Lignocellulosic biomass is a cheap raw material that, thanks to its high carbohydrate content, can be used in fermentation to produce biofuels, biogas and other compounds. Its complex structure, including cellulose, hemicellulose and lignin, requires prior treatment of the biomass to facilitate hydrolysis to simple sugars. Today, biomass is only partially utilized and generates about 14% of the world's energy. This is because the most commonly used physical, chemical and physicochemical treatments are not sustainable. They are energy-consuming but still low in productivity and toxic inhibitors formed during these treatments could hinder later steps of fermentation. Biomass treatment with advanced oxidation techniques has great potential as an environmentally friendly, so-called "green" treatment. These processes generate reactive species (radicals, electrons, ions and peroxides) that attack cellulose, hemicellulose, and lignin components. In this work, the effects of non-thermal plasma, the Fenton process, and the combined treatment of corn stalks with non-thermal plasma/Fenton were compared. Grounded biomass of corn stalks was mixed with Fenton reagent and hydrogen peroxide at different ratios and subjected to non-thermal plasma treatment. Carbohydrate content was decreased in non-thermal plasma treated samples both with and without Fe2+. However, a specific biomass: Fe2+:H2O2 ratio was required to achieve the highest rate of lignocellulose decomposition. The cellulose and hemicellulose fractions were affected and reduced by the treatments studied but resulted in almost no changes in the cellulose crystallinity index. The lower lignin content and cellulose crystallinity allow for more efficient enzyme hydrolysis of the treated lignocellulose and new options for valorization in fermentations.