Response Surface Modeling of Electrospinning

Parameters on Titanium Oxide Nanofibers

Diameter: A Box-Behnken Design (BBD)

Zi Sheng Tang1, Nurmin Bolong1*, Ismail Saad1, Ahmad Fauzi Ismail2, Franklin Tiam Yang Lim1
1Faculty of Engineering, Universiti Malaysia Sabah, Jalan UMS, 88400 Kota Kinabalu, Sabah, Malaysia
2AMTEC, Universiti Teknologi Malaysia, 81310 Skudai, Johor, Malaysia
OUTLINE
Introduction

Materials and Methods

Results and Discussion

Conclusion
Introduction
Objective

The diameter of electrospun nanofibers are affected by

many parameters.
How process parameters affect the fibers diameter?
To study the influence of process factors (applied
voltage, flow rate and tip-to-collector distance) on the
electrospun TiO2 nanofibers diameter.
Response surface methodology was employed to
estimate the size of electrospun TiO2 nanofibers.
Introduction
Response Surface Methodology

RSM offers a quantitative basis for the relationships

between the electrospinning parameters and the fibers
diameter
Response surface methodology design approaches:
1. Full factorial design (FFD)
2. Central composite design (CCD)
3. Box-Behnken design (BBD)
 Materials and Methods
Solution Preparation and Electrospinning Process

Solvent:
Solvent: Ethanol (6 ml)
Ethanol (15 Electrospinning Setup:
ml) Precursor:
TTiP (2 ml) i. High voltage power supply.
Polymer:
PVP (1.29 g) Stabiliser: ii. Syringe set.
6.5 wt.% Acetic Acid iii. Rotating drum collector.
(4ml)
Materials and Methods
Fibers Characterization

Surface Morphology: Examined with scanning electron

microscope (SEM). All the samples were sputter-gold
coated prior to scanning.

Diameter: Measured using JMicroVision software

package.
Materials and Methods
Box-Behnken Experimental Design

TABLE 1: The variables and their levels for BBD.

System Parameters Coded Levels
-1 0 1
A: Applied Voltage (kV) 10 17.5 25
B: Flow Rate (ml/hr) 1 2 3
C: Distance (cm) 6 10 14
Materials and Methods
Box-Behnken Experimental Design
TABLE 2: BBD matrix and the experimental responses.
Experiment A:Voltage B:Flow C:Distance Response:
Run Rate Diameter
(kV) (ml/hr) (cm) (nm)
1 18 2 10 220
2 25 3 10 243
3 25 2 6 248
4 18 2 10 228
5 10 3 10 263
6 18 1 6 242
7 18 1 14 175
8 10 2 6 267
9 25 1 10 191
10 18 3 6 283
11 10 1 10 219
12 18 3 14 214
13 18 2 10 225
14 25 2 14 166
15 10 2 14 200
Results and Discussion
Effect of the Parameters on Fibers

Figure: Effects of electrospinning parameters on fibers

diameter in coded values [Applied voltage = 17.5 kV, flow
rate = 2.0 mL/hr, tip to collector distance = 10 cm].
Results and Discussion
Response surface model development

Backward elimination method remove the

insignificant terms (p-value > 0.05) to reduce the
complexity of the polynomial expression

TiO2 fibers diameter (nm)= +323.9-1.7A-5.23903B -8.9C +6.8B2

TABLE 3: ANOVA for reduced response surface model.

Source SS DF Mean F- p-value
square value
Model 15457.66 4 3864.42 189.49 < 0.0001
Residual 203.94 10 20.39
Lack of Fit 171.27 8 21.41 1.31 0.5026
Pure Error 32.67 2 16.33
R2 = 0.9870, Adj. R2 = 0.9818, Pred R2 = 0.9705.
 Results and Discussion
Model verification and normality test

Normality plot of residuals Model predicted against

experimental plot for fibers
diameter.
 Fiber diameter reduction is controlled by
Result Validation wider tip-to-collector distance.

The jet has longer flight time to reach

collector
Has longer time for solvent evaporation
Offers better thinning effect.
Conclusion
A reduced response surface model based on BBD
technique was developed to predict the diameter of
electrospun TiO2 nanofibers.
The three factors (applied voltage, flow rate and tip to
collector distance) were considered in this model.
Based on the developed model, tip to collector
distance appears to be the most significant factor in
determining the fibers diameter whereas applied
voltage performs less weighty role in the fibers diameter
prediction.