Novel polyether–inorganic hybrid mesoporous silica synthesized through in situ incorporation of organic functionality Mahasweta Nandi a , Nawal Kishor Mal b , Asim Bhaumik a, * a Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032, India b Dynamic Materials Research Group, National Institute of Advance Industrial Science and Technology, Ikeda, Osaka 563-8577, Japan Received 23 March 2006 Available online 29 September 2006 Abstract A new polyether–inorganic hybrid mesoporous silica has been synthesized through in situ incorporation of hydroquinone (HQ) moi- ety bridging between two silica units using tetraethyl orthosilicate (TEOS) as silica source in the presence of the self assembly of cationic surfactant under acidic pH. Samples synthesized with TEOS:HQ mole ratio of 2.0 and 4.0 showed good organic loading, mesoporosity and stability. Decreasing this ratio to 1.0 resulted in a organic-rich mesoporous hybrid material, which collapsed during template removal, whereas, increasing this ratio to 8.0 resulted in very poor incorporation of hydroquinone in the mesoporous silica. XRD and N 2 sorption data suggested the mesopore structure. TEM images indicated the wormhole like structure of these mesoporous samples. Solid state NMR data suggested the existence of (–O–C 6 H 4 –O) 2 Si * (OSi) 2 and (–O–C 6 H 4 –O)Si * (OSi) 3 sites in addition to (Si * (OSi) 4 ) sites. UV–Visible and FT-IR data suggested the incorporation of hydroquinone species and Si–O–Ph bonding in the samples. Ó 2006 Elsevier B.V. All rights reserved. PACS: 81.05.Rm; 81.20.Fw; 82.33.Pt; 82.70.Uv Keywords: Porosity; Polymers and organics; Organic–inorganic hybrids; Adsorption 1. Introduction Zeolites and related microporous and mesoporous mate- rials [1,2] are widely used in academia and industry because of their practical applications in size- and shape-selective catalysis, ion-exchanger, adsorbent, supports, films and separation utilizing its well-defined pores, channels and cavities. Design and synthesis of zeolite-like framework materials with specific structures and functions are thus important. Rational design of these porous materials using the organic linkers to build open framework materials as well as the use of different structure directing agents have received much attention to explore their potential applica- tions [3–6]. Thus the syntheses of organic–inorganic hybrid mesoporous materials with new framework structures are highly desirable [7–14]. Furthermore, these mesoporous materials can be capable for selective sorption of a certain gas, which could be useful in sensing and separating the gases from their mixture depending upon the nature of organic functionality. Many inorganic metal cations viz. Ti 4+ ,V 5+ , Sn 4+ , Zr 4+ , Ga 3+ , In 3+ , Fe 3+ , Co 3+ , etc. have been incorporated into the mesoporous silica material and these materials showed interesting catalytic [15,16], optical [17] and magnetic [18] properties. However, there is no report on the incorporation of organic species into the mesoporous silica material without using the organo- silica precursors. Organosilica precursors, both alkyltrialk- oxysilanes as well as bridging organosilanes are extensively used to improve the hydrophobicity [19] of mesoporous silica material, as hydrophilic Si–OH groups in these mate- rials are detrimental to their applicability to liquid phase partial oxidation reactions in the presence of water. 0022-3093/$ - see front matter Ó 2006 Elsevier B.V. All rights reserved. doi:10.1016/j.jnoncrysol.2006.08.020 * Corresponding author. E-mail address: msab@mahendra.iacs.res.in (A. Bhaumik). www.elsevier.com/locate/jnoncrysol Journal of Non-Crystalline Solids 352 (2006) 5408–5412