The structure of microcrystalline cellulose (MCC) made by mild acid hydrolysis from cotton linter, flax fibres and sulphite or kraft cooked wood pulp was studied and compared with the structure of the starting materials. Crystallinities and the length and the width of the cellulose crystallites were determined by wide-angle X-ray scattering and the packing and the cross-sectional shape of the microfibrils were determined by smallangle X-ray scattering. The morphological differences were studied by scanning electron microscopy. A model for the changes in microfibrillar structure between native materials, pulp and MCC samples was proposed. The results indicated that from softwood or hardwood pulp, flax cellulose and cotton linter MCC with very similar nanostructures were obtained with small changes in reaction conditions. The crystallinity of MCC samples was 54-65%. The width and the length of the cellulose crystallites increased when MCC was made. For example, between cotton and cotton MCC the width increased from 7.1 nm to 8.8 nm and the length increased from 17.7 nm to 30.4 nm. However, the longest crystallites were found in native spruce wood (35-36 nm).

Abstract. Microcrystalline cellulose is a porous natural material which can be used both as a support for nanoparticles and as a reducer of metal ions. Cellulose supported nanoparticles can act as catalysts in many reactions. Cu, CuO, and Cu2O particles were prepared in microcrystalline cellulose by adding a solution of copper salt to the insoluble cellulose matrix and by reducing the copper ions with several reducers. The porous nanocomposites were studied using anomalous small angle x-ray scattering (ASAXS), x-ray absorption spectroscopy, and x-ray diffraction. Reduction of Cu 2+ with cellulose in ammonium hydrate medium yielded crystalline CuO nanoparticles and the crystallite size was about 6 -20 nm irrespective of the copper concentration. The size distribution of the CuO particles was determined with ASAXS measurements and coincided with the crystallite sizes. Using sodium borohydrate or hydrazine sulfate as a reducer both metallic Cu and Cu2O nanoparticles were obtained and the crystallite size and the oxidation state depended on the amount of reducer.

Summary: Copper and nickel nanoparticles were synthesized in the insoluble microcrystalline cellulose support by reduction of metal ions with several reducers in various media resulting in cellulose‐metal nanocomposites. Wide‐angle X‐ray scattering results showed that supramolecular structure of cellulose did not change. Crystalline Cu2O and Cu0 nanoparticles were prepared with reducers NaBH4 and N2H4 · H2SO4, CuO nanoparticles – with cellulose itself as a reducer. Crystalline Ni0 nanoparticles were synthesized with N2H4 · 2HCl and NaBH4; Ni0 nanoparticles in amorphous form were prepared with KH2PO2 · H2O. SEM revealed large agglomerates of metal particles on the fibre surface. ASAXS and TEM have shown the nanoparticles to be in the range 5–55 nm.

Super-swollen hydrogels were prepared in vitro from lignocelluloses of various origins via direct dissolving in N,N-dimethylacetamide/lithium chloride (DMAc/LiCl) followed by regeneration from solutions. The hydrogels retained a large amount of water (up to 2500 wt%) and had high porosity and specific surface areas. Superabsorbance of the hydrogels was confirmed with a wide angle X-ray scattering method. The hydrogels seem to be smart matters due to PH-dependent behavior by swelling and pH change experiments. The gelation mechanism includes spontaneous self-assembly from the solutions in DMAc/LiCl, due to the reconstruction of new hydrogen bond webs between lignocellulose chains and water. The hydrogels exhibited high stability but their morphology changed while drying due to water removal and the collapse of the H-bonds.

Abstract. Polymeric matrices with stabilized metallic nanoparticles constitute an important class of nanostructured materials, because polymer technology allows fabrication of components with various electronic, magnetic and mechanical properties. The porous cellulose matrix has been shown to be a useful support material for platinum, palladium, silver, copper and nickel nanoparticles. In the present study, nanosized cobalt particles with enhanced magnetic properties were made by chemical reduction within a microcrystalline cellulose (MCC) matrix. Two different chemical reducers, NaBH4 and NaH2PO2, were used, and the so-formed nanoparticles were characterized with X-ray absorption spectroscopy, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. These experimental techniques were used to gain insight into the effect of different synthesis routes on structural properties of the nanoparticles. Magnetic properties of the nanoparticles were studied using a vibrating sample magnetometer. Particles made via the NaBH4 reduction were amorphous Co-B or Co oxide composites with diminished ferromagnetic behaviour and particles made via the NaH2PO2 reduction were well-ordered ferromagnetic hcp cobalt nanocrystals.