Er3+ Doped Silica Glass by Sol-Gel Processing with Organic Complexation

1999 ◽  
Vol 560 ◽  
Author(s):  
Xiuhong Han ◽  
Guozhong Cao ◽  
Tom Pratum
Keyword(s):  
Silica Glass ◽  
Sol Gel ◽  
Magic Angle Spinning ◽  
Complexing Agent ◽  
Magic Angle ◽  
Silica Network ◽  
Organic Complexation ◽  
Angle Spinning ◽  
High Level ◽  
Gel Processing

ABSTRACTEr3+-doped silica glass (up to 10 wt%) was synthesized by sol-gel processing with the addition of 3- aminopropyl trimethoxysilane (APS) as a complexing agent. Er3+ ions reacted with amino groups and, thus, linked to the silica network during the sol preparation. As a result, the motion of Er3+ ions was restricted and the formation of Er3+ clusters was inhibited. Both fluorescence spectra and magic-angle spinning (MAS) nuclear magnetic resonance (NMR) indicated that the addition of the complexing agent APS resulted in a homogeneous dispersion of high-level Er+3 doping in the resultant gels. After the removal of organic components, however, Er+3 clustering occurs when firing at a high temperature for a long period of time, e.g. at 1000°C for 10 hrs, due to enhanced Er3+ diffusion.

scholarly journals Chemical and Structural Characterization of Amorphous and Crystalline Alumina Obtained by Alternative Sol–Gel Preparation Routes

Materials ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1761
Author(s):  
Izabela Rutkowska ◽  
Jakub Marchewka ◽  
Piotr Jeleń ◽  
Mateusz Odziomek ◽  
Mateusz Korpyś ◽  
...  
Keyword(s):  
Infrared Spectroscopy ◽  
Aluminum Oxide ◽  
Physicochemical Properties ◽  
Sol Gel ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Bet Method ◽  
Gel Preparation ◽  
Angle Spinning ◽  
Middle Infrared

Aluminum oxide is one of the most commonly used materials in the industry. It is used in the field of catalysis, refractories, and optics. Despite the fact that there are many techniques available, there is still a great challenge in obtaining a material with desired and designed properties. Nevertheless, there is a great flexibility in making customized alumina materials with desired physicochemical properties synthesized by sol–gel methods. This work consists in characterizing the physicochemical properties of sol–gel synthesized aluminum oxide using different sol–gel preparation routes. Three different sols were obtained by using organic precursors and underwent thermal treatment. The structure (Middle Infrared Spectroscopy, Diffused Reflectance Infrared Spectroscopy, X-ray Diffraction, Magic Angle Spinning Nuclear Magnetic Resonance) and microstructure (Scanning Electron Microscopy with Electron Dispersive Spectroscopy) tests of the materials were carried out. The specific surface area was determined by using the Brunauer–Emmett–Teller (BET) method. Thermal analysis was performed for all the powders, in order to analyze the specific temperature of materials transformation.

scholarly journals New Condensation Polymer Precursors Containing Consecutive Silicon Atoms—Decaisopropoxycyclopentasilane and Dodecaethoxyneopentasilane—And Their Sol–Gel Polymerization

Polymers ◽  
2019 ◽  
Vol 11 (5) ◽  
pp. 841
Author(s):  
Sung Jin Park ◽  
Myong Euy Lee ◽  
Hyeon Mo Cho ◽  
Sangdeok Shim
Keyword(s):  
Solid State ◽  
Sol Gel ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Cross Polarization ◽  
Reaction Conditions ◽  
Polymer Precursors ◽  
Sol Gel Process ◽  
Angle Spinning ◽  
Magnetic Resonances

The sol–gel polymerization of alkoxysilanes is a convenient and widely used method for the synthesis of silicon polymers and silicon–organic composites. The development of new sol–gel precursors is very important for obtaining new types of sol–gel products. New condensation polymer precursors containing consecutive silicon atoms—decaisopropoxycyclopentasilane (CPS) and dodecaethoxyneopentasilane (NPS)—were synthesized for the preparation of polysilane–polysiloxane material. The CPS and NPS xerogels were prepared by the sol–gel polymerization of CPS and NPS under three reaction conditions (acidic, basic and neutral). The CPS and NPS xerogels were characterized using N2 physisorption measurements (Brunauer–Emmett–Teller; BET and Brunauer-Joyner-Halenda; BJH), solid-state CP/MAS (cross-polarization/magic angle spinning) NMRs (nuclear magnetic resonances), TEM, and SEM. Their porosity and morphology were strongly affected by the structure of the precursors, and partial oxidative cleavage of Si-Si bonds occurred during the sol–gel process. The new condensation polymer precursors are expected to expand the choice of approaches for new polysilane–polysiloxane.

scholarly journals Hydrocracking of Polyethylene to Jet Fuel Range Hydrocarbons over Bifunctional Catalysts Containing Pt- and Al-Modified MCM-48

Reactions ◽  
2020 ◽  
Vol 1 (2) ◽  
pp. 195-209
Author(s):  
Yanyong Liu
Keyword(s):  
Mesoporous Silica ◽  
Sol Gel ◽  
Mesoporous Structure ◽  
Jet Fuel ◽  
Magic Angle Spinning ◽  
High Yield ◽  
Magic Angle ◽  
Surface Areas ◽  
Angle Spinning ◽  
Post Modification

A low-density polyethylene was hydrocracked to liquid hydrocarbons in autoclave reactors over catalysts containing Pt- and Al-modified MCM-48. Two kinds of Al-modified MCM-48 were synthesized for the reaction: Al-MCM-48 was synthesized using a sol–gel method by mixing Al(iso-OC3H7)3 with Si(OC2H5)4 and surfactant in a basic aqueous solution before hydrothermal synthesis, and Al/MCM-48 was synthesized using a post-modification method by grafting Al3+ ions on the surface of calcined Al/MCM-48. X-ray diffraction (XRD) patterns indicated that both Al-MCM-48 and Al/MCM-48 had a cubic mesoporous structure. The Brunauer–Emmett–Teller (BET) surface areas of Al-MCM-48 and Al/MCM-48 were larger than 1000 m2/g. 27Al Magic Angle Spinning-NMR (MAS NMR) indicated that Al3+ in Al-MCM-48 was located inside the framework of mesoporous silica, but Al3+ in Al/MCM-48 was located outside the framework of mesoporous silica. The results of ammonia temperature-programmed desorption (NH3-TPD) showed that the acidic strength of various samples was in the order of H-Y > Al/MCM-48 > Al-MCM-48 > MCM-48. After 4 MPa H2 was charged in the autoclave at room temperature, 1 wt % Pt/Al/MCM-48 catalyst showed a high yield of C9−C15 jet fuel range hydrocarbons of 85.9% in the hydrocracking of polyethylene at 573 K for 4 h. Compared with the reaction results of Pt/Al/MCM-48, the yield of light hydrocarbons (C1−C8) increased over Pt/H-Y, and the yield of heavy hydrocarbons (C16−C21) increased over Pt/Al-MCM-48 in the hydrocracking of polyethylene. The yield of C9−C15 jet fuel range hydrocarbons over the used catalyst did not decrease compared to the fresh catalyst in the hydrocracking of polyethylene to jet fuel range hydrocarbons over Pt/Al/MCM-48.

Chemical Durability Studies of Waste-Simulant Doped Borosilicate Glasses

2003 ◽  
Vol 807 ◽  
Author(s):  
Adam Duddridge ◽  
Moinul Islam ◽  
Diane Holland ◽  
Charlie R. Scales
Keyword(s):  
Test Procedure ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Borosilicate Glasses ◽  
Nmr Studies ◽  
Mixed Alkali ◽  
Trivalent Cations ◽  
High Level Nuclear Waste ◽  
Angle Spinning ◽  
High Level

ABSTRACTA mixed-alkali modified borosilicate base glass used in the vitrification of high-level nuclear waste (HLW) has been doped with a number of waste simulants to between 2 and 12 mol%. The simulants have been chosen to give two distinct series of glasses: one consisting of trivalent ions having the form M2O3(where M is La, Bi, Al or Fe) and the other consisting of divalent simulants of the form MO (where M is Pb, Zn or Ba). An international standard Soxhlet leach test procedure was performed on each glass to study the effect of prolonged, moderate-temperature, dynamic water corrosion. Results of these studies show that, except for BaO, as the amount of simulant is increased, the amount of Na and Li leached decreases showing them to become more chemically resistant. These corrosion tests have been correlated to ionic (D.C.) conductivity measurements, which show a decrease in the conductivity of the glass as the amount of waste simulant is increased, and 11B magic-angle spinning nuclear magnetic resonance (MAS-NMR) studies, which have shown that, as more waste-simulant is loaded into the glasses the rate of conversion of [BO4] to [BO3] units increases. All of the data from these studies reflect the different network forming abilities of the divalent and trivalent cations.

Interfaces Involving Biomolecules and Inorganic Materials: a Solid State NMR Approach

2007 ◽  
Vol 1008 ◽  
Author(s):  
Christian Bonhomme ◽  
Geoffrey Hartmeyer ◽  
Florence Babonneau ◽  
Michel Wong Chi Man ◽  
Guilhem Arrachart ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Chemical Nature ◽  
Sol Gel ◽  
Magic Angle Spinning ◽  
Inorganic Materials ◽  
Double Quantum ◽  
Magic Angle ◽  
Angle Spinning ◽  
Very High

AbstractMaterials based on ureidopyrimidinone (UPY) dimers and Adenine (A) / Thymine (T) derivatives were synthesized and characterized by advanced solid state NMR (Nuclear Magnetic Resonance) techniques. Silylated UPY molecules were used as model compounds, leading to structured organic-inorganic materials after hydrolysis and condensation processes (sol-gel reactions). High resolution 1H solid state NMR has been extensively used for the in-depth description of the H-bond networks, including very fast MAS (Magic Angle Spinning) experiments at very high field and DQ (double quantum) recoupling experiments. The chemical nature of the organic-inorganic interface has been illuminated by such techniques. In, particular, it has been demonstrated that H-bond networks were preserved during sol-gel reactions and were comparable to those observed in the UPY crystalline precursors.

scholarly journals 14N, 13C, and 119Sn solid-state NMR characterization of tin(II) carbodiimide Sn(NCN)

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Aleksander Jaworski ◽  
Jędrzej Piątek ◽  
Liuda Mereacre ◽  
Cordula Braun ◽  
Adam Slabon
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Chemical Shifts ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Quadrupolar Coupling ◽  
Nmr Study ◽  
Nmr Characterization ◽  
Angle Spinning ◽  
High Level

Abstract We report the first magic-angle spinning (MAS) nuclear magnetic resonance (NMR) study on Sn(NCN). In this compound the spatially elongated (NCN)2− ion is assumed to develop two distinct forms: either cyanamide (N≡C–N2−) or carbodiimide (−N=C=N−). Our 14N MAS NMR results reveal that in Sn(NCN) the (NCN)2− groups exist exclusively in the form of symmetric carbodiimide ions with two equivalent nitrogen sites, which is in agreement with the X-ray diffraction data. The 14N quadrupolar coupling constant | C Q | $\vert {C}_{\text{Q}}\vert $  ≈ 1.1 MHz for the −N=C=N− ion in Sn(NCN) is low when compared to those observed in molecular compounds that comprise cyano-type N≡C– moieties ( | C Q | $\vert {C}_{\text{Q}}\vert $  > 3.5 MHz). This together with the information from 14N and 13C chemical shifts indicates that solid-state NMR is a powerful tool for providing atomic-level insights into anion species present in these compounds. The experimental NMR results are corroborated by high-level calculations with quantum chemistry methods.

Sol-gel synthesis of a nanoparticulate aluminosilicate precursor for homogeneous mullite ceramics

2006 ◽  
Vol 21 (5) ◽  
pp. 1279-1285 ◽  
Author(s):  
Jarkko Leivo ◽  
Mika Lindén ◽  
Cilâine V. Teixeira ◽  
Janne Puputti ◽  
Jessica Rosenholm ◽  
...  
Keyword(s):  
Spinel Phase ◽  
Sol Gel ◽  
Magic Angle Spinning ◽  
Resonance Spectroscopy ◽  
Magic Angle ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Density ◽  
Angle Spinning ◽  
Sol Gel Synthesis

An amorphous nanoparticulate aluminosilicate 3/2-mullite precursor has been synthesized and carefully characterized. The sol contained 2-nm particles of Q3(3Al) silica species together with six-coordinated alumina, which suggested an allophane-like structure of the nanoparticles. The sol remained stable for years, and formed an easily redispersible physical gel upon solvent evaporation. The gel crystallized to mullite at temperatures below 1000 °C, without going through any intermediate spinel phase. Thus, the nanoparticulate precursor is regarded as a homogeneous high-purity mullite precursor with a high Si–O–Al bond density, which is useful in the preparation of various nanostructured Al-rich aluminosilicate materials. The sols and gels were characterized by small-angle x-ray scattering, dynamic light scattering, x-ray diffraction, 27Al and 29Si magic-angle spinning (MAS) nuclear magnetic resonance spectroscopy, and differential thermal analysis.

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