Preparation of SBA-15 and Zr-SBA-15 materials by direct-synthesis and pH-adjustment methods

• Published in: Materials letters 2021-10, Vol.301, p.130326, Article 130326
• Main Authors: Colmenares-Zerpa, J., Chimentão, R.J., Gispert-Guirado, F., Peixoto, A.F., Llorca, J.
• Format: Article
• Language: English
• Subjects: High resolution electron microscopy; Incorporation; Inductively coupled plasma mass spectrometry; Mass spectrometry; Materials science; Mesoporous; Morphology; Photoelectrons; SBA-15; Silica; Silicon dioxide; Structure; Synthesis; X ray photoelectron spectroscopy; X ray powder diffraction; X-ray spectroscopy; Zirconium
• ISSN: 0167-577X; 1873-4979
• DOI: 10.1016/j.matlet.2021.130326

•SBA-15 and Zr-SBA-15 were prepared by direct-synthesis and pH-adjustment methods.•Zirconium incorporation affected the texture, morphology, and structural ordering.•The pH-adjustment method induced better elemental composition and structural order. SBA-15 mesoporous silica materials with zirconium atoms incorporated into its structure were prepared by two methods: direct-synthesis and pH-adjustment. Two nominal ratios of Zr/Si = 0 and 0.10 were evaluated. N2-physisorption, X-ray powder diffraction (XRPD) and, X-ray Photoelectron Spectroscopy (XPS) revealed that the morphology and structural order of the SBA-15 materials were greatly affected by the partial incorporation of zirconium into the SBA-15 structure as well as by the synthesis method. High-resolution transmission electron microscopy (HRTEM) of the materials prepared by pH-adjustment (SBA-15-2 and Zr-SBA-15-2 samples) revealed a more perfectly defined mesoporous structure with long-range ordering when compared with the materials obtained by direct-synthesis (SBA-15-1 and Zr-SBA-15-1 samples). The results by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and Energy-Dispersion X-ray Spectroscopy (EDX) to evaluate the elemental composition of the materials indicated a better correlation using the pH-adjustment method.