Biopolymer based nanocomposites;

Outline
Characterization
• Project description
• Determination of structure
• Where are we today?
• Problems to solve
• Progress plan/publications
Ingvild Kvien

Department of Engineering Design and Materials

1 Department of Engineering Design and Materials
2

Reinforcement Nanocomposite properties

Cellulose crystals
(MCC, Borregaard)
determined by:

• Size and size-distribution of Microscopy

cellulose whiskers TEM (Transmission Electron Microscope)
• Spatial distribution and SEM (Scanning Electron Microscope)
orientation of the whiskers AFM (Atomic Force Microscopy)
in the matrix
• Physical and chemical
bonding between the X-ray technique
Biopolymer reinforcement and matrix WAXD (Wide angle X-ray diffraction)
Matrix
based
PLA (Polylactic acid)
(Cargill Dow) Nanocomposite
CAB (Cellulose ester)
Structure
Material properties Common structure techniques for nanocomposites: TEM and X-ray

Department of Engineering Design and Materials

3 Department of Engineering Design and Materials
4

1
 Goal:
Nanocomposite
to combine microscopy and X-
Cellulose whiskers
ray techniques to have an
overall picture of the
AFM, TEM, SEM TEM
nanocomposite
Challenges:
SEM, AFM
- apply instruments
But: cutting the whiskers developed for metals on
polymers
X-ray - in nanoscale
? Combination of different X-ray - both phases are organic
techniques to determine:
- Size and size-distribution of
whiskers?
- Orientation in the matrix?

Department of Engineering Design and Materials

5 Department of Engineering Design and Materials
6

So far:
Examples

Nanocomposite
2 µm
CAB + cellulose crystals (AFM, NTNU)

TEM-picture of PLA +graft + PEG + cellulose crystals (IPM, NTNU)

Cellulose crystals (TEM, NTNU)

• Preparation But micro…..

• Contrast
• Agglomeration
• Electrons are ”burning” the sample
• Dimensions (orientation) 500 nm
Cellulose crystals (AFM, NTNU)
PLA+graft+PEG+cellulose crystals (TEM, NTNU)

Department of Engineering Design and Materials

7 Department of Engineering Design and Materials
8

2
 1 Separation of MCC (success)
Problems to solve

2. Compatibility between
reinforcement/matrix
1. Separation of micro crystalline
Sulphuric acid
cellulose - chemically modify the polymer 500 nm
(AFM, NTNU)
- surface modification of MCC
chemical: mechanical: - surfactants
- sulphuric acid - ultrasound
(SEM,
MCC NTNU)
- DMAc/LiCl - stirring
(- homogenization) 3. Processing Organic solvent
(DMAc/LiCl)
Investments: - centrifuge - parameters
- feeding (how and where)
- freeze dryer
2.5 µm
- homogeniziser(future studies) (AFM, NTNU)
Moving on to stage 2 and 3….

Department of Engineering Design and Materials

9 Department of Engineering Design and Materials
10

Progress plan
It is possible
Tasks 2003 2004 2005 2006
1. Litterature study xxxx
xx
2. Nanofiber treatments and separation process xxxxxx
3. Characterization of nanofibers (TEM,AFM,X-Ray) xxxxx
xxxxxxx
4. Characterization of nanocomposites properties xxxxxxxxxxxx xxxx
and structure (DMTA, TEM, AFM, XRD, DSC) xxxx
5. Preparation of PhD-thesis and defence of the work xxxxx

Publications
500 nm
1. Dispersion of microcrystalline cellulose in DMAc/LiCl
2. Investigation of structure and distribution of cellulose nano whiskers in
Solution casted nanocomposite (AFM, NTNU) polylactic acid (PLA) by TEM, SEM, AFM and X-ray diffraction
Conference in Madison, May 2005

Department of Engineering Design and Materials

11 Department of Engineering Design and Materials
12