As originally published in the IPC APEX EXPO Conference Proceedings.

A New Method for Measuring Conformal Coating Adhesion

Christopher Hunt and Ling Zou
National Physical Laboratory
Teddington, UK

Abstract
Coating adhesion has been a difficult property to measure, and the industry has made do with a scratch test that is only
capable of qualitative tests. NPL with industrial partners, have developed a tape peel test that can be applied to the PCB or
component surface. The choice of tape is critical in achieving complete wetting of the fabric, and good adhesion to the
coating. The tape is applied with liquid coating to the substrate, and then cured, leaving a flying unbonded section for
clamping on during the pull test. The method shows clear differences in adhesion between different coating types: acrylics,
polyurethanes and silicones. The effect on coating adhesion of surface cleanliness and the cure state of the resist were
investigated. Coatings were generally observed to perform well with these problems. However, coating adhesion to
components and some resists proved much more variable, with some coatings failing to adhere to problematic components.
Surface energy measurements using a wetting angle technique were also used and compared with the peel data.

Introduction
Coatings are increasingly applied across a wide range of applications to offer environmental protection [1,2,3], and some of
these are demanding in terms of the protection offered by the coating in preventing permeation of contaminants [4,5,6]. Of
particular importance is that the coating remains adhered to the substrate. Loss of coating adhesion is primarily a function of
contaminants within the assembly process, and hence a method that can quantify the adhesion within the assembly
environment is needed. Currently there are two methods available. One is the scratch and peel test as described in [7,8,9], but
the method is operator dependent and not quantitative. The second approach is the use of dyne pens to assess substrate
surface energy, and is based on a visual inspection of the pen marks. This again is not quantitative, dependent on operator
interpretation, good condition of the pens, and no compatibility issues between the pen inks and the contaminant surface.

Here we introduce a peel test, based on a tape being cured in the coating and then peeled from the substrate in an instrument,
with additional details given in [10]. The introduction of the tape should not affect the cure process and have a strong
cohesive strength within the coating, so that during the peel the tape lifts the coating from the substrate, rather than pull the
tape from the coating.

Approach
In Figure 1 a cross section schematic is shown of a fully immersed fabric tape in a coating, and an image of a prepared
sample on a laminate substrate. Excess coating is squeegeed off the fabric tape to result in a total thickness of ~200µm.

Liquid Coating Tape

Substrate

Figure 1: Schematic and picture of test sample

Once cured the sample was peel tested, and we achieved this with a Dage bond tester, as shown in Figure 2, although any
suitable peel tester could be used.
 As originally published in the IPC APEX EXPO Conference Proceedings.

Figure 2: Tape peel test

Typical results from this test are shown in Figure 3.

30
A
25
B
Peel force (N)

20
15
10
5
0
0 10 20 30 40
Distance (mm)
Figure 3: An example of peel tests

A significant issue with this approach was the tape material, and a number of meshes: stainless steel, brass, nylon, polyester,
and polypropylene; and a number of cloths were evaluated: glass, polyester, cotton, silk, 20% polyester + 80% cotton, 65%
polyester + 35% cotton, 70% polyester + 30% cotton.

The peel force results from tests on these tapes (25mm width) with an acrylic coating are presented in Figure 4 and 5. The
data reveals that fabrics generally out performed the meshes, and this can be attributed to their fibrous construction, providing
high surface area, and rough fibres, for adhesion to take place on. Also of importance is the open area of the tape, as all
coatings require good access to the atmosphere for curing. Hence, the 65% polyester and 35% cotton mix fabric with 15%
open area, which gave the highest peel force, was selected for all the further tests.
 As originally published in the IPC APEX EXPO Conference Proceedings.

60

50

40
Peel force (N)
30

20

10

0
Polyproplene Stainless steel Nylon Brass Polyester
Mesh material

Figure 4: Average peel forces for different mesh materials

60

50
Peel force (N)

40

30

20

10

0
65% 100% 70% 20% Glass 100% Silk
Polyester Cotton polyester Polyester Polyester
35% 30% 80%
Cotton cotton Cotton
Cloth material

Figure 5: Average peel forces for different fabric materials

1mm

Figure 6: Tape material (65% polyester plus 35% cotton fabric)

 As originally published in the IPC APEX EXPO Conference Proceedings.

Effect of peel speed

The peel speed could be varied from 0.5 to 1.5mm/s with this Dage instrument, and the effect of this on the three coatings is
shown in Figure 7, again using a laminate substrate.

60 Acrylic
Polyurethane
Silicone
Peel force (N) 50

40

30

20

10

0
0.5mm/second 1mm/second 1.5mm/second
Peel speed
Figure 7: Average peel force for three type coatings at different peel speeds

These results show there is little dependence on peel speed over the tested range, but again the low adhesion strength of
silicones is apparent. For the following work, a 1mm/s speed was used.

Tape peel width

The peel forces with different tape widths (5, 10 and 25mm) for three coatings are plotted in Figure 8 respectively. The dotted
lines represent the backward extrapolations of the 25mm tape width values, to check if the force decreases pro-rata with
width. The results show that the force broadly follows tape width, but specifically at 5mm the force is noticeably higher than
expected, and this can be attributed to edge effects. Therefore, it is recommended that a minimum of 10mm tape be used, if
possible.

60

50
Average peel force (N)

40
Acrylic
Polyurethane
30

20
Silicone
10

0
0 5 10 15 20 25 30
Tape width (mm)
Figure 8: Measured and extrapolated peel force from different tape widths
for three coatings
 As originally published in the IPC APEX EXPO Conference Proceedings.

Cure conditions
The sensitivity of the peel test to the cure state of three coating materials was investigated, and the test conditions are
tabulated in Table 1.

Table 1: Cure temperature and time for three coatings

Acrylic A Polyurethane Silicone
Ambient 72°C Ambient 80°C Ambient Ambient (hour)
Hour Minute Hour Minute Hour + 80°C (Minute)
1 20 16 30 24 24 hour + 20 minute
2 40 40 60 48 48 hour + 20 minute
4 70 66 90 72 72 hour + 20 minute
8 120 96 120
24 144
48 216
96

Using the same test procedure as before, i.e. 25mm tape width, 1mm/s peel speed and a peel distance of 35mm, the following
results were obtained, and are presented in Figure 12. All peel test values are for an average between 5 and 35mm of peel for
each of two tests.

60 60
Acrylic Acrylic
50 50
Ambient condition
Peel force (N)

@ 72°C
Peel force (N)

40 40
30 30
20 20
10 10
0 0
0 30 60 90 120 150 0 20 40 60 80 100
Cure time (minute) Cure time (hour)
60 60
Polyurethane
50 50
@80°C
Peel force (N)

Peel force (N)

40 40
30 30
Polyurethane
20 20
Ambient condition
10 10
0 0
0 30 60 90 120 150 0 50 100 150 200 250
Cure time (minute) Cure time (hour)

60 60
Silicone Silicone
50 50
Ambient condition
Peel force (N)
Peel force (N)

Ambient condition
40 40
+ 20 minutes 80°C
30 30
20 20
10 10
0 0
0 20 40 60 80 100 0 20 40 60 80 100
Cure time (hour) Cure time (hour)
Figure 9: Average peel force from different cure conditions for three type coatings
 As originally published in the IPC APEX EXPO Conference Proceedings.

The results in Figure 9 clearly show the role of cure in improving the adhesion, except for the silicone, where the failure was
at the tape interface. In some instances, the cure at elevated temperatures produced bubbling under the tape. This is attributed
to solvent loss issues, where the tape restricts this process. However, elevated temperature definitely accelerates adhesion,
and the test method provides a useful means of checking any given cure schedule. From this work, it was decided to apply the
following cure schedule for the three coating types for subsequent work in this study, summarised in Table 2. The mixed cure
schedule was to allow the initial solvent loss to occur and prevent bubbling during the 80ºC cure.

Table 2: Cure condition for three coatings

Acrylic Polyurethane Silicone
24 hours in ambient 24 hours in ambient 24 hours in ambient
+ 30 minutes @ 80°C + 60 minutes @ 80°C + 20 minutes @ 80°C

Contamination effects on acrylic coating adhesion

With a clean PCB, the failure always occurred at the tape/coating interface, instead of the coating/substrate interface,
reflecting the strong adhesion of the coating to the substrate. To establish the test response as the surface energy decreased,
attempts were made to contaminate the surface. Hence a number of common commercial products were trialled, and these
included solvent and water based solder fluxes, various petroleum based greases with different melting points, a grease with
added slip agents, silicone lubricants and a silicone release spray. All of these failed to impact significantly on the adhesion
force, which can be possibly attributed to the washing action of the co-solvents in the coatings. However, common
surfactants used for general cleaning were found to significantly impact adhesion. For these trials, the laminate substrate was
contaminated with a common proprietary surfactant, which was dissolved in deionised (DI) water at three different
concentrations, as listed in Table 3. For each test, 1.0ml of the contaminant solution was dispensed onto a 25 x 100 mm
laminate sample. The sample was then dried at 100°C oven for 5 minutes before applying the coating with the tape. Two
samples were tested for each contamination level.

Table 3: Contamination levels of surfactant

Coating Contamination (% in DI water)
None
Acrylic A 0.5%
1.0%
3.0%

The average force for each different contamination, are presented in Figure 10. The substrate and peel tape were inspected
under a microscope after testing, and the results are shown in Figure 11.

60

50

40
Peel force (N)

30

20

10

0
3% Surfactant 1% Surfactant 0.5% Surfactant Clean
Contamination
Figure 10: Average peel forces for different contamination samples
 As originally published in the IPC APEX EXPO Conference Proceedings.

Substrate Tape

Clean

0.5% surfactant

1% surfactant

3% surfactant
Figure 11: Substrate and peel tape for different contamination samples after testing

The results in Figure 10 and 11 clearly demonstrate that peel force decreased with increasing contamination, at that the failure
mode changed from the tape/coating interface to coating/substrate interface. As the contamination on the substrate increased
to 3% surfactant, the peel force dropped from 37N to 12N for the clean board. At the intermediate contamination levels, a
mixed failure mode was observed, with failure occurring more at the coating/substrate interface with increasing
contamination. This suggests that the test method can discriminate between different surfactant contamination levels.

60 Acrylic
Polyurethane
Silicone
50
Peel force (N)

40

30

20

10

0
PCB Copper Resist A Resist A Resist B Resist C Resist D
curtain screen
Substrate materials
Figure 12: Average peel force from different materials for three coatings
 As originally published in the IPC APEX EXPO Conference Proceedings.

Effect of resist
Several resists were evaluated, Coates XV501T-4, Coates XV501 CAWN1287, Huntsman Probimer 77 and Electra EMP100.
All resists were applied by screen printing except one which was also curtain coated. The four resists were arbitrary named A
to D. These resists were supplied to NPL from PCB fabricators. The same test method was applied as before and the results
are shown in Figure 12 along with the coatings on bare laminate and copper clad laminate.

The failure mode is given in Table 4.

Table 4: Failure mode from different substrate materials for three coatings
(T: tape/coating interface, S: coating/substrate interface)
Substrate Resist
PCB Cu A A B C D
Coating Curtain Screen
Acrylic T T S T T T T
Polyurethane T S S S T+S T+S T+S
Silicone T T T T T T T

Again the results were not informative for the silicone, with low forces and the failure at the tape/coating interface. The
acrylic out performed the polyurethane with high adhesion forces across the samples with the failures occurring
predominately at the tape/ coating interface. There were many failures at the coating/substrate interface with the
polyurethane, which showed generally poorer adhesion to resists than the acrylic. In addition, one resist (Resist A curtain
coated) gave poor adhesion values revealing a more systematic problem with this coating. Hence, the technique shows the
possibility of quantifying the adhesion between resists for some coatings.

Effect of components
A random selection of plastic encapsulated IC components, see Table 5, were purchased and the adhesion force measured
using the same method as before, except a 10mm tape was used, and therefore the forces are typically 10/25 (40%) of the
values elsewhere in this paper.

Table 5: Components selected for adhesion testing

A (PLCC 68) Texas
B (BGA 380)
C (PLCC68) EXAR
D (BGA177)
E (QFP 532) ANALOG
F (QFP 160) Topline
G (BGA 256) Amkor

30
Acrylic
Polyurethane
25
Silicone

20
Peel force (N)

15

10

0
PLCC BGA PLCC BGA QFP QFP BGA Cleaned PCB
A B C D E F G QFP F
Component

Figure 13: Average peel force from different components for three coatings
 As originally published in the IPC APEX EXPO Conference Proceedings.

The results of the adhesion tests are presented in Figure 13, and the failure mode identified in Table 6.

Table 6: Failure mode from different components for three coatings

(T: coating/tape interface, S: coating/substrate interface)
Component A B C D E F G
Coating
Acrylic S S S S S S S
Polyurethane S S T S S S T
Silicone T S T S T S T

The results of adhesion testing on components clearly show that for a wide range of components adhesion is problematic for
coatings. The acrylic in this test struggled with all the components, the force not exceeding 1N. The polyurethane only
achieved the optimum force on BGA G, with the force being significantly reduced for all the other components, particularly
for BGA B. Even for the silicone coating, on three components the failure was at the substrate interface. Component QFP F
was cleaned in IPA + DI water in an ultrasonic cleaning system for 20 minutes, and tested with the acrylic, but this had no
effect on the adhesion. The low adhesion can be attributed to release agents in the plastic mould compound, and their lack of
solubility in the coatings. Clearly components present a significant adhesion issue for coatings, and where the tape can be
applied to a sufficient area, the technique can clearly differentiate between different coatings.

Post coating application of tape

The method described so far has the tape applied simultaneously with the coating. Here we explore the possibility adhering
the tape by applying a second layer of the original coating. We refer to this as the so-called double coating method, shown
schematically in Figure 14. If successful, this would obviate the need to always embed the tape in the initial coating, allowing
any coating to be tested at any point in assembly without the need for any previous preparation. The experimental parameters
of subsequent tests are shown in Table 7. Here we also explored the effect of state of cure of the first coat, it either being fully
cured, or only cured for 1 hour.

Figure 14: Double coating method

Table 7: Experiment details

Coating Substrate Cure of first coating
Acrylic B Bare laminate Fully cured
Polyurethane Resist A 1 hour cured
Silicone

Figure 15 shows the three possible failure modes as the tape is pulled from the substrate. Ideally the third failure mode should
occur if useful information is to be gained on the adhesion of the original coat.

Tape/coating Coating/Coating Coating/substrate

Failure 1 Failure 2 Failure 3

Figure 15: Three failure modes for the double coating method
 As originally published in the IPC APEX EXPO Conference Proceedings.

Results for testing on coated bare laminate, and on a commercially available resist are presented in Figure 16. The testing of
the double coating method showed poor adhesion of the first coating with resist samples and gave the desired type 3 failures
for both the acrylic and polyurethane coatings. However, on the PCB higher adhesion forces for the acrylic on the PCB were
observed, and the failure was type 1. This is disappointing as the second acrylic coat should dissolve the surface of the
bottom coat and form a single coating. With the polyurethane type 3 failures were not observed, and low forces were
recorded with the tape coming away too easily, type 1 and 2 failures. Low forces were also obtained with the silicone coating.

60 60
Failure 1 Failure 1 Acrylic Polyurethane
50 50

Peel force (N)

Peel force (N)

Failure 1 + Failure 2
40 40
30 30
Failure 3 Failure 3 Failure 2
20 20 Failure 3 Failure 3
10 10

0 0
PCB Full PCB hour Resist Full Resist hour PCB Full PCB hour Resist Full Resist hour
Sustrate material and cure condition Sustrate material and cure condition

60
Silicone
50
Peel force (N)

40
30
20 Failure 1 Failure 1 Failure 1 Failure 1

10
0
PCB Full PCB hour Resist Full Resist hour
Sustrate material and cure condition
Figure 16: Peel force results for the three coatings with the double coating method.

Surface energy
The surface energy of a substrate will have an effect on adhesion, and dyne pens are used as an indicator of surface energy
and hence adhesion. Here we attempted to measure the surface energy using deionised water, with an DAS 100 instrument ,
as shown in Figure 17. The DAS 100 dispensed a 70pl water drop for each measurement, and measured the wetting angles on
both side of each drop, as presented in Figure 17, and took an average reading. Nine measurements were taken for each
substrate coating combination. Wetting angle measurements were made on different substrate materials, bare laminate,
copper clad laminate, and the resists and components identified above, and the results are given in Table 8.

The wetting angle measurements are compared with the adhesion values. The adhesion values are also given in Table 8, and
have been normalised to a 10mm tape values, to enable comparison with the component tests. Unfortunately, a correlation
was not established between these wetting angle measurements and the adhesion values measured in the peel test. For
example, the acrylic testing on components gave universally low adhesion forces, but the wetting angle measurements are
variable. The polyurethane coating on the BGA G gave a low wetting angle and high force, but QFP E had the same wetting
angle but low force. It is possible that further work on selecting the test liquid may yield an improved correlation, for
example selecting a liquid similar to that used in the dyne pens, rather than water. However, there is a potential difficulty in
that hydrogen bonding formed during the coating cure cannot be directly predicted by a wetting angle measurement, as there
is a chemical affinity element of this bonding which is independent of the surface energy. Neither can the solvent action of a
coating be replicated by the dyne pens.
 As originally published in the IPC APEX EXPO Conference Proceedings.

Figure 17: Wetting angle measurement with DSA 100

Table 8: Wetting angles of substrate and peel force from three coatings
Substrate material Wetting angle Peel force (N/10mm)
(°) Acrylic Polyurethane Silicone
FR4 PCB 70.0 21.8 19.7 6.7
Copper 86.9 20.9 12.1 6.9
Resist A (Curtain) 70.1 7.2 5.4 6.9
Resist A (Screen) 68.9 20.7 12.8 7.0
Resist B 71.0 20.7 16.4 6.9
Resist C 84.1 20.4 15.9 6.6
Resist D 72.3 20.1 17.1 7.1
PLCC A 91.3 0.4 7.9 7.2
BGA B 86.2 0.5 2.5 4.8
PLCC C 81.1 0.5 11.9 5.3
BGA D 84.6 0.3 9.5 4.9
QFP E 75.0 0.5 6.5 7.1
QFP F 92.9 0.5 8.0 3.3
BGA G 75.5 0.7 19.9 6.6

Conclusions
• We have demonstrated a adhesion peel test for conformal coatings that can detect when the adhesion becomes less
than optimal for silicone, acrylic and polyurethane coatings.
• Selection of the tape material is critical to achieve the desired coating to substrate failure during peel. A high
surface area woven fabric with a loose weave was found to be ideal, and a 65% polyester and 35% cotton mix cloth
with 15% open area was selected.
• A limitation of the test is that the tape has to be applied with the coating, by fully immersing the tape in the coating
and then curing.
• The peel test is not particularly sensitive to the variables of peel speed, peel length and tape width. It is envisaged
that a wide range of peel test equipment could be utilised.
 As originally published in the IPC APEX EXPO Conference Proceedings.

• Application of the test to a range of material variables was proved successful, and included the cure state of the
coating, contamination of the substrate, surface energy state of resists and components. This test was extremely
effective at revealing the low adhesion of coatings to plastic encapsulated IC packages. The test could be readily
applied to coating process optimisation.
• Separation in the peel test was not always at the coating substrate interface, and both failure surfaces should be
checked to identify the separation path. The silicone revealed low adhesion forces for removing the tape from the
coating, a problem for the test, but on contaminated surfaces, the weaker coating substrate bond could be
investigated. For the acrylic and polyurethane coatings, the force to remove the tape from the coating was
significantly higher than for the silicone. The silicone had the least dependence on substrate surface condition.
• Where low adhesion occurs, the test peeled the coating from the substrate. Where the tape was pulled from the
coating, it is indicative that the coating has sufficient adhesion for its functional purpose.

Acknowledgements
This work was supported under the framework of Joint Industry Projects, part of the Materials Measurement Programme
sponsored by the National Measurement System unit of the UK’s Department for Business, Innovation and Skills. The
authors wish to acknowledge the support and assistance to the project provided by the following companies:
Aero Engine Controls
European Space Agency
Dow Corning
H K Wentworth Ltd
Humiseal Europe
Rockwell Collins

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