dr mohammad sakhawat hussain - institute of …materialsfinishing.org/attach/17. direct nano...
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Dr Mohammad Sakhawat Hussain
PhD (Aston) FIMF FIMMM CEng
Department of Materials Engineering Faculty of Mechanical Engineering Universiti Teknologi Malaysia
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Direct nano-crystalline Ni plating on titanium surfaces
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OUTLINE PRESENTATION
• An innovative process for depositing Ni
directly on Ti surfaces without the need to
pre-treat the substrates with acid/s and pre-
plate with an intermediate metallic layer
• As deposited Ni is nanocrystalline
• Nanomechanical test results to evaluate the
mechanical properties of the as plated
Ti/TiO2/Ni
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Direct plating on Ti
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High speed electroplating, which I have
used for the first time to plate nickel on
aluminium, titanium and stainless steel
without any pretreatment process.
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In order to plate nickel on titanium, oxide layers must be
removed first by acid etching and plated with
displacement reaction.
The function of these immersion coatings is the
replacement of the natural oxide always present on Ti
irrespective of the cleaning process, with an oxide free
metal on which adherent metallic coatings can be
deposited.
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D.C Power Supply
(Rectifier)
+
_
Ni Anode
Cathode Flow
Meter
Filter
Magnetic Pump Ni solution
Control unit Temperature composition
A Schematic diagram of the plating equipment designed for depositing Ni directly on titanium.
Out In
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Low Speed solution Movement
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High Speed solution Movement
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Ti base metal
Oxide layer
Ni Deposit
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Schematic Diagram: Aluminium has a porous and a fine compact oxide layer before pure Al can be exposed (the thickness of these oxide layers is less than 10 nanometer).
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Aluminium has a porous and a fine compact oxide layer before pure Al can be exposed (TEM images showing oxide structures enlarged after anodizing )
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TEM images showing oxide structure
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HIGH SPEED ELECTROPLATING PARAMETERS
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Research Methodology
SOLUTION PREPARATION
Type Constituents Typical Concentration
g/l pH
Watt’s Solution NiSO4.7H2O
NiCl2.6H2O
H3BO3
300 45 38
3.5 – 5.5
Nickel Sulphate Solution
NiCl2.6H2O
H3BO3
300 38
2.5
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MORPHOLOGY ANALYSIS
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Research Methodology
• Specimen were cut by cross
section
• Specimen were mounted
using cold mounting
• Sample were grinding and
polished with different
abrasive paper.
• The thickness of nickel layer
were measured using SEM to
determined the effect of
different solution, current
density and temperature
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Mechanism of electroplating and structure of electroplated coatings.
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SEM image – surface view of the Ni deposits showing the mechanism nucleation and growth of nano-crystalline Ni layer
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ADHESION TESTING
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Research Methodology
• Adhesion testing is required to quantify the
strength of the bond between the nickel layer
and aluminium substrate.
• Adhesion testing according to ASTM D6677
and ASTM D3359
• ASTM D6677 - Adhesion testing by knife
• ASTM D3359 - Adhesion testing by tape test
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ADHESION ANALYSIS
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Results & Discussion
• The sample of nickel layer which electroplated
on high current density were easily to peeled off
compared to sample which electroplated on low
current density.
I = 1 A at 55 oC I = 1 A at 65 oC
Figure 4.: Nickel plating samples after adhesion testing.
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• Hardness – resistance to penetration of a hard indenter • Load is applied • Plastic zone forms • Hardness determined from optical measurements
Background: hardness testing
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Micro- vs nanoindentation
• Force, displacement and time are recorded throughout the test • Optical inspection of hardness impression is not required • No other technique provides quantitative information on both elastic and plastic
properties of thin films and small volumes • Ideal for thin films, coatings, nanocomposites, biomaterials…
Nanoindentation
• Force is applied and optical inspection of hardness impression necessary • No information on elastic modulus • Results less useful for wear prediction • Not suitable for thin films or coatings, or highly localised measurements…
Hardness and micro-hardness testing
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Fig.5. Nanomechanical test results – carried out on plated Al/(Al2O3)/Ni layers. The measured indentation modulus (Er) and hardness shows significant differences between the Ni plated layer and the aluminium base, however, the interface i.e. the oxide layer has very different measured values compared to Ni and Al.
Ni
Al
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HRTEM Image showing 3 distinct layers i.e. Al, the oxide layer and the Ni coating. There is no sign of any porous Al layer.
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Improved equipment for direct electroplating by using high speed electroplating process
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Product of new equipment
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CONCLUSIONS • It has been possible to plate nickel directly on titanium without any pre-
treatment process, using a basic power supply and without any additives
• As plated the Ni is nanocrystalline
• Nanomechanical tests show Ni, aluminium oxide and Al all have different modulus and Hv, however, the oxide layer is much softer than expected and has shown inconsistent properties which indicates that the natural oxide was responsible for this inconsistencies.
• By increasing the temperature, the weight and thickness of the layer also increase.
• Nickel sulphate solution gives higher rate of deposition compare to the watt’s solution.
• Adhesion between nickel and aluminium became low at current above 1 A. Nickel layer is easily to peel off.
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Acknowledgement This work has been sponsored by Research
Management Centre (RMC), Universiti Teknologi
Malaysia.
Industrial Partners:
• Hysitrion Inc. USA
• Micro Materials Ltd, UK
• MEng Research students (Nanomaterials Synthesis Group),
Dept of Materials Engineering, UTM
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THANK YOU
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