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Regional Conference on Solid State Science and Technology (RCSSST 2014)

Cellulose Micro/Nano fibers (CMNF) from Bioresources in Malaysia Fauziah Abdul Aziz Physics Department Centre For Defence Foundation Studies National Defence University of Malaysia (NDUM) Sg. Besi, Kuala Lumpur. Regional Conference on Solid State Science and Technology

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Regional Conference on Solid State Science and Technology (RCSSST 2014)

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  1. Cellulose Micro/Nano fibers (CMNF) from Bioresources in MalaysiaFauziah Abdul AzizPhysics DepartmentCentre For Defence Foundation StudiesNational Defence University of Malaysia (NDUM)Sg. Besi, Kuala Lumpur

  2. Regional Conference on Solid State Science and Technology (RCSSST 2014) Copthorne Hotel, Cameron Highlands, Pahang 25 – 27 November 2014

  3. OUTLINE • Introduction • Term CMNF • Why Used CMNF? • Bioresources of CMNF • Some Analysis • Potential Benefits of CMNF • Conclusions

  4. INTRODUCTION • Cellulose is a renewable, biodegradable & the most abundant natural biopolymer in the world • Natural cellulosic fibers are synthesized mainly in plants • cellulose constitutes 40 to 50% of wood

  5. TERM CMNF(Chakraborty et al., 2006) • Microfibres are defined as fibres of cellulose of 0.1-1 µm in diameter • corresponding minimum length of 5-50 µm nanofibrils are at least 1-D at the nanometer scale (1-100 nm)

  6. TERM CMNF (con’t) • While the small fibrils isolated from natural fibers normally have a wide range of diameters, most are below 100 nm & some are above 0.1 µm • A term of cellulose micro/nanofibrils (CMNF) used

  7. Hardwoods-Tropical • dicot angiosperm trees; flowers / seeds ; • broad leaves; evergreen • presence of pores / vessels (obvious) • Gardening plants – shrubs, non-woody • Due to physical structure, hardwood tend to be more expensive than softwood

  8. SUPRASTRUCTURES FIBRE CMNF

  9. Hierarchical structure of the wood cell wall

  10. Some eg of cellulose (whiskers) from different cellulosic sources

  11. Scale of Cellulose (Wang, 2008)

  12. Structural Formula of Cellulose, (C5H10O5)n (Cave & Walker, 1994)

  13. Lattice parameter for various cellulose allomorphs

  14. Unit Cell of Cellulose Iβ Parallel mode of repeating unit of cellulose Iβ (Nishiyama et al., 2002; Penttilä, 2013) along the a-axis (left, centre chain only) and along the b-axis (right)

  15. Cellulose I • Natural cellulose = native cellulose = cellulose I - ordered • best crystalline allomorph of cellulose • two allomorphs ie • cellulose Iα • cellulose Iβ

  16. Cellulose I (con’t) • The parallel packing of native cellulose make it metastable arrangement • this irregular chain arrangement

  17. Cellulose I (con’t) • the microfibrils, consisting of about • 36 parallel cellulose chains in a crystal are arranged into bundles with outer lateral dimensions in the order of 20 nm

  18. Cellulose Iβ & Cellulose Iα • cellulose Iβ is more disordered of cellulose than cellulose Iα • cellulose Iα is more crystalline than cellulose Iβ • Iβ allomorph is recognized to be dominant in higher plants • higher stability of cellulose Iβ compared to cellulose Iα

  19. WHY USED CMNF? • Renewable materials from nature • Most environmentally friendly materials combined with a biogradable polymer as a matrix • Low abrasion compared to glass-fibre • Non-toxic

  20. WHY USED CMNF? (con’t) • Light • Porous • High mechanical strength

  21. WHY USED CMNF? (con’t) • nonlinear • optical behavior has been the subject of many - design of smart materials

  22. BIORESOURCES OF CMNF • Once upon a time, a living cell of biological origin • Natural sources • Organic • In this work, used plants • Non-Woody • Hardwood

  23. Non-Woody Plants • Banana (Musa acuminata) pseudo-stem • Pineapple (Ananascomosus) leaf

  24. Hardwood • Resak (Vatica spp.) waste • Merbau(Intsiabijuga) waste

  25. Methods & Techniques • chemical treatment • Amorphous region - removed • Purification (lessen DP=no of repeating units per molecule) • Segal’s method • Scherrer equation

  26. SOME ANALYSIS

  27. DIFFICULTY • producing purely single solid crystal due to its polymorphic behaviour • The increase of defibrillation of cellulose molecule & rearrangement of hydrogen bonds during isolation

  28. STRUCTURAL CHARACTERIZATION • x-ray diffraction (XRD) • field emission scanning electron microscopy (FESEM)

  29. Chemical composition of various plants samples

  30. Abbreviations of bioresources

  31. Hardwood Merbau (Intsia bijuga) sample

  32. The cellulose residue before dry of alkali treatment process

  33. Cellulose delignification cellulose (DL) of Merbau (Intsia bijuga) After deliglification cellulose (DL) powder

  34. Micrographic of FESEM of after delignification cellulose (DL) of Merbau (Intsia bijuga) Structure and appearance of CMNF by SEM - Regenerated cellulose fiber - nano-scale, Wang et al, 2006

  35. Commercial celluloses, Moran et al, 2008 Product acid-bleached cellulose (BA) of Merbau (Intsia bijuga)

  36. Micrographic of FESEM of acid-bleached cellulose (BA) of Merbau (Intsia bijuga) SEM Microstructure of PP/CMNF composites – overview (Wang et al, 2006)

  37. Structure and appearance of CMNF by SEM, Wang at al, 2006 FESEM images of untreated :R1, M1, P1 & B1

  38. FESEM images of treated samples : R2, M2, P2 and B2

  39. Simulation Diffractogram [XRPD] of microcrystalline states of cellulose (Crowder & Fawcett, ICDD) • Estimates crystallites size parameters • Compute comparable FWHMs for peaks, 3.5nm • Software simulates pattern using d-space & intensity values

  40. Simulation Diffractogram of microcrystalline states of cellulose (Crowder & Fawcett, ICDD)

  41. Diffractogram (XRPD) - Experimental & Standard of Cellulose Iβ Crowder & Fawcett, ICDD

  42. Diffractograms of untreated various CMNF of plants samples Diffractograms of cotton & tunicate cellulose whiskers, Pullawan, 2012

  43. Simulation Diffractogram of microcrystalline states of cellulose (Crowder & Fawcett, ICDD) Diffractograms of treated various CMNF plants sample

  44. CMNF Crystalline cellulose Iα & cellulose Iβ • Presents of cellulose Iα & cellulose Iβ • cellulose Iβ more dorminant than cellulose Iα • Lack of long range order means have no conventional Bragg diffractions • Broad features due to interatomic distances within the disordered structure

  45. XRD of CMNF Pattern • Presents at least more than one phase system • Maxima are shifted from the underlying positions of the major Bragg peaks due to the significant overlap

  46. ICDD Data Base • Best integral index fit is 50-2241, cellulose Iβ

  47. Crystallite size, D (nm) & crystallinity, Xc ( % ) of various CMNF plants samples

  48. Some XRD Results

  49. Some XRD Results • The percentages of crystallinity of CMNF of all samples increased after passing the chemical treatment • CMNF banana (Musa acuminata) is more crystalline (79.29%) than other CMNF samples

  50. Some Results (con’t) • Significance size reduction in diameter were seen when the fiber was treated during the chemical treatment process

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