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OUTLINE
Introduction
Materials
Results and Discussion
Conclusions
Acknowledgements
Introduction
Barrier Films?
Designed to reduce/retard gas
migration
industries
toxic chemicals
Chemical Vapor
Barrier
To prevent the diffusion of toxic chemical
vapors, while allowing water vapor to
pass through
Hydrophilic barriers to protect from
hydrophobic toxins
Should be tough and flexible
Useful in protective clothing
Materials
Structure:
Poly(acrylic acid)-PAA
Poly(acrylic acid) PAA:
Source: Sanli, O., et al. Journal of applied polymer science, 91( 2003)
Cellulose Nanocrystals(CNXLs)
Native cellulose
Crystalline regions
Acid hydrolysis
Individual nanocrystals
Proposed structure
PAA
PVOH
Objectives
Prepare chemical barrier films with
treatment
Methods
Film Preparation
Testing methods
degradation
Chemical Vapor Transmission Rate (CVTR)
Preparation of the
Blends
5 wt % solution of PVOH and PAA
1 wt % solution of dispersed CNXLs in DI water
Composition
0%
CNXL
10% CNXL
20% CNXL
0% PAA
0/0
0/10
0/20
10% PAA
10/0
10/10
10/20
20% PAA
20/0
20/10
20/20
Film Preparation
Compositions were mixed, sonicated and
Heat treatment
optimization
Evaluate via water solubility test
At 125 C/1 hr films were completely soluble
in water after a day
At 185 C/1hr color of the films changed to
brown
At 150 C and 170 C/45 min films were clear
and had good water resistance
(Weight 1 Weight 2)
*100%
Weight 1
Lower = Better
PAA
Blue: Non heat treated film
Absorbance
Absorbance
3500 cm-1
2500 cm-1
1500 cm-1
3500
2500
Wavenumbers (cm-1)
1500
1715 cm-1
Absorbance
1723 cm-1
0.0
3500
3000
2500
2000
Wavenumbers (cm-1)
1500
1000
a) 5% CNXL/ 10%PAA
Water Permeability
Water Vapor Transmission Rate
D
M
Mass change( g )
J ( Flux )
2
A * t Area (m ) * time(day )
dogbone shape
Span: 20 mm
Stress, MPa
Ultimate Tensile
Strength
150 %
Increase
Tensile Modulus
Almost
Double
Elongation
Elongation, % mm/mm
20%
reduction
70%
reduction
Toughness
2.5 times
increase
Thermal degradation
Thermo gravimetric Analysis
Change in weight with
increasing temperature
Test is run from room
temperature to 600C
Ramping 20C/min
Chemical Vapor
Transmission Rate-CVTR
ASTM standard F 1407-99a (Standard method of
CVTR Assumptions
The assumptions made for the
2500
100% PVOH
2000
flux = slope of steady state
1500
1000
breakthrough
500
20
40
60
Time, h
80
100
120
2000
100% PVOH
1500
1000
500
20
40
60
Time, h
80
100
120
Surface Modification of
CNXLs OBJECTIVES
To improve the interaction between CNXLs and
PVOH
To understand if the CVTR observations are
Surface modification of
CNXLs
TEMPO
NaBr
NaClO
CNXLs
C.CNXLs
% Carboxylate Content
1.32 mmols/g
of acid groups.
Methods
Polarized optical microscopy
Water vapor transmission
Thermal degradation
Chemical vapor transmission
Dispersion of C.CNXLs
CNXLs
C.CNXLs
10%
10%
15%
15%
Flux : g / m2 * day
Thermal degradation
DTGA
Conclusions
170 C temperature and 45 minutes of heat