surfaces pretreated with SIP. In contrast,
aluminum surfaces blasted with corundum and duro-

0.64
1.17

Ca

Ti

0.18
0.48

0.37

0.18

plast have a different chemical composition. This

chemical composition strongly depends on the blasting
agent applied.
The examination of the pretreatment method in terms
of the adhesive strength of aluminum samples shows
that through dry ice blasting, an improvement can be
achieved for all glues investigated (Fig. 5). Under
constant circumstances, the feed speed v of the jet
nozzle as a scale for blasting intensity and the IPS were
varied for the examined glues. Three feed speeds, 0.1, 0.5
and 1.0 m/min, as well as two IPSs, 0.1 and 0.5 mm, were
investigated. In the case of the feed speed v of 0.1 m/min,
the effect of a subsequent treatment with SIP was
additionally analyzed. The investigation shows a qualitatively similar reaction of all glues. Compared with the
state as received, an increase of the adhesive strength
could be achieved through dry ice blasting. The lower
feed speed of 0.1 m/min results in higher adhesive
strengths for all glues than the adhesive strength of
samples treated with a feed speed of 1.0 m/min. An
increase of the adhesive strength can be achieved for the
two epoxy glues by an additional SIP-treatment.
In the case of epoxy glues, the inuence of the IPS on
the adhesive strength is different from polyurethane
glues. The samples joined with epoxy glues show higher

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

76

Glue EP 1
IPS = 0.5 mm

IPS = 0.1 mm

Adhesive strength [MPa]

20

v = 0.1 m/min + SIP

v = 1.0 m/min

v = 0.1 m/min

v = 0.5 m/min

v = 0.1 m/min + SIP

v = 1.0 m/min

10
v = 0.5 m/min

F = testing force
l = overlapping length
t = material thickness
d = glue film thickness

v = 0.1 m/min

15

as delivered

Shear tension test

according DIN EN 1465

Pretreatment method
Glue EP 2
IPS = 0.5 mm

Glue PU

IPS = 0.1 mm

IPS = 0.5 mm

IPS = 0.1 mm

Pretreatment method

v = 0.1 m/min + SIP

v = 1.0 m/min

v = 0.1 m/min

v = 0.5 m/min

v = 0.1 m/min + SIP

v = 1.0 m/min

v = 0.5 m/min

v = 0.1 m/min

as delivered

v = 0.1 m/min + SIP

v = 1.0 m/min

v = 0.5 m/min

v = 0.1 m/min

v = 1.0 m/min

v = 0.5 m/min

v = 0.1 m/min

10

v = 0.1 m/min + SIP

15

as delivered

Adhesive strength [MPa]

20

Pretreatment method

Fig. 5. Adhesive strength of EP 1, EP 2 and PU glues dependent on the pretreatment method.

adhesive strengths for smaller IPSs, in the case of joining

with polyurethane glues however, higher adhesive
strengths can be achieved with bigger IPSs. The highest
absolute adhesive strength was achieved when using EP
1. It reached approximately 20 MPa. The highest
increase in adhesive strength was reached with samples
joined with EP 2. The adhesive strength was increased
by 99% with SIP treatment and by 77% without it. In
the case of the epoxy glue EP 1, the adhesive strength
was increased by 48% with SIP treatment and by 12%
without it. The adhesive strength of samples joined with
polyurethane glue deteriorated on blasting with an IPS
of 0.1 mm. An additional SIP-treatment also leads to a
reduction of the cohesive strength of the polyurethane
glue.
After material failure, the bonding surfaces were
examined by a scanning electron microscope. The
samples of EP 1 failed adhesively on the aluminum
surface in macroscopic terms, independently of the
pretreatment parameters (Fig. 6). The topographic
structures of the fractional surfaces of the aluminum
samples after dry ice blasting are largely identical to the
structures after compressed air blasting. However, traces
of glue residues are detectable at some parts of the
fractional surface. In contrast, the SEM images of the
fractional surfaces of the samples with EP 2 show both a
cohesive fraction within the glue lm and an adhesive

fraction on the aluminum surface. After an additional

pretreatment of the samples with SIP, the ratio of
the cohesive fractional behavior in the glue lm
increased markedly. The samples of the PU glue failed
in the glue lm cohesively, independently of the
pretreatment parameters and some samples showed
traces of adhesive fraction at the aluminum surface. In
the state as delivered however, the samples fractured
mostly adhesively on the aluminum surface. With a
lower adhesive strength, all fractional surfaces have a
porous structure.
The EDX-analysis of the samples glued with EP 1
detected the same elements of largely similar concentrations on one of the two fractional surfaces (A) (Table 5)
as directly after dry ice blasting (Table 4). On the
opposite fractional surface (B), the elements silicon and
chlorine were detected, whereas iron and manganese
were not found. Furthermore, the concentration of
aluminum and magnesium is very low. This suggests
that alongside an adhesive fraction on the aluminum
surface, traces of a cohesive fraction occurred in the glue
lm. The elements aluminum and magnesium are
detectable on both fractional surfaces. Largely the same
elements and concentrations were found on different
fractional surfaces independently of the pretreatment
parameters and the application of SIP. The analysis of
the fractional surface (A) of samples joined with EP 2

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

77

Fig. 6. SEM images of the fractional surfaces dependent on the pretreatment method and the glue.

with a pretreatment without the use of scramblers, i. e.

with an IPS of 0.5 mm, detected the same elements with
largely the same concentrations as after dry ice blasting.
On the opposite fractional surface (B), magnesium and
aluminum were found in a low concentration, whereas
the concentration of carbon was markedly higher.
Additionally, the elements silicon, chlorine and calcium
were veried, whereas manganese and iron were not
detected. In contrast, the EDX-analysis of both
fractional surfaces of an aluminum sample pretreated
with dry ice blasting with scrambler and glued with EP
2, carbon, oxygen, magnesium, aluminum, silicon,
chlorine, calcium, and titanium were found. Additionally, on one fractional surface only, a low concentration
of manganese was detected. The concentration of
magnesium (2.41%) and aluminum (0.89%) on the
surface (B) without manganese and iron is very low,

whereas the percentage of carbon (69.60%) is very high.

This leads to the conclusion that the fraction occurred
cohesively in the glue lm close to the boundary layer as
well as in the aluminum and magnesium-oxide lm. The
macroscopic view of the fractional surfaces shows that
the fraction occurs in the middle of the glue lm if
samples were blasted with scrambler (IPS=0.1 mm) in
contrast to samples blasted without it (IPS=0.5 mm).
The EDX-analysis of the fractional surfaces of the
aluminum samples joined with PU glue, shows independently of the IPS and the feed speed the same
elements with similar concentrations on all samples. In
contrast to the samples joined with epoxy resin, the
elements sodium and potassium are additionally detectable in low concentrations; samples pretreated with
SIP however, have only a low sodium concentration on
one side.

78

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

Table 5
Chemical composition on the fractional surfaces dependent on the pretreatment method and on the glue (A and B are the opposing fractional
surfaces of a sample)
Adhesive; Type of pretreatment

Concentration of the elements (counts of roentgen quanta) (%)

C

EP 1; Dry ice blasting, v 0:1 m/min, IPS=0.5 mm

Mg

Al

Si

Cl

Ca

Ti

A 0.77
B 90.93

1.32
6.60

7.29
0.44

90.53
1.10

0.67

0.27

EP 1; Dry ice blasting + SIP, v 0:1m/min, IPS =0.5 mm A 1.48

B 86.35

1.25
7.96

6.86
0.77

90.07
1.94

0.25
2.73

0.26

EP1; Dry ice blasting, v 0:1 m/min, IPS=0.1 mm

A 2.03
B 91.15

0.88
7.18

6.41
0.18

90.60
0.35

0.93

0.20

A 1.08
B 88.84

0.85
8.61

6.53
0.15

91.47
0.37

2.03

A 1.05
B 83.79

1.26
11.79

6.87
0.90

90.72
1.89

1.17

0.16

0.31

EP 2; Dry ice blasting + SIP, v 0:1 m/min, IPS=0.5 mm A 27.08

B 70.67

4.97
9.50

5.21
2.62

56.50
1.13

3.85
8.54

0.55
0.86

1.84
6.45

0.23

EP 2;Dry ice blasting, v 0:1 m/min, IPS=0.1 mm

A 5.59
B 69.60

1.57
9.00

6.36
2.41

84.67
0.89

0.91
9.50

0.28
1.01

0.49
7.40

0.05
0.19

EP 2; Dry ice blasting +SIP,v 0:1 m/min, IPS=0.1 mm

A 39.60
B 74.81

5.99
14.03

4.19
2.82

39.80
0.15

5.96
6.16

0.83
0.39

3.44
1.56

0.19
0.08

PU;Dry ice blasting, v 0:1 m/min, IPS=0.5 mm

A 53.35
B 46.89

13.95
16.76

0.57
0.24

1.26
1.33

3.97
4.07

25.47
29.09

0.52
0.66

PU;Dry ice blasting +SIP, v 0:1 m/min, IPS=0.5 mm

A 51.20
B 50.43

14.44
13.71

0.36
0.25

2.16
1.92

3.86
3.95

27.27
29.19

0.48
0.54

PU;Dry ice blasting,v 0:1 m/min, IPS=0.1 mm

A 51.52
B 57.98

13.37
15.53

3.40
0.67

2.89
2.73

27.86
22.27

0.48
0.39

EP 1; Dry ice blasting +SIP, v=0.1 m/min, IPS=0.1 mm

EP 2;Dry ice blasting,v 0:1 m/min, IPS=0.5 mm

7. Summary
The adhesive strength of aluminum components can
signicantly be improved with dry ice blasting. Depending on the respective gluing system, the adhesive
properties can be enhanced through the optimization
of the dry ice blasting parameters IPS and feed speed.
Compared to the state as received, an increase of the
adhesive strength by up to 99% was achieved for
the two-component epoxy resin glues EP 1 and EP 2 as
well as 27% for the two-component polyurethane
glue PU.
A lower feed speed leads to higher adhesive strengths
for all gluing systems. A higher blasting intensity results
in improved adhesive properties. Samples joined with
epoxy glues have higher adhesive strengths with an IPS
of 0.1 mm. In the case of polyurethane glues however,
higher adhesive strengths were achieved with an IPS of
0.5 mm. In the latter case, a pretreatment with an IPS of
0.1 mm leads to a deterioration of the adhesive strength.
In the case of epoxy glues the additional pretreatment of

Mn

Fe

0.05

0.04

0.05

0.04

0.05

0.03

Na

0.52
0.62

0.37
0.34

0.06

0.05

0.05

0.05

0.03

0.24

0.47
0.43

the aluminum samples with SIP results in a signicant

increase of the adhesive strength. In contrast, the
consequence of an additional pretreatment of the
samples with SIP in the case of PU glue is the reduction
of the adhesive strength. After a signicant improvement of the adhesion, the samples glued with EP 1 fail
in adhesive terms on the aluminum surface, samples
glued with EP 2 fail in adhesive terms on the
aluminum surface as well as in cohesive terms in the
glue lm. The PU bonds too, broke both adhesively and
cohesively.
Compared to the state as received, dry ice blasting
provokes only slight changes in the topographic surface
structure and, in contrast to conventional pretreatment
methods, leads to no signicant increase in surface
roughness. Through dry ice blasting, the carbon,
oxygen, and magnesium concentration is strongly
reduced on the surface, whereas the concentration of
aluminum increases from 86% to 91% for the investigated alloy. Additionally, manganese and iron
were detected. Consequently, the improvement of the

F. Elbing et al. / International Journal of Adhesion & Adhesives 23 (2003) 6979

adhesive strength is due to the removal of the disturbing

lubricant, aluminum-oxide, and magnesium-oxide lms.

Acknowledgements
The authors thank Ciba, Permabond, and Tivoli,
manufacturers of adhesives, as well as VAW AluminumNorsk Hydro, producer of aluminum, for the
provision of materials.

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