Spectroscopic and Thermal Studies of Polyalkoxysilanes and Silica-Chitosan Hybrid Materials

2015 ◽  
Vol 5 (1) ◽  
pp. 1 ◽  
Author(s):  
Antonio Sanchez-Fernandez ◽  
Laura Pena-Paras ◽  
Elisa M. Mendoza ◽  
Alejandra Leyva ◽  
Luis A. Bautista ◽  
...  

Polymers of organoalkoxysilanes (or polyalkoxysilanes) were synthesized through sol-gel process using different organosilanes: Tetraethylorthosilicate (TEOS), (3-Glycidyloxypropyl) trimethoxysilane (GPTMS), Trimethoxy(propyl)silane (TMPS), and/or Triethoxy(octyl)silane (EOS). Different carboxylic acids (acetic, formic, and citric) were used to prepare polyalkoxysilanes, with citric acid acting as a reactant rather than a catalyst for the sol-gel reaction. Silica-chitosan hybrid materials were synthesized reacting polyalkoxysilanes and chitosan, one of the most important and most studied natural polymers, through sol-gel process. The synthesized materials were characterized using Fourier transform infrared spectroscopy (FT-IR), thermogravimetrical analysis (TGA), differential Scanning Calorimetric (DSC) and solid-state Carbon-13 Nuclear Magnetic Resonance (solid-state   13C-NMR) spectroscopy, obtaining information on the structural properties of each modified materials. The results obtained by NMR indicate that the oxirane group of GPTMS remains in all reaction products to form different polyalkoxysilanes.

2008 ◽  
Vol 396-398 ◽  
pp. 481-484
Author(s):  
Rodrigo Jiménez-Gallegos ◽  
L. Téllez-Jurado ◽  
Luis M. Rodríguez-Lorenzo ◽  
Julio San Román

This paper focuses on the preparation of siloxane-polyurethane hybrid materials using a sol-gel method. The global aim of the project is to tailor mechanical properties, degradability rate, bioactivity and biocompatibility to design scaffolds for musculoskeletal applications. A series of seven hybrid materials were synthesized with varying the proportion of polydimethylsiloxane (PDMS), and Polyurethane (PU). The organic part ratios (by weight) employed were (% PDMS:% PU) 30:0, 35:5, 20:10, 15:15, 10:20, 5:25, and 0:30. The organic part was reacted with constant 70 % TEOS to obtain the hybrid materials. A sol-gel process was selected for the synthesis of the hybrids. The characterization of materials was carried out by the fourier-infrared spectroscopy (FT-IR), x-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electronic microscopy (SEM) and proton nuclear magnetic resonance (1H-NMR) techniques in order to analyze the structure, microstructure and chemical composition of the hybrid materials. Gelification time depends on the proportion of PU used. When no PU is employed, the gel time is 8 hours but it rises up to 18 days for 30 % of polyurethane. Materials range from opaque to translucent but with a greater fragility for greater amounts of polyurethane. No differences in the bonding of materials could be appreciated.


2000 ◽  
Vol 78 (11) ◽  
pp. 1519-1525 ◽  
Author(s):  
Jean-Philippe Bezombes ◽  
Claude Chuit ◽  
Robert JP Corriu ◽  
Catherine Reyé

The hydrolysis-polycondensation by the sol-gel process of the aromatic diphosphines (X3SiC6H4)2PC6H4P(C6H4SiX3)2, which are rigid molecules bearing four hydrolysable SiX3 groups (X = OiPr, H), leads to new organic-inorganic hybrid materials, characterized by solid state 13C, 29Si, and 31P NMR spectroscopies. The accessibility of the phosphorus centres incorporated into the xerogel obtained from the diphosphine with X = OiPr has been studied. All the phosphorus atoms reacted quantitatively with H2O2, S8, and CH3I but only 20% with the more bulky reagent W(CO)5·THF. This result is explained by the rigidity of the inorganic network resulting from the high number of hydrolysable Si-OiPr groups in the precursor.Key words : Diphosphines, sol-gel process, xerogels, solid 31P NMR.


2004 ◽  
Vol 847 ◽  
Author(s):  
Marcus Örtenblad ◽  
Stephane Parola ◽  
Frédéric Chaput ◽  
Cédric Desroches ◽  
Catherine Sigala ◽  
...  

ABSTRACTMaterials based on alkynyl platinum derivatives and thiacalixarenes were prepared through the sol-gel process The molecular species were grafted to the matrix (class II hybrid) in order to maximise the concentration and the stability of the final solid-state material Broadband optical limiting performance in the visible wavelength region was observed in the prepared materials Thermomechanical characterisation of the matrix is also discussed.


2000 ◽  
Vol 628 ◽  
Author(s):  
Guang-Way Jang ◽  
Ren-Jye Wu ◽  
Yuung-Ching Sheen ◽  
Ya-Hui Lin ◽  
Chi-Jung Chang

This work successfully prepared an UV curable organic-inorganic hybrid material consisting of organic modified colloidal silica. Applications of UV curable organic-inorganic hybrid materials include abrasion resistant coatings, photo-patternable thin films and waveguides. Colloidal silica containing reactive functional groups were also prepared by reacting organic silane and tetraethyl orthosilicate (TEOS) using sol-gel process. In addition, the efficiency of grafting organic moiety onto silica nanoparticles was investigated by applying TGA and FTIR techniques. Experimental results indicated a strong interdependence between surface modification efficiency and solution pH. Acrylate-SiO2 hybrid formation could result in a shifting of thermal degradation temperature of organic component from about 200°C to near 400°C. In addition, the stability of organic modified colloidal silica in UV curable formula and the physical properties of resulting coatings were discussed. Furthermore, the morphology of organic modified colloidal silica was investigated by performing TEM and SEM studies‥


2012 ◽  
Vol 217-219 ◽  
pp. 733-736
Author(s):  
Xiu Mei Han ◽  
Shu Ai Hao ◽  
Ying Ling Wang ◽  
Gui Fang Sun ◽  
Xi Wei Qi

Zn2SiO4:Eu3+, Dy3+ phosphors have been prepared through the sol-gel process. X-ray diffraction (XRD), thermogravimetric and ddifferential thermal analysis (TG-DTA), FT-IR spectra and photoluminescence spectra were used to characterize the resulting phosphors. The results of XRD indicated that the phosphors crystallized completely at 1000oC. In Zn2SiO4:Eu3+,Dy3+ phosphors, the Eu3+ and Dy3+ show their characteristic red(613nm, 5D0-7F2), blue (481nm, 4F9/2–6H15/2) and yellow (577nm, 4F9/2–6H13/2) emissions.


1994 ◽  
Vol 6 (1) ◽  
pp. 43-52 ◽  
Author(s):  
Yoshitake Iyoku ◽  
Masa-aki Kakimoto ◽  
Yoshio Imai

Poly(methylsilsesquixoane) network (silicone)-polyimide hybrid materials were successfully prepared by the sol-gel reaction of methyltriethoxysilane (MTES). The ethoxysilyl group in MTES was hydrolyzed and polycondensed in the solution of the polyamic acid, derived from pyromellitic dianhydride and bis(4-aminophenyl)ether, in N,N-dimethyl-acetamide (DMAc). The hybrid films were obtained by casting the reaction mixture, followed by heating up to 300°C. The hybrid materials containing 0-60wt% of silicone afforded flexible films. The films containing less than 7 wt% silicone were yellow and transparent, whereas the films with higher silicone content were yellow and opaque. Silicone particles with a diameter of around 1-10 μm were observed in the fracture surface of the hybrid films by scanning electron microscopy. Although the tensile strength and tensile modulus of the films obtained decreased with increasing silicone content. the value of the elongation at break remained at 60% up to 30% silicone content.


2022 ◽  
Author(s):  
Monika Patel ◽  
Sunita Mishra ◽  
Ruchi Verma ◽  
Deep Shikha

Abstract Nanotechnology is a completely unique branch of technology that offers with substances in a very small size between (1-100 nm) with various crystal shapes which include spherical nanoparticles, flower shaped, Nano rods, Nano ribbons, and Nano platelets. Metals have ability to produce large number of oxides. These metal oxides play an major role in many areas of chemistry, physics, material science and food science. In this research, Zinc Oxide (ZnO) and Copper (II) oxide nanoparticles were synthesized via sol-gel process using zinc nitrate and copper (II) nitrate as precursor respectively. The characterization of CuO and ZnO nanoparticles was done by using various techniques. X-ray Diffraction (XRD) indicates the crystallinity and crystal size of CuO and ZnO nanoparticle. Fourier transform infrared spectroscopy (FT-IR) was used to get the infrared spectrum of the sample indicating composition of the sample which contains various functional groups. XRD result shows the particle size of CuO at highest peak 29.40140 was 61.25 nm and the particle size of ZnO at highest peak 36.24760 was 21.82 nm. FT-IR spectra peak at 594.56 cm-1 indicated characteristic absorption bands of ZnO nanoparticles and the broad band peak at 3506.9 cm-1 can be attributed to the characteristic absorption of O-H group. The analysis of FT-IR spectrum of CuO shows peaks at 602.09, 678.39, and 730.19cm−1 which refer to the formation of CuO. A broad absorption peak noticed at 3308.2 cm−1 attributed to O–H stretching of the moisture content.


2007 ◽  
Vol 1007 ◽  
Author(s):  
Sorin Ivanovici ◽  
Christoph Rill ◽  
Claudia Feldgitscher ◽  
Guido Kickelbick

ABSTRACTHybrid materials based on polysiloxanes and metal oxides (SiO2, TiO2, ZrO2) were prepared by hydrosilation of allyl acetoacetate (AAA) modified metal alkoxides (M(OR)4; M = Ti, Zr; R = ethyl, isopropyl) or vinyl triethoxysilane with poly(dimethylsiloxane-co-hydrosiloxane) (PDMS-co-PMHS). The obtained compounds acted as single-source precursors in the sol-gel process. Various spectroscopic methods showed the complete functionalization of the polysiloxane chains with the complexes. When alcohols were used as solvents in the sol-gel process, hybrid nanoparticles were obtained, as observed by dynamic light scattering (DLS) measurements, transmission electron microscopy (TEM), and spectroscopic methods such as NMR and FT-IR.


2010 ◽  
Vol 434-435 ◽  
pp. 231-234
Author(s):  
Li Guan ◽  
Bing Bing Fan ◽  
Ming Liang Li ◽  
He Jing Wen ◽  
Kai Li ◽  
...  

SiO2-SiC composite particles were prepared using a sol-gel process. BaTiO3 powders were synthesize through solid-state reaction. They were mixed as microwave absorbents with Fe3O4 powders to obtain the complex absorption. Epoxide resin (EP) was used as matrix and solidified with the mixtures. The techniques of DSC-TG, XRD were used to characterize the composite particles and the obtained compacts. A vector network analyzer was used to measure the reflectivity of the SiO2-SiC-based composites. The effects of the aborbents’ contents on the reflection of the microwave absorption materials were disscussed. It was found that SiO2-SiC composites could be prepared using sol-gel process and BaTiO3 powders could be synthesize through solid-state reaction. The results indicated that SiO2-SiC composite is contribute to absorb microwave, where SiO2-SiC: BaTiO3: Fe3O4 = 6:2:2 (vol %), the frequency region in which the maximum reflectivity is more than -10 dB is 5.4-7.6 GHz.


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