Lignocellulosic fibres are attractive materials that can replace traditional fossil-based alternatives due to their superior mechanical, thermal, and chemical properties. These fibers are biological materials precisely organized from the nano to the macroscale to fulfill their biological functions, providing stability and strength against mechanical and osmotic stress to plant cells. However, the production of lignocellulosic fibers typically involves harsh chemical processes for their extraction from woody feedstock, degrading the lignin. This results in a combined loss of carbohydrates, hemicellulose in particular, that could be used for diverse applications. E.g. Hemicelluloses can enhance the bonding between cellulose fibrils, improving the mechanical properties of cellulose fibrillar networks. In this context, wood-based holocellulose fibres retaining most of the hemicellulose around the cellulose fibrillar structure, emerge as a high-quality sustainable building block. Amongst delignification methods, peracetic acid (PAA) has been demonstrated to show high selectivity towards lignin removal. In this work, we aim to produce holocellulose fibers with high hemicellulose content via PAA treatment, by optimizing temperature and pH condition, and comparing the compositional and structural properties of the derived holocellulose materials, including hemicellulose content, delignification efficiency, and fiber morphology to determine optimal conditions.