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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).
0143-7496/03/$ - see front matter r 2003 Elsevier Science Ltd. All rights reserved.
doi:10.1016/S0143-7496(02)00083-0
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
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
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
Fig. 1. Schematic depiction of the experimental equipment for the pretreatment with dry ice blasting.
72
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
economic parameters
- manufacturing cost
- quantities
- disposal cost
Fig. 2. Relevant parameters for the pretreatment of bonding surfaces with dry ice blasting.
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.
73
Table 1
Technical data and SEM images of the surface of the metallic joint partners
Material
Manufacturer
Trade name
Chemical formula
Material thickness
Arithmetical mean deviation of the prole
Mean roughness
Prole depth
Chemical composition of the surface
Surface topography
Table 2
Technical data of the glues
Adhesive basis
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
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
PU
Tivoli
Tivopur 1667
Tivopur 1667
Tivopur 1600/07
100:30 (m%)
14 min, 201C
Manual
48 h, 201C+3 h, 1001C
74
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.
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
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
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
0.64
1.17
Ca
Ti
0.18
0.48
0.37
0.18
76
Glue EP 1
IPS = 0.5 mm
IPS = 0.1 mm
20
v = 1.0 m/min
v = 0.1 m/min
v = 0.5 m/min
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
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 = 1.0 m/min
v = 0.1 m/min
v = 0.5 m/min
v = 1.0 m/min
v = 0.5 m/min
v = 0.1 m/min
as delivered
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
15
as delivered
20
Pretreatment method
77
Fig. 6. SEM images of the fractional surfaces dependent on the pretreatment method and the glue.
78
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
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
1.25
7.96
6.86
0.77
90.07
1.94
0.25
2.73
0.26
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
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
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
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
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
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
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
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
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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Dorn
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79