Biopolymer based nanocomposites; Characterization

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

Ingvild Kvien

Department of Engineering Design and Materials

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Department of Engineering Design and Materials

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Reinforcement Cellulose crystals (MCC, Borregaard)

Nanocomposite properties determined by:
• Size and size-distribution of cellulose whiskers • Spatial distribution and orientation of the whiskers in the matrix • Physical and chemical bonding between the reinforcement and matrix
Microscopy TEM (Transmission Electron Microscope) SEM (Scanning Electron Microscope) AFM (Atomic Force Microscopy)

Matrix PLA (Polylactic acid) (Cargill Dow) CAB (Cellulose ester)

Biopolymer based Nanocomposite
Structure Material properties

X-ray technique
WAXD (Wide angle X-ray diffraction)

Common structure techniques for nanocomposites: TEM and X-ray
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Department of Engineering Design and Materials

Department of Engineering Design and Materials

4

Goal:
Nanocomposite Cellulose whiskers AFM, TEM, SEM

TEM SEM, AFM

to combine microscopy and Xray techniques to have an overall picture of the nanocomposite

Challenges:
- apply instruments developed for metals on polymers - in nanoscale - both phases are organic

But: cutting the whiskers
X-ray

?

Combination of different X-ray techniques to determine: - Size and size-distribution of whiskers? - Orientation in the matrix?

Department of Engineering Design and Materials

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Department of Engineering Design and Materials

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Examples

So far:
Nanocomposite
2 µm CAB + cellulose crystals (AFM, NTNU) TEM-picture of PLA +graft + PEG + cellulose crystals (IPM, NTNU) Cellulose crystals (TEM, NTNU)

• • • • •

Preparation Contrast Agglomeration Electrons are ”burning” the sample Dimensions (orientation)

But micro…..

500 nm Cellulose crystals (AFM, NTNU) PLA+graft+PEG+cellulose crystals (TEM, NTNU)

Department of Engineering Design and Materials

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Department of Engineering Design and Materials

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Problems to solve
2. Compatibility between reinforcement/matrix 1. Separation of micro crystalline cellulose
chemical: - sulphuric acid - DMAc/LiCl mechanical: - ultrasound - stirring (- homogenization)

1 Separation of MCC (success)

- chemically modify the polymer - surface modification of MCC - surfactants
MCC
(SEM, NTNU)

Sulphuric acid

500 nm (AFM, NTNU)

3. Processing - parameters - feeding (how and where)

Organic solvent (DMAc/LiCl)

Investments: - centrifuge - freeze dryer - homogeniziser(future studies)
Department of Engineering Design and Materials

2.5 µm

Moving on to stage 2 and 3….
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Department of Engineering Design and Materials

(AFM, NTNU)

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It is possible

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

Publications

500 nm

1. Dispersion of microcrystalline cellulose in DMAc/LiCl

Solution casted nanocomposite (AFM, NTNU)

2. Investigation of structure and distribution of cellulose nano whiskers in polylactic acid (PLA) by TEM, SEM, AFM and X-ray diffraction Conference in Madison, May 2005

Department of Engineering Design and Materials

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Department of Engineering Design and Materials

12

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