24th International

Elementz Fair
Project code: JC17

Title: Utilising poly-L-lactic acid for fabrication of smart

fabric catered for mechanical energy harvesting at human
joints for powering of delicate devices
 Introduction to the Team:

Cheong Yang Liu Jingxian

Xiang, Zenden
Abstract: Utilising electrospun Poly-L-lactic acid for fabrication of Smart Fabric
catered for Mechanical Energy harvesting for powering of delicate devices
PURPOSE
Enhance the shear piezoelectricity (d14) of poly-l-lactic acid (PLLA) through optimisation of
precursor solution and electrospinning process parameters.

METHODS MAIN FINDINGS

- Solution mixing containing PLLA powder using a Final results obtained
magnetic stirrer under heat suggested that PLLA fiber
- Electrospinning to obtain PLLA fibers annealing to alignment directly increase
increase crystallinity d14
- A Scanning Electron Microscope (SEM) and
Differential Scanning Calorimetry (DSC) were used to
conduct characterisation tests
Introduction

Problems with conventional

Piezoelectric materials are
piezoelectric material is that they
essential in our daily life, it’s
are made of bulky ceramic, non-
functions ranges from: power
biodegradable, and toxic. e.g Lead
generation, signal detection etc.
zirconate titanate (PZT).

However, PLLA exhibit Solution: PLLA, a biodegradable,

relatively low shear flexible, and biocompatible material
piezoelectricity compared that exhibits shear piezoelectricity is
to conventional materials an excellent alternative
Introduction
Optimise solution
parameters, increasing the
concentration of PLLA
solution within the solubility
and viscosity limit Improved PLLA
Low PLLA
d14, hence leading to
d14 compared to
more practical
conventional
piezoelectric PURPOSE applications, stronger
substitute for conventional
materials
piezoelectric materials
Optimise the drum
electrospinning parameters,
(e.g applied voltage, solution
feeding rate, drum speed)
Investigative Approach / Theoretical Background
Literature review:
- Increasing drum speed lead to
higher fiber alignment
- Enhances d14
+ Electrospinning is the currently
most effective method to
manufacture PLLA
+ Potential for further improvements
of experimental designs
PDLA
PLLA
Hypothesis:
Increasing [PLLA] in solution within
the solubility and viscosity limit
improves the quality of the
electrospun PLLA fibres. Also, higher
drum speed improve alignment of the
fibres, enhancing d14.
Investigative Approach / Theoretical Background
Why electrospinning?

PLLA piezoelectric nano fibres Electric dipole component along

can be fabricated using
electrospinning
the main carbon chain of the
PLLA polymer can be
polarized along the direction of
alignment during the process
electrospinning using an applied
electric field
Resources
Equipment: Reagents:

Electrospinning machine SEM machine DSC machine PL15 powder

(Purasorb, PL15 Corbion) Dimethylformamide

Annealing oven Magnetic stirrer XRD machine Chloroform

Procedure: Preparation of solution
1. 36 ml of chloroform, warm at
70℃ and stir at frequency
300rpm.
2. Add 2.25g of PL15 powder into
bottle containing chloroform
3. After a homogeneous solution is
formed after 3h of stirring, add 9 ml
of DMF into the mixture
5. Procedure 1 to 4 repeated with
PL15 mass 4.5g and 6.75g
to obtain 5w%, 10w% and 15w%
solution
6. Basic physical properties of
various solutions are tested
(viscosity & gelling time)

4. The mixture bottle is put in

ultrasonic shaker to remove
bubbles in solution
Procedure: Electrospinning and annealing
Needle nozzle
1. The PLLA solution of 10w% is the most
ideal in terms of viscosity and gelling time for
best electrospinning results

2. Electrospin at 1000 rpm, 18 kV, 10 cm,

and 1.0 ml/h jet speed with aluminium foil.

3. Repeat step 2 with 1500, 2000 and 3000

rpm

4. Anneal all the amorphous samples at 120℃ Electrospinning machine

for 1h to increase crystallinity Electrospinning drum
wrapped in aluminium foil
Characterisation: DSC
1. Electrospun PLLA fibres are highly
amorphous

2. Glass transition process (Tg) results in

significant changes in the thermal & electric
properties by increasing crystallinity

3. Anneal temperature above Tg (60℃) and

below it’s melting temperature (173-178℃)

4. Annealed at 120℃ under atmospheric

conditions maximises crystallinity
 Characterisation: SEM
Coating machine Metal Stand

1. PLLA fibre sheet are coated with gold

using a coating machine

2. Samples are cut into small pieces and

attached to metal stand using carbon tape

SEM machine
3. Samples are delivered into the vacuum
scanning chamber of SEM machine

4. SEM scanned at an appropriate

magnification to yield an image
Findings: SEM Image processing
1. Most random fibre is
with lowest rotation speed at
1000rpm

2. Most aligned fibre is with

highest at 3000rpm
1000 RPM 1500 RPM
3. Fibre alignment increases
with increasing drum
rotational velocity, fibre is
also more closely packed

4. Improve the alignment of

nanofibre
2000 RPM 3000 RPM
Characterisation: XRD
XRD machine
1. Irradiated sample with X-
ray at angle 𝛉

2. Detected X-ray due to

constructive interference
governed by Bragg’s Law

3. Higher the crystallinity,

higher the peak intensity,
and narrower the peak

4. Plot graph intensity

against 2𝛉
 Characterisation: XRD

Higher
peak

Lower
peaks

Three samples 1. Aligned-Annealed

Reference
(arranged in order of 2. Aligned-Non Annealed
peaks
intensity of peak) 3. Random-Non Annealed
Findings: XRD graph analysis

1. Random, non-annealed 2.Aligned, non-annealed 3.Aligned, annealed

2. Baseline 3. Integrating
1. Analysis of 4. Find
correction by area under
data using the percentage
subtracting the peak using
Origin Lab crystallinity by
base line using Peak Analysis
software formula
Peak Analysis function
Findings: XRD graph analysis

1. XC is the 2. AC is the 3. AA is the 4. Find percentage

degree of area under the area under the crystallinity by
crystallinity. crystalline non- multiplying Xc to
peaks. crystalline 100%.
peaks.
 Findings: XRD

1. Non-annealed, 2. Annealed, aligned 3. Result aligned with

random sample has the sample has the highest theory. Annealing and
lowest percentage percentage crystallinity higher fibre alignment
crystallinity at 31.4% at 73.9% yield higher crystallinity

Non-annealed, Non-annealed, Annealed,

Units (a.u) random aligned aligned 4. 3000rpm annealed
Area peak 1 0.943 1.640 7.067
sample will exhibit the
Area peak 2 0.177 0.356 0.510
most ideal d14 due to
increased crystallinity,
Area peak 3 0.077 0.077 0.173
hence it is used for
Total area (Ac+Aa) 3.812 4.924 10.494
device testing.
% crystallinity 31.4 42.1 73.9
Summary of analysis of findings
DSC SEM XRD

Annealing temperature Increasing rpm in

between Tg and Tm electrospinning Aligned and annealed
fibres results in XRD graph
have more intense peaks
Appropriate annealing Increases the alignment
temperature at 120℃ of fibres

Increases AC, hence

Increases crystallinity Increases the crystallinity
of the fibres percentage crystallinity

Best fibre sample: 10w% PL15, 3000 rpm, annealed

 Testing
Accelerometer
OSCILLOSCOPE

Cantilever
beam

Shaker base

Energy
harvesting
sample

1. Bond copper 2. Secure the PLLA

3. Set shearing 4. Measure the
tape onto one sheet with electrode
frequency of 100 voltage
PLLA surface, and onto mechanical
Hz at acceleration generated using
aluminum on the shaker using double
of 0.1 m/s2 oscilloscope
other surface sided tapes
Testing

Oscilloscope

1. Maximum
2. Sufficient to 3. Charge battery
stable voltage 4. Power
charge up in chemical
generated at 0.9 V delicate devices
capacitors potential energy
peak to peak
Application

2. Supersede 3. Save athletes or 4. More accurate

1. Power devices
replaceable & patients extra measurement. Also
that monitor
rechargeable weight when more advantageous:
biological signals
batteries & PZT measuring these flexible, biocompatible
(e.g heart rate)
generating 0.6V biological signals and biodegradable.
 Conclusion

Successful synthesis of the PLLA fibre sheet capable

of generating peak to peak voltage of 0.9V

1. Disadvantages: Still lacking in 1. Advantages: Having 0.9V peak to

terms of voltage generation peak, which is close to that of
compared to conventional PZT conventional PZT.
material (0.9V compared to 1.2V 2. Flexible, biocompatible and
peak to peak) biodegradabe compared to PZT
Areas for improvements
Experimentation: Optimise other
parameters such as humidity and
temperature during fibers deposition.

Practical: Set up proposed energy

harvesting circuit which will be wearable
to examine the kinetic energy harvested to
test the energy harvesting efficiency under
practical conditions

Application: research on more potential

microsystem applications, such as health
care, medical rehabilitation, athletic
training, and outdoor equipment
 References
Research Papers
1. Narolia, T., Gupta, V., & Parinov, I. A. (2020). Design and analysis of a shear mode piezoelectric energy harvester for
rotational motion system. Journal of Advanced Dielectrics, 10(03), 2050008. https://doi.org/10.1142/s2010135x20500083
2. Zhai, W., Ko, Y., Zhu, W., Wong, A., & Park, C. B. (2009). A Study of the Crystallisation, Melting, and Foaming Behaviours
of Polylactic Acid in Compressed CO2. International Journal of Molecular Sciences, 10(12), 5381–5397.
https://doi.org/10.3390/ijms10125381
3. Gray, A. W. (1970). Polymer crystallinity determinations by DSC. Thermochimica Acta, 1(6), 563–579.
https://doi.org/10.1016/0040-6031(70)80008-9
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