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. 2022 Oct 20;8(10):677.
doi: 10.3390/gels8100677.

Novel Silica Hybrid Xerogels Prepared by Co-Condensation of TEOS and ClPhTEOS: A Chemical and Morphological Study

Guillermo Cruz-Quesada  1 , Maialen Espinal-Viguri  1 , María Victoria López-Ramón  2 , Julián J Garrido  1
Affiliations

Novel Silica Hybrid Xerogels Prepared by Co-Condensation of TEOS and ClPhTEOS: A Chemical and Morphological Study

Guillermo Cruz-Quesada et al. Gels. .

Abstract

The search for new materials with improved properties for advanced applications is, nowadays, one of the most relevant and booming fields for scientists due to the environmental and technological needs of our society. Within this demand, hybrid siliceous materials, made out of organic and inorganic species (ORMOSILs), have emerged as an alternative with endless chemical and textural possibilities by incorporating in their structure the properties of inorganic compounds (i.e., mechanical, thermal, and structural stability) in synergy with those of organic compounds (functionality and flexibility), and thus, bestowing the material with unique properties, which allow access to multiple applications. In this work, synthesis using the sol-gel method of a series of new hybrid materials prepared by the co-condensation of tetraethoxysilane (TEOS) and 4-chlorophenyltriethoxysilane (ClPhTEOS) in different molar ratios is described. The aim of the study is not only the preparation of new materials but also their characterization by means of different techniques (FT-IR, 29Si NMR, X-ray Diffraction, and N2/CO2 adsorption, among others) to obtain information on their chemical behavior and porous structure. Understanding how the chemical and textural properties of these materials are modulated with respect to the molar percentage of organic precursor will help to envisage their possible applications: From the most conventional such as catalysis, adsorption, or separation, to the most advanced in nanotechnology such as microelectronics, photoluminescence, non-linear optics, or sensorics.

Keywords: ORMOSILs; TEOS; chemical-textural properties; chlorophenyltriethoxysilane; hybrid materials; ordered structures; silica species; xerogels.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Mechanism in acidic media of (a) the first hydrolysis reaction of tetraethoxysilane (R = OEt) or triethoxysilane (R = alkyl or aryl), and (b) the co-condensation reaction of tetraethoxysilane with a triethoxysilane (R = alkyl or aryl).
Figure 2
Figure 2
FT-IR spectra (range 1600–400 cm−1) of the reference (100%TEOS) and the hybrid materials at different molar percentages of organic precursor (ClPhTEOS).
Figure 3
Figure 3
FT-IR spectra (range 1400–900 cm−1) of the reference, 15ClPh, and both phases of 20ClPh and 100ClPh.
Figure 4
Figure 4
From left to right: 4-fold ring, short ladder (SLd), open-cage (T7), and close-cage (T8).
Figure 5
Figure 5
Experimental and calculated spectra of (a) reference and (b) 100ClPh.
Figure 6
Figure 6
(a) Normalized 29Si NMR spectra of the hybrid xerogels. (b) Variation of the relative abundance of the condensed species with respect to the percentage of ClPhTEOS.
Figure 7
Figure 7
XRD diffractograms of the hybrid xerogels (reference, 1ClPh, 5ClPh, 10ClPh, and 15ClPh).
Figure 8
Figure 8
Skeletal density of the hybrid materials with respect to the percentage of ClPhTEOS.
Figure 9
Figure 9
Isotherms of the hybrid xerogels: (a) N2 (−196 °C), and (b) CO2 (0 °C).
Figure 10
Figure 10
Pore size distribution of the materials calculated from (a) N2 isotherms and (b) CO2 isotherms.
Figure 11
Figure 11
FE-SEM micrographs of: (a) 0ClPh, (b) 1ClPh, (c) 5ClPh, (d) 10ClPh, and (e) 15ClPh.
Figure 12
Figure 12
HR-TEM micrographs of (a) 0ClPh, (b) 1ClPh, (c) 5ClPh, (d) 10ClPh, and (e) 15ClPh.
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