A Multifunctional Coating for

Autonomous
Corrosion
Control
N early a ll me tals a nd t heir a lloys a re
subject to corrosion that causes them
to l ose t heir s tructural in tegrity o r
other f unctionality. I t i s e ssential t o
detect corrosion when it o ccurs, a nd
preferably at its early stage, so that action can be taken to
avoid structural damage or loss of function of metals and
their alloys. Because corrosion is mostly an electrochem-
ical p rocess, pH a nd ot her e lectrochemical cha nges a re
synthesis, as well as selected test results of the smart
coating w ith pH- sensitive m icrocapsules fo r c orrosion
indication and inhibition.

Corrosion and pH
Corrosion i s la rgely a n e lectrochemical phe nomenon,
because, in most cases, it involves the transfer of electrons
between a metal surface and an aqueous electrolyte solu-
tion. F or i nstance, whe n i ron c orrodes i n ne ar neu tral
often ass ociated w ith it, s o it is expected that materials environments, the typical electrochemical reactions are:
that a re pH o r ot herwise e lectrochemically r esponsive
can be used to detect and control corrosion. The authors Cathodic reaction: O2 + 2H 2O +4e – N 4 OH –
developed a s mart c oating w ith a c ontrolled-release
system that uses pH-triggered release microcapsules for Anodic reaction: Fe N Fe2+ + 2e –
early detection of corrosion and for corrosion protection.
This article describes the relation between pH and corro- In the case of localized corrosion, such as pitting cor-
sion, t he design of pH- sensitive m icrocapsules a nd t heir rosion as shown in Figure 1, the anodic reaction hap-
pens i n a c onfined a rea, t he me tal ion s p roduced a re
precipitated a s s olid c orrosion p roducts, s uch a s i ron(II)
FIGURE 1 | The electrochemical cell set up between anodic and cathodic sites on
an iron surface undergoing pitting corrosion.
oxide, F e(OH)2, (of ten f urther o xidized t o i ron(III) o xide,
Fe(OH)3), wh ich c overs t he mou th of t he p it. Th is c over-
ing traps the solution in the pit and allows the buildup of
Porous cap
hydrogen ion s, H +. The o verall e ffect i s t hat, wh ile lo cal-
O2 + H2O
ized corrosion happens, the anode area often has an acidic
Passive film pH and the cathode has an alkaline pH.1
O2 + H2O CI- Besides p itting, c revice c orrosion a nd d issimilar me tal
OH- corrosion result in pH changes as illustrated by the simple
Fe(OH)3
demonstration sho wn i n F igure 2 , whe re a u niversal pH
indicator was used to show the pH cha nges that occur dur-
ing corrosion of a metal, such as steel. In this demonstra-
e- CI-+ H2O tion, most of t he steel was exposed to agar gel while a s trip
Fe(OH)2
in the middle was wrapped in copper tape. The color change
of the pH i ndicator shows that the exposed steel tends to be
+CI-+ H+ acidic ( yellow c olor) wh ile t he s trip w rapped i n t he c opper
Fe2+ tape tends to be basic (purple color) due to the oxygen reduc-
e- Acid chloride tion reaction and the release of the hydroxide ion, OH-.
pit electrolyte Since pH a nd ot her e lectrochemical cha nges a re of ten
associated w ith c orrosion, i t is e xpected th at m aterials
Iron that are pH or otherwise electrochemically responsive can
be u sed t o d etect a nd c ontrol c orrosion. Various pH a nd

By Luz M. Calle | NASA, Kennedy Space Center, FL; and Wenyan Li, Jerry W. Buhrow and Scott T. Jolley | ASRC Aerospace, Kennedy
Space Center, FL

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068-NASA-FT.indd 68 10/21/11 1:20 PM

 electrochemically r esponsive m aterials a s w ell a s t heir FIGU RE 2 | pH changes associated with corrosion.
potential applications in smart coatings for corrosion con-
trol c an b e fou nd i n ou r p revious r eview.2 A s elf-healing
coating i s a nother new d evelopment i n m aterial d esign
that is important to corrosion control.3,4,5 Acidic

pH-Sensitive Microcapsules
The a uthors d eveloped a c ontrolled-release s ystem t hat
combines the advantages of corrosion sensing and protec- Slightly 0h 5h
tion by using pH-triggered release microcapsules for early Acidic
corrosion d etection a nd p rotection.2,6,7,8 The key c om-
ponent of th is technology is a pH-sensitive m icrocapsule Neutral
with a wall designed to break down and release the encap-
sulated contents in response to the pH of the cathodic site
Slightly
of localized corrosion (Figure 3).
Basic

Smart Coating Based On 1h 3 days

pH-Sensitive Microcapsules Basic
Microencapsulation is a versatile approach because it can
be used to encapsulate an unlimited number of materials, FIGU RE 3 | The key component of the smart coating system: pH-sensitive microcap-
in both solid and liquid phase, and even in the gas phase sules.
when entrapped in aerogel. It is possible to incorporate
microcapsules i nto c omposites o r c oatings. F or c orro- Microcapsule containing pH
sion ap plications, va rious c ompounds, s uch a s c orrosion indicator (inhibitor, self healing agents)
indicators, inhibitors, self-healing agents and dyes can be
encapsulated. The se m icrocapsules c an b e i ncorporated
into va rious c oating s ystems fo r c orrosion d etection, OH-
protection a nd s elf-repair of me chanical coating da mage
(Figure 4). The versatility of t he design is of s pecial inter- The shell of the microcapsule breaks
est in corrosion-inhibition applications. Almost all corro- down under basic pH (corrosion)
sion inhibitors are chemically active reagents. Very often,
conditions
the reactivity that makes them effective corrosion inhibi-
tors also causes them to be environmentally unfriendly, OH-
such as in the case of chromates. Because of this, research
for new and environmentally friendly corrosion inhibitors
is an on-going effort in the corrosion protection industry.
pH indicator changes color and is
After a new i nhibitor is developed, it u sually takes a lon g
time t o i ncorporate it i nto a p aint fo rmulation. A s mart released from the microcapsule
coating that includes encapsulated inhibitors and releases when corrosion starts
them on demand when corrosion starts can shorten this
long r eformulation p rocess fo r new i nhibitors by s imply
FIGU RE 4 | Smart coating with pH-sensitive microcapsules for corrosion detection
changing the core content of the microcapsules. and protection applications.
The pH controlled-release microcapsule design has,
1. Corrosion indicators
in ad dition t o a ll t he adva ntages of t he r egular m icro-
capsule d esign, t he t rue c ontrolled-release f unction fo r 2. Corrosion inhibitors
corrosion ap plications. Re gular m icrocapsules r elease 3. Healing agents
their c ontents whe n t hey a re me chanically br oken; pH-
sensitive m icrocapsules r elease t heir c ontents whe n c or- O2 + H2O
OH-
rosion o ccurs. Me chanical da mage i n a c oating i s one of
the important causes for corrosion of the base metal. How- Incorporated into
ever, m any c oating d efects, s uch a s a ir bubble s, u neven coating Fe2+ e-
thickness, permeation, porosity or edge effects, will also
result i n p oor c orrosion p rotection of t he c oating a nd
Mechanical damage Corrosion
allow corrosion to occur. pH-sensitive microcapsules will causes capsule causes capsule
release their content for corrosion detection or protection to rupture to rupture
regardless of the corrosion cause. OH-

Chemistry of the pH-Sensitive Microcapsules

The che mistry of t he pH- sensitive m icrocapsules i s ba se- Ruptured microcapsule:
catalyzed e ster h ydrolysis. The p olymeric w alls of t he - indicates corrosion Fe2+ e-
microcapsules i nclude a c rosslinking a gent t hat ha s one - protects metal from corrosion
- repairs damaged area

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 A Multifunctional Coating for Autonomous Corrosion Control

or mo re e ster a nd me rcapto g roups. A t ypical c ross- Capsule w all br eakdown u nder ba sic c onditions c an
linker is pe ntaerythritol te trakis ( 3-mercaptopropionate be ob served v isually. F igure 5 sho ws s uch br eakdown
or PTT), a tetra-functional molecule. occurring i n r esponse t o ex posure t o a s mall a mount
Since this crosslinker is not a good film former, other of w ater c ontaining s odium hydroxide, N aOH, ( pH 12).
prepolymers o r mon omers a re ne eded t o p rovide t he Soon a fter t he N aOH s olution w as ad ded, t he s olution
structural integrity of the microcapsule wall. Examples starts to penetrate the microcapsule wall, as indicated by
of f ilm-forming m onomers an d p repolymers in clude the color change inside the microcapsules (Frames b-d).
urea formaldehyde and melamine formaldehyde mono- In Frame e, the microcapsule begins to slowly release its
mers and prepolymers. contents (a s ev idenced by t he s mall d roplet t hat b egins
to form on the bottom left quadrant of the frame). The
FIGU RE 5 | Microcapsule breakdown in basic solution. content c ontinues t o b e r eleased u ntil ( Frame i) it d issi-
pates into the solution. The microcapsule wall eventually
a b c d e f g collapses as shown, in Frames j through n.

Encapsulation Process
h i j k l m n
Encapsulation Methods
pH-sensitive microcapsules are the key c omponent of t he
smart c oatings. S everal me thods s uch a s s pray d rying,
emulsion p olymerization, i nterfacial p olymerization, a s
well as in-situ polymerization have been used to synthe-
FIGU RE 6 | Schematic representation of the steps involved in the interfacial poly- size p H-sensitive m icrocapsules. I nterfacial p olymeriza-
merization of an oil-in-water microemulsion for making oil core microcapsules. Oil tion is illustrated in Figure 6 as an example. There are
is shown in yellow and water in blue. two main steps involved in the interfacial polymerization
Capsule with process: microemulsion formation and microcapsule wall
Surfactant Prepolymer formation. This technique can be used to form both oil (or
polymer wall
hydrophobic) core and water (or hydrophilic) core micro-
capsules. F igure 6 sho ws a s chematic r epresentation of
Oil the s teps i nvolved i n forming oi l c ore m icrocapsules: t he
microemulsion i s fo rmed by ad ding t he oi l pha se ( with
prepolymer, sho wn i n y ellow) t o t he w ater pha se ( with
surfactant, shown in blue) and mixing; the last step is the
formation of the microcapsule wall (shown in green) by
interfacial p olymerization. F igure 7 sho ws a s chematic
representation of the steps involved in forming water core
microcapsules: in this case, the microemulsion is formed
Water by adding water (shown i n blue) to the oi l (with prepoly-
mer and the surfactant, shown in yellow) followed by mix-
ing; the last step is the formation of the microcapsule wall
Addition of oil and Mixing Polymerization (shown in green) by interfacial polymerization.
prepolymer These two illustrations involve the use of oi l, or hydro-
phobic s olvent-soluble w all-forming p repolymer. A s im-
ilar p rocess ha s b een d eveloped t o u se w ater-soluble
FIGU RE 7 | Schematic representation of the steps involved in the interfacial poly- wall-forming ma terials b y d issolving t he wa ll-forming
merization of a water-in-oil microemulsion to synthesize water core microcapsules. prepolymer in the water phase and the catalyst in the oil
Oil is shown in yellow and water in blue. phase. The reaction at the interface will form the capsule.
In situ polymerization is also used to form pH-sensitive
Prepolymer Surfactant Capsule with microcapsules. T he in si tu po lymerization p rocess is
polymer wall
similar t o i nterfacial p olymerization; t heir d ifference i s
the lo cation whe re t he p olymerization r eaction o ccurs.
For i nterfacial p olymerization, r eaction o ccurs at t he
interface; the polymerization reaction occurs in the con-
tinuous phase for in situ polymerization and the polymer
is formed th rough the reaction deposits at the i nterface
Water to form the capsule wall.
Spray d rying i nvolves d ispersing t he wa ll-forming
prepolymer and substance to be encapsulated (the core
material) into a c ontinuous phase (water for instance).
Oil Oil The mixture is sprayed into a mist and in a hot gas flow
where t he l iquid d roplets a re d ried i nto s olid p articles.
In the process, the core material is encapsulated inside
Addition of water Mixing Polymerization the wall materials.

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 A Multifunctional Coating for Autonomous Corrosion Control

size s olid c ore m icrocapsules a nd a s a u seful me thod fo r

FIGURE 8 | Oil core microcapsules of different sizes.
drying m icrocapsules i nto a f ree-flowing p owder fo rm
without forming clusters.

Microcapsule Synthesis
Different a ctive core co ntents h ave b een en capsulated,
including c orrosion i ndicators, c orrosion i nhibitors, dy e
50 μm
and s elf-healing a gents. B oth w ater c ore m icrocapsules
and oi l c ore m icrocapsules w ere s ynthesized u sing t he
FIGURE 9 | SEM images of the water core microcapsule. methods described above.
To t ailor t hese p rocesses fo r e ncapsulating c orrosion
inhibitors an d in dicators, v arious in dicators an d inhi bi-
tors w ere s elected a nd t ested fo r t heir i ndicating a nd
inhibiting e fficiency r espectively. The s olubility a nd d is-
persibility of t he ac tive c ompounds w ere s urveyed o r
tested to find a suitable method for their encapsulation.
An active compound that can be dissolved or dispersed
in a hydrophobic solvent, such as oil, can be encapsulated
into oi l core m icrocapsules. Normally, oi l core m icrocap-
sules a re used for encapsulating oil-soluble materials but
not w ater-soluble m aterials, s uch a s s alts o r p olar mol -
1 µm NASA 10/22/2009 1 µm NASA 10/22/2009
X 3,000 0.30kV SEI GB_HIGH WD 3mm X 7,000 0.30kV SEI GB_HIGH WD 3mm
ecules. However, these materials can still be encapsulated
by dissolving them first into a polar co-solvent and adding
Interfacial p olymerization a nd in si tu po lymerization the r esultant s olution t o t he oi l pha se. A lternatively, a
are t he m ain ap proaches u sed by t he a uthors fo r m icro- surfactant can be added to the oil phase. This will dissolve
capsule synthesis. Spray drying has been used to synthe- or disperse the polar or water-soluble reagents into the oil

Read about the next generation,

“0 VOC”, Borchi® OXY – Coat 1101 in the
Emerging Technologies Section, page 83

PCI11114OMG.indd 1 10/14/11 9:37 AM PCI11114

068-NASA-FT.indd 72 10/21/11 1:21 PM
 phase. The oil-in-water emulsion can then be formed and
FIGURE 10 | SEM images of a water core microcapsule obtained by using a transmis-
the i nterfacial r eaction c an b e u sed t o e ncapsulate t hese
sion electron detector.
reagents into the oil core of the microcapsules.
Similarly, if a compound can be dissolved or dispersed in
water, with or without the aid of a c o-solvent, or a s urfac-
tant, it is possible to encapsulate it into water core micro-
capsules. For example, phenolphthalein does not dissolve in
water, but ethanol can be used as a co-solvent to dissolve a
moderate amount of the indicator in water, making it pos-
sible to encapsulate it into water core microcapsules.
Various c ompounds of i nterest fo r c orrosion c ontrol
applications have been encapsulated into oil core micro-
capsules. These compounds i nclude: corrosion i ndicators
100 nm NASA 10/22/2009 100 nm NASA 10/22/2009
such a s phe nolphthalein, phe nol r ed, a nd f luorescein; X 35,000 30.0kV TED SEM WD 5 mm X 80,000 30.0kV TED SEM WD 5 mm
dyes such as Rhodamine B; healing agents such as epoxy
and p olysiloxane; a nd va rious s olvents, s uch a s ch loro- cation. The c apsule size can b e controlled by adju sting
benzene, which can be used as a healing agent. the emulsion formula or by varying the mixing speed of
Various c orrosion i nhibitors a nd i ndicators ha ve b een the m ixer du ring the emulsion formation. These meth-
encapsulated into water core microcapsules, such as ods can be used to obtain microcapsules of a desired size
the c orrosion i ndicator phe nolphthalein, a nd c orrosion within a na rrow ra nge of d istribution. Si zes f rom 2 00
inhibitors s odium m olybdate ( Na2MoO4), ce rium ni trate nm to 200 µm (micron) can be obtained, with a typical
(Ce(NO3)3), s odium pho sphate (N aH 2PO4), c alcium size f rom ab out 1 t o 5 µ m. O il c ore m icrocapsules of
metaborate, and phenylphosphonic acid. various sizes are shown in Figure 8.
Af ter a m icrocapsule fo rmula i s d eveloped, a n op ti- The SEM images in Figure 9 show capsules of spherical
mization p rocess u sually fol lows t o obt ain m icrocap- shape w ith less than 1 μm i n d iameter s ize. The c apsule
sules of suitable size and desired properties for its appli- wall thickness is about 50-100 nm as shown in the micro-

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068-NASA-FT.indd 73 10/21/11 1:22 PM
 A Multifunctional Coating for Autonomous Corrosion Control

graphs of t he m icrocapsules obt ained u sing a t ransmis- Corrosion Indication Tests

sion electron detector (Figure 10). Corrosion indication can be incorporated into the coating
by e ncapsulating a c orrosion i ndicator i nto pH- sensitive
Experimental microcapsules. F igure 11 shows t he r esults f rom t he s alt
Microcapsules were incorporated into dif ferent c ommer- immersion test of steel panels coated with a clear urethane
cially available coatings in order to test their corrosion coating containing 10% of m icrocapsules w ith corrosion
indication an d inhi bition f unctions. P reliminary r esults indicator. The panels were scribed and observed for visual
of these tests are presented below. changes over time. It w as observed that the indicator sig-
naled the onset of c orrosion in the scribe about 1 m inute
FIGURE 11 | Corrosion indication test results. after immersion, which is considerably earlier than the 2
hours for the appearance of the typical rust color.
Initial 30 sec 2 min 3 min 5 min In ad dition t o e arly c orrosion d etection, a nother
potential ap plication of t he s mart c oating i s t o d etect
hidden corrosion, for example on structural bolts. Bolts
tend t o c orrode on t he h idden sha ft a rea b efore v isible
corrosion is seen on the bolt head or nut. Often, the head
and nut are in pristine condition, even when significant
corrosion has occurred on the shaft. There is no method
to identify the degree of corrosion without removing the
bolt f rom s ervice. A c oating t hat cha nges c olor on t he
bolt he ad o r n ut whe n c orrosion s tarts w ould g reatly
20 min 30 min 1h 2h 5h speed up the inspection process.

Corrosion Inhibition Tests

Test panels coated with Carboline Carbomastic 15 FC
epoxy m astic c ontaining w ater c ore m icrocapsules w ith
an i nhibitor w ere t ested u sing a s alt fog cha mber, fo r
approximately 6 months, following the ASTM B 117 stan-
dard method. Panels were evaluated for both rust grades
(ASTM D 610) and scribe ratings (ASTM D 1654). Several
coating systems were tested; the coating containing 10%
20 h 48 h 74 h 116 h 139 h
phenylphosphonic acid m icrocapsule performed the best.
The corrosion ratings of these panels are shown in Table 1
in comparison with the controls.
After s ix mont hs of s alt fog t esting, t he c ontrol
showed bl isters a nd c orrosion u nder t he p aint, wh ile
the phenylphosphonic acid (PA) microcapsule-containing
panel showed no sign of corrosion. In order to evaluate
the s cribe a reas, t he c oating a round t hese a reas on t he
panels was scraped off for easy observation (Figure 12). It
was fou nd t hat t he PA m icrocapsule-containing c oating
showed much better adhesion than the control.

FIGURE 12 | Six-month salt fog test results of selected coating systems. Summary
B1-1 B1-2 B1-3
A m ultifunctional s mart c oating fo r t he a utonomous
control of c orrosion i s b eing d eveloped u sing pH- sen-
sitive m icrocapsules. The m icrocapsules a re d esigned
specifically to detect the pH changes that are associated
with the onset of c orrosion a nd respond autonomously

TABLE 1 | Rust grade and scribe rating of Carbomastic 15 FC

experimental coatings.
Control Carbomastic 15 FC
Carbomastic 15 FC Scribe
B7-1 B7-2 B7-3 Sample # Rust Grade
Coating Systems Rating
1 5 5
Control 2 10 5
3 6 5
10% (w/v) 1 10 5
phenylphosphonic 2 10 5
10% Phenylphosphonic Acid Water Core Capsules in Carbomastic acid microcapsule 3 10 5

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 A Multifunctional Coating for Autonomous Corrosion Control

to indicate its presence early, to control it by deliver- References

ing c orrosion i nhibitors, a nd t o d eliver s elf he aling o r 1 Maile, F. J.; Schauer, T.; and Eisenbach, C.D. Evaluation of Corro-
film-forming ag ents ca pable o f repa iring m echanical sion and Protection of Coated Metals with Local Ion Concentration
damage to the coating. Technique (LICT), Progress in Organic Coatings 38, 111 (2000).
Various pH- sensitive m icrocapsules w ith h ydrophobic 2 Li, W. and Calle, L.M. pH and Electrochemical Responsive Mate-
or hydrophilic cores were synthesized through interfacial rials for Corrosion Control Applications (Invited), NACE Corro-
polymerization r eactions i n a n e mulsion. T he m icroen- sion 2008, New Orleans, LA, March 2008.
capsulation p rocess w as op timized t o obt ain mon odis- 3 Kessler, M.R. Self-Healing: A New Paradigm in Material Design,
persed microcapsules in a s ize range suitable for incorpo- Proc. I MechE Vol. 2 21 P art G : J . A erospace E ngineering, p age
ration i nto c ommercially a vailable c oatings. The m icro- 479-495 (2007).
capsules can be obtained in suspension or in free-flowing 4 Andersson, Magnus; Wilson, G erald O.; Wh ite, S cott R. E valu-
powder form. ation o f S elf-Healing P olymer Che mistries fo r A pplication i n
Preliminary r esults f rom s alt fog t esting of p anels Anti-Corrosion Coatings, American Coatings Conference 2008
coated w ith co mmercially available co atings i n w hich at Charlotte, NC (June 2-4, 2008).
the m icrocapsules a nd p articles w ere i ncorporated 5 Cho, Soo Hyoun, PhD Thesis “Polydimethylsiloxane-Based Self-
indicate t hat m icrocapsules a nd p articles c an b e u sed Healing Composite and Coating Materials”, University of Illinois
to d etect c orrosion b efore v isible r ust ap pears a nd t o at Urbana-Champaign, Urbana IL (2006).
deliver corrosion inhibitors. 6 Li, W . a nd C alle, L .M. C ontrolled Re lease M icrocapsules fo r
Current w ork i s fo cused on op timizing t he c oncen- Smart Coatings, NACE Corrosion 2007, Paper 07228, Nashville,
tration of i ndicator i n t he m icrocapsules o r p articles TN, March 2007.
as well as on optimizing the release properties of the 7 Li, W. a nd C alle, L .M. A Sm art C oating for t he E arly D etec-
microcapsules a nd p articles whe n i ncorporated i nto tion a nd I nhibition of C orrosion, P roceeding of t he Sm art
coatings of i nterest. E ncapsulation me thods fo r s elf- Coatings 2007, p.191, Orlando, Florida, February 2007.
healing agents a nd f ilm-forming compounds a re being 8 Calle, L .M. a nd L i, W. C oatings a nd Me thods fo r C orrosion
developed t o i ncorporate t he s elf-healing f unction i nto Detection and/or Reduction, U.S. Patent No. 7,790,225, U.S.
the multifunctional coating. 䡲 Patent and Trademark Office, September 7, 2010.

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