This study was done to investigate the microstructures of nanocrystalline cellulose (NCC) after hydrolysis with mineral acid concentrated. The optimum NCC was achieved through acid hydrolysis and the NCC was used as a reinforcement in nitrile butadiene rubber composites. The Field Emission Scanning Microscopy (FESEM) was used to study the structures and surfaces of the NCC and composites produced. The NCC that was synthesis from microcrystalline cellulose (MCC) found to be more individual and agglomerated due to hydrogen bonding between the NCCs, the more individual NCC produced would create more surface area to be bonded with NBR as a reinforcement. More surface area of NCC was good to create physical bonding with NBR and increase mechanical performance of composites. The NCCs in NBR composite found to form agglomeration caused by different properties that exhibited by both materials. This can restrict and reduce the performance of composite produced. A combination of these materials can be used as a reinforcement but need more attention on the modification to make these materials more compatible. Further research can be done to find the best way to prevent agglomeration between these both materials.
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