Investigation of thick film carbon electrode surface treatment techniques

SUPERVISOR: Mr. ANANDAN SHANMUGAM

DEPARTMENT OF ELECTRICAL AND ELECTRONIC ENGINEERING

By Tamil selvan Ramadoss

WHAT IS A CAPACITOR? capacitor is a device used for storing charges and energy in its simplest form. A capacitor consists of two conducting surfaces separated by an insulating material ( Dielectric). WHAT IS A BATTERY Batteries store electricity using chemical reactions happening between an electrolyte , a positive electrode, and a negative electrode WHAT ARE SUPERCAPACITORS Supercapacitors store more energy than ordinary capacitors by creating a double layer of separated charges between two plates made from porous, typically carbon-based materials. The plates create the double-layer by polarizing the electrolyte in between them

 The term electrochemical double layer capacitor is most commonly used for carbon based double layer capacitors because of its high capacitance value. It generally denotes the supercapacitor having non- faradaic reactions at both electrodes

Activated carbon Black carbon Binder (PTFE) Aluminium foil

Equivalent series resistance High capacitance

 Different surface treatment techniques on aluminium and investigate the adhesion property of carbon on aluminium surface

Etch the aluminium foil based on alkali and acid etchant Alkali ( NaOH) Acid ( HCl and H2SO4 )

The main aim of this research work is to keep the resistance between the carbon and aluminium metal sheet as low as possible, this in effect will help to ESR (Equivalent Series Resistance) of the electrode minimum. In order to meet these aim the following objectives to be carried out. Undertake the study of different surface treatment techniques of the aluminium and investigate the carbon adhesion property to the same Optimize the aluminium surface in terms etching. Prepare the carbon- carbon electrodes and assemble the supercapacitor cells Run the Cyclic voltammetry tests to determine specific capacitance for the fabricated supercapacitor cell. Measure the internal resistance between carbon and metal by means of Impedance spectroscopy.

 Alkali etching Acid etching

Cyclic voltammetry Impedance spectroscopy

1) refers to an ideal capacitor, in parallelogram structure where charging and discharging is perfect. 2) refers to capacitor with resistivity 3) refers to capacitor with carbon material and 4) refers to influence of redox reactions, where U is voltage delay Ic is capacitance current

Comparison of ideal and real cyclic voltammograms

Complex impedance plot of conventional capacitor and EDLC

 Alkaline Etching using NaOH (0.1M,0.2M,0.3M) at 55oC Acid Etching using H2SO4 (0.1M,0.2M,0.3M) at room temperature Acid Etching using H2SO4 (0.1M,0.2M,0.3M) with constant temperature(55oC) and increased time Acid Etching using HCl (0.1M,0.2M,0.3M) with constant temperature(55oC) and increased time Acid as a surface cleaner and alkali as an etchant 0.1M of HCl at 15min+0.2M of NaOH at 5min 0.1M of HCl at 15min+0.3M of NaOH at 4min 0.1M of at H2SO4 15min+0.2M of NaOH at 5min 0.1M of at H2SO4 15min+0.3M of NaOH at 4min

0.1M of at H2SO4 15min+0.3M of NaOH at 2min

0.1M of at H2SO4 15min+0.3M of NaOH at 3min

Optimised etching profile obtained from following etching techniques 0.2 M conc of NaOH at 15min 0.3 M conc of NaOH at 10min 0.1M of at H2SO4 15min+0.3M of NaOH at 2min

0.1Mconc of NaOH (55oC) )

5min

10min

15min

0.2Mconc of NaOH (55oC)

5min

10min

15min

0.3Mconc of NaOH (55oC)

5min

10min

15min

Variation in orientation of pit size for alkali etching

 Acid Etching using H2SO4 at room temperature have not produced better etching profile but yields clean surface Acid etching using H2SO4 (55oC)

5min

10min

15min

Acid etching using HCl (55oC)

5min

10min

15min

0.1M of at H2SO415min+0.2M of NaOH at 5min

0.1M of at H2SO4 15min+0.2M of NaOH at 2min

Cyclic voltammogram test for 0.2 M of NaOH at 15min

Specific capacitance (Cspe) = 0.4/0.0136 =29.4 F/g.

0.2M of NaOH at 15min was not subjected to impedance testing due to the fabrication error

Cyclic voltammogram test for 0.3 M of NaOH at 10min

Specific capacitance (Cspe) = 0.4/0.0136 =38.94 F/g.

Cyclic voltammogram test for 0.1M of at H2SO4 15min+0.2M of NaOH at 2min

The specific capacitance (Cspe) = 0.5/0.01225= 40.81F/g

Impedance versus frequency

Impedance versus resistance

Impedance versus frequency

Impedance versus resistance

 Metal oxides and Conducting polymers are being in growth steadily as an electrode material in future. Unlike carbon, conducting polymers utilize the entire bulk of film to store charge and therefore it is possible to achieve high capacitance. The charge storage mechanism is quite dissimilar to carbon based material. The charging takes place when the ions transferred to back bone of conducting polymer during Oxidation similarly the discharging takes place when ions released to solution from the backbone during Reduction. On the other hand Metal oxides have been extensively used as an electrode material due high capacitance and low internal resistance. These material drawn attentions because of their fast charging and discharging profile and can be operate in both organic and aqueous type electrolyte. These materials remarkably yield 720 to 760 F g1 of specific capacitance. Metal oxides as an electrode is still under researching, since they are expensive and slight degradation during charging and discharging cycles.