Functional materials of high porosity and hierarchical structure, based on renewable building blocks, are highly demanded for material applications. In this regard, substantial progress has been made by functionalizing micro- and nano-sized cellulose followed by its reassembly via bottom-up approaches. However, bottom-up assembly processes are still limited in terms of upscaling and the utilization of these building blocks presupposes the disassembly of the plant feedstock inherit hierarchical cellulose scaffold. To maintain the three-dimensional structure, delignification processes from pulp and paper production were recently adapted for the treatment of bulk wood. Yet, a detailed chemical analysis and the determination of macroscopic swelling/shrinkage parameters for the scaffolds, necessary for a systematic design of cellulose scaffold based materials, are still missing. Here, acidic bleaching and soda pulping were used for producing cellulose scaffolds, for functional materials under retention of their inherent hierarchical structure. Spatially resolved chemical investigations on thin sections by Raman microscopy provided detailed information on the induced alterations at the cell wall level, revealing significant differences in dependence of the chemistry of the pre-treatment. An adaption to bulk wood samples proved the applicability of these treatments at larger scales and volumetric alterations at different atmospheric conditions indicated the effect of the altered porosity of the scaffolds on their hygroscopic behaviour.
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