G. Parida, D. Chaira, A. Basu* Department of Metallurgical and - - PowerPoint PPT Presentation

Synthesis and Characterization of Nano-TiO2 Dispersed Composite Coating by Electro-co-deposition

• G. Parida, D. Chaira, A. Basu*

Department of Metallurgical and Materials Engineering National Institute of Technology, Rourkela Odisha, India

www.nitrkl.ac.in

• Electro-co-deposition and Ni coating
• Plane of work
• Results (effect of texture and particle on properties)
• Results (effect of texture and particle on properties)
• Summary

Contact *: basua@nitrkl.ac.in, anindya.basu@gmail.com

International Conference on Materials for advanced Technologies (ICMAT 2011) 26 June – 1 July 2011, Suntec, Singapore

Electro-co-deposition

Mechanism for solution deposition Mechanism for ceramic powder (electro phoretic) deposition

Parameters

deposition

Additives pH of the solution Electrolyte temperature Current density Electrolyte agitation l Metal ion concentration

Dispersed particle Aggregated particle

Ni coating Ni coating

Electro deposition

Corrosion resistance Electrical conductivity

Low cost Low temperature requirement

Electro‐deposition

Nickel y Thermal conductivity Magnetostriction property Physical appearance

p q Low energy requirement Capability to handle complex geometry

Physical appearance

Simple scale‐up with easily maintained equipment Good chemical stability

Electro co deposition

Improve mechanical properties Electro-co-deposition Particle and grain size

control pH Wear resistance Protection against high temp Corrosion and oxidation Ceramic particles pH Organic surfactant Agitation Corrosion and oxidation resistance Hardness particles

Plan o Plan of Wor Work f k f k

Ultrafine TiO2 dispersed Ni coating on the mild steel substrate using Electro-co-deposition method.

Electro deposition for nano‐dispersed coating

g p

Characterization Microstructure

(SEM, FESEM,AFM)

Chemical Analysis

(EDS)

Mechanical

(Hardness, wear)

Correlation with process parameter

Effect of surfactant and texture study

Deposition Parameters Deposition Parameters

Electrolyte (Watt’s bath) Nickel sulphate (NiSO4.6H2O): 350 g/l Nickel chloride (NiCl 6H O): 45 g/l (Watt s bath) Nickel chloride (NiCl2.6H2O): 45 g/l Boric acid (H3BO4): 37 g/l Wetting agent Sodium dodecyl sulphate: 0.2 g/l Surfactant Hexadecylpyridinium bromide: 0, 0.1, 0.3 g/l Dispersion Titania (TiO2): 5, 10, 15 g/l pH 4 pH 4 Temperature (oC) 60 Current density 5 A/dm2 Plating time 30 minutes Potential Flat DC

Results

TiO2 Particle Characterization

Particle size IEP XRD TEM

XRD and Texture study (of Ni)

/ I I

Coating/sample Grain size Texture coefficient

% 100 ) / ( /

) ( ) ( ) ( ) ( ) (

× = ∑

hkl hkl hkl hkl hkl

I I I I TC

(nm) (111) (200) (220) (311) Ni, no TiO2 and surfactant 31 0.18 0.25 0.08 0.50 5 g TiO no 5 g TiO2, no surfactant 30 0.17 0.10 0.63 0.10 10 g TiO2, no surfactant 20 0.21 0.11 0.54 0.15 15 g TiO2, no 24 0 14 0 07 0 71 0 07

Deposition without surfactant

nlarged

surfactant 24 0.14 0.07 0.71 0.07 5 g TiO2, 0.1 g/l surfactant 30 0.29 0.33 0.09 0.29 10 g TiO2, 0.1 g/l surfactant 40 0.29 0.32 0.08 0.30

En

su ac a 15 g TiO2, 0.1 g/l surfactant 33 0.15 0.70 0.03 0.12 5 g TiO2, 0.3 g/l surfactant 35 0.22 0.08 0.56 0.13 10 g TiO 0 3 g/l 10 g TiO2, 0.3 g/l surfactant 28 0.24 0.10 0.56 0.10 15 g TiO2, 0.3 g/l surfactant 33 0.15 0.06 0.70 0.09

EDS study

10 g/l TiO2 without surfactant Particle deposition rate

SEM Micrograph

5 g/l TiO2 without surfactant 15 g/l TiO2 without surfactant

2

Parida et al., Surf. Coat. Technol., 205 (2011), 4871

AFM Study

5 g/l TiO2 without surfactant 10 g/l TiO2 without surfactant

Microhardness and Wear Study

Microhardness Wear with varying TiO2 % Wear with varying surfactant %

SEM Micrograph of Wear Track MAGNIFIED

Pure Nickel 15 g/l TiO2 without surfactant

Summary

Orientation of nickel in composite coating hard [110] in zero or 0.3 g/l surfactant whereas it is softer ([100] & [211]) in 0.1 g/l surfactant. TiO2 co‐deposition rate increases more in zero or 0.3 g/l surfactant compared to 0.1 g/l surfactant. With increase in TiO2 surface roughness increases marginally. Due to soft orientation and less powder loading hardness increase is less in zero or 0.3 g/l surfactant compared to 0.1 g/l surfactant. Maximum hardness reported with 0.3 g/l surfactant and 15 g/l TiO2. The wear test results show similar trend as microhardness due to combined effect of The wear test results show similar trend as microhardness due to combined effect of nickel orientation and TiO2 amount in the coating. Wear mechanism primarily adhesive in nature and the worn out particle shifts it nominally to abrasive regime.

Acknowledgment A k g

Department of Science and Technology (DST), India [G t N SR/FTP/ETA/A 10/08] [Grant No. SR/FTP/ETA/A-10/08]

Thank You! Thank You!