o Ie
Ing
BY INDUMATHI S.N. A, T. VASUDEVANB, S. SUNDARRAJANA, BV.sUBBA RAOA,
cvs. MURTHYA AND D.R. YADAVA
ADEFENCE RESEARCH AND DEVELOPMENT LABORATORY, KANCHANBAGH
P.O, HYDERABAD - 500 058, ANDHRA PRADESH, INDIA
BKALASALINGAM UNIVERSITY, KRISHNANKOIL - 626190 VIRUDHUNAGAR
DISTRICT, TAMIL NADU, INDIA
Cadmium- and Chromate-Free
Coating Schemes for Corrosion
Protection of 15CDV6 Steel
ABSTRACT
Electrodeposits of cadmium- and
chromate-based inorganic inhibitor
pigments in paint formulations are
extensively used in the aerospace
industry to provide long-term cor-
rosion protection for high-strength
steel hardware. Due to environmen-
tal concerns and worker safety
issues, there is a pressing need to
identify and adopt alternative eco-
friendly coatings with equivalent
performance. In this work, an eco-
friendly cadmium- and chromate-
free coating scheme comprised of
zinc nickel alloy plating, trivalent
chromium- based passivation, fol-
lowed by a primer based on polyani-
line phosphate, is studied for its
anticorrosive properties. Long-term
performance evaluation studies of
this eco-friendly coating scheme
were carried out on 15CDV6 steel,
an ultra-high- strength steel used in
the aerospace industry.
For comparative purposes, two
extensively used cadmium- and chro-
mate-based schemes complying to
aerospace and military specifications
comprised of cadmium plating,
hexavalent chromium-based passiva-
tion followed by two different chro-
mate-based primers were studied on
15CDV6 steel substrate.
Electrochemical impedance spectro-
scopic studies and salt fog exposure
tests were carried out to evaluate the
anticorrosive properties of the coat-
www.organicfinishing.com
ing schemes. Cadmium- and chro-
mate-free scheme exhibited excellent
performance in the long-term corro-
sion evaluation studies. The results
obtained in accelerated tests show
the possibility of replacement of cad-
mium- and chromate-based schemes
for corrosion protection of steels
with an ceo-friendly option.
INTRODUCTION
Cadmium coatings and chromate-
based corrosion inhibitors in pro-
tective coatings are extensively used
in the aerospace industry at present
to protect high-strength structural
steel. 15CDV6 steel is a low carbon,
low alloy, ultra-high-strength steel
possessing yield strength of 950 to
1000 MPa. This steel also possesses
good weldability and toughness,
and is extensively used for the fabri-
cation of pressure vessels, rocket
motor casings and other structural
hardware in the aerospace and
defense industries. A proven and
preferred scheme for long-term cor-
rosion protection of this structural
steel is cadmium plating carried out
either by electrodeposition or physi-
cal vapor deposition followed by an
efficient painting scheme. The cad-
mium coating on steel acts both as a
barrier coating, separating the steel
substrate from the environment,
and as a sacrificial coating, provid-
ing protection when the coating
becomes damaged. A chromate pas-
sivation treatment is applied to the
cadmium plating to promote adhe-
sion of the subsequent paint layer
and to improve the corrosion resist-
ance of the cadmium coating.
Cadmium plating is provided as
an undercoat to chromate-based
primers on steel hardware demand-
ing longer service life.
Electroplating of cadmium is car-
ried out from hazardous, cyanide-
based chemicals. The usage of cad-
mium and chromates is regulated
worldwide due to environmental
concerns and the adverse health
effects surrounding the usage of
such hazardous chemicals. Studies
are being carried out extensively to
identify potential alternatives [1].
Electrodeposited zinc nickel alloy
coatings being tested worldwide,
particularly zinc nickel alloy coat-
ings with 10 to 15% nickel in the
deposit, were found to possess supe-
rior corrosion resistance and lesser
susceptibility to hydrogen embrittle-
ment when compared to the exten-
sively used electrodeposits of cadmi-
um [2-5]. Zinc cobalt alloy plating
with 1% cobalt in the deposit and a
thin nickel interlayer on high-
strength steel was found to possess a
lower hydrogen embrittlement index
when compared to electrodeposits
of cadmium [6].
Chromate compounds are exten-
sively used in the protective coatings
to protect industrial ferrous and
nonferrous alloys. Here, chromates
refer to compounds containing hexa-
valent chromium (Cr 6 +). They are
employed in the coating systems
through various means, such as pig-
ments in paints like strontium chro-
mate and zinc chromate, chromate
conversion coatings and chromic
acid anodization of the aluminum
alloy substrate [7]. Chromates are the
commonly used pigments in the
primer coating [8]. Apart from their
impact on the environment, usage of
chromate-containing compounds
ApriVMay 2011 I metalfinishing I 15
ORGANIC
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pose serious worker safety issues.
In finding a replacement for chro-
mate inhibitors, Kendig er al studied
the characteristics of Cr 6+ that make
it an effective inhibitor [9]. Some of
the most promising chromate
replacement inhibitors are derived
from cerium salts [10]. Zinc phos-
phates were the initial replacement
pigments for zinc chromate; they dis-
play no toxic effects and provide
some corrosion protection by form-
ing a Zn 3(P04) 2' 4 H 20 film [11]. Yl,
Kuznetsov et al studied organic cor-
rosion inhibitors as possible chro-
mate replacements. This resulted in a
thin (up to 20 nrn) but tenacious
passive layer [12].
Electroactive conducting polymers
continue to be of considerable inter-
est as components of corrosion-
resistant coating systems.
Electroactive conducting polymers,
in addition to being conductive, are
redox active materials with poten-
tials that are positive of most metals
and alloys such as aluminum, mag-
nesium, steel, and zinc. As with chro-
mate, interesting and potentially
beneficial interactions of electroac-
tive conducting polymers with active
metals and alloys are anticipated
Table 1. Chemical composition of 1SCDV6 steel
[13]. Polyaniline is an important can-
didate material for anticorrosive
coatings in the family ofelectroactive
conducting polymers. Polyaniline-
containing paints are studied for
their anticorrosive properties on
steel [14-16].
Barbucci et. aL reported the study
on chromate-free pretreatments and
primers for the corrosion protection
of galvanized steel sheets and recom-
mended a chromate-free coating sys-
tem consisting of nitro-cobalt chem-
ical conversion with fluoro zincate
passivation coated by an epoxy
polyurethane primer having ionic
exchange active pigments [17].
Studies finding alternatives to haz-
ardous chromate pretreatments,
primers and cadmium coatings are
available individually, but little infor-
mation is available on cadmium- and
chromate-free coating schemes for
structural steel demanding longer
service life. This paper deals with the
performance evaluation studies car-
ried out to assess the efficacy of cad-
mium- and chromate-free coating
scheme comprised of zinc nickel
alloy plating + trivalent chromium
based passivation + polyaniline
phosphate-based primer on ultra-
high-strength 15CDV6 steel against
the conventionally used scheme of
cadmium plating + hexavalent
chromium-based passivation + chro-
mate based primer.
EXPERIMENTAL
Three coating schemes on 15CDV6
steel substrate, two based on cadmi-
um plating, hexavalent chromium-
based passivation and chromate-
based primers conforming to mili-
tary specifications and aerospace
standards and a cadmium- and chro-
mate-free coating scheme were evalu-
ated for their anticorrosive proper-
ties by means of electrochemical
impedance spectroscopy and salt fog
exposure tests. The chemical compo-
sition of 15CDV6 steel substrate
taken up for experimental work is
provided in Table 1.
The details of cadmium- and chro-
mate-based coating schemes taken

Order of treatment Process step details Cadmium and Cadmium and Cadmium and
chromate based chromate based chromate based
scheme 1 scheme 2 scheme
1. Electroplating Cadmium plating of Cadmium plating of Zinc nickel alloy plat ing
8-10 I.l thickness from 8-10 I.l thickness from of 8-10 I.l thickness
cyanide bath as per cyanide bath as per the from non-cyanide bath
the specification SAE specification SAE AMS - as per the specification
AMS -QQ-P-416 QQ-P-416 SAE AMS 2417G
2. Passivation treatment Hexavalent chromium Hexavalent chromium Trivalent chromium
based passivation as based passivation as based passivation as
per the specification per the specification per ASTM B633-07
SAE AMS -QQ-P-416 SAE AMS -QQ-P-416
3. Primer Coating Commercially available Commercially available Polyaniline phosphate-
zinc chromate-based strontium chromate- based epoxy primer of
epoxy primer of 301.l based epoxy primer of 301.l thickness prepared
thickness in compliance 30 I.l th ickness in com - in the laboratory whose
with specifications of pliance with specifica- details are provided in
MIL-P-23377G , Type I, tions ofMIL-P-23377G , section 2.1
Class C Type I, Class C
Table 2. Details of coating schemes taken up for experimental study on 1SCDV6steel substrate

161 metalfinishing I ApriVMay 2011 www.organicfinishing.com

ORGANIC
-fTnlshing II
•
•
• •
.'
ZnNi Jlloy plJting +tri vJI nt chromium b ased pJssi vJtion+
Pol YJniline phosphJte prim ron 15CDV6 steel subsuJte
,-
•
. •
.
............... .
,
to HUt!!e
•
up for study and its cadmium and
0' • ···.1. •• •
" '
'

chromate free counterparts are pro-

....•. • .., e. ...
x
•
. . .. - 00··.
-"
, 0
vided in Tab le 2. . t.:.~ •
7 ", •. oo ~ ; ••
I 00 0 • • • •
2.1 Formulation details ofPolyaniline 000 ' "
00 ' .
phosphate-based epoxy p rim er. I
c ; ,t
.t
Polyani line phosphate pigment was •.:
prepared by th e oxidative polymer-
'\ 0 \ 1ogCl) Z J
• I

ization of anili ne monomer in phos-

Figure 1. Bode plots as a funct ion of t ime for cadmium- and chromate-free coat ing scheme on
phoric acid medi um using ammoni-
15CDV6 steel substrate.
um per su lphate as an oxidant. The
reactio n was conducted at 5± 10°e.
All the che micals us ed were AR
• •••• • Cadmium platine + he xavalent chromium b a sed pa ssivation +
gra de. A dark green colored conduct- Zinc chromate ba sed primer on 15CDV6 st e e l su bs t r a te
.
ing polyaniline phosphate salt thus
formed was filtered and repeated ly
was hed with distilled water to
rem ove excess acid co ntent. T he
0'
~
J •
•
• ~!!!~' I h
7

7
•
·i •••
~··
'" "
....
•••
~ At"
.... . 9~?0
0 0
•
1:0
so ...
&0.,.,
IOO.~
.ay,

po lyme r was drie d in an oven at ". •••• .? ?2

750° C for two hours. The dried
• ••••• • •• • • • • i i i
0
polyaniJine ph osphate salt was fine 0
grinded using mortar. A pri mer with 't e
•.: ., 0 , Z J • 0
50% volu me solids and 30% PVC was 10010
prepared by usin g polyan ilin e phos-
ph ate, talc an d titaniu m diox ide as Figure 2. Bode plots as a function of time for cadmium- and chromate-based coating scheme 1 on
pigments. An epoxy resin with epoxy 15CDV6 steel substrate.

equiva len t of 500 (M/S Atul po ly-

mers, Gujarat) was used in the for-
mulation and th e pr imer was cured • '" '" Cadmium plating + he xa valent chromium based passi vation +
••••••• Strontium chromate based primer on 15CDV6 steel substrate
usin g ami ne ha rdener. The concen-
trat ion of polyaniJine phosphat e in
the pr im er was 1% by weigh t. The
p repar ed paint was pneumat ically
0'
X
~
.2
•
7
• •• •• • •
.0. ' , " . • ~ o ~ ·
00000000000000000
. .,
..... ...
• so ...

000
.. .....,. ~

•
.- • .,
' •
•
•
o ':Olllm
&O..... t.
IOOcl~

sprayed to a dry film thickness of 30 I ooooooooooooo ! ••

microns on 15CDV6 st eel pan els of •• ••
100mm x 50mm x 3mm size coated
with th e scheme provided in Tabl e 2.
T he pr im er coated panels were cured
0

•.: .\ 0 , Iog(l) Z J
••••
•
••• .... 0

for seven days at room tem perature

before procee ding for fu rt her evalua- Figure 3. Bode plots as a funct ion of time for cadm ium- and chromate-based coat ing scheme 2 on
tio n stu dies. For comparative st ud- 15CDV6 steel substrate .

ies, 15CDV6 steel pan els were also

coated with cadmiu m platin g and
chromate-based passiva tion, and
with two chromate-based primers as
per the scheme provided in Table 2.
2.2 Evaluation of anticorrosive prop-
erties. The evaluation of anticorrosive
properties of the coating schemes on
15CDV6 steel substrate (Table 2) was
carrie d out using AC impedan ce spec-
troscop y an d salt fog exposure tests.
Altern ating current impedance tech-
nique was used to evaluat e th e pro-
tect ive value of th e various coa tings meas urements were cartie d ou t peri-
sche mes . I cm 2 area of the coa ted odical ly and the resultant dat a was
sam ple was continuously exposed to analyzed for prot ective ability of the
a corrosive solution of 3.5% sodium various coating schemes.
chloride contained in a three elec- Imp edan ce measurem ents were car-
tro de pol arizat ion cell. Silver/ silver ried out using computer-controlled
chloride was used as reference elec- Porenriostar/ Galvanosrar of AUTO-
trode and platinum as auxiliary elec- LAB PGSTAT3 0 equipment. The
trode. An AC signal of lOmV ampli- electroc hemi cal im pedance monitor-
tude was applied to th e meta l solu- ing of the various coating schemes
tion interface at the op en circuit was carried out for 120 days in order
potential in th e freque ncy range of to assess th e capability of the
100KHz to lOmH z. The impedance schemes to provide long-term corro-

www.organicfin ishing.com April/May 2011 I metalfinishing I 17

ORGANIC
-fTnlshing
sion protection of the hardware.
In salt fog exposure tests, the sam- 5 5.40 X 10 9 6.05 X 10 9 8.80 X 10"
ples were continuously exposed to
alternate wet and dry cycles of salt
30 4.10 X 10 9 1.10 X 10 9 2.10 X 10"
fog generated from 5% sodium chlo-
ride solution as per MIL STO 810F
and the chamber temperature was 60 2.00 X 10 9 7.80 X 10 8 1.20 X 10 '0
maintained at 350°C throughout
the test duration. The test was con- 100 9.90 X 10 8 5.10 X 10 8 9.80 X 10 9
tinued until the failure of a particu-
lar sample by visual appearance. 120 7.80 x 10 8 6.50 X 10 7 8.30 X 10 9
Since the coating schemes studied
were intended to provide long time
Table 3. Logarithmic impedance values measured at 'OmHz for the coating schemes studied at
service life for the structural hard- various exposure durations.
ware, Taber abrasion tests were con-
ducted on the different coating
schemes as per the ASTM 0 4060
Details of coating schemes on 15CDV6 steel Salt fog resistance in hours
test method. The adhesion of the
substrate
coating schemes to the 15COV6 sub-
. strate material was evaluated by Chromate and cadmium free coating scheme 1290
sandwich pull-off method as per Chromate and cadmium based coating scheme 1 1230
ASTM 04541.
Chromate and cadmium based coating scheme 2 1225
RESULTS AND DISCUSSION Table 4. Results of salt fog exposure tests.
3.1 Electrochemical impedance
spectroscopic measurements
The evaluation of protective proper- Details of coating scheme Adhesive strength in Weight loss in
ties of different schemes studied N!mm 2 mg!1000cycles
was carried out using electrochemi- Chromate and cadmium 5 0.0096
cal impedance measurements over a free coating scheme
range of frequencies. Since the
Chromate and cadmium 4.7 0.0085
schemes taken up for study were
based coating scheme 1
complex, monitoring the total
impedance of the coating scheme Chromate and cadmium 4.9 0.0077
analyzed at the low frequency of based coating scheme 2
10mHz as a function of time was Table 5. Results of adhesion and abrasi on resista nce measurements.
chosen as an effective way to deter-
mine the condition of the deterio-
rating system. The relatively small studied at a low frequency of lOmHz tored in terms of impedance in elec-
decrease in the impedance of the as a function of exposure time is trochemical impedance spec-
system at the low frequency region given in Table 3. The decrease in low troscopy [18-25]. The data from
from its initial value even after pro- frequency impedance values as a impedance spectra can be divided
longed exposure to the corrosive function of exposure time is repre- into two major parts: the high fre-
electrolyte is a good sign for the sented graphically in Figure 4. quency region and low frequency
effectiveness of the system. This cri- An organic coating on the metal region. The low frequency part of
teria was considered to grade the surface can be considered as multi- the spectra represents the reactions
systems under study for their per- phase heterogeneous system and occurring at the bottom of the pores
formance in impedance studies. the corrosive species such as water, of the coating and is characteristic
The superimposed Bode plots of oxygen, ions of corrosive electrolyte of the metal-coating interface in
the impedance data of the different penetrate through the defects (i.e., terms of anticorrosive or corrosive
coating schemes studied as a func- pores in the coating) and reach the property [26-27].
tion of exposure time is provided in metal/coating interface, leading to From the impedance srudies car-
Figures 1, 2 and 3. the corrosion processes. The ried out on the coating systems
The logarithmic impedance values response of the coating system to taken up for srudy, it is observed
for the different coatings schemes this corrosion process can be moni- that the cadmium- and chromate-

18 I metalfinishing I April/May 2011 www.organicfinishing.com

ORGANIC
-finishing 1 .00e·1 2

free coating scheme shows a rela-

tively small decrease in the logarith-
mic impedance value at a low fre-
"[

f
.e-
N
l.OOE + l0

1 .00E .. 08

1 .00 e"0 6
-
- ----
quency of lOmHz after an exposure
duration of 120 days compared to
the other two cadmium- and chro-
ii 1 .00e" 04 - . - c a d m lu m + he •• Yo' ent c hr o m a'. + . tro n tl u m c h romate b ••ed
prtm.r
_ - c a d m iu m . he . 8v lent c h ro m ote + z inc c tvornar. ba• • dpnm .r
mate-based systems taken up for 'Ii 1 .00 E+0 2
~~nc nic ke l a ll oy + tri v alent c h ro m iu m'" PAN' pho apha,e baaed
8' rtmer
study. The cadmium- and chro- -'

mate-free coating based on zinc 1 .00E +OO

5 30 60 100 12 0
nickel alloy plating, trivalent E xpo sure d l¥ot lon ( days)

chromium-based passivation and

polyaniline phosphate- based Figure 4. GraphicaL representation of variation of Logarithmic impedancevaLues for the different coat-
ingschemes studied as a function of exposure duration
primer exhibited a low frequency
impedance value of 8.30 x 109 at a
measurement frequency of 10mHz
even after continuous exposure for
120 days to the corrosive 3.5% sodi-
um chloride solution. The imped-
ance value of the order of 10 9 after
prolonged exposure to corrosive
solution indicates the highly protec-
tive nature of the coating. The rela-
tively high order of impedance of
cadmium- and chromate-free Figure 5. Photographsof test specimen after faiLure in saLt fog tests

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www.organicfinishing.com April/May 2011 I metalfinishing I 19

ORGANIC
-finishing
scheme after 120 days when com-
pared to the other two chromate
and cadmium-based coating
schemes studied indicates it has bet-
ter anticorrosive properties on
15CDV6 steel substrate.
3.2 Salt fog exposure tests. Salt fog
resistance of the coating schemes
studied in terms of time taken for
the appearance of first failure on
prolonged exposure to salt fog is pre-
sented in Table 4. From the results, it
is evident that the cadmium- and
chromate-free coating scheme stud-
ied exhibits better anticorrosive
properties on 15CDV6 steel sub-
strate when compared to the other
two cadmium- and chromate-based
schemes studied. (The photographs
of the test panels after exposure to
salt fog tests are shown in Figure 5.)
From the photographs, it is evident
that the cadmium and chromate
scheme is less affected at the time of
occurrence of first failure when com-
pared to the other two cadmium-
and chromate-based schemes taken
up for experimental study.
3.3 Adhesion and abrasion resistance
measurements. The results of adhe-
sion and abrasion resistance meas-
urements carried out on different
coating schemes are provided in
Table 5. From the results of adhe-
sion measurements, it is evident
that cadmium- and chromate-free
coating scheme possesses compara-
ble adhesive strength to that of the
chromate- and cadmium-based
schemes studied. The abrasion
resistance of the coating schemes is
also comparable and, hence, the
cadmium- and chromate-free
scheme studied shows comparable
mechanical properties to that of
cadmium- and chromate- based
schemes. It is also seen that trivalent
chromate based passivation process
used in the present study for
improving the adhesion of the sub-
sequent paint layer serves the pur-
pose when compared to the hexava-
20 I metalfinishing I ApriVMay 2011
lent chromate based passivation
carried out on cadmium plating.
From the electrochemical imped-
ance spectroscopic and salt fog expo-
sure studies, it is evident that zinc
nickel alloy plating, trivalent chromi-
um-based passivation and an anti-
corrosive primer based on polyani-
line phosphate provide superior cor-
rosion resistance when compared to
the cadmium- and chromate-based
schemes selected for study in compli-
ance with military and aerospace
specifications.
Due to the basic nature of the
amine hardener used to cure the
polyaniline phosphate-based primer,
deprotonation of polyaniline phos-
phate salt is possible, thus convert-
ing the salt form to emeraldine base
form of polyaniline, liberating the
phosphate species. This emeraldine
base form of polyaniline plays an
active role in corrosion protection
due to the ability of emeraldine base
species to intercept electrons from
the corrosive ions at the metal sur-
face and to transport these electrons
outside the primer surface [28].
This conductive property of
polyaniline species was demonstrat-
ed in as little concentration of
0.6-0.9% polyaniline in the organic
matrix[29]. To enable this protective
role by polyaniline species, some
electrochemical activity at the metal
polymer interface needs to start. As
soon as water and ions of corrosive
species diffuse through the pores
and defects present in the coating
and reach the metal surface, the
emeraldine base form of polyaniline
protects the substrate by the mecha-
nism explained previously. This
mechanism is also supported by an
initial decrease in low frequency
impedance values due to the trans-
port of corrosive ions into paint
film and relatively higher imped-
ance values after 120 days of expo-
sure to corrosive electrolyte when
compared to the cadmium- and
chromate-based scheme.
From the results of accelerated cor-
rosion tests and evaluation of
mechanical properties-such as
adhesion and abrasion resistance of
the coating schemes-it is evident
that cadmium- and chromate-free
coating scheme exhibits superior
performance when compared to the
widely used cadmium- and chro-
mate-based schemes.
CONCLUSIONS
Efficient and eco-friendly alterna-
tives to cadmium- and chromate-
based coatings is a major require-
ment in the area of protective coat-
ings for aerospace and defense
applications. In this paper, experi-
mental work to evaluate and find
an efficient alternative to cadmi-
um- and chromate-based coating
schemes used to comply with aero-
space and military specifications
was carried out.
The proposed cadmium- and chro-
mate-free scheme comprised of zinc
nickel alloy plating, trivalent chrorni-
urn-based passivation and polyani-
line phosphate-based primer offers
superior corrosion protection to the
15CDV6 steel substrate when com-
pared to the cadmium- and chro-
mate-based schemes taken up for
study. The mechanical properties of
the cadmium- and chromate-free
schemes are also comparable to the
cadmium- and chromate-based
counterparts. These promlslllg
results show the possibility of
replacement of the widely used cad-
mium and chromate based schemes
for corrosion protection of 15CDV6
steel with an eco-friendly scheme
comprised of zinc nickel alloy plat-
ing, trivalent chromium based passi-
vation and polyaniline phosphate
based primer.
ACKNOWLEDGMENTS
The authors would like to express
their sincere gratitude to Shri. P.
Venugopalan, director, DRDL,
Hyderabad for his constant support
to carry out this work. The authors
also thank Shri. N. Viswanathan,
Scientist G (retd), Shri. B.
Madhusudana rao, Scientist F (retd)
of DRDL, Hyderabad for their
encouragement to initiate work III
the area of ceo-friendly coatings.
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www.organicfinishing.com
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