AbstractEffects of dual-treatment on cellulose fiber quality, micro-structure appearance, crystalline structure, hydrogen bonds, and surface elements were analyzed using a fiber quality analyzer (FQA), scanning electron microscope (SEM), wide-angle X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS), respectively. In comparison to the untreated pulp, the brightness of pulp increased by 51.71%, whereas the apparent density and burst strength index of the pulpboard decreased by 11.76% and 48.18%, respectively. The absorption time, absorbability, and bulk of the fiber obtained by defibering the pulpboard decreased by 47.40%, 8.33%, and 5.32%, respectively, when it had been subjected to supplementary alkali. With the analysis of FQA and SEM, fiber swelled and curled, its surface was relatively smooth, and filaments of its partial surface area were exposed as a result of the supplementary alkali. Additionally, XRD analysis, FT-IR analysis, and XPS scanning spectra all showed that the crystallinity degree of fiber decreased by 45.10%, indicating more crystal structures were converted into amorphous structures. The proportion of total intra-molecular hydrogen bond intensity to total hydrogen bonds increased. The –OH content on fiber surface only decreased by 4.15%, compared with those of the untreated pulp, when the fiber was subjected to the two-step chemical treatment.