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Rapid Preparation of Free- standing
Nanocellulose Films using spray coating
Co-authors : Kirubanandan Shanmugam, Prof. Gil Garnier and Dr. Warren
Batchelor
Australian Paper and Pulp Institute, Monash University,
Australia.
Swambabu Varanasi
Introduction and Background of the research
Research Objective
Methods
Results
Conclusion
OUTLINE
Bio-degradable
Bio-renewable
Bio-compatible
Characteristics
High Specific Strength
Thermal Stability
Hydrophilicity
Chemical
Modification
Hierarchical structure of wood fibers, Network of micro fibrils (Zhu et al., 2014)
INTRODUCTION
APPLICATIONS OF NANOCELLULOSE
Solar Cell (Georgia Tech News, 2013) Water and Air Filtration
Touch Screens (Zhu et al., 2014) High performance barrier materials
Images from web
NANOCELLULOSE FILMS PREPARATION TECHNIQUES
2. Vacuum filtration
Filtration Separation Drying
1. Casting and Solvent evaporation
Processing Method Processing Time Basis Weight (g/m2)
Casting 3 min 10 to 30
Vacuum Filtration 3 min to 4 hours 60
Sehaqui et. al. Biomacromolecules 2010, 11 (9), pp 2195–2198
Processing time –10-27 mins
3. Spray Coating
FREE STANDING FILMS PREPARATION TECHNIQUES
Beneventi, D. et. al. Industrial Crops and Products, 2015. 72: p. 200-205.
Our aim – Developing a spray coating technique to prepare lab scale films with very
minimum processing time ( less than minute)
EXPERIMENTAL SETUP
A Professional spray gun for performing spray
coating process
Experimental Conditions :
• Spray distance - 30 cm
• Suspension concentration - 1.0 to 2.0 wt %
• Velocity of conveyor – 0.34 cm/sec
Shanmuagam et. al. Cellulose - DOI: 10.1007/s10570-017-1328-4
SUSPENSION CONSISTENCY Vs BASIS WEIGHT & THICKNESS
0
50
100
150
200
250
300
0
50
100
150
200
250
0.8 1 1.2 1.4 1.6 1.8 2 2.2
BasisWeighting/m2
Concentration of nanocellulose in wt%
Basis Weight Vs Suspension Concentration
Thickness Vs Suspension Concentration
Thicknessinµm
THICKNESS MAPPING
SprayDirection
Surface exposed to atmosphere - rough
Surface adjacent to plate - Smooth
THICKNESS DISTRIBUTION
Spray Coated Film Film made by Vacuum Filtration
1 2 3 4
1
2
3
4
Region
Region
111.0
116.0
121.0
126.0
131.0
136.0
141.0
146.0
151.0
1 2 3 4
1
2
3
4
Region
Region
109.0
111.4
113.8
116.1
118.5
120.9
123.3
125.6
128.0
SEM IMAGES OF NANOCELLULOSE SHEET
1µm 10 µm 100 µm
1 µm 10 µm 100 µm
Rough
surface
Smooth
surface
SURFACE ROUGHNESS
Rough Smooth
AFM Image of the nano-fibrillated sheet – Rough and Smooth surface at 500 nm
Technique used Surface RMS Roughness (nm)
AFM Rough 414.0 nm (10µm
x10µm)
51.4 nm (2µm x
2µm)
Smooth 81.1 nm (10µm
x10µm)
16.7 nm (2µm x
2µm)
Parker Print
Surface
Instrument
Roughness 10.8±0.17µm -
Smoothness 5.5±1.4 µm -
Parker Print
Surface
Instrument
Sheet prepared
via the vacuum
filtration
10.6±0.3 µm
9.9±0.1 µm
-
SURFACE ROUGHNESS
OPTICAL PROFILOMETRY
Rough Smooth
MECHANICAL AND BARRIER PROPERTIES
Properties Spray Coated Sheet Sheet Prepared by
Vacuum filtration
Tensile Index (Nm/g) 60.2±1.5 62.3±3.4
Tensile stiffness (KN/m) 946±86 941±78
Air permeability
(µm/Pa.s)
<0.003 <0.003
Water Transmission Rate
(g/ m2 day)
35.6±8.5 33.9±3.5
CONCLUSION
• A rapid technique to prepare lab scale nanocellulose films
was developed.
• Processing time to prepare lab-scale nano-cellulose films is
less than a minute.
• Spray coated films has similar uniformity, mechanical and
barrier properties compared to films prepared by Vacuum
filtration.
• Spray coated films has one highly smooth and glossy surface.
ACKNOWLEDGEMENT
• Kirubandan Shanmugam, Dr. Warren Batchelor and Prof. Gil
Garnier
• Monash Centre for Electron Microscopy, Monash University
• Dr. Natasa, Dr. Rico Tabor for help with AFM
• Dr. Hemayet Uddin, Melbourne Centre for Nanofabrication
Thank you
PRESENTED BY
Swambabu Varanasi
Research Fellow
Monash University
Australia

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Spray coating – a rapid method for preparation of free-standing nanocellulose film

  • 1. Rapid Preparation of Free- standing Nanocellulose Films using spray coating Co-authors : Kirubanandan Shanmugam, Prof. Gil Garnier and Dr. Warren Batchelor Australian Paper and Pulp Institute, Monash University, Australia. Swambabu Varanasi
  • 2. Introduction and Background of the research Research Objective Methods Results Conclusion OUTLINE
  • 3. Bio-degradable Bio-renewable Bio-compatible Characteristics High Specific Strength Thermal Stability Hydrophilicity Chemical Modification Hierarchical structure of wood fibers, Network of micro fibrils (Zhu et al., 2014) INTRODUCTION
  • 4. APPLICATIONS OF NANOCELLULOSE Solar Cell (Georgia Tech News, 2013) Water and Air Filtration Touch Screens (Zhu et al., 2014) High performance barrier materials Images from web
  • 5. NANOCELLULOSE FILMS PREPARATION TECHNIQUES 2. Vacuum filtration Filtration Separation Drying 1. Casting and Solvent evaporation Processing Method Processing Time Basis Weight (g/m2) Casting 3 min 10 to 30 Vacuum Filtration 3 min to 4 hours 60 Sehaqui et. al. Biomacromolecules 2010, 11 (9), pp 2195–2198
  • 6. Processing time –10-27 mins 3. Spray Coating FREE STANDING FILMS PREPARATION TECHNIQUES Beneventi, D. et. al. Industrial Crops and Products, 2015. 72: p. 200-205. Our aim – Developing a spray coating technique to prepare lab scale films with very minimum processing time ( less than minute)
  • 7. EXPERIMENTAL SETUP A Professional spray gun for performing spray coating process Experimental Conditions : • Spray distance - 30 cm • Suspension concentration - 1.0 to 2.0 wt % • Velocity of conveyor – 0.34 cm/sec Shanmuagam et. al. Cellulose - DOI: 10.1007/s10570-017-1328-4
  • 8. SUSPENSION CONSISTENCY Vs BASIS WEIGHT & THICKNESS 0 50 100 150 200 250 300 0 50 100 150 200 250 0.8 1 1.2 1.4 1.6 1.8 2 2.2 BasisWeighting/m2 Concentration of nanocellulose in wt% Basis Weight Vs Suspension Concentration Thickness Vs Suspension Concentration Thicknessinµm
  • 9. THICKNESS MAPPING SprayDirection Surface exposed to atmosphere - rough Surface adjacent to plate - Smooth
  • 10. THICKNESS DISTRIBUTION Spray Coated Film Film made by Vacuum Filtration 1 2 3 4 1 2 3 4 Region Region 111.0 116.0 121.0 126.0 131.0 136.0 141.0 146.0 151.0 1 2 3 4 1 2 3 4 Region Region 109.0 111.4 113.8 116.1 118.5 120.9 123.3 125.6 128.0
  • 11. SEM IMAGES OF NANOCELLULOSE SHEET 1µm 10 µm 100 µm 1 µm 10 µm 100 µm Rough surface Smooth surface
  • 12. SURFACE ROUGHNESS Rough Smooth AFM Image of the nano-fibrillated sheet – Rough and Smooth surface at 500 nm
  • 13. Technique used Surface RMS Roughness (nm) AFM Rough 414.0 nm (10µm x10µm) 51.4 nm (2µm x 2µm) Smooth 81.1 nm (10µm x10µm) 16.7 nm (2µm x 2µm) Parker Print Surface Instrument Roughness 10.8±0.17µm - Smoothness 5.5±1.4 µm - Parker Print Surface Instrument Sheet prepared via the vacuum filtration 10.6±0.3 µm 9.9±0.1 µm - SURFACE ROUGHNESS
  • 15. MECHANICAL AND BARRIER PROPERTIES Properties Spray Coated Sheet Sheet Prepared by Vacuum filtration Tensile Index (Nm/g) 60.2±1.5 62.3±3.4 Tensile stiffness (KN/m) 946±86 941±78 Air permeability (µm/Pa.s) <0.003 <0.003 Water Transmission Rate (g/ m2 day) 35.6±8.5 33.9±3.5
  • 16. CONCLUSION • A rapid technique to prepare lab scale nanocellulose films was developed. • Processing time to prepare lab-scale nano-cellulose films is less than a minute. • Spray coated films has similar uniformity, mechanical and barrier properties compared to films prepared by Vacuum filtration. • Spray coated films has one highly smooth and glossy surface.
  • 17. ACKNOWLEDGEMENT • Kirubandan Shanmugam, Dr. Warren Batchelor and Prof. Gil Garnier • Monash Centre for Electron Microscopy, Monash University • Dr. Natasa, Dr. Rico Tabor for help with AFM • Dr. Hemayet Uddin, Melbourne Centre for Nanofabrication
  • 18. Thank you PRESENTED BY Swambabu Varanasi Research Fellow Monash University Australia