Fourth Derivative FTIR-ATR & UV-Vis DRS Investigation on

Photo -Thermal stability of CNFs

R. Pavithra Marthandam
Research Scholar
PG & Research Department of Physics
Pachaiyappas College, Chennai 600 030.
Under the Guidance of
Dr. E. Sailatha
SpectroPhysics Research Laboratory / ISPA
PG & Research Department of Physics
Pachaiyappas College
Chennai 600 030
Under the Supreme Guidance of
Dr. S. Gunasekaran, Ph.D.,D.Sc.
TANSA Awardee
Dean (R&D), SPIHER
St. Peters University
Avadi, Chennai 600 054.
Smart Materials
Eco-friendly
Toxin-free
In Abundance
Renewable
Cost effective
Versatility
Reinforcing Materials and
Composites
 Cellulose Nanofibrils
Organic Polymer

Cellulose - Found in Plant Cell walls / Cotton/ Bacterial Cellulose

replenished by Photosynthesis

Cellulose Nanofibrils (CNFs) are derived from plant biomass are

particularly desirable group of nano-products

CNFs are usually prepared by liberation from the constituent fiber

matrix and microfiber bundles

Top-down approach

Combination of Physical and Chemical refining

Major Constituents of Wood & Non-wood Plant
Resources
Cellulose Lignin
 Lignocellulosic Resources
Teak
Acacia nilotica
Casuarina
Sugarcane Bagasse
Banana Fibers
Plantain Fibers
 Extraction of CNFs
Ground Precursors Acetone + Double Distilled Water at 120c for 5h

NaOH + Double Distilled Water at 120C for 5h Discoloration While Bleaching with NaCl2O2
at 120C for 5h
 Extraction of CNFs
Bleached fibers - Cellulose Cellulose

Introduction of Sulfuric Acid While Acid hydrolysis at

Washed CNFs Sonicated for 15 Min
60C for 5h
 Extraction of CNFs
CNFs Dry CNFs

Sonicated Ethanol Suspension of

CNFs

Sheet Made up of CNFs

Extraction of CNFs
 Characterization Techniques
Fourier Transform Infrared-Attenuated Total Reflectance (FTIR ATR)

Powder X-Ray Diffraction (PXRD)

Scanning Electron Microscopy (SEM)

Atomic Force Microscopy (AFM)

Transmission Electron Microscopy (TEM)

Dynamic Light Scattering (DLS)

Thermo Gravimetric Differential Thermal Analyses (TG-DTA)

Dielectric Studies
Characterization Results
The Green Option for 3-D Printing
 Discoloration
Biggest challenge
How to maintain CNFs properly?
Suitable optical vicinity
Suitable temperature
Causes of Discoloration
Is Light absorption due to restorement of lignin?
Methods to predict discoloration
 Reflectance Molecular Spectroscopic
Techniques
Fourth Derivative FTIR ATR Spectroscopy

and

Diffuse Reflectance UV-Vis Spectroscopy

Determination of impact of UV irradiation on Cellulosic
fibers Zeroth Derivative FTIR Spectroscopy
 Determination of impact of UV irradiation on Lignocellulosic
fibers Fourth Derivative FTIR Spectroscopy

Fourth derivative spectra in the region of 3000-2800cm-1 Fourth derivative spectra in the region of 1800-1200cm-1

Fourth derivative spectra in the region of 1200-800cm-1

 Determination of impact of UV irradiation on Cellulose fibers
Fourth Derivative FTIR Spectroscopy

Fourth derivative spectra in the region of 3000-2800cm-1 Fourth derivative spectra in the region of 1800-1200cm-1

Fourth derivative spectra in the region of 1200-800cm-1

 Determination of impact of UV irradiation on CNFs
Fourth Derivative FTIR Spectroscopy

Fourth derivative spectra in the region of 3000-2800cm-1 Fourth derivative spectra in the region of 1800-1200cm-1

Fourth derivative spectra in the region of 1200-800cm-1

 Overlaid Reflectance and K-M Spectra of Cellulosic fibers

Overlaid UV-Vis reflectance spectra of Lignocellulose fibers (LCF), Cellulose fibers (CF) and Cellulose Nanofibrils (CNF)

Overlaid UV-Vis K-M spectra of Lignocellulose fibers (LCF), Cellulose fibers (CF) and Cellulose Nanofibrils (CNF)
 Overlaid Reflectance and K-M Spectra of UV irradiated Cellulosic fibers

Overlaid UV-Vis reflectance spectra of UV irradiated Lignocellulose fibers (LCFUV), Cellulose fibers (CFUV) and Cellulose Nanofibrils (CNFUV)

Overlaid UV-Vis K-M spectra of UV irradiated Lignocellulose fibers (LCFUV), Cellulose fibers (CFUV) and Cellulose Nanofibrils (CNFUV)
Determination of Thermal Degradation of Cellulosic fibers
FTIR-ATR Spectra of fibers at 270C

Overlaid FTIR-ATR spectra of thermally degraded Lignocellulose fibers (LCF),

Cellulose fibers (CF) and Cellulose Nanofibrils (CNF) at 270C
 Conclusion
Sensitiveness of C-H regions

Advantages of UV-Vis Reflectance spectroscopy

Lucid representation of Fourth Derivative FTIR-ATR

Spectroscopy

Thermal withstanding ability of CNFs

Stability of CNFs over its precursors

CNFs for future

 Acknowledgements
Dr. S. Gunasekaran, Ph.D.,D.Sc.

TANSA Awardee Dean (R&D), SPIHER, St. Peters University, Avadi, Chennai 600 054.

Dr. E. Sailatha, My Research Supervisor

Dr. S. Srinivasan, My DC Expert

SAIF St. Peters University, Avadi, Chennai 600 054.

Dept. of Chemistry, IIT-M , Crystal Growth Centre, Department of Nanotechnology Anna

University, NCNSNT UNOM

ISPA Members

All My Professors

Ms. Kamatchi, Mr. P. Ramesh, Ms. P. Sasirekha and all my friends, Fellow Researchers.