Induron Adhesiaon_MP White Paper 2024 FINAL COPY
Induron Adhesiaon_MP White Paper 2024 FINAL COPY
Induron Adhesiaon_MP White Paper 2024 FINAL COPY
Abstract
Here we examine the notion of “adhesion” as it relates to thermosetting organic coatings on metallic substrates. The chemistry
and physics of coatings adhesion is reviewed and considered. Commonly used standard methodologies for adhesion testing
used by paint manufacturers, by field inspectors and others are reviewed and examined. Suggestions are made for recom-
mended field and inspection practice. Adhesion testing’s role in the engineering standard literature is examined.
Philosophy of Coatings Testing in the fog chamber; what about 115ºF? A form of “salt fog perfor-
mance” would still be measured. It would not be ASTM B117 salt
When engineers specify coatings materials for any industrial ap- fog or ISO 9227 salt fog testing though. It would be testing by
plication the process often involves the comparison of various so- some non-standard methodology but still distinctly a form a salt
lutions through the lens of physical and chemical properties of the fog testing and still measuring some form of corrosion resistance
cured coating. Standards organizations such as ASTM Interna- in high salinity environments.
tional (formerly the American Society for Testing and Materials, Choice of precise testing methodology is somewhat arbitrary. This
now having adopted the international moniker), and AMPP (Asso- is not a problem per se. Testers often have a large collection of
ciation for Materials Protection & Performance) produce stand- standardized methodologies to choose from and they may select
ards documents which are widely disseminated and used very ef- one or another for a variety of reasons. The only problem arises
fectively by the entire industry. when “apples to oranges” comparisons are attempted.
There are two ways one may speak of the properties of a com- In the following sections we address such philosophical issues
mercial material. There are the results of an actual standard meth- around the topic of adhesion testing in commonly used organic
odological assessment (a lab test) that may be traced back to a coating systems such as epoxies, urethanes, alkyds and acrylics.
specific version of a specific standard, and there is the actual un- We propose, and at least suggest answers to the following ques-
derlying property of a coating that said methodology is attempting tions: What is adhesion in coatings? How is it measured? What
to measure. As in all scientific measurements, the choice of meth- physical phenomena are at play behind the phenomena of adhe-
odology used to check a particular physical property is somewhat sion and its measurement and how do certain types of measure-
arbitrary. ment best (or worst) capture that? Which form of measurement
Take for example salt fog testing. This is a common corrosion re- and ontological understanding of adhesion best serves the coat-
sistance assay for organic coatings over steel. The test samples ings community and non-expert coatings decision maker?
are carbon steel panels coated with the material in question. The
coated panels are then put inside a “salt fog cabinet” where they Coatings and Adhesion
are exposed to a high humidity, high salinity, warm temperature
environment for extended periods. There are a variety of stand- Adhesion is perhaps the most important property of a coating sys-
ards written that detail procedures one may carry out for such a tem. Without adhesion to substrate, all other properties of the
“salt fog” testing regime. Amond them are ASTM B117 “Standard coating are unhelpful. Simply speaking adhesion is the strength
Practice for Operating a Salt Spray (Fog) Cabinet”[1] and ISO 9227 of a coating’s bond to the underlying substrate. The concept is
“Corrosion Tests in Artificial Atmospheres – Salt Spray Tests”[2]. applicable to almost any combination of coating and substrate.
But what are salt fog tests measuring really? Strictly speaking salt One may speak of the adhesion of an epoxy lining to the carbon
fog tests only measure the coating’s performance in a salt fog steel substrate of a tank interior just as one may speak of the ad-
cabinet. Pragmatically, the testers are often seeking some form of hesion of an overcoat paint job applied to an already painted sub-
information concerning corrosion or creep resistance in the con- strate. Hot dip galvanizing has a certain amount of adhesion to
text of highly corrosive atmospheric services. The 2019 version of raw steel and a coating may later be applied to that same galva-
the standard itself reads (under the heading “significance and nizing and we may inquire about its adhesion as well. The concept
use)[1]: is nearly ubiquitous in coatings.
“3.1 This practice provides a controlled corrosive environment The adhesion of an industrial coatings system may be measured
which has been utilized to produce relative corrosion resistance by a multitude of parties for many commercial reasons. Including
information for specimens of metals and coated metals exposed but not limited to:
in a given test chamber ”
• The paint manufacturer measuring the adhesion of their
Would salt fog testing still serve its purpose if the standard tem- products on various substrates under various applica-
perature at which the test was run was increased one degree tion and curing conditions during the course of re-
Fahrenheit? What about if the salt concentration was just a little search, development and marketing of said coatings
higher than the specified 5 parts NaCl to 95 parts water? Or a little
lower? What if the angle of the panels sitting in the test chamber • An in-field inspector measuring the adhesion of a paint
was shifted one degree? ASTM B117 calls for a 95ºF temperature system installed on-site as part of an applicator quality
control process (either as mandated by a specification,
or in response to some perceived application issue in-
field during the course of the work) • Dipole Interactions: Molecular substances such as the
polymers that constitute cured paint are inherently com-
• A third party science, engineering or industrial services posed of uneven distributions of charge. Atoms at their
provider vetting technical claims about coatings in the core are composed of discrete units of charge such as
interest of consulting, producing a specification or simi- protons (+1 unit of charge), electrons (-1 charge) and
lar technical writing neutrons (no electric charge). As such, for coatings pol-
ymers there are always large sections of the molecules
• During the course of a failure analysis being conducted in question that posses a “net dipole moment”; or areas
i.e. some problem has occurred in the field and there is of a molecule that have a partially positive or negative
reason to seek the root cause of the failure electric charge. As positive and negative charges are
attracted to each other, and like charges repel, this type
Adhesion may be measured both under laboratory conditions and
under field conditions. The standard literature does not differenti-
ate in any way that necessitates one over the other.
It cannot be reiterated enough, the extent to which nearly all con-
ceivable variables are crucial and relevant in the reporting of coat-
ings adhesion data. The methodology used, the cure time and
conditions [temperature and relative humidity] the coating experi-
enced prior to testing, the substrate used, the substrate surface
preparation method used, and precise details of the test as con-
ducted are all hyper-relevant and may skew results significantly.
For the remainder we restrict our scope to thermosetting [chemi-
cally cured] organic coatings applied to metallic substrates as the
topic of concrete adhesion is complex and an entire topic mostly
unrelated to coatings over metallic substrates. This also limits the
scope in terms of resin technologies discussed to the commonly
used two component or moisture cured industrial coatings types;
namely epoxies, two component urethanes, novolacs, vinyl es-
ters, epoxy poly-siloxanes, moisture cured urethanes and alkyds.
In pragmatic terms adhesion on metallic substrates is measured Pull-off adhesion testing also offers additional information in addi-
by a variety of testing methodologies. A few of which are detailed tion to the adhesion value itself, it also captures the precise mode
below: of failure well; the modes discussed in the prior section. Pull-off
adhesion allows the testing technician to examine the dolly and
substrate after the test and determine which layer is exposed.
When there is coating on the dolly underside, remaining on the
substrate post-pull that indicates that the coating failed cohe- not simple in practice and is subject to many methodological ca-
sively. In cases where bare substrate is exposed there was at veats.
least some degree of adhesive failure at the substrate. See Fig-
ures 7-9 for demonstrative examples of adhesive and cohesive ASTM D4541 allows for the use of five different types of testing
failure on adhesion dollies. apparatus with corresponding methods. The five are enumerated
below:
Figure 7: Side view representation of adhesion dollies
showing complete adhesive failure to substrate (left) • Type I (discontinued) – This type of adhesion tester is a
and cohesive failure within film (right) crank driven dynamometer that mechanically pulls the
dolly from the substrate from turning the crank. These
are an older model of adhesion tester not in common
use today. As of the 2022 version of the standard this
method has been discontinued.
Figure 8: Image of polyamide epoxy primer, one coat • Type III (Method C) – Tester than pulls the dolly in an
system showing adhesive failure to unprepared alumi- automated fashion with hydraulic force.
num substrate from ASTM D4541 pull
• Type IV (Method D) – These are often referred to at
“patty-style” devices as the pulling action is imparted
onto the dolly by a metallic pancake shaped device con-
nected to an airline. Type IV devices typically have pre-
cise controls for the ramp speed of pulling force based
on the expected value of failure. Type IV adhesion test-
ing devices are often encountered in laboratory environ-
ments and are rarely practical in field.
Tape Adhesion
ASTM D3359 is a fairly common standard that comes with two
methods (Method A, and Method B). Both methods involve the
use of some kind of cuts to a film followed by adhering a certain
standard type of masking tape to the cut area. The tape is then
pulled away in a controlled manner and resultant amount of de-
lamination is observed.
Method A is the “X-cut” method where an “X” is cut into the film
with a knife in a manner similar to that described in the pick back Figure 17: Scoring rubric from ASTM D6677 as written.
knife adhesion method ASTM D6677. Here instead of picking at
the central cross of the “X” the tester will apply tape that is com-
pliant with ASTM D3359 [the standard defines the strength and
width of the tape, these tapes are commercially available and usu-
ally labelled “ASTM D3359 Tape” or similar].
In both methods the standard explicitly calls for the tape to pulled
back onto itself at a 180º angle. This tends to be the largest source
of error in the method as it is difficult to pull the tape at precisely
180º repeatably and variation in the angle of the tape being pulled
may result in relatively large variation in the compressive and ten-
sile forces experienced at the substrate.
Both methods use a 0-5 rating scale, the letter after the number
denoting the respective methods A and B. Both visual scoring ru-
brics have been reproduced below
“1.2 Test Method A is primarily intended to rate the adhesion In the context of paint specification and system selection it is im-
of coatings and coating systems greater than 125 μm (5 mils) in portant to note that adhesion only matters in so far as it is suffi-
total thickness, while Test Method B is primarily intended to cient to not be a hindrance to service life. That is, additional meas-
rate the adhesion of coatings and coating systems less than ured adhesion value beyond a certain value does not enhance
125 μm (5 mils) in total thickness. Test Method B is not performance or increase service life as has been examined thor-
considered suitable for films thicker than 125 μm (5 mils) oughly by Jaimal et Al[9]. In the same work just cited, it is important
unless wider spaced cuts are employed and there is an explicit to note that a correlation was found between corrosion prevention
agreement between the purchaser and seller.” [proxy for service life] and the degree of surface roughness in the
underlying metallic substrates. That would suggest that the con-
Tape adhesion is a robust qualitative method that, similar o knife ditions that lead to long paint service life also tend to lead to higher
adhesion offers a simple, qualitative assay to spot-assess adhe- adhesion values but the adhesion is the dependent variable in this
sion. Like all methods it is imperfect and suffers from a general view and not the causative agent for long service life once a cer-
lack of sensitivity and lack of discrimination between high adhe- tain minimum value is reached.
sion coatings and the standard itself says this explicitly.
Engineers should always use caution when selecting paints for a
Conclusions & Recommendations to Specifying specification. However they should especially use caution when
using paint manufacturer provided adhesion data. Adhesion
Engineers and Painted Asset Owners should not be a highly weighted factor to determine one coating’s
superiority to another for specifications. All major paint manufac-
Adhesion is a complex topic for which there are many variables turers are capable of producing very large pull-off adhesion values
driving the final outcome. When a coating’s adhesion is measured for public consumption due to the surface prep conditions in la-
it must be measured according to some methodology. The choice boratories and their access to Type IV, V and VI testing apparat-
of that methodology may have a large impact on how results area uses. These numbers are real measurements and say something
interpreted and decisions are made. It is crucial, to asset owners, about a coating’s potential maximum adhesion under ideal condi-
inspectors, engineers and paint manufacturers to understand the tions. However these numbers in no way reflect the numbers that
limitations of the testing methods they use. It is of even greater are likely to be measured on a real jobsite connected to the same
importance that results be compared “apples to apples” and re- said specification. This can be attributable to both the work con-
sults are not overinterpreted outside of their window of statistical ditions on site during real large scale surface preparation or vari-
power. ance in the testing methodology used on site versus the control
material laboratories use to test. Either way the adhesion pull data
An adhesion test conducted on a jobsite where coating has been submitted to engineers for specification acceptance is likely to
applied is likely not comparable to any testing conducted by the show much higher numbers than one would expect from the same
paint manufacturer. Both numbers are valid within their respective product in-field.
domains but both values may appear to be in conflict at first
glance. Where adhesion data is used to discriminate between coatings at
the specification level the following particular points should be
In the context of on-jobsite adhesion testing that may lead directly considered:
to decision making by the asset owner or engineer it is imperative
• Whether the specification is for in-shop fabricated new o The adhesion of the epoxy primer to the sub-
construction steel or is for on-site maintenance work is strate
not trivial when considering if reported manufacturer ad-
hesion numbers are comparable. The relative small o The adhesion of the intermediate coat to the
size of test panels virtually guarantees most data re- primer
ported as being taken over an SSPC-SP10 near white
metal blasted substrate was taken over a substrate o The adhesion of the topcoat to the intermedi-
blasted with angular grit to near SSPC SP-5 level. In ate coat.
reality, shop primed new construction steel is blasted to
a very clean level but usually with a mixture of shot and Facts such as say, the adhesion of the topcoat to the
grit rather than pure angular carbon steel or aluminum substrate are not relevant. However, all of this is cap-
oxide grit. This has an appreciable effect on profile tured holistically by pull-off testing of the entire system.
depth, angularity and adhesion to the subsequent coat- The coating will fail at the weakest bond point in the
ing[11]. On-site maintenance work is very unlikely to ever course of the test and as such gives you all limiting in-
achieve the same level of surface cleanliness as labor- formation about the system’s pull-off adhesion with one
atory blast operations or in-shop fabricators. number.
• In the context of ASTM D4541 adhesion pulls, high PVC • The use of different dolly adhesives, the use of scoring
(pigment volume concentration, a measure of the ratio around dollies (which ASTM D4541 allows for) and
of pigment to resin in a paint formulation) coating mate- other methodological variations allowed by the standard
rials inherently show lower numbers. The important ca- may have additional effects on ASTM D4541 or any
veat is that these lower numbers tend to be cohesive other methodology’s results.
failures rather than adhesive failures i.e. cured material
is left behind on the substrate that continues to protect. Closing Remarks
This effect is not negative as long as such materials
pass other reasonable measures of robustness. In fact Those who are involved in the writing of coatings specification lit-
cohesive failure by design is highly preferable to large erature, have input on such committees, and private engineers,
surface area adhesive failures seen in high cohesive consultants and specifiers working in the field actively should con-
strength materials such as elastomers, many water- sider these myriad of aforementioned variables when thinking
borne materials and thick film aromatic urethane/poly- about adhesion in coating’s during the course of their daily work
ureas. High PVC and/or low cohesive strength materi- and problem solving. Contained in the preceding paragraphs
als “breakaway coupling” materials include but are not there is no truly novel information though perhaps this may be the
limited to ceramic epoxies, glass flake epoxies, ethyl sil- first time such facts and principles have been complied into one
icate inorganic zincs and correctly water balanced ce- place for such an audience. The author hopes that by reading you
mentitious epoxy overlay materials. Moisture cured ure- have become more educated on the topic of industrial coatings
thane zincs are notably absent from this class [tending adhesion. Of all the m methodologies discussed, and all the vari-
to fail adhesively rather than cohesively]; speculatively ous ways to look at adhesion it is clear that there is no best meth-
due to their low zinc loadings. odology or absolute best current precise scientific understanding
of the topic.
• Pull-off and tape adhesion are useful methods but do
not simulate any meaningfully likely real world condi-
tion. That is not a criticism of them as methods per se,
but such things should be taken in context. Knife pick-
back adhesion also does represent much of a real world
R E F E R E N C E S:
condition (instances of scoundrels attacking our poor
1) ASTM B117-19 Standard Practice for Operating Salt
steel with bladed weapons are rare) but the method
Spray (Fog) Apparatus; ASTM International, 2019
does inherently approximate some form of gouge or cut
resistance assay and as such speaks to general film ro-
2) ISO 9227:2022; Corrosion tests in artificial atmos-
bustness. ASTM D6677 is explicit that a cut must be
pheres — Salt spray tests; International Organization
made to all the way to substrate and so for samples
for Standardization, 2022
where a cut cannot be made with a knife and hand pres-
sure that offers information about the adhesion of the
3) Epoxy Adhesion to Metals; Schmidt, Bell, Advances in
film in itself.
Polymer Science, 33–37 1975
• Adhesion testing for induvial coatings is interesting but
4) The Critical Humidity Effect in the Adhesion of Epoxy to
not particularly relevant where multi-coat systems are
Glass: Lefebvre, D.R.; Elliker, P.R.; Takasahi K.M.;
specified. Teka for example a typical industrial atmos-
Ragu, V.R.; Kaplan, M.L.; Journal of Adhesion Science
pheric service system, two coats of epoxy at 2-3 mils
& Technology 2012
each followed by a urethane topcoat at 2-3 mils. Only
the following facts area relevant at all with respect to
5) Paint Adhesion, Corrosion Protection & Interfacial
adhesion:
Chemistry; Dickie, R.A.; Ford Research Laboratory
Ford Motor Company; 1994
6) Theory of Adhesion & its Practical Applications, Butt,
M.A.; Chughati, A; Ahmad, J.; Ahmad, R.; Majeed, U.;
Kahn, I.H.; Journal of Faculty of Engineering & Technol-
ogy 2007-2008