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Author’s Accepted Manuscript

The effect of sandblasting on surface properties for


adhesion

Anna Rudawska, Ing. Izabela Danczak, Miroslav


Müller, Petr Henc

www.elsevier.com/locate/ijadhadh

PII: S0143-7496(16)30133-6
DOI: http://dx.doi.org/10.1016/j.ijadhadh.2016.06.010
Reference: JAAD1864
To appear in: International Journal of Adhesion and Adhesives
Received date: 11 January 2015
Accepted date: 25 June 2016
Cite this article as: Anna Rudawska, Ing. Izabela Danczak, Miroslav Müller and
Petr Henc, The effect of sandblasting on surface properties for adhesion,
International Journal of Adhesion and Adhesives,
http://dx.doi.org/10.1016/j.ijadhadh.2016.06.010
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Anna Rudawska1, Ing. Izabela Danczak2 Miroslav Müller3, Petr Henc3
1
Lublin University of Technology, Department of Production Engineering
36 Nadbystrzycka Str. 20-618 Lublin, Poland, e-mail: a.rudawska@pollub.pl
phone number: (+48 81) 53-84-232
2
Technical University of Dresden, Institute of Lightweight Engineering and Polymer
Technology (ILK), Holbeinstr. 3, 01307 Dresden, Germany
3
Department of Material Science and Manufacturing Technology, Faculty of Engineering
Czech University of Life Sciences, Kamycka 129, Praha - 6 Suchdol, 165 21, Czech Republic

The effect of sandblasting on surface properties for adhesion

Abstract:

The paper presents the effect of sandblasting on surface properties of steel for
adhesion. The investigated parameters included pressure (1, 2 and 4 bars) and four types of
abrasive material, each material type being of different granulation. In the experiments the
effect of the above variables on the surface roughness, contact angle , work of adhesion
Wa and surface free energy  was investigated. It has been shown in this research that
surface properties are more affected by abrasive material type applied rather than by the
sandblasting process parameters.

Keywords: surface properties, work of adhesion, surface free energy, sandblasting

1. Introduction

Surface treatment is one of the most important factors governing the strength of
adhesive joints [1-5]. There are numerous methods of pre-treatments of joining materials [6-
9]. The most common treatments are mechanical, chemical and electrochemical methods.
The mechanical methods consist of roughening processes by, for example, grit-blasting,
sandblasting or abrasion [4,10-12].
Roughening surfaces prior to bonding generally enhances adhesive joint strength. An
increase of adherend roughness should lead to an increase of effective area for the bond
[13]. However, it is reported that excess roughness decreases the ability for adhesive
penetration, increasing void formation and therefore introducing localized stress
concentration [14,15]. Indeed, a decrease of strength is often found when the adherend
surface is too rough. The value of critical roughness depends on many parameters, such as,
for example, the roughening pre-treatment applied, the type of adherend, the type of
adhesive, the geometry of the joint and the stresses applied. It has also been found that
roughening may introduce physico-chemical changes, which affect wettability and surface
free energy [1]. Surface roughness can also affect the spreading of the adhesive, either
because the adhesive cannot penetrate the adherend or because it gels before it completes
the penetration. The relationship between roughness and adhesion is not very simple.

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Optimum surface profile varies from one adhesive to another, and depends upon the type of
stress applied [16].
The effect of surface roughness on wettability has been studied by many researchers
using surface roughness factors such a the Wenzel roughness factor [17,18]. The effect of
density and height of peaks on adhesion fracture strength has been discussed by Kunio and
Mitsuru [19]. The effect of grit-blasting on surface properties for adhesion has been
presented by Harris and Beevers [12]. The same issue of surface pre-treatment on an
aluminium surface has been investigated by Prolongo and Urena [14]. Shahid and Hashim
[20] examined the influence of surface roughness of a steel adherend on cleavage strength.
Hay, Dragila, and Liburdy [21] presented some information on the influence of surface
roughness on wettability.
Sandblasting is the operation of forcibly propelling, under high pressure, a stream of
abrasive material against a surface in order to clean the surface or influence its shape.
Sandblasting is recommended to be used prior to the application of a paint coating to a
surface. The first sandblasting process was patented by Benjamin Tilghman in 1870 [22].
Sand is the most commonly used abrasive material, yet other fine materials can be used,
including copper slag, shot, glass, metal, dry ice, garnet (mineral), as well as bits of coconut
shell or other plants.
Sandblasting is often recommended to be applied to surfaces of various structural
materials prior to adhesive bonding, these materials including steel [23], titanium or
titanium alloys [24,25], aluminum alloys [4, 13] and polymers (polyester, polyethylene) or
composites [26,27]. Bresson et al [13] investigated the different conditions of sandblasting:
the pressure and also the type of grit. Some information of description of sandblasting test is
presented in [20,25,26,28].
Although sandblasting produces effects similar to those of grinding, sandblasted surfaces
are less rough and more uniform compared to those subjected to grinding operations. In
addition sandblasting can be applied to surfaces of irregular shape. Roughness of adherend
surfaces has frequently been used as design parameters for adhesive joints [20,21,29,30].

The purpose of this work was to study the effect of sandblasting parameters on the surface
properties of steel and thus identify the surface characteristics vital for optimum adhesive
joint strength performance.

2. ANALYSIS

For ideal surfaces, which are considered to be rigid, smooth (surface roughness << 0.5 μm)
and chemically homogeneous [31-33], there exists only one contact angle, which is the true
equilibrium contact angle [34,35]. However, for real surfaces, there may be several observed
contact angles (advancing and receding contact angles), which results in contact angle
hysteresis [36-41].

2.1. Contact angle hysteresis

When a liquid drop is placed on a solid, it spreads until it attains an equilibrium state. If
additional liquid is added to the drop, the contact line advances and stops. The drop exhibits
an advancing contact angle a in the cases of each time motion (Fig. 1a). If liquid is removed
from the drop, the contact angle decreases without movement of the contact line. If enough

2
liquid is removed, the contact line retreats. The drop exhibits a receding contact angle r.
The difference between a and r is referred to as contact angle hysteresis [37].

a) b)

Fig 1. Side view of a sessile liquid drop on the solid surface: a) advancing contact angle a,
b) receding contact angle r

Contact angle hysteresis H (1), exists when there is inequality of the advancing angle a and
receding contact angle r [38]
H   a  r (1)

Contact angle hysteresis is most often defined empirically as arithmetic difference (2) [37],

 = a - r (2)

And a ratio H (3), has been used to denote the hysteresis for a surface [39].

H = (a - r )/ a (3)

The advancing contact angle is less sensitive to surface roughness and heterogeneity than
the receding contact angle. Therefore, advancing contact angle data are commonly used to
calculate surface and interfacial tension components [42,43].

The advancing angle a and receding contact angle r are often defined in dependence on
the triple line motion on formerly non-wetted or wetted area. This kind of definition is
dependent on the image resolution, the frame rate and the conditions used for the optical
identification of the drop shape [44].

Contact angle hysteresis has been attributed to solid surface roughness, surface chemical
heterogeneity, penetration of liquid into solid surface, swelling, and also surface
reorientation of functional groups [45-47]. Surface roughness is not expected to result in
contact angle hysteresis for relatively smooth surfaces (roughness surfaces less than
approximately 0.5 m) [38].

2.2. Work of adhesion Wa

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The work of adhesion Wa describes the work required to create a surface unit due to
separating the measuring liquid and tested material. Wa can be defined by the following
equation (4) [17,48,49]:
Wa= L (1+cos) (4)

The Young-Dupree equation is fulfilled if the contact angle depends only on the solid surface
tension but not roughness and ranged from 180 to strictly zero degree. If spreading of the
liquid over solid surface is observed it is difficult to state that this equation is fulfilled.

Most existing theoretical models assume that imperfections such a roughness or


heterogeneities, cause hysteresis of contact angle [17,36,40,41,50]. One approach is to
ignore the details of the interface and use a thermodynamic approach to describe hysteresis
[37]. A model based on Young’s equation has been used to calculate the work of adhesion
from contact angle hysteresis W [37,51,52],

W = L (cos r – cos a) (5)

where:
L – the surface free energy of contact liquid,
r – receding contact angle,
a – advancing contact angle.

The work of adhesion from the contact angle hysteresis W (eq. 5) value agrees reasonably
well with the hysteresis in solid-solid surface energy measurements for finite contact angles
on low-energy surfaces [53,54].

2.3. Wetting and wetting criteria

Wetting of liquids on solid surfaces is a topic of fundamental interest with widespread


technological implications, for example during bonding. Adhesives with surface energies less
than that of an adherend will readily wet the surface and form good bonds. The adhesive will
spread on the adherend when the surface free energy of the adherend is greater than that
of the adhesive [17]. If sufficiently intimate contact is achieved between the adhesive and
adherend a physical interaction develops between the atoms of the two surfaces, which
results in wetting.

Wetting may be due to: van der Waals forces (dipole-dipole and dispersion forces), acid-base
interactions and weak hydrogen bonding [17]. The extent of wetting depends on the
differences in the surface free energies of the solid, liquid and subsequent interface.
For wetting to occur spontaneously, the following condition should be applied (eq. 6 and eq.
7 [55]:
sv  sl + lv, (6)

where:
sv – interfacial surface free energies for solid-vapor,
sl – interfacial surface free energies for solid-liquid,
lv – interfacial surface free energies for liquid-vapor.

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sv  lv, or adherend  adhesive, (7)

The criterion for estimating the wetting process is defined as the magnitude of the spreading
coefficient S [56] described by the following equation (8) [17,57] and equation (9) [58]:

S = sv - sl - lv  0 (8)


or
S = Wa - 2 (9)
where:
Wa – work of adhesion,
L – surface free energy of a wetting liquid.

According to this theory, wetting can be considered thorough when S is positive, the liquid
droplet at equilibrium will be spread completely over the solid [18]. When the spreading
coefficient S is negative, partial wetting will occur, leading to a non-zero contact angle  at
the junction of solid-liquid-vapor [59]. However, the geometric aspect or processing
conditions, such as the surface roughness of the solid and applied external pressure, can
restrict the applicability of this criterion [17].

2.4. Surface free energy

The surface free energy of a solid s can be obtained from equilibrium contact angle
measurements of a series of test liquids on the solid surface, providing the relationship
between sl and the solid s and liquid lv surface energies [17,18,56].
The surface free energy of solid S can be expressed by the sum of the dispersive (Sd) and
polar (non-dispersive) (SP) components [17,48,60,61]:

S = Sd + SP (10)

The London forces are connected with dispersive intermolecular interactions (included
dipole-induced dipole interactions) The apolar or dispersion component results from
induced-dipole-induced dipole (dispersion) interactions. The polar component contains the
dipole-induced dipole (Debye-van der Waals interactions) and dipole-dipole (Keesom-van
der Waals) interactions as well as hydrogen bond and pi-electron interactions. [62].
Owens and Wendt used equation 10 to derive a relation for the work of adhesion W a (eq.
11) [17]:

Wa = Wad+ Wap (11)

where:
Wad – derived from the London dispersion forces,
Wap – derived from non-dispersive forces.

For the liquid-solid system interacting by dispersion forces only, equation (11) can be
further developed by taking into account the geometric mean of the dispersion component
of both liquids, resulting in equation (12) [17,56]:

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sl = S + L -2 (SdLd)1/2 (12)

or equation (13)
L(1+ cos) = 2 (SdLd)1/2 (13)

Many researchers have developed a geometric mean approach which is an extension of


Fowkes’ models for the interfacial free energy between two phases, which can be applied to
a liquid drop on a solid surface. This theory considers also the polar term. The geometric
mean was used to combine the polar and dispersive components together (eq. 14 and eq.
15) [17]:

sl = S + L -2 (SdLd)1/2 - 2 (SpLp)1/2 (14)

L(1+ cos) = 2 (SdLd)1/2 + 2 (SpLp)1/2 (15)

To calculate the dispersive and polar components of the surface free energy of a solid the
values of contact angle measured for two liquids is needed [17,49].

3. EXPERIMENTAL TESTS
3.1. Materials
The tests were conducted on samples made of one type of carbon steel sheet: C45 (EN
10083-2/1.0503). C45 is a medium carbon steel and it is used when greater strength and
hardness is desired [63]. This carbon steel has good mechanical properties (Table 1 and Fig.
2).
Table 1. Some mechanical properties of C45 steel [64].
Rm,, MPa 580
Re, MPa 305
Minimum
A, % 16
mechanical properties
E, MPa 2.1105
Hardness, HB 207

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Fig. 2. Tempering temperature versus mechanical properties of C45 steel [65]

The main chemical composition of C45 steel is: carbon (C) from 0.42%, to 0.50%,
manganese (Mn) from 0.50%, to 0.80%, sulphur (S) max 0.025%, phosphorus (P) max
0.025%, silicon (Si) from 0.15% to 0.35% [66].

3.2. Surface treatment


The C45 steel specimens were subjected to sandblasting as surface treatment. The
variables applied in this mechanical treatment operation were: three different types of
abrasive material and pressure. General characteristics of the applied abrasive materials are
given in Table 2. The time of surface treatment in all variants of the process was maintained
the same.

Table 2. Technological parameters of sandblasting


Granulation, μm
No. Symbol Sandblasting medium
1 A brown fused alumina 150 ÷ 180
2 B brown fused alumina 2.5 ÷ 3.5
3 C white fused alumina 1400 ÷ 1700
4 D glass beads 70 ÷ 110

The pressure of the sandblasting media was set to 1 bar, 2 bar and 4 bar, respectively.
The operations were performed using the German sandblasting machine Clemco HS 200 P-1.
The process was performed at right angles to the substrate surface (to the horizontal) and at
a distance of about 100 mm from the nozzle for the duration of about 1 minute (Fig. 3).

Fig. 3. Schematic representation of the distance between sandblasting process nozzle and
substrate surface

The applied variants of sandblasting are characterized in Table 3.


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Table 3. Sandblasting variants applied

No. Sandblasting variant Symbol


1 No sandblasting applied, surface degreasing only O
2 Sandblasting with abrasive A, pressure: 1 bar, time: 1 min A-1-1
3 Sandblasting with abrasive A, pressure: 2 bar, time: 1 min A-2-1
4 Sandblasting with abrasive A, pressure: 4 bar, time: 1 min A-4-1
5 Sandblasting with abrasive B, pressure: 1 bar, time: 1 min B-1-1
6 Sandblasting with abrasive C, pressure: 1 bar, time: 1 min C-1-1
7 Sandblasting with abrasive C, pressure: 2 bar, time: 1 min C-2-1
8 Sandblasting with abrasive C, pressure: 4 bar, time: 1 min C-4-1
9 Sandblasting with abrasive D, pressure: 1 bar, time: 1 min D-1-1
10 Sandblasting with abrasive D, pressure: 2 bar, time: 1 min D-2-1
11 Sandblasting with abrasive D, pressure: 4 bar, time: 1 min D-4-1

For comparative reasons, the analysis of surface geometrical structure, adhesive


properties and strength was conducted also on specimens that were only degreased with an
acetone-based degreaser. Given that A and B is the same type of abrasive (the only
difference being its granulation), we investigated only the sandblasting variant with abrasive
B.

3.3. Surface roughness parameters


Surface roughness parameters were measured using a Perthrometr 2 profilometer and
NanoFocus scan AF2 in compliance with standard ISO 4278 requirements [67]. In the tests,
we measured the following parameters: Ra, Rz, Rp, Rv, Rk, Rpk, Rvk, Mr1, Mr2. The
parameters are briefly characterized in Table 4.

Table 4. Characteristics of surface roughness parameters

No. Parameters Characteristics


1 Ra Roughness average Ra is the arithmetic mean of the absolute values
of the roughness profile ordinates.
2 Rz Mean roughness depth Rz is the arithmetic mean value of the single
roughness depth Rzi of consecutive sampling lengths. Single
roughness depth Rzi is the vertical distance between the highest
peak and the deepest valley within a sampling length.
3 Rp Rp is the maximum peak height of the roughness profile within one
sampling length.
4 Rv Rv is the maximum valley depth of the roughness profile within one
sampling length. Previously, the parameter symbol Rm was used in
place of Rv.
5 Rk Core roughness depth Rk is the depth of the roughness core profile.
6 Rpk Reduced peak height Rpk is the mean height of the peaks

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protruding from the roughness core profile.
7 Rvk Reduced valley depth Rvk is the mean depth of the valleys
protruding from the roughness core profile.
8 Mr1 Mr1 is the lowest material ratio of the roughness core profile.
9 Mr2 Mr2 is the highest material ratio of the roughness core profile.

The overall height of the roughness profile Rz is the sum of the maximum peak height of
the roughness profile Rp and the maximum valley depth of the roughness profile Rv within
one sampling length.

The material ratio curve provides reliable information about profile shape and even about
the maximum valley depth of a profile. This curve can be used to describe variations in
properties of a profile depending on the profile's depth. The parameters defined using the
information provided by the material ratio curve include:
- Rk - core roughness depth,
- Rpk - reduced peak height,
- Rvk - reduced valley depth,
- Mr1 - the lowest material ratio of the profile peak,
- Mr2 - the highest material ratio of the profile valley.

The above parameters are usually sufficient to identify surfaces with the same Ra. Not
only do they provide information about roughness depth, but also roughness shape. Given
this, it seems that the material ratio curve and parameters determined thereby can be used
to analyze the suitability of a given surface for adhesive bonding, for example.

The above parameters are graphically illustrated in Fig. 2.

Fig. 2. Material ratio curve [67]

The reduced peak height Rpk is defined as the mean height of the peaks protruding from
the roughness core profile. This parameter describes behavior of sliding and running
surfaces in abrasion. A low Rpk means high resistance to abrasive wear.

The reduced valley depth Rvk is the mean depth of the valleys protruding from the
roughness core profile. The parameter defines oil retention capacity of the surface. For
example, lubricated surfaces are required to have a high Rvk. It might seem then that this

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parameter could be applied to determine the degree of roughness depth filling by an
adhesive in making adhesive joints. However, due to differences in viscosity of adhesives and
lubricants, it is the width of valleys that plays a significant role here.

Surface roughness is one of the major causes of thermodynamic hysteresis with contact
angles. The Wenzel equation [18] defines the effect of surface roughness on contact angle. It
is generally assumed that at Ra < 0.5 μm, roughness has a negligible effect on contact angle.
According to the Wenzel equation, an increase in Ra can either improve (when  < 90°) or
deteriorate (when  > 90°) wetting conditions [58].

3.4. Wettability and work of adhesion

The wettability of a steel surface can be examined by comparing the contact angles for water
(distilled water) and diidomethane since two solvents are often used as reference liquids in
analyses of the interactions of polar and apolar solvents with solid surfaces [38]. The contact
angle hysteresis was calculated according to eq. 1.

3.5. Surface free energy


The Owens-Wendt [17,68,69] method for calculation of solid surface free energy were
applied. The measurements were taken using two measuring liquids: polar (distilled water)
and apolar (diiodomethane), with known surface free energies and their non-dispersive
(polar) and dispersive components. Values of the surface free energy S and its components
as determined with the above measuring liquids are given in Table 5.

Table 5. Values of the surface free energy L and its components determined using measuring liquids
[17,48,70,71,72].
Surface free energy and its components Wetting liquids
Distilled water Diiodomethane
L, mJ/m2 72.8 50.8
Ld, mJ/m2 21.8 48.5
Lp, mJ/m2 51.0 2.3

The contact angle measurements were made with distilled water and diidomethane
taking an average of 8-12 drops with each type of liquid of each variant of treatment. Every
sandblasting variant was tested on 3-5 specimens, with the number of measurements for
each specimen ranging from 25-30 (for: 4 to 6 drops of each measuring liquid).

About 2 l of distilled water [58] and 1 l diiodomethane [58] was used for each
measurement at a temperature of 21±1oC and air humidity of 30±1%. Contact angles were
assessed within 5 s of drop formation. Final contact angle measurements were recorded
(usually within 10-15 s) once their values did not change after drop placement. Repeat
measurements of a given contact angle were all within 2.

The tests were conducted using a PGX goniometer manufactured by Fibro System and
computer image analysis software PG v.3.4.0.1. This goniometer has an integrated camera
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and captures 80 images/sec (640x480 pixels). The instrument automatically pumps out a
droplet, captures the liquid/substrate interaction and graphs the results. An illuminated
enlarged image of the droplet is projected onto the built-in groundglass screen. A 7-times
magnifying lens allows the contact angle to be read off precisely (at an accuracy of better
than 2°) using a rotated tangential ruler.

Some test conditions of contact angle measurement are derived from the ASTM D5946
standard [73]. The surface free energy of steel was calculated only apparently because the
contact angle values were used to SFE calculating not fulfilled the Young equation.

To calculate the surface free energy of steel, in terms of dispersive and polar components,
the Fowkes equation modified by Owens and Wendt (eq. 14) was used.

The components Sd and Sp of the examined materials may be calculated from the
formulas (17) and (18) – Owens-Wendt approach [74].

dp
 d cos  d  1   w cos  w  1
wp
 
s
d 0,5

 
(17)
p 
p

2  d   d w p 
d
 w 
 
 w cos  w  1  2  s d  w d
 
s
p 0,5
 (18)
2 w
p

where: sd – dispersive component of surface free energy of the materials examined, sp
– polar component of surface free energy of the materials examined, d - surface free
energy of diiodomethane, dd – dispersive component of diiodomethane surface free
energy, dp – polar component of diiodomethane surface free energy, w – surface free
energy of water, wd – dispersive component of water surface free energy, wp – polar
component of water surface free energy, Θd – contact angle of diiodomethane, Θw –
contact angle of water.
4. RESULTS AND DISCUSSION
4.1. Surface roughness
Surface roughness was investigated by measuring selected surface roughness parameters,
determining surface roughness profile and geometrical structure of surfaces of the tested
materials.
Surface roughness parameters produced by sandblasting were estimated from 3 locations
on each surface of 5 samples of each variant of sandblasting (15 measurements of each
variant of sandblasting).
Examples of the roughness profile and view of steel sheet surfaces after degreasing are
shown in Fig. 5.

a)

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b)

Fig. 5. Roughness profile (a) and surface (b) of C45 steel sheet after degreasing

The surface of a C45 steel sheet that was subjected to degreasing exhibits slight surface
roughness (Ra = 0.086 μm, Rz=0.665 μm) as well as a considerable uniformity of roughness
across the entire area of the specimen.
Examples of the roughness profile of steel sheet surfaces following the application of three
variants of sandblasting with abrasive A are illustrated in Fig. 6, while Fig. 7 shows the
surface treated with sandblasting variant A-2-1.
a)

b)

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c)

Fig. 6. Roughness profile of a C45 steel sheet surface after sandblasting:


a) A-1-1, b) A-2-1, c) A-4-1

Fig. 7. C45 steel sheet surface after sandblasting A-2-1

Examining the obtained roughness profiles (Fig. 6) and of the surface itself (Fig. 7), it can
be observed that the value of pressure in sandblasting with abrasive A does not have any
significant effect on the surface roughness profile.
An example of the roughness profile of a steel sheet surface sandblasted with abrasive B
(B-2-1) and a view of the surface after the application of this sandblasting variant are shown
in Fig. 8.

a)

13
b)

Fig. 8. Roughness profile (a) and surface (b) of a C45 steel sheet after sandblasting B-2-1

The surface roughness and profiles of surface roughness after the application of the
highest applied sandblasting pressure (4 bar) and different abrasive materials are compared
in Fig. 9 and in Fig. 10.
a) b)

c)

14
Fig. 9. Surface roughness of a C45 steel sheet: a) A-4-1, b) C-4-1, c) D-4-1

a)

b)

c)

15
d)

Fig. 10. Roughness profile of a C45 steel sheet surface after sandblasting: a) A-4-1,
b) B-4-1, c) C-4-1, d) D-4-1

The results given in Figs. 5-8 reveal a certain relationship between the application of a
higher sandblasting pressure and surface roughness, depending on the type of abrasive
used. The surfaces subjected to sandblasting with abrasive D (glass beads) have the smallest
roughness.
Moreover, comparing the results of the sandblasting variant wherein the pressure was
set to 2 bar (Fig. 5b and Fig. 8b), it can be observed that the geometrical structure of the
tested steel sheet surfaces is clearly different - when abrasive B is applied, the results are
nearly twice as high.
Bresson et al. [13] tested sandblasting under various conditions: the effect of relative
distance between the sandblasting nozzle and the aluminium surface (“far” and “near”).
They observed that increasing the period of sandblasting for ‘far” configuration decreased
dispersion of the results in terms of roughness measurement, but it does not modify the
average significantly. For the “near” configuration an arithmetic mean roughness of about
2.850.17 m was found and for “far” configuration – 2.720.16 m was evaluated.

4.2. Contact angle hysteresis and work of adhesion Wa


The values of advancing contact angle a, receding contact angle r and contact angle
hysteresis H for steel samples after sandblasting variants are listed in Table 6.

Table 6. Advancing contact angle a, receding contact angle r and contact angle hysteresis
H for steel samples after sandblasting variants
No. Surface treatment Water Diidimethane
a/r,  Hw,  a/r,  Hd, 

16
1 O 84.6/81.1 3.5 34.7/30.0 4.7
2 A-1-1 105.5/88.9 16.6 16.8/12.1 4.7
3 A-2-1 111.5/78.2 33.3 18.3/12.2 6.3
4 A-4-1 107.9/100 7.9 16.7/12.3 4.4
5 B-2-1 82.3/79.2 3.1 13.8/10.3 3.5
6 C-1-1 96.0/84.4 11.6 12.5/8.0 4.5
7 C-2-1 96.8/84.1 12.8 13.7/8.0 5.7
8 C-4-1 89.9/84.1 5.8 15.8/11.1 4.7
9 D-1-1 49.7/42.4 7.3 30.2/23.9 6.3
10 D-2-1 46.4/42,2 4.2 32.7/26.9 5.8
11 D-4-1 41.7/36,7 5.0 33.0/24.7 8.3

The hysteresis varies widely and generally decreases with contact angle. The contact
angle hysteresis for all investigated surface treatment variants are given in Fig. 11 and Fig.
12.

Fig. 11. Comparison of the water contact angle hysteresis Hw after the application of
different variants of sandblasting

17
Fig. 12 Comparison of the diidomethane contact angle hysteresis Hd after the application of
different variants of sandblasting

The lowest water contact angle hysteresis Hw after sandblasting was obtained
sandblasting variant D-2-1 (H = 3.1º) and in variants of sandblasting with abrasive D (Fig. 11).
The highest water contact angle hysteresis Hw was observed for the surfaces subjected to
sandblasting with abrasive A (Table 6, Fig. 11). The surface of steel sheets treated with
distilled water exhibited an intermediate wetting state only after degreasing.
When the nonpolar liquid (diiodomethane) was applied, the surfaces subjected to
sandblasting with abrasive B had the lowest water contact angle hysteresis Hw (Table 6, item
5), while the highest water contact angle hysteresis Hw values were observed for the
surfaces subjected to sandblasting with abrasive D (Table 6, items 9-11).
The abrasive material C was characterized by the largest size of particles, while abrasive B
had the smallest particles. Also, abrasives A and B are brown fused alumina with different
sizes of abrasive particles. Given the above results, it can be observed that the size of
abrasive material particles does not affect the contact angle and contact angle hysteresis H.
Rather, this effect depends on the type of abrasive material used.
The work of adhesion from contact angle hysteresis W for wetting liquids was calculated
from equation (5). The results of the work of adhesion from contact angle hysteresis
regarding the applied surface treatment variants and measuring liquids are listed in Table 7
and in Fig. 13.

18
Table 7. The work of adhesion from contact angle hysteresis of distilled water (Waw) and
diiodomethane (Wad)
No. Surface treatment Work of adhesion, mJ/m2

Waw Wad
1 O 4.4 2.2
2 A-1-1 2.9 1.0
3 A-2-1 41.6 1.4
4 A-4-1 9.7 1.0
5 B-2-1 3.9 0.6
6 C-1-1 14.7 0.8
7 C-2-1 16.1 1.0
8 C-4-1 7.4 1.0
9 D-1-1 6.7 2.5
10 D-2-1 3.7 2.6
11 D-4-1 4.0 3.5

Waw

Wad

Fig. 13. Comparison of Waw and Wad after the application of the investigated surface
treatment variants

Analyzing the results given in Table 7 and Fig. 13, the following observations can be made:
- the application of the polar liquid (distilled water) produced the highest Waw (41,.6
mJ/m2) in the sandblasting variant marked as D-2-1, while the lowest Waw was obtained in
sandblasting A-1-1. Bearing in mind that the above results were obtained for the same
sandblasting abrasive materials, it can therefore be claimed that adhesion work is more
affected by the type of abrasive used rather than surface treatment parameters;
- sandblasting with abrasive A and C (i.e. two types of alumina with different granulation)
produced the highest values of Wa, while other abrasive materials (D) produced generally
the lowest Wa; Consequently, it can be claimed that the application of glass beads as
abrasive material leads to obtaining less satisfactory values of Wa than when using alumina;
19
- the work of adhesion from contact angle hysteresis of diiodomethane (Wad) of abrasive D
was the higher than other abrasive materials and for abrasive material D there is the
smallest differences between Waw and Wad;
- following the application of different surface treatment variants, the adhesion work Wad
was less varied than the adhesion work Waw;
- with regard to conditions of wetting the most favorable wetting conditions for polar liquids
can be obtained using sandblasting with abrasive A and C.

4.3. Surface free energy S


Surface free energy and its components of the surface-treated specimens, obtained from
the mean contact angle measurement using distilled water and diiodomethane (geometric
mean), are given in Table 8.

Table 8. Surface free energy S and its components of a steel sheet surface following
different surface treatments – geometric mean (Owens-Wendt method)

No. Surface treatment Surface free energy


and its components, mJ/m2
S  Sd  Sp
1 O 45.51.4 43.5 2.0
2 A-1-1 49.10.5 49.1 0.0
3 A-2-1 49.21.4 49.2 0.0
4 A-4-1 49.60.1 48.7 1.1
5 B-2-1 51.60.6 49.7 1.7
6 C-1-1 50.30.8 50.1 0.2
7 C-2-1 50.21.0 50.0 0.2
8 C-4-1 50.10.9 49.4 0.7
9 D-1-1 63.32.7 45.3 18.0
10 D-2-1 63.51.9 44.0 19.4
11 D-4-1 66.52.2 44.7 21.8

Analyzing the results of surface free energy and its components (Table 8), it can be
observed that the highest values were obtained in sandblasting with abrasive D (glass
beads), while the lowest ones were produced by degreasing. Sandblasting with abrasive D
(Table 8, Items 9-11) also produced the highest ratios of the polar component of surface free
energy.
It was found that the type of abrasive used is of more significance to surface treatment
than pressure. The results of the experiments in table 8 show that, in general, glass beads
(abrasive D) display the higher surface free energy values than brown or white fused
alumina. Moreover white fused alumina displays the higher surface free energy values than
brown fused alumina. Harris and Beevers [12] also observed during grit-blasting that white
grit compositions usually cause the higher values of surface free energy than brown. The
surface free energy values after grit-blasting are from 45 mJ/m2 to 70 mJ/m2 for mild steel
and 43-68 mJ/m2 for aluminium alloy.
Values of surface free energy and its components obtained after the application of
different surface treatment variants are given in Figs. 14, 15 and 16.
20
Fig. 14. Effect of abrasive material type on surface free energy and its components –
sandblasting: pressure - 1 bar, time - 1 minute

Fig. 15. Effect of abrasive material type on surface free energy and its components –
sandblasting: pressure - 2 bar, time - 1 minute

21
Fig. 16. Effect of abrasive material type on surface free energy and its components –
sandblasting: pressure - 4 bar, time - 1 minute

The results of surface free energy and its components (Figs. 14-16) after the application of
all investigated surface treatment variants demonstrate that the lowest S is exhibited by the
surfaces that were only degreased at 45.5 mJ/m2 (Table 8, item O). In contrast, the highest
values were obtained in sandblasting with abrasive D. This variant of surface treatment also
yields the highest ratios of polar component of the total surface free energy, these ratios
ranging from 28 to 33% of the surface free energy. This regularity is observed for every
pressure variant applied in sandblasting.

Surface treatment where the same abrasive material was applied produced similar values
of S. Nonetheless, it was found that for every type of abrasive material used, the variant
wherein the highest pressure was applied (Fig. 16) exhibited the highest ratio of the polar
component Sp, compared to the operations in which other pressures were applied.

Harris and Beevers [12] also observed during grit-blasting that, in general, the dispersive
component of surface free energy is higher than the polar component and the brown and
white grit composition produced different values of surface free energy. Also the brown grit
composition has a lower surface free energy with higher dispersive and lower polar
components than other grit sandblasting medium. In this study (Figs. 14-16) similar
observations were obtained.

It can be claimed that this type of abrasive material (glass beads of particular dimensions)
helps produce surfaces with considerably different energy parameters than is the case with
sandblasting variants based on the use of other types of abrasive material.

22
4.4. Surface free energy and surface roughness
Tables 9-13 compare the obtained dispersive and polar components of surface free
energy as well as surface roughness parameters Ra, Rz, Rp, Rv.

Table 9. Dispersive and polar components of surface free energy and parameters Ra, Rz, Rp,
Rv – different abrasives used, sandblasting: pressure - 2 bar, time - 1 min, degreasing

No. Surface Parameter


treatment  d
S ,  p
S , Ra, μm Rz, μm Rp, μm Rv, μm
mJ/m2 mJ/m2
1 A-2-1 49.2 0.0 1.630.13 10.40.42 5.080.40 5.060.75
2 B-2-1 49.7 1.7 4.151.86 34.612.7 10.902.45 10.902,67
3 C-2-1 50.0 0.2 1.620.62 10.90.57 4.590.17 5.930.40
4 D-2-1 44.0 19.4 0.700.04 4.090.56 2.350.40 2.140.16

Table 9 presents the results of sandblasting when different types of abrasive material were
used but surface treatment parameters were maintained the same. The results (Table 9)
point to certain dependencies between the dispersive component of surface free energy and
the investigated surface roughness parameters; these dependencies can be described using
coefficient of correlation () or (r). In the analysis the Pearson correlation coefficient [75,76],
commonly called simply "the correlation coefficient", which is sensitive only to a linear
relationship between two variables, was used. It is obtained by dividing the covariance of the
two variables by the product of their standard deviations. The correlation coefficient ρX,Y
(19) between two random variables X and Y with expected values μX and μY and standard
deviations σX and σY is defined as:

(19)

where E is the expected value operator, cov means covariance, and corr is a widely used
alternative notation for the correlation coefficient.
The Pearson correlation is +1 in the case of a perfect direct (increasing) linear relationship
(correlation), −1 in the case of a perfect decreasing (inverse) linear relationship
(anticorrelation) [75], and some value between −1 and 1 in all other cases, indicating the
degree of linear dependence between the variables. As it approaches zero there is less of a
relationship (closer to uncorrelated). The closer the coefficient is to either −1 or 1, the
stronger the correlation between the variables.
The highest correlation coefficient was observed between Sd and Rp (maximum peak
height of the roughness profile). It was found that an increase in Rp leads to an increase in
the dispersive component of surface free energy. In contrast, the correlation between Rp
and the polar component is weak. The lowest values of the examined parameters were
obtained with two surface treatment variants: sandblasting with abrasive D (glass shot) and

23
degreasing. It can therefore be claimed that the type of abrasive used has a significant effect
on surface roughness and adhesive properties.

Fig. 17. The correlation coefficient between the surface free energy components and surface
roughness parameters for results in Table 9

The highest correlation coefficient (0.72) was observed between Sd and Rv (the maximum
valley depth of the roughness profile within one sampling length). It was found that an
increase in Rv leads to an increase in the dispersive component of surface free energy. In
contrast, the correlation between Rv and the polar component is different. It can therefore
be claimed that the type of abrasive used has a significant effect on surface roughness and
adhesive properties.

Table 10. Dispersive and polar components of surface free energy and parameters Ra, Rz,
Rp, Rv – sandblasting with abrasive A

No. Surface Parameter


treatment  d
S ,  p
S , Ra, μm Rz, μm Rp, μm Rv, μm
2 2
mJ/m mJ/m
1 A-1-1 49.1 0.0 1.510.12 9.470.89 4.870.43 5.200.44
2 A-2-1 49.2 0.0 1.630.13 10.40.42 5.080.40 5.060.75
3 A-4-1 48.7 1.1 1.310.02 8.510.31 4.290.11 4.440.20

Table 10 gives the results of sandblasting with abrasive A (brown fused alumina, grain
size: 150-180 m). These results reveal a correlation between the dispersive and polar
components of surface free energy and the tested roughness parameters. The correlation
coefficients of the dispersive component Sd and roughness parameters are as follows: Ra =
0.98; Rz – 0.95; Rp – 0.99; Rv – 0.93. The close the coefficient is to 1 the stronger the
correlation between the dispersive component of surface free energy and surface roughness
parameters.

24
Fig. 18. The correlation coefficient between the surface free energy components and surface
roughness parameters for results in Table 10

The correlation coefficients of the polar component Sp were: -0.92; -0.87; -0.97; and -
0.98, respectively. This means that an increase in roughness leads to a proportional increase
in the dispersive component Sd and to a parallel decrease in the polar component Sp. The
close the coefficient is to -1 the stronger the correlation between the variables.
The example of the correlation coefficients of the dispersive component Sd and Rp
roughness parameter (Table 10) is presented in Fig. 19.

Fig. 19. The correlation coefficients of the dispersive component Sd and Rp roughness
parameter (Table 10)

25
Table 11. Dispersive and polar components of surface free energy and parameters Ra, Rz,
Rp, Rv – sandblasting with abrasive C
No. Surface Parameter
treatment  d
S ,  p
S , Ra, μm Rz, μm Rp, μm Rv, μm
mJ/m2 mJ/m2
1 C-1-1 50.1 0.2 1.240.11 8.290.37 4.090.40 4.460.03
2 C-2-1 50.0 0.2 1.620.62 10.90.57 4.590.17 5.930.40
3 C-4-1 49.4 0.7 1.410.13 8.941.66 3.520.84 4.330.48

In sandblasting with abrasive C (white fused alumina), where particle dimensions ranged
from 1400 - 1700 μm, a correlation was observed between the two components of surface free
energy and the Rp parameter (maximum peak height of the roughness profile). The correlation
coefficient of the dispersive component is 0.81, while that of the polar component is -0.88.

Fig. 20. The correlation coefficient between the surface free energy components and surface
roughness parameters for results in Table 11

This means that an increase in Rp causes an increase in the dispersive component and a
parallel decrease in the polar component. Observed dependencies between other surface
roughness parameters are negligible.

Table 12. Dispersive and polar components of surface free energy and parameters Ra, Rz,
Rp, Rv – sandblasting with abrasive D
No. Surface Parameter
treatment Sd, Sp, Ra, μm Rz, μm Rp, μm Rv, μm
2 2
mJ/m mJ/m
1 D-1-1 45.3 18.0 0.840.02 5.120.08 2.660.12 2.400.03
2 D-2-1 44.0 19.4 0.800.01 4.300.11 2.010.25 2.210.13
3 D-4-1 44.7 21.8 0.700.04 4.090.56 2.350.40 2.140.16

26
The application of sandblasting with abrasive D (glass beads) produced the highest values
of the polar component of surface free energy and the lowest values of the investigated
roughness parameters.

Fig. 21. The correlation coefficient between the surface free energy components and surface
roughness parameters for results in Table 12

Fig. 22. The correlation coefficients of the dispersive component Sp and Ra roughness
parameter (Table 12)

A certain dependence was observed between the following parameters: Sd and Rp; Sp
and Ra, Sp and Rz, Sp and Rv. The correlation coefficients were: 0.99; -1.0; -0.89; and -0.92,
respectively (Table 12, Fig. 21, Fig. 22). The results of sandblasting with abrasive D reveal a
relationship between the dispersive and polar components and surface roughness
parameters.

27
The results presented in Fig. 17, Fig. 18, Fig. 20 and Fig. 21 show that with all the
sandblasting variants investigated, parameters that increase surface roughness result in
decreasing values of the polar component of surface free energy. In some cases the closer
the coefficient is to −1, the stronger the correlation between the variables.
Harris and Beevers [12] presented that, in general, smoother grit-blasted surfaces display
higher surface energy values. Hitchcock et al. [77] also observed that, within certain limits,
roughening a substrate usually causes its wettability to decrease. Some researchers have
suggested that the peaks, ridges and asperities form barriers which restrict the spreading of
the droplet.
Shanahan [78] reported that heterogeneities such as surface roughness could produce a
positive influence on wetting characteristics of a drop by “pulling” the liquid mass towards
the abnormality but the negative effect of peaks and asperities on wetting characteristics
was observed.
Birkeman [79] suggested that wetting was independent of roughness on grooved and
ridged surfaces and implied that as drop front moves across a ridge the true contact remains
constant.
Packham [18] reported that the contact angle between a liquid and a rough surface
depends on the details of the topography. For example penetration into an idealized pore,
occurs until the back pressure of trapped air equals the capillary driving pressure.
Several researchers have compared the various surface roughness parameters with
surface free energy or wetting or contact angle. Although some research [37] suggested that
surface roughness was relatively unimportant during contact angle measurement. The
various surface roughness parameters were used to characterize the surface topography for
example to bonding also. Harris and Beevers [12] presented the effect of the surface
roughness parameter Rq on surface free energy. Bresson et al. [13] used the arithmetic
mean roughness Ra. Shahid and Hasim [20] studied the surface roughness parameters Ra
and Rlo after polishing and grit-blasting. Jiang et al. [25] measured the Ra after sandblasting
titanium. Moghadamzadeh et al. [11] used the Ra and Rz (also Sa and Sz) surface roughness
parameters to characterize the surface topography after surface treatment. The same
parameters were measured by da Silva et al. [1].

5. SUMMARY

Summing up, it can be observed that the application of sandblasting produces surfaces
with different roughness parameters and surface properties for adhesion. The above factors
play a significant role in the treatment of surfaces which are, for example, to be bonded.
In the experiments, we applied three types of abrasive material and variable pressures.
The experiments demonstrated that both surface roughness and adhesive properties are
more affected by the type of abrasive material used rather than by variations in pressure. It
is commonly known that surface free energy and surface characteristic for adhesion are
dependent on a complex interaction between surface texture and chemical components. But
other factors such as sandblasting media and its particle size have an influence on the
adhesion characteristics of surfaces.
The application of abrasive material D (glass beads) leads to the highest values of surface
free energy as well as a much higher value of the polar component than is the case with
other surface treatment variants. What is more, in sandblasting with abrasive material D, the

28
roughness parameters Ra, Rz, Rp, Rv are the lowest in the tested range. Also, this surface
treatment variant reveals a relationship between the polar component and roughness
parameters.
The majority of sandblasting variants applied demonstrate that, irrespective of the type of
abrasive used, the highest correlation occurs between Sd and Rp, i.e. the maximum peak
height of the roughness profile. It was found that an increase in Rp leads to an increase in
the dispersive components of surface free energy. It was also observed that an increase in
surface roughness leads to a proportional increase in the dispersive component of surface
free energy, while the polar component of surface free energy decreases.
Ii was noted that the various surface roughness parameters could be compared with
surface free energy or wetting or contact angle. However, the surface roughness parameters
which provide information about roughness depth and also roughness shape can be used to
analyze the suitability of a surface for adhesive bonding.

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