Fabrication of Polyaniline

Nanofiber via Electrospinning

for the Development of
Carbon Monoxide Sensor
A TERMINAL REPORT

Office of the Vice Chancellor for Research and Extension Building

February 23, 2011, 8:30AM

forging the foundations for the future

People

Project leader Marvin U. Herrera

Materials Physics Laboratory, Physics Division
Institute of Mathematical Sciences and Physics
on study leave for PhD at Kyoto University

Proponent IMSP IC
Prof. Emmanuel A. Florido Dr. Ernesto J. del Rosario, Jr.
Ms. Melody Joy Gamboa Mr. Jesse Cervantes
Ms. Diane Denise Tabernilla
Mr. Francis Emralino
Mr. John Cerry dela Rosa
Funding Details

Implementing Unit Institute of Mathematical Sciences and Physics

Cooperating Unit Institute of Chemistry

Funding Source PCASTRD Fellowship Grant

Project Duration February 1, 2009 to January 31, 2010

Total Budget PhP 500,000.00

 WALKTHROUGH
Polyaniline Nanofiber via Electrospinning for the Development of Carbon Monoxide Sensor
A Terminal Report

PEOPLE/FUND PANI SYNTHESIS WB-type CHEMISTOR

Resistor 1 PANI fiber

Resistor 2 Resistor 3

power supply

ABSTRACT SPINNER eSPUN FIBERS STUDIES

A WheatstoneBridge-type
chemistor was fabricated to
measure the sensitivty of
electrospun PANI fiber.
Several electrospinning
parameters were varied to
produce fibers with nanometer
diameter. Fiber morphology
and composition were
analyzed as parameters were
adjusted.
Abstract
Development of a Wheatstone Bridge-type Chemistor
Characterization of electrospun fibers
Fabrication of electrospinning set-up

PANI synthesis
Abstract
PANI synthesis
Development of a Wheatstone Bridge-type Chemistor
Characterization of electrospun fibers

Fabrication of electrospinning set-up

syringe pump

syringe

needle (cathode)

aluminum foil (anode)

DC power supply
Abstract
Fabrication of electrospinning set-up
Characterization of electrospun fibers

Development of a Wheatstone Bridge-type Chemistor

Resistor 1 PANI fiber

Resistor 2 Resistor 3

power supply
Abstract
Fabrication of electrospinning set-up
Development of a Wheatstone Bridge-type Chemistor

Characterization of electrospun fibers

Pictures insert here

PANI synthesis
Polyaniline-emeraldine was synthesized following standard oxidative
polymerization by Stejskal (2005).

mixed while in ice bath

aniline HClO4

added dropwise
APS
stored under 4oC

polyaniline solution
washed
filtered
vacuum dried

PANI powder
The Spinner

Custom-built vertical electrospinning set-up

The Spinner

Syringe pump

The syringe pump controls the flow rate being

ejected from the needle.
INSERT UNIT
The Spinner

Syringe

Contained in the syringe was the solution of certain

concentration. Needle gauge was chosen so as to
produce the desired fiber diameter. The needle
was connected to the positive terminal of the
power supply.
The Spinner

Collector

The collector used in the study is a commercially

available aluminum foil. This allowed the
researchers flexibility in setting the area for
collection of electrospun fibers. It also gave ease in
extraction/harvesting of fibers. The aluminum foil
served as ground which was connected to the
negative terminal of the high power supply.
The Spinner

Collector holder

To vary the distance between electrodes (needle

tip and collector), the aluminum foil was fixed to an
adjustable holder. The holder could be translated
along the vertical position.
The Spinner

Power supply

A high voltage power supply (AHV 100) was utilized

in the study. The instrument is capable of providing
constant voltage supply from 0 to 100kV.
The Spinner

Stand

The stand supports the components described

earlier into place. It is made of wood to prevent
short circuiting and unwanted random deposition of
fibers onto it.
The Spinner

Cover

A plastic sheet for safety covers the entire anode-

cathode system. It contains off-course fibers from
flying off. This also prevented accidental contact
with the electrodes while running an experiment.
The Spinner and its parameters

Parameters varied

1. voltage
2. tip to collector distance
3. viscosity
Wheatstone Bridge-Type Chemistor

Resistor 1 PANI fiber

Resistor 2 Resistor 3

power supply

Schematic diagram of Wheatstone bridge-type chemiresistor

Wheatstone Bridge-Type Chemistor

Variable resistors

Three variable resistors (R1, R2, and R3) along with the
PANI fiber were connected to form a Wheatstone bridge.
The resistances were adjusted to balance the bridge.
Voltage across the bridge was measured using a high
precision nanovoltmeter (Keithley).

V
Wheatstone Bridge-Type Chemistor

Power supply

A constant dc voltage (Keithley 2410C) is supplied

across the bridge.
Wheatstone Bridge-Type Chemistor

Chemiresistor

Electrospun PAni fibers fixed on an interdigitated Interdigitated circuit

copper tracks.

fix
etche-spun
PCB pani
Wheatstone Bridge-Type Chemistor

Sensing

Electrospun PAni fibers fixed on an Gas chamber

interdigitated copper tracks.

to the bridge and voltmeter

valve

reaction chamber CO generator

Wheatstone Bridge-Type Chemistor

Sensing

Electrospun PAni fibers fixed on an Gas chamber

interdigitated copper tracks.
Voltage difference before and during
exposure to CO is measured across the to the bridge and voltmeter
bridge.
Sensitivity of the device is determined valve
following

S = |VCO-Vi| / Vi X 100%

VCO voltage across the bridge in the

presence of CO static gas chamber CO generator
Vi voltage before exposure
S sensitivity
Electrospun Fibers

Electrospinning

PAni powder were dissolved in NMP were mixed with different polymers (i.e. PVC, PVAc).

Binder Solvent Mixture (volume) Stirring time

PANI:binder

polyvinyl acetate none varied 20-30 minutes

polyvinyl chloride tetrahydrofuran 1:2 10 minutes
Elastomer none 1:1 ~
Electrospun Fibers

Morphology

PAni-PVC PAni-PVAc Pani-elastomer

Scanning electron microscope images of composite fibers.
Electrospun Fibers

Morphology: Electrode voltage and fiber diameter of Pani-elastomer

Electrospun Fibers

Morphology: Electrode distance, solution conductivity, and

fiber diameter of PAni-PVC
Electrospun Fibers

Morphology: Viscosity and fiber diameter of PAni-PVAc

Electrospun Fibers

Sensitivity: Solution conductivity and sensitivity

FIBER 1

high fiber gap suggests high barrier gap prevents conduction

FIBERS

Active material Pani-EB Pani-ES

CO sensitivity (%) 93.45 29.72
Standard deviation 8.10 1.31
|Stdev/Sensivity| (%) 8.67 4.40
Electrospun Fibers

Sensitivity: Solution conductivity and sensitivity

FIBER 1

CO CO CO CO CO CO CO CO
CO CO CO CO
CO CO CO CO CO CO CO
CO
CO
FIBERS

CO “connects” the fibers thus changing the bulk electric resistance

Active material Pani-EB Pani-ES

CO sensitivity (%) 93.45 29.72
Standard deviation 8.10 1.31
|Stdev/Sensivity| (%) 8.67 4.40
Electrospun Fibers

Sensitivity: Solution conductivity and sensitivity

FIBER 1

CO CO CO CO CO CO CO CO
CO CO CO CO
CO CO CO CO CO CO CO
CO
CO
FIBERS

Or, CO blocks oxidation sites in the PAni structure, thus, decreases

resistance

Active material Pani-EB Pani-ES

CO sensitivity (%) 93.45 29.72
Standard deviation 8.10 1.31
|Stdev/Sensivity| (%) 8.67 4.40
Electrospun Fibers

Sensitivity: Solution conductivity and sensitivity

FIBER 1

CO CO CO CO CO CO CO CO
CO CO CO CO
CO CO CO CO CO CO CO
CO
CO
FIBERS

Lastly, CO acts as dopant.

Active material Pani-EB Pani-ES

CO sensitivity (%) 93.45 29.72
Standard deviation 8.10 1.31
|Stdev/Sensivity| (%) 8.67 4.40
Summary

A custom-built electrospinning set-up was assembled. The set-up was

made such that electrospinning parameters like voltage and tip-to-
collector distabce could be varied.

A Wheatstone Bridge-type chemiresistor was successfully fabricated as

CO sensor.

Fiber diameter are as follows: PAni-PVAc, 100 nm; PAni-PVC, 200nm,

and PAni-elastomer, 250nm.

Fiber diameter grows exponentially with electrode voltade in Pani-

elastomer.
Summary

Decrease in fiber diameter as distance between electrodes was varied in

PAni-PVC. Smallest fiber diameter was observed at 16-cm tip-to-
collector distance.

Bead formation was observed in PAni-PVAc with low viscosity.

PAni-EB was observed to be more sensitive in detecting CO than

H2SO4-doped PAni.
Studies conducted

Student

Ms. Melody Joy Gamboa

Ms. Diane Denise Tabernilla
Mr. Francis Emralino
Mr. John Cerry dela Rosa
Mr. Jesse Cervantes
Mr. Nathaniel Carolina
Ms. Stephanie Tumampos
Acknowledgement

PCASTRD for the grant.

Dr. EJ del Rosario for allowing the students to work in his lab at the Institute of
Chemistry-UPLB.
Prof. AKG Tapia for continuing and supervising the work on heme assisted CO
sensing.