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Manufacturing and measurement of superhydrophobicity for paperbased active packaging
COST Action FP1405Active and intelligent fibre-‐based packaging – innovation and market introduction
Charlène REVERDY, PhD student, LGP2
STSM project partners
“Chemistry, Materials and Surfaces”
Expertise on surface modification andformulation of coatings, advancedassessment of surface functionality andmaterials properties.
“Multiscale BiobasedMaterials”
Expertise on nanocellulose and papertechnology. Special interest in activepackagingwith antimicrobial properties.
Involved persons:Julien Bras, associate professorCharlène Reverdy, PhD student
Involved persons:Agne Swerin, research director
Maziar Sedighi Moghaddam, post-‐doc
PROJECT GLOBAL PLAN
PROJECT
-‐Cellulose nanofibrils hydrophobization
-‐ Nanofibrils/ Calcium carbonate coatingelaboration-‐ Surface characterization
-‐ Surface mapping-‐ Effect of superhydrophobicity on bacterialadhesion and growth
INTRODUCTION − WHAT IS NANOCELLULOSE?
Cell structure
Adapted from Pääkkö, et al. 2007Wood cell
NANOCELLULOSE
D 2-‐10 nmL 150-‐1000 nm
Cellulose nanocrystals (CNC)Cellulose nanofibrils (CNF)
D 2-‐20 nmL ˃ 1000 nm
INTRODUCTION − WHAT IS SUPERHYDROPHOBICITY?
5
Lowwater adhesionWater contact angle > 150°Water Roll-‐off angle < 10°
• Actually, contact angle is affected by surface roughness.• Surface with a r roughness (Wenzel)
𝐜𝐨𝐬𝜽& = 𝒓𝒄𝒐𝒔𝜽𝑬• Surface non chemically homogeneous (Cassie
Baxter)𝒄𝒐𝒔𝜽& = 𝒇𝟏𝒄𝒐𝒔𝜽𝟏 + 𝒇𝟐𝒄𝒐𝒔𝜽𝟐
f1 et f2 probability to encounter solid 1 or 2, and Ѳ1
and Ѳ2Young angle for eache solid. (Air pocketmodel)
• A contact angle measurement is done ideally with(Young ѲE):• Plane surface• Chemically homogeneous surface
Surface wettability can be control by roughness and chemistry
INTRODUCTION − WHAT IS SUPERHYDROPHOBICITY?
Latex
Hydrophobizedacicular aragonite
Cellulose nanofibrils
Cardboard
STSM PROJECT
• Learn how to make a superhydrophobic coating
• Learn how to measure superhydrophobicity
Antimicrobial hydrophobic CNF : CNF-‐APMS
Hydrophobic reference CNF (InoFib, France) : CNF-‐AKD
Static, Roll-‐off, WaterShedding Angle, Advancingand receding
Advancing and recedingangles, wettability(multicycles)
WILHELMY PLATE
OPTICAL CONTACT ANGLE
Force measurement duringpenetration of the sample inthe known liquid
Image recording of acontrolled water drop.Tilting of the surfacecontrolled.
METHOD
MATERIAL AND METHODS
PROBLEM N°1 : Facing dry matter content
78% pigments2% oleate20% Latex
33% Dry matter
78% pigments2% oleate20% CNF
9% Dry matter
r489% pigments2% oleate9% CNF-‐APMS
r10
15% Dry matter
PROBLEM N°2 : Oleate excess disrupt CNF-‐AKD hydrophobization
15% Dry matter
91% pigments0,3% oleate9% CNF-‐AKD
r1095% pigments0,3% oleate5% CNF-‐AKD
18% Dry matter
r20
Rod Coater
MATERIAL AND METHODS
CNF AKD r20 CNF APMS r10
CNF
RESULTS
0.0
20.0
40.0
60.0
80.0
100.0
120.0
140.0
160.0
Advancing Receding
θw (°)
CNF-‐AKD
CNF-‐APMS
CNF-‐AKD r20
CNF-‐APMS r10
Latex r4
Roughness
Wetting measurements
Water adhesion probably due to CNF high affinity with water (evenafter hydrophobisation) and/or enlargement of pitch
WSA
CNF-‐AKD r20 17°Latex r4 2,5°
RESULTSStatic water contact angle
0
20
40
60
80
100
120
140
160
180
θw (°)
CNFCNF-‐APMSCNF-‐AKDCNF-‐APMS r10CNF-‐AKD r20
Latex r4
SH
• Superhydrophobic static contact angle obtained but not roll-‐off (Water shedding yes)• More a « rose petal effect »• Leaching of PCC observed
Water shedding angle
• Poster presentation at N.I.C.E conference, October 2016, Nice, France
• Conference on material science based on biomimetism
SCIENTIFIC VALORIZATION
“ Superhydrophobic surfaces manufacturing with nanocellulose ”
• Adaptation of LGP2 laboratory tools for measurearement of superhydrophobic properties
PERSPECTIVES ON THE PROJECT
• Assessement of bacterial adhesion and growth on a superhydrophobic surface with antimicrobial and non-‐antimicrobial CNF
• Stronger hydrophobization of CNF, not interacting with fatty acid
THANK YOU FOR YOURATTENTION