Article

The Influence of Sandblasting Process Parameters of Aerospace

Aluminium Alloy Sheets on Adhesive Joints Strength
Izabela Miturska-Barańska *, Anna Rudawska and Elżbieta Doluk

Department of Production Engineering, Faculty of Mechanical Engineering, Lublin University of Technology,

Nadbystrzycka 36, 20-618 Lublin, Poland; a.rudawska@pollub.pl (A.R.); e.doluk@pollub.pl (E.D.)
* Correspondence: i.miturska@pollub.pl

Abstract: In this study, the influence of sandblasting process parameters as a surface preparation
method on the strength of single-lap adhesive joints of EN AW 2024 T3 aerospace aluminium alloy
sheets was determined. Eleven sets of sandblasting parameters were used, which were determined
according to a determined experimental plan. The variable factors in the sandblasting process were
pressure, nozzle distance, and workpiece displacement speed. The sand jet incidence angle was con-
stant. Garnet 80 E+ was the abrasive material that was used. The joints were made using an epoxy
adhesive composition of Epidian 5 epoxy resin and a PAC curing agent. The influence of the surface
preparation method on the surface roughness and contact angle to determine the surface free energy
was evaluated. The shear strength of the adhesive joints was also determined, which finally allowed
the evaluation of the applied surface treatment variants. The obtained results were subjected to sta-
tistical analysis, which indicated that the highest shear strength of the adhesive joints was obtained
Citation: Miturska-Barańska, I.;
Rudawska, A.; Doluk, E. The
for samples whose surfaces were treated by sandblasting at parameter configurations in which the
Influence of Sandblasting Process pressure was 5–6 × 105 Pa; the distance between the nozzle and the sandblasted surface should not
Parameters of Aerospace be greater than 97 mm, and the speed at which the workpiece moves in relation to the nozzle should
Aluminium Alloy Sheets on not be greater than 75 mm/min.
Adhesive Joints Strength.
Materials 2021, 14, 6626. Keywords: shear strength; single-lap adhesive joints; EN AW 2024 T3 aluminium alloy; sandblasting
https://doi.org/10.3390/ma14216626

Academic Editor: Raul D. S. G.

Campilho 1. Introduction

Received: 7 October 2021

One of the most developed methods of joining materials that has been in recent times
Accepted: 2 November 2021
is adhesive bonding, the key advantage of which is the possibility of joining elements
Published: 3 November 2021 made of materials that are characterized by various mechanical, physical, and chemical
properties [1–4]. Through adhesive bonding, it is possible to make structures that are
Publisher’s Note: MDPI stays neu- much larger than they can be made as a single element or that can be transported as a
tral with regard to jurisdictional single unit [5]. The bonding technology also contributes to the design and the manufac-
claims in published maps and insti- ture of lightweight yet strong structures with specific properties [6]. Because of this ver-
tutional affiliations. satility, this technology is used in a wide range of industries, such as the aerospace, auto-
motive and rail, and civil engineering industries as well as other industrial sectors where
an effective high strength-to-weight ratio is important for the development of the innova-
tive structures [7–15]. As Messler describes in his publications [16,17], adhesive bonding
Copyright: © 2021 by the authors. Li- technology creates the possibility of replacing other bonding methods without causing
censee MDPI, Basel, Switzerland. microstructural changes in the joined elements. A number of the advantages resulting
This article is an open access article
from the use of this joining method are due to the fact that the adhesive joints can also be
distributed under the terms and con-
successfully applied in the electronics and construction industries as well as in medicine
ditions of the Creative Commons At-
and material engineering [9,18,19]. As indicated by the authors of Saboori et al. [20] and
tribution (CC BY) license (http://crea-
Ziółkowski and Dyl [21], structural bonding may be a worthwhile alternative in repair
tivecommons.org/licenses/by/4.0/).
and sealing processes, where regenerating parts in the repairs of machine structure ele-

Materials 2021, 14, 6626. https://doi.org/10.3390/ma14216626 www.mdpi.com/journal/materials

Materials 2021, 14, 6626 2 of 21

ments, allows costs being able to be reduced. During vehicle construction, adhesive tech-
nology can be used to fix linings, brake pads, glass panes, joining elements of door skins,
engine covers, and the boot [13,14,22,23]. Adhesive technology is also used in bus manu-
facturing due to the excellent damping properties of the adhesives. An important share is
also recorded in the construction of self-supporting vehicle bodies [13,24]. These adhe-
sives are also used to seal internal combustion engines, differentials, and transmissions
and can also be used to reinforce thrust-bearing contact surfaces. Structural adhesive
bonding is also now widely used in the construction of aircraft airframes [25–27].
The correct execution of the bonding process consists of several steps [12,15,28]. The cor-
rect implementation of the individual stages of the technological process affects the correct
execution of adhesive joints that are characterized by a specific strength. The most important
and initial stage is the preparation of the surface of the joined materials. Surface preparation
has a very large influence on the strength and resistance of the adhesive joints. When choosing
the appropriate surface treatment method, it is necessary to know the type, structure, and
properties of the adherends [15,29–31].
In this study, aerospace aluminium alloys were used. Aluminium and aluminium
alloy surfaces are usually processed chemically and electrochemically. Anodizing, chro-
mating, and phosphating are frequently used [3,10,11,22,31–34]. However, due to the
availability of materials and the safety of the process, the most commonly used process is
mechanical treatment [35–37]. Mechanical treatment is one of the most frequently used
methods for the surface treatment of construction materials to be used in the bonding
process [32,38–41]. One of the reasons for the use of mechanical treatment is to clean var-
ious impurities from the surface that have managed to become stuck to the surface
through various means (e.g., oxides, fine impurities) as well as to change the geometric
structure of the adherend surfaces. These are important activities that are related to ob-
taining the appropriate (favorable) stereometric structure of the surface and that influence
the adhesive properties of the adherend surfaces. As a result, the surface is geometrically
developed, and this affects the increase in mechanical adhesion, which is related to the
increase in the active area where the adhesive is in contact with the adherent [42]. When
using mechanical processing, the correct choice of abrasive grain size is crucial. Too small
a grit size can cause the contaminants to be smeared across the surface, whereas coarse
grit sizes create deep scratches and craters on the surface, which can cause changes in the
properties of the surface layer [43,44]. The machining process should be followed by a
final degreasing process to remove dust, dirt, grease, and other contaminants. Degreasing
can be accomplished by using trichloroethylene, acetone, carbon tetrachloride, extraction
gasoline, or other agents to emulsify the contaminants.
When considering machining methods, various methods that have been the subject
of analysis in scientific works can be distinguished, including abrasive blasting (including
sandblasting), shot blasting, shot blasting, grinding, and others [45–49]. Among the me-
chanical treatments, sandblasting is recommended and is the most favorable, while the
coarse-grained abrasive cloth method is the least favorable. During sandblasting, it is to
the use of an aluminium oxide, silicon carbide, and a quartz as the abrasives which is
recommended due to their irregular shape and the sharp edges, making them effective in
imparting a certain roughness to the treated surface [47,50,51]. Abrasives in the form of
glass beads, porcelain beads, or metal shot should not be used on aluminium and its al-
loys, as they only cause surface crushing [52].
The aim of this study was to determine the influence of the parameters of the sand-
blasting process as a surface preparation method on the strength of the single-lap adhesive
joints of EN AW 2024 T3 aerospace aluminium alloy sheets. The adhesive joints were
made using an epoxy adhesive composition. The tests also included surface roughness
and contact angle measurements to determine the surface free energy. The shear strength
of the adhesive joints was also determined. The obtained test results were subjected to
statistical analysis.
Materials 2021, 14, 6626 3 of 21

2. Materials and Methods

2.1. Adherend
In this study, an EN AW 2024 T3 aluminium alloy was used. This material is charac-
terized by lower corrosion resistance and poorer weldability than other aluminium alloys,
but it contains a high amount of copper and has very high strength—compared to
AW2014, for example—and high fatigue strength. The chemical composition of the alloy
that was used is given in Table 1. This material is most often used in structures requiring
high strength but is also used where the risk of corrosion is low. It is used in parts where
a high strength-to-weight ratio is required; therefore, it is used in the construction of air-
craft equipment, gears and shafts, screws, computer parts, clutches, hydraulic valve parts,
rocket and munitions parts, pistons, worm gears, and orthopedic equipment. Table 2 pre-
sents the mechanical properties of the material used in this study.

Table 1. Chemical composition of EN AW 2024 T3 aluminium alloy [53].

The Element Contents, %

Si 0.1671
Fe 0.2153
Cu 4.0975
Mn 0.4281
Mg 1.4405
Cr 0.0053
Zn 0.0154
Ti 0.0191
Al 93.5699

Table 2. Mechanical properties of EN AW 2024 T3 aluminium alloy [53,54].

Mechanical Properties Value

Tensile strength 447.2 MPa
Yield strength 302.5 MPa
Elongation 16.5%
Hardness 123 HB
Thermal conductivity 170 W/mK
Thermal conductivity 2.78 g/cm3

The specimens used in the study were cut from a sheet of a plate with a thickness of
2.00 ± 0.12 mm to dimensions of 101.60 ± 0.25 mm × 177.80 ± 3.17 mm by means of a hy-
droabrasive jet using a Waterjet Eckert Combo portal cutting machine (Eckert AS Ltd.,
Legnica, Poland). The cutting process speed was 200 mm/min at a water pressure of
3500 × 105 Pa. The distance between the nozzle and the material being cut was 3 mm,
and the abrasive flow rate during the cutting process was approximately 0.4 kg/min. The
abrasive used was Garnet 80 E+ sand. Subsequently, two holes with a diameter of 2.5 mm
were drilled into each of the cut sheets to grind the fixing pins, which made it possible to
assemble the adhesive panels in a defined geometry while maintaining a constant overlap
length.

2.2. Surface Preparation Methods

The surface of the cut sheets was prepared for the bonding process by sandblasting
and degreasing the surface with acetone. The process of sandblasting the samples for ad-
hesive bonding was carried out on a specially modernised cabin sandblaster (Cormak,
Siedlce, Poland). The sandblasted sample was placed in a holder and was driven by an
electric motor so that a constant speed of nozzle movement over the sample was achieved.
Materials 2021, 14, 6626 4 of 21

The pressure was set on a regulator, and parameters such as the angle of incidence of the
sand jet and the distance of the nozzle from the workpiece were achieved by keeping the
nozzle and the sample stationary. Garnet 80 E+ sand was used in the sandblasting process.
A diagram of the sandblasting process is shown in Figure 1. The sample was moved at a
constant speed V and was sandblasted with the nozzle placed at a distance h from the
sandblasted surface using a specific pressure P.

Sandblasting nozzle

Abrasive
h

Sandblasted
sample
V

Figure 1. Sandblasting process diagram.

In order to select the optimal sandblasting parameters, tests were carried out accord-
ing to the Hartley PS/DS-P:Ha3 determined selection plan [55]. The Hartley plan allowed
for a significant reduction in the number of experiments that needed to be carried out. The
basic principle of creating poliselection plans is the deliberate selection of the combination
of input values (within the previously assumed range) in such a way that it is possible to
obtain the required scientific information with limited effort, i.e., a relatively small num-
ber of measurements. This plan belongs to the static, determined, policy-selective plans
for three input quantities, where five different values are used for each input quantity.
The test plan included different combinations of sandblasting parameters in which the
variables were sample displacement speed, sandblasting pressure, and nozzle distance
from the sample surface. The angle between the sample and the jet direction was assumed
to be constant at 90°. The number of sample displacements was also assumed to be two.
To perform the calculations to determine the parameter sets according to the Hartley Plan,
it was necessary to establish the minimum and maximum values achievable for each pa-
rameter, which are summarized in Table 3. The minimum and maximum values of the
parameters were determined on the basis of our own preliminary tests to check the capa-
bilities of the machine on which the sandblasting process was carried out.

Table 3. Range of values for selected parameters of the sandblasting process.

Parameter Parameter Value

X1—distance of the nozzle from the sample surface 40 ≤ X1 ≤ 155 [mm]
X2—speed of sample displacement 50 ≤ X2 ≤ 100 [mm/min]
X3—sandblasting pressure 3 × 105 ≤ X3 ≤ 7 × 105 [Pa]

The parameter sets determined according to the test plan are presented in Table 4.
Materials 2021, 14, 6626 5 of 21

Table 4. Hartley plan PS/DS—P: Ha3 for actual input values.

X1 X2 X3
Number of Parameter Distance of the Nozzle Sandblasting
Speed of Sample Dis-
Sets Sandblasting from the Sample Surface Pressure
placement (mm/min)
(mm) (Pa)
1 69 62 6 × 105
2 126 62 4 × 105
3 69 87 4 × 105
4 126 87 6 × 105
5 48 75 5 × 105
6 147 75 5 × 105
7 97 53 5 × 105
8 97 96 5 × 105
9 97 75 3 × 105
10 97 75 6 × 105
11 97 75 5 × 105

The samples were sandblasted according to the specified parameters and were then
cleaned of dust and any contaminants in an acetone bath. The samples were immersed in
the acetone bath for 20 min at 23°C ± 2 °C, after which the surfaces were wiped with a
cleaning rag, cleaned a second time, and allowed to dry internally for 10 min.

2.3. Shape and Dimension of Adhesive Joints and Specimen Preparation Conditions
Single-layer adhesive joints of aluminium alloy sheets were prepared using an epoxy
adhesive composition of Epidian 5 epoxy resin (CIECH S.A., Sarzyna, Poland) and the
PAC curing agent (CIECH S.A., Sarzyna, Poland), which were mixed in a stoichiometric
ratio of 100:80 (identification of composition—E5/PAC/100:80). Epidian 5 is a pure form
of epoxy resin, which is a product of the reaction of bisphenol A with epichlorohydrin. It
is characterised by excellent adhesion to most plastics, chemical resistance as well as re-
sistance to aggressive environmental factors, and good electrical properties [56,57]. Ep-
idian 5 resin and compositions based on it are used in the manufacture of glass fiber lam-
inates, joining metals, ceramics, and thermosetting plastics. Adhesives prepared on the
basis of this resin are also used in building structures that are used as anti-corrosive and
electro-insulating coatings. The performance properties of the resin used in this study are
presented in Table 5.

Table 5. Physical and chemical properties of Epidian 5 epoxy resin [56,57].

Properties Epidian 5 Epoxy Resin

Epoxy number 0.48–0.52 mol/100 g
pH value approx. 7
Viscosity at 25 °C 20,000–30,000 mPa·s
Density at 20 °C 1.16 g/cm3
Flash point 266 °C
Auto-ignition temperature 490 °C
Melting point 30–50 °C
Boiling point initial not indicated—decomposition

PAC curing agent (CIECH S.A., Sarzyna, Poland) (fatty acids, C18-unsaturated, di-
mers, polymeric reaction products with triethylenetetramine) is used to harden liquid
epoxy resins. This hardener causes the flexibility and impact strength of the composition
to increase, which is why it is used for joints that are exposed to deformations, e.g., in
Materials 2021, 14, 6626 6 of 21

boatbuilding to join wooden elements or elements made of polyester-glass laminates; to

join rubber with metal, thin sheets and plywood; and to pour elements in electrical engi-
neering and electronics. The PAC curing agent belongs to a group of slow curing agents.
Full cure is achieved in 7–14 days. The functional properties of the hardener used in this
study are shown in Table 6.

Table 6. PAC curing agent functional properties [57,58].

Properties Polyamide Hardener (PAC Curing Agent)

Viscosity at 25 °C 10,000–25,000 mPa·s
Density at 20 °C 1.10–1.20 g/cm3
Amine number 290–360 mg KOH/g
Gel time
(for example, for a composition with Ep- 180 min
idian 5 at 20 °C, for a 100 g sample)

Adhesive composition was prepared straight before the bonding process. The com-
ponents of the mixtures were carefully weighed using a KERN CKE 3600-2 laboratory
scale (Kern, Albstadt, Germany) with a measurement accuracy of 0.01 g. Before the mixing
process, the epoxy resin was preheated to 50 °C to reduce its viscosity. The epoxy resin
heating stage was conducted using an electric heater—DEPILUX 400 (Activ, Wroclaw,
Poland)—with the power of 100 W, which allows for the smooth regulation of the liquid
heating from 45 to 105 °C. The temperature of the heated epoxy resin was monitored using
an electronic thermometer (Amarell Electronic, Kreuzwertheim, Germany) with the meas-
uring range of −50 to 200 °C and with the measuring accuracy of ±0.1 °C. Then, the heated
epoxy resin was mixed with a mechanical mixer Güde GTB 16/5 A (Güde, Wolpertshau-
sen, Germany) equipped with a propeller mixer. The mixing process used a speed of 460
rpm lasted for 2 min. Next, the adhesive compositions were deaerated for 2 min in order
to remove any gas bubbles that had formed as a result of mixing the components. The
finished adhesive compositions were applied to the surfaces to be bonded using a roller
for adhesive application, which made it possible to achieve a homogeneous joint thickness
across the entire adhesive surface. In the next stage, the elements were joined together.
The adopted curing conditions for the adhesive joints are presented in Table 7.

Table 7. Parameters of curing conditions for adhesive bonds.

Curing Process Parameter Parameter Value

Pressure 0.6 × 105 Pa
Temperature 23 °C ± 2 °C
Humidity 23% ± 3%
Time 7 days

Constant pressure throughout the curing period for the adhesive joints was ensured
by the vacuum bag method, which was implemented using a SVAGG vacuum pump
(Schunk, Lauffen/Neckar, Germany). The vacuum bag method is illustrated in Figure 2.
Pictures of the real joint-making process are shown in Figure 3.
Materials 2021, 14, 6626 7 of 21

Manometer
Air valve

Diaphragm foil

Delamination fabric

Perfored foil

Bonded specimens
Separation foil

Butyl tape
Fixing plate

Figure 2. Layout of vacuum bag components with bonded specimens.

Figure 3. View of bonded specimens in a vacuum bag.

The adhesive joints used in the tests were prepared in accordance with the require-
ments of the ASTM D1002 standard [59] in the form of panels. The general appearance of
the prepared panels with a fixed overlap length, which, according to the standard, is 12.7
mm, is shown in Figure 4.

Figure 4. Method of assembling the bonded panels used in the tests.

After the joint seasoning time, the panels were cut on a Waterjet Eckert Combo ma-
chine using the same parameters as those used for sheet cutting. From one panel, five
samples were obtained for each sandblasting variant. The geometry and dimensions of a
single adhesive specimen intended for testing are shown in Figure 5.
Materials 2021, 14, 6626 8 of 21

2.00u0.12

2.00u0.12
adhesive joint thickness

12.7u0.25

25.4u0.25
101.6u0.25
190.5u0.25
Figure 5. Single-lap adhesive bonding used in the tests performed in accordance with the ASTM
D1002 standard.

The overlap length and adhesive bond thickness were measured using a Keyence
VHX-5000 digital microscope (Keyence, Itasca, IL, USA). Figure 6 shows an example
photo of the measurement of the overlap length and adhesive joint thickness of the tested
adhesive joints.

Figure 6. Sample images of overlap joint taken with the Keyence VHX-5000 microscope.

The average adhesive joint thickness was 0.100 mm ± 0.025 mm.

2.4. Surface Roughness

Before the bonding process, the surface roughness and 3D topography features of the
EN AW 2024 T3 aluminium alloy samples were evaluated after the sandblasting process
was complete using a T8000 RC120-400 contour, roughness, and 3D topography measur-
ing device (Hommel-Etamic, Berlin, Germany). Tests were conducted in accordance with
the EN ISO 25178 standard [60]. A TKU300 measuring tip was used in the study. The
measuring range was 80 μm. The tests were conducted at a speed of 0.50 mm/s. The sam-
pling length was set to lr = 0.8 mm. The area that was scanned included a 4.8 mm × 4.8 mm
section of the surface, and the roughness profile parameters were determined from 241
measurements. The following amplitude parameters of the roughness profile and surface
topography were analysed: Ra—arithmetic mean deviation of roughness, Rz—highest
profile height, Sa—arithmetic mean surface height, and Sz—maximum surface height.
Ten measurements were taken for each sample.
Materials 2021, 14, 6626 9 of 21

2.5. Surface Energy

Before the bonding process, the contact angle of the aluminium alloy sheet surface
was also measured after the sandblasting process to determine the surface free energy.
The surface free energy was determined using the Owens–Wendt method, which is based
on direct measurements of the contact angle [42,61,62]. The Owens–Wendt method is
based on the determination of two components: polar and dispersion surface free energy,
according to Equation (1) [47,63]:
𝑝𝑝
𝛾𝛾𝑠𝑠 = 𝛾𝛾𝑠𝑠𝑑𝑑 + 𝛾𝛾𝑠𝑠 (1)
𝑝𝑝
where 𝛾𝛾𝑠𝑠 —surface free energy (SFE),𝛾𝛾𝑠𝑠𝑑𝑑 —dispersioncomponent of SFE, 𝛾𝛾𝑠𝑠 —polar com-
ponent of SFE.
To determine the total surface free energy, two measuring liquids (non-polar and
polar) with known polar and dispersion component values were used to determine the
surface free energy. Distilled water and diiodomethane CH2I2 were used as measuring
liquids, and the droplet size that was used was approximately 2 μL. The polar component
of the distilled water was 51 mJ/m2 and had a total surface free energy equaling 72.8 mJ/m2
[42,62]. The individual components of the surface free energy of diiodomethane equaled
dispersion—48.6 mJ/m2, and polar—2.4 mJ/m2 [63], respectively. The components 𝛾𝛾𝑠𝑠𝑑𝑑 and
𝑝𝑝
𝛾𝛾𝑠𝑠 for the surface free energy of the adherend surface could be calculated from the equa-
tions presented in [42].
The droplet size of the measuring liquids was approximately 2 μL. There were 15
measurement respetitions on the measurement on each aluminium alloy sample with each
measuring liquid. The reading of the contact angle value was made 5 s after the liquid
drop was formed. Contact angle measurements were made at a temperature of 21 ± 1 °C
and at an air humidity of 30 ± 1%. The tests were conducted using a PGX pocket goniom-
eter (Kontech, Lodz, Poland).

2.6. Strength Test

Strength tests of single-lap adhesive joints of EN AW 2024 T3 aluminium alloy sheets
under shear stress were conducted on a Zwick Roell Z150 testing machine (Zwick/Roell,
Ulm, German) according to the ASTM D1002 standard [49]. This is a standard for testing
the apparent shear strength of single-lap specimens by tensile loading. The crosshead dis-
placement during the test was 1.5 mm/min at an initial force of 5 N.

3. Results and Discussion

3.1. Surface Roughness
The results of the surface quality assessment for the samples after the sandblasting
process are presented below (Figure 7 and Table 8).
Materials 2021, 14, 6626 10 of 21

14
Parameter Rz
12.16 Parameter Ra
12 11.82
11.05

10.08 9.93
10 9.58
Parameter Ra i Rz [μm] 8.84
8.52
Surface roughness

8 7.45
6.92
6.64

2 1.46 1.52
1.29 1.27 1.39 1.26 1.41
0.79 0.79 0.94 0.96

0
1 2 3 4 5 6 7 8 9 10 11
Set of sandblasting parameters

Figure 7. Ra and Rz surface roughness parameters of EN AW 2024 T3 aluminium alloy samples after
sandblasting.

Table 8. Surface topography of EN AW 2024 T3 samples after sandblasting.

Number of Surface Profile Height

Surface Topography
Parameter Sets Sandblasting Parameters

Sa = 1.49 μm
1
Sz = 26.8 μm

Sa = 0.82 μm
2
Sz = 14.8 μm
Materials 2021, 14, 6626 11 of 21

Sa = 0.90 μm
3
Sz = 17.7 μm

Sa = 1.41 μm
4
Sz = 23.5 μm

Sa = 1.57 μm
5
Sz = 22.6 μm

Sa = 0.97 μm
6
Sz = 19.0 μm

Sa = 1.43 μm
7
Sz = 32.8 μm
Materials 2021, 14, 6626 12 of 21

Sa = 1.31 μm
8
Sz = 21.8 μm

Sa = 1.02 μm
9
Sz = 22.7 μm

Sa = 1.51 μm
10
Sz = 28.3 μm

Sa = 1.58 μm
11
Sz = 25.3 μm

Figure 7 presents the results of surface roughness testing of the samples after sand-
blasting. The highest average values of the Rz and Ra parameters were obtained for 1, 7,
and 11 sets of the sandblasting parameters (described in Table 4). In the mentioned vari-
ants of the process, the sandblasting pressure was 5 and 6 bar, the distance of the nozzle
for one set of parameters was 69 mm, and for the other two, it was 97 mm, while the
sandblasting speed for one sandblasting variant was 62 mm/min, for seven set of param-
eters it was 53 mm/min, and for ten variants, it was 75 mm/min. For comparison, the sur-
face topography of the samples after sandblasting is presented in Table 8.
From the surface topographies shown in Table 8, it can be seen that the sandblasting
process did not create any deformation on the surfaces of the samples that were to be
bonded. This could only be observed on the uniformly distributed surface depressions,
Materials 2021, 14, 6626 13 of 21

which are desirable in the adhesive process since in the next stage, the adhesive penetrates
into the created depressions, anchoring itself and forming mechanical bonds between the
surfaces. Analyzing the surface topography parameters Sa and Sz, it can be observed that
the distribution of the obtained results is similar to that of the surface roughness profile
parameters Ra and Rz.

3.2. Surface Energy

Figure 8 presents the calculated surface free energy results for the sandblasted sur-
faces.

Figure 8. Surface free energy of EN AW 2024 T3 aluminium alloy sheet samples after sandblasting.

For comparison, the surface free energy results for a reference aluminium alloy sur-
face not treated with sandblasting are also included. As it can be seen, the untreated sur-
face is characterised by a significantly lower surface free energy value (23.5 mJ/m2). Such
a surface is characterised by lower wettability, which may consequently lead to the weak-
ening of adhesive bonds in the adhesive joint. As it can be seen, the highest surface free
energy value can be observed in the sample surfaces that were subjected to the 5th sand-
blasting method (42.8 mJ/m2) as well as to the 7th and 11th set of sandblasting parameters
(in both cases 42.4 mJ/m2). The results obtained were statistically processed. The statistical
analysis of these three values showed no significant differences at the adopted significance
level α = 0.05. The lowest surface free energy value was observed in the case of the 6th
sandblasting method (30.2 mJ/m2). As an example, Table 9 shows the appearance of the
droplets for the sandblasting methods described as well as the values of the contact angles
for all of the surfaces that were analysed.
Materials 2021, 14, 6626 14 of 21

Table 9. Droplet measuring the surface contact angles of EN AW 2024 T3 aluminium alloy sheet samples after sandblasting
and values of the contact angles.

Number of Droplet and Value of Contact Angle Measure- Droplet and Value of Contact Angle Measure-
Parameter sets Sandblasting ment with Diiodomethane ment with Water

reference
surface

𝜃𝜃𝑑𝑑 = 79.11° 𝜃𝜃𝑤𝑤 = 89.74°

𝜃𝜃𝑑𝑑 = 38.52° 𝜃𝜃𝑤𝑤 = 117.75°

2 𝜃𝜃𝑑𝑑 = 47.72° 𝜃𝜃𝑤𝑤 = 101.06°
3 𝜃𝜃𝑑𝑑 = 44.10° 𝜃𝜃𝑤𝑤 = 118.85°
4 𝜃𝜃𝑑𝑑 = 43.20° 𝜃𝜃𝑤𝑤 = 107.87°
5 𝜃𝜃𝑑𝑑 = 40.47° 𝜃𝜃𝑤𝑤 = 123.95°

𝜃𝜃𝑑𝑑 = 57.62° 𝜃𝜃𝑤𝑤 = 113.28°

𝜃𝜃𝑑𝑑 = 37.05° 𝜃𝜃𝑤𝑤 = 113.88°

8 𝜃𝜃𝑑𝑑 = 43.96° 𝜃𝜃𝑤𝑤 = 107.70°
9 𝜃𝜃𝑑𝑑 = 43.85° 𝜃𝜃𝑤𝑤 = 101.90°
10 𝜃𝜃𝑑𝑑 = 45.20° 𝜃𝜃𝑤𝑤 = 113.12°
Materials 2021, 14, 6626 15 of 21

11

𝜃𝜃𝑑𝑑 = 45.70° 𝜃𝜃𝑤𝑤 = 115.56°

3.3. Strength Test Results

The obtained results of the shear strength tests of adhesive joints depending on the
parameters of the surface preparation treatment of the specimens are shown in Figure 9.

22
Average
19.26 Standard deviation
20
17.68
18 17.04
13.13
16 13.87
13.31
12.22
Shear strength Rt [MPa]

14
12.28
11.92
12 8.84

10

7.60
8

0
1 2 3 4 5 6 7 8 9 10 11

Number of parameter sets sandblasting

Figure 9. Results of shear strength tests of EN AW 2024 T3 aluminium alloy sheet adhesive joints as
a function of sandblasting parameters.

From the results obtained here, it can be seen that the highest shear strength (mean
value) was obtained for the samples whose surfaces were prepared according to the 7th
set of sandblasting parameters. In order to be able to analyse the test results in more detail,
a statistical analysis of the obtained results was conducted. The results of the Shapiro–
Wilk test are summarised in Table 10.

Table 10. Results of the W Shapiro–Wilk test for normality of the tensile shear strength distribution
of EN AW 2024 T3 sheet adhesive joints as a function of sandblasting parameters.

Number of Parameter Sets Sand- The Value of the W Level p for the W
blasting Shapiro–Wilk Shapiro–Wilk
1 0.946 0.711
2 0.939 0.649
3 0.726 0.017
4 0.974 0.905
Materials 2021, 14, 6626 16 of 21

5 0.791 0.087
6 0.884 0.357
7 0.889 0.352
8 0.844 0.177
9 0.927 0.580
10 0.973 0.898
11 0.791 0.068

Based on the results obtained here, it can be noted that the conditions for a normal
distribution were not met in any of the groups (in group 3—p < 0.05). Therefore, in a later
part of the study, a post hoc test was performed where homogeneous groups were deter-
mined. The results of this test are presented in Table 11.

Table 11. Post hoc test results of homogeneous groups of mean tensile shear strength as a function
of sandblasting parameters.

Number of Parameter Sets Average Shear Strength Homogeneous Groups

Sandblasting Rt (MPa) 1 2 3 4 5
7 19.26 ***
1 17.68 ***
10 17.04 *** ***
3 13.87 *** ***
8 13.31 ***
5 13.13 ***
4 12.28 *** ***
11 12.22 *** ***
2 11.92 *** ***
6 8.84 *** ***
9 7.60 ***
where: ***—indication of group assignment.

When analyzing the results obtained here, it can be observed that group 1 contains
the averaged results of three groups: sandblasting parameter sets 7, 1, and 10. However,
in the case of adhesive joints whose surfaces were prepared using sandblasting parameter
set 7, the highest result repeatability was also obtained (standard deviation of 3.9%). The
lowest shear strengths were obtained in the case of sandblasting methods 6 and 9 for the
surfaces of the bonded samples.

4. Discussion
Some machining methods are not only used to treat the surfaces of construction ma-
terials before adhesive processes but are also used to modify surface properties, such as
abrasive blasting. This treatment includes sandblasting, shot blasting, and shot peening.
Such a modification may contribute to increasing the fatigue strength of the components
that are subjected to high stresses. For example, the machined elements (e.g., after milling,
cutting or heat treatment) contain residual tensile stresses. Shot peening transforms these
stresses into compressive stress, which significantly extends the service life of these com-
ponents. The surface subjected to shot peening slightly deforms plastically, which causes
a change in the direction and nature of the stresses occurring in the surface layer. This
issue was emphasized in many works, e.g., in Al-Obaid [45]. Shot blasting is similar to
sandblasting, except that it works using a plasticity mechanism instead of an abrasion
mechanism. In turn, the use of surface shot peening [64] and laser shock peening [65] em-
phasize the importance of plastic deformation in improving the surface properties of var-
ious construction materials. Abrasive blasting, which includes sandblasting, can cause
Materials 2021, 14, 6626 17 of 21

plastic deformation that roughens the surface and that can cause significant subsurface
grain refinement. In [66], Multigner et al. show that the plastic strain gradient and volume
increase associated with α′-martensite-induced deformation is responsible for the devel-
opment of compressive residual stresses with a maximum value near the surface. The dif-
ferent results are related to the specific morphology of the particles and their specific role
in the blasting process. Li, Du et al. present similar conclusions in their work [67].
In order to determine the influence of individual parameters, both roughness and
surface free energy, a correlation study analysis was performed. The results of this analy-
sis are summarised in Table 12.

Table 12. Results of the correlation study.

Correlations
Indicated Correlation Coefficients are Significant with p < 0.05
Standard
Average r (X,Y) r2 t p
Deviation
Shear strength (MPa) 13.38 3.54
Parameter Ra (μm) 1.19 0.27 0.57 0.33 2.10 0.07
Shear strength (MPa) 13.38 3.54
Parameter Rz (μm) 9.40 1.96 0.39 0.15 1.27 0.24
Shear strength (MPa) 13.38 3.54
Parameter Sa (μm) 1.27 0.29 0.53 0.29 1.90 0.09
Shear strength (MPa) 13.38 3.54
Parameter Sz (μm) 23.21 5.07 0.67 0.44 2.68 0.03
Shear strength (MPa) 13.38 3.54
SFE (mJ/m2) 38.65 3.48 0.58 0.34 2.14 0.06
Where r(X,Y)—Pearson correlation coefficient; r2—determination coefficient; t—value of the t sta-
tistic testing the significance of the correlation coefficient; p—the calculated significance level for
the t-test.

Analyzing the results obtained here, it can be seen that the value of the correlation
coefficient oscillates between 0.53 and 0.67 (except for the Rz parameter), which indicates
strong linear dependence of the strength on the roughness and surface free energy param-
eters. The coefficient of determination ranges from 0.30 to 0.44 in all cases, which means
that the variation in shear strength is almost 44% and can be explained by the variation in
the individual parameters. The significance level p for the t-statistic is only less than 0.05
in the case of the Sz parameter, which means that the correlation coefficient is significantly
different from 0. Despite the previously mentioned similar distribution of the roughness
profile parameters Ra and Rz with the surface topography parameters Sa and Sz, some
discrepancies could be observed in the correlation study. They may have resulted from
the fact that the Rz parameter is only determined only in the 2D cross-section in one ori-
entation, while the Sz parameter informs the size of the elevations on the tested surface.
In the conducted studies, it was noticed that the sandblasting parameters have a sig-
nificant influence on the adhesive joint strength. It was shown in [47] that both the surface
roughness and the adhesive properties, such as surface free energy, are more dependent
on the type of the abrasive material that is used and not on differences in the sandblasting
pressure value. Other factors such as sandblasting agent and its abrasive particle size also
influence adhesion. In this work, increasing the ratio of the valley depth to the tip height
as a result of changing sandblasting parameters, as evidenced by the change in Ra and Rz
surface roughness parameters, has a positive effect on the adhesive joint strength. In turn,
Staia et al. [68] emphasized that the sandblasting process allows a favorable adherend
surface roughness to be obtained and provides the mechanical anchoring between the ad-
hesive and the adherend surface and also depends on one of the sandblasting parameters,
which is the pressure during this treatment. In another work [69], the strength and the
Materials 2021, 14, 6626 18 of 21

surface roughness parameters were compared, and it was noticed that in the case of the
adhesive joints in which there is a significant roughness of the surfaces of the adherends,
there is a greater relationship between the values: the set of Rz and Rt surface roughness
parameters and the adhesive joints strength. Mandolfino et al. [70] indicated that the prop-
erties of bonded surfaces obtained after the sandblasting process affect the strength of the
adhesive joints and also indicated that the type of the sand and the sandblasting pressure
also had an effect on the strength of the adhesive joints.

5. Conclusions
An important aspect affecting the strength of the adhesive joints, apart from the
proper selection of the adhesive composition, is the proper preparation of the adherend
surfaces. In the case of the bonding aluminium alloys, the recommended method is the
sandblasting. Studies were carried out on the influence of the sandblasting parameters as
a method of the surface treatment on the static strength of EN AW 2024 T3 aluminium
alloy adhesive joints. This surface treatment method for the bonding was a variable factor
in the tests, while factors such as the type of the adhesive and other bonding conditions
remained constant during the tests. The roughness measurements of the treated surfaces
and surface free energy measurements were also carried out. Based on the strength results
obtained for the adhesive joints of the aluminium alloy sheets, the following conclusions
can be drawn:
• Both the properties of the adhesive (in particular its viscosity) and the geometric
structure of the adhesion surface, after the application of certain surface treatment
methods, significantly influence the formation of the actual adhesive–binder inter-
face, as this ensures relatively the high strength due to, among other things, the sig-
nificant role of the mechanical adhesion;
• Increasing the ratio of valley depth to tip height as a result of changing sandblasting
parameters, as evidenced by the change in Ra and Rz parameters, has a positive effect
on the strength of the adhesive joints;
• Sandblasting parameters have a significant influence on the strength of adhesive
joints. The selection of appropriate parameters is a key factor for obtaining a well-
developed surface. The tests conducted here have determined that the pressure of
the sandblasting process should not be less than 5 × 105 Pa, the distance of the noz-
zle from the sandblasted surface should not be greater than 97 mm, and the speed at
which the workpiece is displaced in relation to the nozzle should not be greater than
75 mm/min. Exceeding these parameters results in a decrease of the roughness profile
parameters as well as the value of the surface free energy and thus in a decrease of
the shear strength of the constituted adhesive joints;
• The joints with the highest strength were prepared by abrasive blasting with the fol-
lowing parameters: nozzle distance from the sample—h = 97 mm, blasting speed—V
= 53 mm/min, pressure—P = 5 × 105 Pa. In the case of these joints the highest result
repeatability was also obtained.

Author Contributions: Conceptualization, I.M.-B.; methodology, I.M.-B., A.R., and E.D.; software,
I.M.-B.; validation, I.M.-B.; formal analysis, I.M.-B.; investigation, I.M.-B., A.R., and E.D.; resources,
I.M.-B., A.R., and E.D.; data curation, I.M.-B.; writing—original draft preparation, I.M.-B.; writing—
review and editing, I.M.-B.; visualization, I.M.-B.; supervision, I.M-B.; project administration, I.M.-
B.; funding acquisition, I.M.-B. All authors have read and agreed to the published version of the
manuscript.
Funding: This project/research was financed in the framework of the project Lublin University of
Technology-Regional Excellence Initiative, funded by the Polish Ministry of Science and Higher Ed-
ucation (contract no. 030/RID/2018/19).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Materials 2021, 14, 6626 19 of 21

Data Availability Statement: The raw/processed data required to reproduce these findings cannot
be shared at this time due to technical or time limitations. Data can be made available on individual
request.
Acknowledgments: Faculty of Mechanical Engineering, Lublin University of Technology, Lublin,
Poland.
Conflicts of Interest: The authors declare no conflicts of interest.

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