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IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
1234567890‘’“”

Performance Evaluation of Nano Additives and Surfactants

on the properties of Electroless Nickel Phosphorous Coating
on Aluminium – Magnesium Alloy

1
Shetha Daniel, 2 Manik C Majumder, 3 Sudhir CV
1
Lecturer, Caledonian College of Engineering, Oman.
2
Professor, NIT Durgapur, West Bengal, India
3
Professor, Caledonian College of Engineering, Oman.

* Corresponding Author: shethamanu80@gmail.com

Abstract: Corrosion occurs as a result of the interaction of a metal with the environment. The
extent of corrosion depends on the type of the metal and the surrounding environment. This
paper focuses on the investigation of the corrosion problem in Aluminum–Magnesium alloys
and experimentally develops an Electroless Nickel - Phosphorouscoating with different nano
additives and surfactants. This paper investigates the different types of Electroless Nickel -
Phosphorouscoatings done to reduce corrosion in Al-Mg alloys. Two types of nano particles
such as nano Al2O3 and nanoZnO with two types of surfactants such as SDS and CTAB were
used in this investigation. Different corrosion evaluation tests such as atmospheric exposure
test, and wet corrosion test were carried out on the coated samples. Coated samples were
characterized with help of Scanning Electron Microscope and Energy Dispersive X-ray
Spectrometry. Mechanical evaluation tests such as surface roughness and hardness were
measured on the coated samples. Comparison was done between the different EN-P coatings to
optimize the concentration ofnano additives and surfactants.
Key word: corrosion, coating, AL–Mg alloys, Aluminum oxide (Al2O3). Zinc oxide (ZnO),
nickel-phosphorus(Ni-P), surfactants.

1. Introduction
1.1 Motivation
Corrosion of Al-Mg alloys one of the major problems in automobile industry. Several coatings were
developed and tested previously to prevent corrosion. However, Nickel coatings have not been tested
in the Omani environment. Different surfactants in the EN-P coating along with nano additives is used
tooptimise the best coating by changing the concentration of surfactants in EN-P coating[5].

1.2Problem Definition
During the summer season in Oman high ambient temperature contributes to corrosion of Al-Mg
alloys and is one of the major problems facing in industrialequipment’s. The effect of corrosion
ranges from a simple appearance of crack to complete damage of Al-Mg alloys leading to several
million riyals revenue loss [6]. Though several types of coatings are used to prevent corrosion,
Electroless Ni-P is a unique surface protective coating which is not tried in Oman environment.

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distribution
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Published under licence by IOP Publishing Ltd 1
IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
1234567890‘’“”

Electroless Ni-P is a chemical metal deposition process. In this process Nickel is deposited on the
substrate by means of an auto catalytic reduction reaction [7].

2. Literature Review
Corrosion is a chemical reaction between metal and environment. Al-Mg alloy is the most chemically
active of all the metals used in aircraft construction, marine constructions and many part in
automobiles and is the most difficult to protect. Corrosion can be concentrated to a certain area or wide
spread almost uniformly corroding the surface. Due to this problem the life time of the alloy is reduced
and resulted in high replacement cost every year [1]. To overcome the existing problem of corrosion,
an EN-P coating with different Nano additive and surfactant is developed. Electroless Nickel
Phosphorus coating is an auto catalytic reaction used to deposit a coating of nickel on the substrate.
This plating technique prevents corrosion and develops uniform coating thickness [2].The EN plating
of metallic nickel from aqueous solution in presence of hypophosphate was first noted by Wurtz in
1844 [3].In this paper a new technique of protection coating is done in Electroless Nickel Phosphorus
coating (EN –P) with nano Al2O3 and nano ZnO with two types of surfactants such as SDS and CTAB.
In this method coating is done uniformly with uniform thickness to the entire surface [4, 5].

3. Experimental Set up
3.1 Sample preparation:
A total number of 48 samplesof size 25mm x 25mm were taken for coating. Samples were polished
with wet 400,600 and 2000 grit SiC paper. The surface of each sample was cleaned with distilled
water, thencleaned with acetone followed by a methanol wash and dipping into acid Pickling
(1%HF+3%HNO3 by volume) [6].Then take the initialweight of each sample by using digital
analytical balance. The size of nano additives used for coating has a particle size of 50nm.
•Samples were coated with the following different types of coating:

 EN-P
 EN-P+nanoAL2O3
 EN-P+ nanoAL2O3 +SDS1%
 EN-P +nanoAL2O3+CTAB1%
 EN-P+nano AL2O3+SDS1.5%
 ENP+nanoAL2O3+CTAB1.5%
 EN-P+nanoZNO
 EN-P+nanoZNO+SDS1%
 EN-P+nanoZNO+CTAB1%
 EN-P+nanoZNO +SDS1.5%
 ENP+nanoZNO+CTAB1.5%
3.2. Electroless Nickel Coating Bath Composition
The coating bath consists of the chemical composition as shown in the table.
Table 1. Chemical composition of EN-P bath.
Materials & Chemicals Amount
Nickel Chloride 6g*12=24g+200ml Dw
Sodium hypophosphite 8g*4=32g+200ml Dw
Sodium Tri citrate 5g*4=20g+200ml Dw
Ammonium Chloride 10g*4=40g+200ml Dw
Acetone 200ml
Methanol 200ml

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IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
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Sulfuric Acid 200ml

Ammonia Solution 200ml
Nano (Al2O3) <50 nm 0.5 g
Nano (ZnO) <50 nm 0.5 g
CetylTrimethyl Ammonium Bromide (CTAB) 0.3+10ml Dw
Sodium Dodecul Sulfate (SDS 0.24+10ml Dw

The various process parameters such as pH, concentration of nano additives and surfactants were
varied. The pH level is maintained by the addition of ammonia. The pH value maintained is 9-10, at a
temperature around 850C.The coating process is kept for 1 hour in 200 ml of coating bath [6].

3.3. Sample preparation for Atmospheric Exposure Test

Samples were exposed to the atmospheric conditions for 60 days. The atmospheric test is carried out in
the climatic condition of Oman with an average temperature of 400C, average relative humidity of 60
to 65%.

4. Result and Discussion

4.1 Wet and dry corrosion Test
The basic idea of the test was to dip the samples in filtered sea water and dry it in atmospheric air [8].
Filtered sea water had a pH value of 7.8.

4.1.1Weight loss Test

In this weight loss technique the samples were coated with different types of chemicals. The initial
weight before exposure to test was taken. After 8 weeks the samples were taken out and cleaned and
final weight was taken. The difference gives the weight loss. The weight loss for different coated
samples are recorded in figure 1.

Figure 1. Weight loss in samples coating using dry/wet test.

4.1.2 Corrosion Rate
The rate can also be calculated as follows: Crate=87.6*(W/ADT) where:
W = total weight lost
T = time taken for the loss of metal
A = the surface area of the exposed metal
D= the metal density in g/cm³
Calculation of area of the Sample:
Samplesize =25*25=625 mm Thickness=0.4mm
Area= (25*25)*2+ (25*0.4)*4=1290 mm²=12.9 cm²

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IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
1234567890‘’“”

Figure 2. Corrosion rate by wet/dry test

From figure 2 shows that sample without coating has highest value of corrosion rate due to its less
corrosion resistance However EN-P in present of nanoAL2O3and nanoZnO and concentration of
surfactant (SDS1.5% and CTAB1.5%) have lowest corrosion rate because of high corrosion
resistance.

4.2 Atmospheric Exposure Test

Atmospheric test was conducted for a period of 60 days with ambient conditions as stated above.

4.2.1Weight loss Test

Figure 3.Weight loss in samples coating usingatmospheric test.

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IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
1234567890‘’“”

4.2.2 Corrosion Rate

Figure 4. Corrosion rate by atmospheric exposure test.

The above figure shows the results in terms of corrosion rate for the atmospheric test. The sample without
coating has highest corrosion rate with a rate of1.54 mm/y. The best coating was EN-P coated with Nano-
Al2O3, and concentration of surfactant (SDS 1.5% and CTAB1.5%) because corrosion rate was between
(0.2 mm/y-0.26 mm/y) for atmosphericexposure test.

4.3 Mechanical Properties

4.3.1 Rockwell hardness Test

Figure 5. Hardness test.

5
IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
1234567890‘’“”

The hardness test was used to measure the hardness of the Al-Mg alloy for different coating, where the
sample without coated has lowest value of hardness when compared with others samples [7]. The
samples coated with EN-P and nano-additives (Al203&ZnO) have approximately similar value. The
samples coated with EN-P + nano additives and surfactant have good result in hardness [7].The best
result was for EN-P coated with Nano-additive(Al2O3, ZnO),and concentration of surfactant (SDS
1.5%,CTAB1.5%) because it is has the highest value of hardness when compared with others
samples.

4.3.2 Coating Thickness Test

For further evaluation the samples coating thickness were measured using thickness gauge.

Figure 6. Coating thickness.

As we see in the above figure, the samples coated with EN-P +nano-additive (Al2O3, ZnO)and
concentration of surfactant(SDS 1.5%,CTAB1.5%)have highest coating thickness when compared
with another samples .

4.4Characterization Testing
Surface morphology and composition of the EN P coatings were analyzed by scanning electron
microscope(SEM) and X-ray diffraction (XRD) as shown below [8].

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IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
1234567890‘’“”

Figure 8. Characterization test in sample (EN-

Figure 7. Characterization test in sample (EN- P+nanoAl2O3+CTAB 1%) coating.
P+nanoAl2O3+SDS 1%) coating.

Figure 9. Characterization test in sample (EN- Figure 10. Characterization test in sample (EN-
P+nanoAl2O3+SDS 1.5%) coating. P+nanoAl2O3+CTAB 1.5%) coating

Figure 11. Characterization test in sample (EN-P+ Figure 12. Characterization test in sample (EN-
nanoZnO+ SDS 1%) coating P+ nanoZnO + CTAB 1%) coating.

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IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
1234567890‘’“”

Figure 14. Characterization test in sample (EN-

Figure 13. Characterization test in sample (EN-P+ +nanoZnO +CTAB 1.5%) coating
nanoZnO +SDS 1.5%) coating

Moreover the surface area of the sample without any coating can be completely corroded [12].

5. Conclusion
Corrosion is a natural phenomenon and needs to be handled with all techniques to protect the Al-Mg
alloys .The degradation of a materials properties as a result of it is interaction with the operating
environment, plays a critical role in determining the life –cycle performance, safety and cost [9].
Investigations done to study the behavior of the corrosion in different conditions was promising as it
met the project objectives. Corrosion cannot be terminated from the metals, but it can be isolated by
applying good coating [10]. Corrosion rate for different coating is tested by conducting atmospheric
exposure test and dry/wet test and results areconcluded in terms of corrosion rate. Characterization
tests like SEM and XRD was also done.
The purpose of this paper is to provide a study about corrosion analysis of different coating on Al-Mg
alloy. The metal coatings and their thickness plays a vital roleagainst corrosion [11]. From the various
corrosion tests it is concluded that, EN-P in presence of nanoAL2O3and nanoZnO and concentration of
surfactant (SDS1.5% and CTAB1.5%) have lowest corrosion rate because of high corrosion
resistance.However, when surfactant like (SDS & CTAB) where added with less concentration to the
EN-P bath, less number of cracks were observed on the deposits. The main reason for improved
corrosion resistance in presence of surfactant is due to structural change from crystalline to amorphous
nature.
At higher concentration of surfactant the coated samples exhibit more amorphous fraction than
crystalline. This improved the corrosion resistance.

6. Recommendation and Future Work

The recommendation is to use surfactants like (SDS & CTAB) but with high concentration (1.5%, 2%,
2.5% and 3%) and it can be observed that there are no cracks formed on the deposits.

References
[1] Amer J 2014 Influence of Multiple Electroless Nickel Coatings on Beech Wood: Preparation and
CharacterizationComposite Interfaces21(3)191-201.
[2] Mainier FB, Fonseca MP, Tavares SS andPardal J M2013 Quality of Electroless Ni-P (Nickel-
Phosphorus) Coatings Applied in Oil Production Equipment with Salinity Journal of Materials
Science and Chemical Engineering1(6).

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IConMMEE 2018 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 376 (2018) 012048 doi:10.1088/1757-899X/376/1/012048
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[3] Riddle YW and McComas C E 2005 Advances in Electroless Nickel-Boron Coatings:

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