EFFECT OF PARTICLE

INCLUSION, ELECTROLYTE ADDITIVES ON

PLASMA ELECTROLYTIC OXIDATION
COATING FOR ENHANCING CORROSION
RESISTANCE OF AZ31 B-ALLOY

Group Members: Guided By:

Amareesh MM 31 Madhu Mohan
Anandhakrishnan V 32 Asst. Professor
Ananthu Krishnan C 33 Mechanical Departm
Aswani NK 50 ent
CONTENTS
1. ABSTRACT
2. NOVELTY
3. INTRODUCTION
4. PROPERIES OF Mg & Mg AZ31 B-ALLOY
5. PLASMA ELECTROLYTIC OXIDATION
6. EXPERIMENTATION AND ANALYSIS
7. OBJECTIVES
8. METHODOLOGY
9. RESULTS AND DISCUSSION
10. CONCLUSION
11. REFERENCES
ABSTRACT
Magnesium and its alloys, which are esteemed for their lightweight attributes,
offers a promising solutions in automotive and aerospace sectors. Despite their
advantages in machinability and recyclability, magnesium alloys encounter
challenges with corrosion susceptibility, particularly in harsh environments,
presenting durability concerns. This research explores about the impact of
incorporating particle inclusions and electrolyte additives on Plasma Electrolytic
Oxidation (PEO) coatings to enhance the mechanical properties of AZ31B alloy.
PEO treatment, known for its corrosion resistance and mechanical strength
enhancement, is investigated through systematic experimentation and analysis.
By modifying the structure and composition of coatings via particle inclusions and
electrolyte additives, this study aims to optimize PEO processes, offering insights
into enhancing the mechanical properties of AZ31B alloy for tailored applications.
NOVELTY AND IMPLEMENTATION SCOPE

• The PEO and electrolyte composition of glass particles on the same

specimen was not identified in any of the researched journals.

• As we are considering multiple factors simultaneously, the project

seeks to tailor PEO coatings specifically for AZ31B alloy, offering
customized solutions for corrosion protection.

• The findings from this project have the potential to significantly impact
various industries such as automotive and aerospace reliant on
magnesium alloy components by improving their durability and
longevity in corrosive environments.
INTRODUCTION
● Magnesium's remarkable lightweight properties make it ideal for applications
needing strength without added weight, such as transportation, electronics, and
construction.

● While magnesium offers benefits, it's prone to corrosion. Scientists are

exploring alloying with elements like manganese and aluminum to enhance
resistance, with zinc improving both corrosion prevention and weldability.

● Plasma Electrolytic Oxidation (PEO) coating enhances magnesium's durability

by forming a protective layer. Challenges arise with potential tiny holes in the
coating, prompting innovative solutions like using sodium silicate and glass
particles for effective sealing.

● Magnesium-zinc alloys show promise in maintaining pH balance in biological

environments, suggesting diverse potential applications.
PROPERTIES OF MAGNESIUM
● Magnesium is a lightweight and versatile metal.
● It has an atomic number of 12 and an atomic weight of 24.305.
● It belongs to the alkaline earth metals group on the periodic table.
● Magnesium exhibits properties such as high strength-to-weight ratio, excellent
machinability
● It is preferred in aerospace and automotive industries.
COMPOSITION OF Mg AZ31B ALLOYS
● Mg - 93% to 95% of the composition by weight.

● Al - Typically around 2.5% to 3.5% by weight.

● Zn - Comprising approximately 0.6% to 1.4% by weight.

● Mn - Present in small quantities, usually around 0.2% to 1.0% by weight.

 PLASMA ELECTROLYTIC OXIDATION (PEO)
● Plasma Electrolytic Oxidation (PEO) revolutionizes metal surface treatment by
creating thick, dense oxide coatings to enhance wear and corrosion resistance.

● PEO utilizes environment friendly electrolytes to produce ceramic coatings, ranging

from tens to hundreds of microns in thickness.

● The process involves electrochemical, plasma chemical, and thermal oxygen

diffusion reactions, resulting in three-layer coatings: porous outer layer, dense
middle layer, and thin but dense interior layer.

● PEO offers advantages over other coating techniques, such as simplicity, reduced
costs, enhanced durability, and the ability to create diverse colors and textures while
improving wear and corrosion resistance, thermal stability, and biocompatibility.
Layers of PEO coating Experimental set up of PEO

Mechanism of PEO
EXPERIMENTATION & ANALYSIS
● Contact Angle Testing : Contact angle testing measures how a liquid droplet
interacts with a surface, indicating its wetting properties. The angle formed
between the droplet and the surface reveals surface energy and chemistry. It's
crucial for assessing material characteristics in diverse fields like coatings,
biomaterials, and electronics.

● Corrosion Testing : Corrosion testing assesses how materials withstand

degradation from corrosion in different environments. It involves subjecting
materials to conditions like salt spray or acidic solutions to evaluate their
durability. Through this process, weaknesses are identified, guiding
improvements in material composition or protective coatings.
EXPERIMENTATION & ANALYSIS
● Taguchi Method : The Taguchi method is a statistical approach for optimizing
product or process design. It minimizes variability in manufacturing processes
to enhance product reliability and reduce costs. By systematically analyzing
factors using orthogonal arrays and signal-to-noise ratios, it helps determine
the optimal design parameters for robustness against variations, leading to
higher quality and more reliable products.
 OBJECTIVES

1. Surface conditioning of AZ31B

2. To produce a PEO coating over AZ31B magnesium alloy
3. To study the corrosion resistance and wear resistance
4. Optimizing PEO coating parameters based on the regression analysis
METHODOLOGY
● Procurement of the MgAZ31B Alloy

● Preparation of the specimens

● Preparation of the glass particles

● PEO coating of the samples

● Measurement of contact angle of the samples

● Corrosion test of the samples

PREPARATION OF SPECIMEN

● Polish the surface of samples using sandpapers of various grades (800, 1200,
2000).

● Eliminate oil and water content by treating the surface with ethanol.

● Material is sectioned into samples of dimension 2cm x 2cm each facilitated by

the use of a hacksaw.
 Surface polishing
AZ31B Substrate

Samples after cutting and cleaning After Cleaning and polishing

PREPARATION OF GLASS PARTICLES
● Silica glass crushed and turned into fine powder using ball milling machine
from NSSCE measurement lab.

● The crushed powder is passed through a 75 micrometer sieve.

● Size of the obtained glass particles is measured.

Ball milling for glass particle preparation Image of glass particles
PEO COATING
● Electrolyte Preparation: The mixture of Na3PO4.12H2O and KOH is used as the
electrolyte in this process.

● Immersion in the electrolyte: The well cleaned sample is immersed into the
electrolyte solution.

● Application of voltage: High DC voltage is applied between the electrodes.

● Oxide Formation: The high heat and pressure on the surface quikly make
magnesium turn into a thick, hole-filled layer of magnesium oxide and other stuff
like magnesium hydroxide.
PEO COATING
● Coating Growth: As the PEO process continues, the oxide layer grows
thicker and denser, gradually covering the entire surface of the magnesium
substrate.

● Cooling and Rinsing : The PEO-treated magnesium substrate is cooled and

rinsed to remove residual electrolyte.
PARAMETERS VARIED DURING PEO COATING
Samples Current density Particle wt% KOH
(A/CM^2) Concentration
1 1.5 0.0 2
2 1.5 2.5 3
3 1.5 5.0 4
4 2.0 0.0 3
5 2.0 2.5 4
6 2.0 5.0 2
7 2.5 0.0 4
8 2.5 2.5 2
9 2.5 5.0 3
MEASUREMENT OF CONTACT ANGLE
● To determine the contact angle on a PEO coated material, the software used
was imageJ software, and the experimental set up as follows:

schematic diagram of contact angle measurement

The mechanism of contact angle testing :
1. Preparation of Sample : The solid surface is prepared by cleaning and drying

2. Application of Liquid :A small droplet of deionized liquid of interest is carefully

dispensed onto the surface of the solid

3. Image Capture :A high-resolution camera or imaging system is used to capture images

of the droplet on the solid surface.

4. Image Analysis :The captured images are analyzed using image processing software.

5. Measurement : The contact angle is measured as the angle between the tangent to the
droplet at the contact line and the solid surface.
Flat surface Camera
CORROSION TEST

Schematic view of corrosion testing

 CORROSION TEST

● The three-electrode mechanism is a common setup in corrosion testing,

particularly in electrochemical techniques like Potentiodynamic
Polarization (PDP) testing. It consists of three main components:

● Working Electrode: This electrode is the material being tested for

corrosion. It is immersed in the electrolyte solution and subjected to
various electrochemical measurements to assess its corrosion behavior.

● Reference Electrode: The reference electrode provides a stable

reference potential against which the potential of the working electrode
CORROSION TEST
● Counter Electrode: Also known as the auxiliary electrode, this electrode
completes the electrical circuit in the corrosion testing setup. It provides the
necessary current flow between the working and reference electrodes during
electrochemical measurements.
RESULTS AND DISCUSSION

WATER CONTACT ANGLE

1. Examined water contact angles of Plasma Electrolytic Oxidation (PEO)

coated AZ31B magnesium alloy surfaces.
2. Contact angles consistently exceeded 90 degrees, typically ranging between
95 to 100 degrees.
3. Significantly hydrophobic surfaces indicated strong resistance to water.
4. Hydrophobic behaviour attributed to unique PEO coating characteristics:
- Roughened texture
- Low surface energy discouraging water adhesion.
Sample CA Left CA Right

Base Metal 72.54 72.36

1 97.200 91.564

2 92.644 91.739

3 98.660 97.712

4 84.607 86.342

5 74.669 72.079

6 91.042 90.568

7 100.169 96.194

8 90.782 83.617

9 85.811 92.368

Contact angles of samples

CORROSION TEST RESULTS
Sample I_CORR E(I=0) CORROSION Cathodic Anodic
mV RATE Beta (Mv) Beta (Mv)
(mpy)
BASE 824.097nA -1.811 0.29937 179.266 433.514
METAL
1 277.046pA -852.421 0.00010068 528.209 528.209
2 9.017nA -857.916 0.0032869 317.571 798.838
3 47.293nA -814.408 0.017181 366.079 925.799
4 42.87nA -786.435 0.015582 199.613 147.094
5 1.095μΑ -1.133V 0.39797 632.912 632.912
6 482.723nA -1.077V 0.17537 580.816 580.816
7 40.563pA -1.17V 1.4356e-05 590.644 590.644
8 1.592nA -957.906 0.00056223 746.403 746.403
9 420.657pA -762.377 0.00014887 1885 1130
PDP & NYQUIST CURVES
Base Metal Sample 1

Sample 2 Sample 3

Sample 4 Sample 5

Sample 6 Sample 7

Sample 8 Sample 9
Base Metal Sample 1

Sample 2 Sample 3

Sample 4 Sample 5

Sample 6 Sample 7

Sample 8 Sample 9
CORROSION RESULTS
● Sample 7:
- Minimum corrosion current: 40.563 pA
- Corrosion rate: 1.4356e-05 mpy
- Ranked as the best sample
● Sample 5:
- Maximum corrosion current: 1.095 µA
- Corrosion rate: 0.39797 mpy
- Ranked as the worst sample
OPTIMIZATION OF PARAMETERS VIA TAGUCHI METHOD

Response Table for Signal-to-Noise ratio SN ratio curve for corrosion

for Corrosion
● The SN curve indicates that the best parameter values are 2.5 A/cm2 for
current density, 0.0 for particle wt%,3 g/l for KOH concentration.

● According to figure given above , the maximum–minimum value for the

current density has the highest delta value. Hence, the current density is the
most significant parameter affecting the corrosion resistance (rank 1) whereas
the concentration of glass particles wt% has the less effect on comparing with
current density (rank 2)
CONCLUSION
● The water contact angle measurements consistently surpassed 90 degrees on the
surfaces of AZ31B magnesium alloy coated with Plasma Electrolytic Oxidation
(PEO). This observation is important as it signifies a pronounced hydrophobic
characteristic, essential for applications requiring water repellence.

● For enhancing the corrosion resistance of the samples, we employed the Taguchi
method. This approach allowed us to systematically vary key parameters, including
current density and concentration. By conducting a series of controlled experiments
and analyzing the results, we were able to identify the optimal combination of
parameters that significantly improves the corrosion resistance of the
magnesium alloy.
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