precise and quantitative assessment of automotive coating
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© 2019 The Korean Society of Rheology and Springer 89
Korea-Australia Rheology Journal, 31(2), 89-96 (May 2019)DOI: 10.1007/s13367-019-0010-9
www.springer.com/13367
pISSN 1226-119X eISSN 2093-7660
Precise and quantitative assessment of automotive coating adhesion
using new microgap pull-off test
Chi Hyeong Cho1,†
, Intae Son1,†
, Ji Yong Yoo1, Gitae Moon
1, Eunbi Lee
1, Sung Ho Yoon
2,
Jae Sik Seo2, Choon Soo Lee
2 and Jun Hyup Lee
1,*1Department of Chemical Engineering, Myongji University, Yongin 17058, Republic of Korea
2Interior System Plastic Materials Development Team, Material Development Center, Hyundai Motor Company, Hwaseong 18280, Republic of Korea
(Received December 19, 2018; final revision received March 21, 2019; accepted March 27, 2019)
The quantification of coating adhesion on substrates is an important technology that has recently receivedmuch attention in automotive industry because the adhesion characteristics of automotive paints have agreat influence on color and appearance of automobiles. Here, we present a robust and precise method forquantifying the coating adhesion of automotive paints on flat substrates using new microgap pull-off testbased on the application of a micrometer-thick layer of adhesive to the divided compartments. The influenceof water and organic material penetration on the coating adhesion between paint and plastic substrate isinvestigated in order to quantitatively measure the water resistance and organic compound resistance ofautomotive paints. When the paint absorbed moisture and organics, they penetrated through the paint sur-face to interfere with the coating adhesion between the plastic substrate and the paint layer, thereby reducingthe initial coating adhesion. In addition, we investigated the effect of chlorinated polyolefin (CPO) contenton the coating adhesion between nonpolar plastic substrate and polar paint coating. As the CPO content inpolar acrylic paints increased, the coating adhesion of the polar paint to nonpolar plastics was increased dueto the compatibilization effect of CPO resin in the coating interface.
Keywords: automotive paint, coating adhesion, microgap, pull-off test, quantification method
1. Introduction
Paint plays an important role in the purchase of auto-
mobiles because it dictates the color and appearance, but
paint also prevents car body corrosion (Akafuah et al.,
2016; Dosdat et al., 2011; Guo, 2012). Therefore, the
automotive paint characteristics are important, including
color and appearance, corrosion resistance, impact resis-
tance, and coating adhesion. Among these properties, the
adhesion characteristics have a great influence on the
long-term stability of the coating layer, and corrosion
starts when the coating peels off due to low adhesion
strength. Generally, polar plastics, such as polycarbonate
(PC) and acrylonitrile butadiene styrene copolymer
(ABS), and nonpolar plastics, such as polypropylene (PP),
are used for automotive interior materials (Liu and Qiu,
2013). PC and ABS are thermoplastic resins, which are
characterized by high impact resistance and rigidity (Pham
et al., 2000; Zhang et al., 2001). They are also used for
exterior materials of many products, such as mobile
phones and monitors. These polar plastics are commonly
painted using polar paints, such as acryl and urethane
polymers. In contrast, PP is a nonpolar plastic substrate, so
it cannot achieve sufficient adhesion to polar coating resin.
Therefore, it is technically painted with chlorinated poly-
olefin (CPO) mixed with polar acrylic coating resin. CPO
crystals functioned as compatibilizers grow epitaxially on
the PP crystals during baking, which leads to intimate
interactions between PP and acrylic resin, and thus
enhances coating adhesion of polar paints (Schmitz and
Holubka, 1995; Tomasetti et al., 2001). For this reason,
the content of CPO greatly affects the interfacial adhesion
between the nonpolar plastic substrate and the polar paint
coating (Clemens et al., 1994; Ryntz and Buzdon, 1997).
Also, the adhesion of these coatings can be greatly
affected by the external environment such as humidity and
organic contaminants. The chemical and physical proper-
ties of automotive paint materials mainly made of poly-
mers can be deteriorated by contact with foreign substances,
such as the water or cosmetics. Therefore, it is necessary
to evaluate the coating adhesion of the paint to confirm
these external effects on the coating layer. Various assess-
ment methods are conducted to evaluate the coating adhe-
sion of paint, such as the cross-cut method (Huang et al.,
2007) and dolly test (Wolkenhauer et al., 2008). In case of
cross-cut method, it is difficult to quantitatively measure
the coating adhesion of paint because the area of coating
detachment is roughly determined by the naked eye after
tape peel-off process. While the dolly test based on the
pull-off adhesion testing can provide the adhesion strength
of coating paints, this method is problematic because the
†These authors are equally contributed to this work.*Corresponding author; E-mail: junhyuplee@mju.ac.kr
Chi Hyeong Cho, Intae Son, Ji Yong Yoo, Gitae Moon, Eunbi Lee, Sung Ho Yoon, Jae Sik Seo, Choon Soo Lee and Jun Hyup Lee
90 Korea-Australia Rheology J., 31(2), 2019
accurate and reproducible quantification of coating adhe-
sion is difficult due to the failure of coating layer detach-
ment.
In this study, we established a precise and quantitative
method to reproducibly assess the coating adhesion of
automotive paints using the newly designed microgap
pull-off test. The proposed approach is founded on the
application of a micrometer-thick layer of highly adhesive
material to the divided compartments of coating sub-
strates, leading to the clear detachment of coating layer
from plastic substrate. By using this microgap pull-off
test, we investigated the effect of penetration of external
substances such as moisture and cosmetics on the coating
adhesion of automotive urethane paints. In order to exam-
ine the effect of water penetration on the adhesion between
the polar coating layer and plastic substrate, water was
absorbed into the coating layer through a heating bath
under different time and temperature conditions, and to
investigate the effect of penetration of cosmetics, the coat-
ing surface was treated with commercial cosmetics at dif-
ferent temperatures. Furthermore, in order to examine the
effect of CPO content on the coating adhesion between
nonpolar PP substrate and polar paint layer, the ratios of
acryl and CPO resins were varied and compared. The rela-
tionship between the coating adhesion and various mate-
rial parameters involving water, organic contaminant, and
compatibilizer was demonstrated by using the proposed
quantitative method for automotive coating adhesion.
2. Experimental
2.1. MaterialsEach coated substrate (urethane-coated ABS, CPO-
coated PP) was obtained from Hyundai Motor Company
(Hwaseong, Korea). Urethane-based paint material was
prepared by mixing polyurethane and acryl resins, and
CPO-based paint coatings were manufactured by mixing
CPO and acryl resins in 1:3 (CPO-1), 2:2 (CPO-2), and
3:1 (CPO-3) ratios. The adhesive (Araldite 2014-1) used
to assess the coating adhesion of the automotive paints
was purchased from Huntsman Co., Ltd. (Woodlands,
Texas). The sunscreen (NIVEA Fresh Sun Lotion) used
for evaluation of resistance to organic compound was pur-
chased from NIVEA Co., Ltd. (Hamburg, Germany).
2.2. Preparation of test specimens for water and organic
compound resistanceA urethane-coated substrate prepared for water resis-
tance evaluation was impregnated in a heating bath (Jeio-
tech, BS-11) containing 1000 ml of water. The water-
resistance evaluation was carried out for 7 days at 40°C in
a low temperature environment (Water-L) and for 1 day at
80°C in a high temperature environment (Water-H). Then,
the specimens were dried at 50°C for 2 days in a vacuum
oven (Jeiotech, OV-11) to remove the residual moisture.
The organic resistance evaluation was performed by
applying 0.25 g of sunscreen per 50 mm length and 50
mm width on the surface of the urethane-coated substrate.
And then the coated surface was covered with a cotton
cloth, pressed with an acrylic plate, and treated at 80°C for
1 h (Sun-L) in a convection oven (Jeiotech, OV-11E). In
order to examine the effect of thermal treatment tempera-
ture on the coating adhesion strength under the above con-
ditions, we treated sunscreen-covered substrates at a
relatively higher temperature of 100°C (Sun-H). After the
treated test specimens were cleaned with a neutral deter-
gent, the surface of specimens was wiped with a tissue
paper, and they were dried at room temperature.
2.3. Preparation of test specimens for the microgappull-off testing
As shown in Fig. 1a, the test specimen consists of a top
plate and a bottom plate. The top plate is a substrate made
of aluminum, and the bottom plate is made of a plastic
substrate coated with an automotive paint. The overall size
of the specimen is 50 mm in length and 25 mm in width
for both substrates. To measure the adhesion strength of
the coating paint in a certain area, the center of the lower
plastic plate is divided into a section with 3 mm length
and 3 mm width, as shown in Fig. 1b. In order to apply a
micrometer-thick layer of highly adhesive material to the
divided compartments, a 5.75 μm ball spacer dispersed in
ethanol was sprayed on the surface of the lower plastic
plate, and then dried to adhere to the plate for 10 min at
room temperature. After applying adhesive to the inside of
the compartment, the upper plate and lower plate are
bonded to each other and heat-treated at 70°C for 2 h in
a convection oven for curing the adhesive while pressing
it in a clamp with a pressure of about 5 kgf/cm2.
2.4. Coating adhesion measuring principleThe adhesive strength of the coating paints was mea-
sured by pull-off test using a universal testing machine
(UTM; Lloyd Instruments, LR-5K), and the adhesive
strength was recorded by quantifying the required force to
separate the upper and lower plates of the test specimen.
As shown in Fig. 1c, a UTM machine is equipped with the
test specimens prepared by connecting a jig made for the
pull-off test. The mounted specimens were tested in a pull-
off test mode of UTM. The jig connected to the bottom
plate is fixed to the bottom of the UTM, and the jig con-
nected to the top plate rises vertically at a rate of 1000
mm/min. As the upper jig rises, the divided portion
adhered to the coating paint falls off and the force at that
time is measured by the UTM. The measured force is cal-
culated into stress using
(1)N
cm2
--------- =
Fmax
Ad
----------
Precise and quantitative assessment of automotive coating adhesion using new microgap pull-off test
Korea-Australia Rheology J., 31(2), 2019 91
where is the adhesive strength at failure, Fmax is the
maximum force, Ad is the detached area by adhesive, as
shown in Fig. 1d. In order to measure the precise detach-
ment force, the area of the coating layer desorbed on the
actual aluminum plate was calculated as the actual detached
area (Ad). The adhesive strength was determined using the
highest force (Fmax) during the microgap pull-off test.
2.5. CharacterizationThe structures of the pure coating paints, the detached or
residual parts of the coating paints, and the adhesives were
compared by using Fourier-transform infrared spectros-
copy (FTIR; Jasco, FT/IR-460 plus). The surface mor-
phology of the test specimens was examined by optical
microscopy (OM; Olympus, BX51). The surface penetra-
tion depth of the coating layers was determined by using
a nanoscratch tester (Anton Paar, NST3). The condition for
the scratch test was set with the speed of 2 mm/min, force
of 79.8 mN/min, and total length of 1 mm. In addition, the
hardness of the coating layer was measured by using
nanoindentation (Anton Paar, NHT3) at loading and un-
loading rates of 20 mN/min.
3. Results and Discussion
3.1. Effect of water absorption on the coating adhe-
sion of automotive paint
Figure 2a shows the FTIR spectra of the adhesive, pure
paint layer of coated substrate, and desorption regions of
the upper and lower plates from the pull-off test specimen.
The pure coating paint fabricated on the basis of urethane
resin showed N-H stretching and C=O stretching peaks at
3323 cm1 and 1734 cm1, respectively. The FTIR spectra
of the detached regions of the upper and lower plates
showed similar spectral features to that of pure paint layer,
which indicates that the coated paint material is present on
both substrates due to the breakdown in the bulk layer of
the coating paint after pull-off test. In order to further ver-
ify the interlayer separation of the coating paint, the sur-
face morphology of the upper and lower plates of the
specimen was examined through the OM experiment, as
shown in Fig. 2b. The OM image was measured at 100×
magnification and it was confirmed that the optical texture
of the upper plate was almost identical to that of the lower
plate, which suggests that the delamination occurred in the
bulk layer of the coating paint. These results confirmed
that the proposed microgap pull-off test provides the suc-
cessful detachment of coating paint from plastic substrate.
Figure 3 shows the result of the coating adhesive strength
for the pristine urethane-coated substrate and water-treated
specimens with different treatment temperatures. While
the coating adhesion strength of a pure specimen before
water absorption was 405.6 N/cm2, the coating adhesion
of Water-L specimen with a long-term water absorption at
Fig. 1. (Color online) Photographic images of (a) the upper and lower plates of the specimen, (b) the divided sections of the coating
layer, and (c) the pull-off test jig. (d) Basic principle of the coating adhesion testing mechanism.
Chi Hyeong Cho, Intae Son, Ji Yong Yoo, Gitae Moon, Eunbi Lee, Sung Ho Yoon, Jae Sik Seo, Choon Soo Lee and Jun Hyup Lee
92 Korea-Australia Rheology J., 31(2), 2019
low temperature of 40°C decreased to 105.6 N/cm2. Since
the water can penetrate into the bulk layer inside the coat-
ing film to reduce the cohesive strength between the res-
ins, the coating adhesive strength is greatly reduced after
the water absorption (Arslanov and Funke, 1988; Kim and
Kim, 2015). Comparing Water-L and Water-H specimens
under different treatment conditions, the coating adhesion
of Water-H specimen decreases even more when the water
absorption is performed at a high temperature of 80°C for
a short period of time. Therefore, it is inferred that the
coating adhesion of automotive paint may be greatly influ-
enced by the water absorption temperature rather than the
absorption time.
3.2. Effect of organic compound absorption on thecoating adhesion of automotive paint
Figure 4a shows the FTIR spectra of the adhesive,
untreated paint layer, and the separated regions of the
upper and lower plates from the sunscreen-treated speci-
men. Similar FTIR spectra to those of water absorption
evaluation were observed for the organic compound resis-
tance assessment due to the use of the same urethane-
coated substrate. The separated regions of the upper and
lower plates showed similar spectra, which suggests that
the delamination occurs in the bulk layer of the coating
paint after pull-off experiment. For further verification, the
OM images of the upper and lower plates had similar opti-
cal textures, which is analogous to that of water absorp-
tion test, as shown in Fig. 4b. Figure 5 shows the results
of coating adhesion strength of the urethane-coated spec-
imen after absorbing the sunscreen. Compared to the
unprocessed substrate, the Sun-L specimen treated at a rel-
atively low temperature of 80°C exhibited a reduced adhe-
sion strength of 76.3 N/cm2. Since the desorption of the
sunscreen-treated specimen occurs inside the bulk layer of
the coating paint, the organic compound of the sunscreen
transfers from the surface of the coated substrate to the
bulk layer, thereby reducing the cohesion between the res-
ins in the coated paint. The Sun-H specimen treated at a
higher temperature of 100°C had a coating adhesion of
231.6 N/cm2, which is an increased strength compared to
that of the Sun-L specimen. Previous studies have shown
that some of the penetrated organic compounds can improve
the cohesion of the resins by inducing a curing reaction
with the resin in the polymer film at high temperatures
(Daniels and Klein, 1991). It is inferred that the organic
compound such as sunscreen weakens the coating adhe-
sion of the paint layer when it is absorbed into the interior
of the coating layer like water absorption, but unlike
water, the organic compound may increase the coating
adhesion by bonding with the resin in the paint layer.
Since the nanoscratch and indentation tests are often
used to analyze the viscoelastic-plastic characteristics of
the coating film (Pelletier et al., 2008), the influence of the
Fig. 2. (Color online) (a) FTIR spectra of the adhesive, pure paint layer, and water-desorption regions of the upper and lower plates
from the pull-off test specimen. (b) OM images of the surface of the upper and lower plates.
Fig. 3. Coating adhesive strength of the pristine urethane-coated
substrate and water-treated specimens with different treatment
temperatures.
Precise and quantitative assessment of automotive coating adhesion using new microgap pull-off test
Korea-Australia Rheology J., 31(2), 2019 93
water and organic compounds on the viscoelastic-plastic
properties of the coating films was analyzed. Figure 6a
shows the penetration depth results according to scratch
length. During the scratch test, the variation in penetration
depth of Water-L and Sun-L specimens was significantly
higher than that of the pure coating layer. The final pen-
etration depths at the endpoint of Water-L and Sun-L
specimens were 10163.3 nm and 11019.8 nm, respec-
tively. This result is ascribed to the increased viscoelastic
properties stemming from the absorption of water and
organic compounds in the coating layer. Similarly, nanoin-
dentation measurements demonstrated that the Water-L
and Sun-L specimens exhibited a lower indentation hard-
ness of 222.9 MPa and 208.4 MPa than pure coating layer,
as shown in Fig 6b.
3.3. Effect of chlorinated polyolefin content on the
coating adhesion of automotive paintFigure 7 presents the FTIR spectra of CPO-1 on the
nonpolar PP substrate before and after the evaluation of
coating adhesion. While the unvalued CPO-1 paint layer
exhibited the characteristic stretching vibrations of CPO
and acryl resins, the totally different spectra were found
for desorption regions of the upper and lower plates of the
CPO-1 specimen. These spectra were very similar to that
of the pure PP substrate, which indicates that the failure
occurred at the side of PP substrate near the interface
between paint layer and substrate. Since the polar acryl
resin-rich CPO-1 layer and nonpolar PP substrate are
incompatible, the low interfacial adhesion between the
nonpolar substrate and the polar paint coating is expected,
leading to the delamination of paint coating layer on PP
substrate. To verify this failure of CPO-1 coating paint,
photographic and OM images were additionally measured
and shown in Fig. 8. After pull-off test of CPO-1, the dark
coating paint layer was confirmed to be completely
attached to the upper aluminum substrate through the pho-
tographic image. For further confirmation, the OM images
of CPO-1 showed that the surface microscopic image of
the unvalued CPO-1 paint layer was different from those
of the detached upper and lower plates of the specimen.
These results indicate that the delamination of CPO-1
coating paint occurs in the middle layer of PP substrate
rather than the bulk layer of the coating paint. The CPO-
1 coating layer is inferred to have a higher cohesive
strength between the polar resins than the interfacial adhe-
sion between the nonpolar PP and the polar coating paint,
resulting in complete desorption of the coating paint.
To examine the effect of CPO content on the coating
adhesion of paint, the photographic and OM images of the
CPO layer on the PP substrate after the pull-off test were
observed according to the CPO content, as shown in Fig.
8. In case of CPO-2 specimen, the dark desorbed paint
area and the bright adhesive area were found for the upper
Fig. 4. (Color online) (a) FTIR spectra of the adhesive, pure paint layer, and the separated regions of the upper and lower plates after
the sunscreen treatment. (b) OM images of the upper and lower plates.
Fig. 5. Coating adhesion strength of the urethane-coated speci-
men before and after absorbing the sunscreen.
Chi Hyeong Cho, Intae Son, Ji Yong Yoo, Gitae Moon, Eunbi Lee, Sung Ho Yoon, Jae Sik Seo, Choon Soo Lee and Jun Hyup Lee
94 Korea-Australia Rheology J., 31(2), 2019
aluminum substrate under photographic observation. In
addition, a comparison of the surface of the unvalued
CPO-2 with that of the detached lower plate through the
OM image revealed that the coating paint was partially
peeled off from the PP substrate. Since CPO-2 has a
higher CPO content than CPO-1, the interfacial coating
adhesion between the polar paint and the nonpolar sub-
strate is expected to be strengthened, leading to the partial
desorption of CPO paint layer on PP substrate. In case of
CPO-3 with the highest CPO content, the photograph
showed that only the bright adhesive area was present on
the upper aluminum substrate, indicating that the coating
paint was not desorbed from substrate. The OM observa-
tion also revealed that the surface of the unvalued CPO-3
was similar to that of the lower PP substrate. As a result,
since the content of CPO in paint layer is very high, CPO-
3 has a very strong coating adhesion to nonpolar PP sub-
strate, resulting in the failure at interface between the
adhesive and the coating paint. The cause of the increased
coating adhesion according to the CPO content was found
in the literature (Aoki, 1968; Bonnerup and Gatenholm,
1993; Tomasetti et al., 2000). Previous study showed that
the Cl content controls properties such as melting point,
glass transition temperature, solubility, and polarity of the
material, and that the CPO layer improves the coating
adhesion of polar paint to nonpolar PP substrate by com-
patibilization effect of chlorinated polyolefin resin in the
coating interface. The CPO crystals in paint layer grow
epitaxially on the PP crystals of substrate during paint cur-
ing process, resulting in the increased interactions between
PP substrate and polar paint resin (Schmitz and Holubka,
1995; Tomasetti et al., 2001). Therefore, as the CPO con-
tent increases, the coating adhesion of the polar paint on
nonpolar substrate increases.
Based on the above results, the coating adhesion strength
of CPO paint layer according to the CPO content is shown
in Fig. 9. While the CPO-1 specimen showed the lowest
coating adhesion strength of 843 N/cm2, the coating adhe-
sion of CPO-2 and CPO-3 gradually increased to 971 N/
cm2 and 1085 N/cm2, respectively. Therefore, as the CPO
content in the polar paint layer increases, the coating adhe-
sion with the nonpolar PP substrate gradually increases.
Since the coating layer of CPO-3 specimen was not detached
from the PP substrate, the coating adhesion strength of
Fig. 6. (Color online) (a) Scratch penetration depth and (b) indentation hardness of the urethane-coated specimen before and after
absorbing the water and sunscreen.
Fig. 7. (Color online) FTIR spectra of CPO-1 specimens before
and after the evaluation of coating adhesion.
Precise and quantitative assessment of automotive coating adhesion using new microgap pull-off test
Korea-Australia Rheology J., 31(2), 2019 95
CPO-3 is expected to be higher than the measured value.
As a result, it is confirmed that the chlorinated polyolefin
content in polar acrylic paints played a crucial role in
improving the coating adhesion on nonpolar PP substrate
through the proposed new microgap pull-off test.
In order to investigate the effect of chlorinated polyole-
fin on the viscoelastic characteristics of the coating layer,
the nanoscratch and indentation experiments were con-
ducted. As shown in Fig. 10a, the penetration depth of the
CPO-3 specimen was 14099.8 nm, which was lower than
that of the CPO-1 (20821.8 nm). This result suggests that
the plastic tendency of the coating layer becomes more
pronounced as the content of the polar CPO increases. In
addition, indentation hardness was measured for the CPO-
Fig. 8. (Color online) The photographic and OM images of the CPO layers according to the CPO content after the pull-off test.
Fig. 9. Coating adhesion strength of CPO paint layer according
to the CPO content.
Fig. 10. (a) Scratch penetration depth and (b) indentation hardness of the CPO paint layer according to the CPO content.
Chi Hyeong Cho, Intae Son, Ji Yong Yoo, Gitae Moon, Eunbi Lee, Sung Ho Yoon, Jae Sik Seo, Choon Soo Lee and Jun Hyup Lee
96 Korea-Australia Rheology J., 31(2), 2019
treated coating layers, as shown in Fig. 10b. Similar to the
surface scratch test results, it is confirmed that CPO-3
specimen with high CPO ratio exhibited higher indenta-
tion hardness of 192.6 MPa than CPO-1 (178.3 MPa).
4. Conclusions
A quantitative method to measure the coating adhesion
of automotive paints has been presented. The proposed
microgap pull-off approach applied a micrometer-thick
layer of adhesive material to the divided compartments of
coating substrate, leading to the reproducible detachment
of coating layer from plastic substrate. By using this
microgap pull-off test, the relationship between the coat-
ing adhesion and various material parameters such as
water, organic contaminant, and CPO compatibilizer was
confirmed. The absorption of water and organic com-
pound reduced the cohesive strength between the paint
resins, resulting in the decrease in the coating adhesion.
The increased CPO content in polar paints improved the
coating adhesion of the automotive paint on the nonpolar
plastics due to the increased compatibilization between
nonpolar PP and polar acrylic resin. This study provides a
method for quantifying the coating adhesion of automo-
tive paint and defines a relationship between coating adhe-
sion and various parameters involving materials and
environment. These results will help facilitate the appli-
cation of functional paints to automotive exterior and inte-
rior materials.
Acknowledgments
This work was supported by Hyundai NGV and the
National Research Foundation of Korea (NRF) grant
funded by the Korea government (MSIT) (No. NRF-
2018R1A5A1024127).
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