An NMR Study of Hydrogen in Si02 Films on Silicon

1989 ◽  
Vol 159 ◽  
Author(s):  
David H. Levy ◽  
K. K. Gleason

ABSTRACTWe have used solid state nuclear magnetic resonance (NMR) spectroscopy to study both “wet” and “dry” thermally grown films of SiO2 on silicon substrates. For the 5000 § wet film, grown at 1050 °C we observed a single Lorentzian line of 6 kHz HWHM (half width at half maximum). For the 500 § dry film, we observed a convolution of two lines: a) a Lorentzian of 4 kHz HWHM and b) a Gaussian of 20 kHz HWHM. The hydrogen distributions in both oxides are interpreted as a function of these lines.

2018 ◽  
Vol 11 (1) ◽  
pp. 485-508 ◽  
Author(s):  
Sharon E. Ashbrook ◽  
John M. Griffin ◽  
Karen E. Johnston

The sensitivity of nuclear magnetic resonance (NMR) spectroscopy to the local atomic-scale environment offers great potential for the characterization of a diverse range of solid materials. Despite offering more information than its solution-state counterpart, solid-state NMR has not yet achieved a similar level of recognition, owing to the anisotropic interactions that broaden the spectral lines and hinder the extraction of structural information. Here, we describe the methods available to improve the resolution of solid-state NMR spectra and the continuing research in this area. We also highlight areas of exciting new and future development, including recent interest in combining experiment with theoretical calculations, the rise of a range of polarization transfer techniques that provide significant sensitivity enhancements, and the progress of in situ measurements. We demonstrate the detailed information available when studying dynamic and disordered solids and discuss the future applications of solid-state NMR spectroscopy across the chemical sciences.


Clay Minerals ◽  
1986 ◽  
Vol 21 (5) ◽  
pp. 879-897 ◽  
Author(s):  
M. A. Wilson ◽  
S. A. McCarthy ◽  
P. M. Fredericks

AbstractThe structure of synthetic aluminosilicates prepared at pH 6 has been investigated by 29Si and 27Al high-resolution solid-state nuclear magnetic resonance (NMR) spectroscopy. Fourier transform infrared (FTIR) spectroscopy and electron microscopy have also been used to characterize the products. The amount of Si and Al in protoimogolite, disordered allophane and other structures has been measured. There is a fair correlation between the intensity of the 349 cm−1 band in the FTIR spectra and the proportion by weight of protoimogolite Si measured by NMR. It is shown that disordered allophanes have similar structures to those proposed by van Reeuwijk and de Villiers (Soil Sci. Soc. Am. Proc. 32 (1968) 238–240), i.e. octahedral Al surrounding a tetrahedral core. Moreover, it is clear that at high Al:Si ratios (⩾1:1), protoimogolite can compete with disordered allophane precursors for aluminum. The driving forces for formation of protoimogolite rather than allophane appear to be long range Al-Al repulsive forces through oxygen.


Biochemistry ◽  
2008 ◽  
Vol 47 (15) ◽  
pp. 4369-4376 ◽  
Author(s):  
Karsten Seidel ◽  
Ovidiu C. Andronesi ◽  
Joachim Krebs ◽  
Christian Griesinger ◽  
Howard S. Young ◽  
...  

2011 ◽  
Vol 34 (5-6) ◽  
pp. 153-153
Author(s):  
Libasse Diop

Abstract Solid-state and solution 117Sn nuclear magnetic resonance studies of C2O4(SnPh3)2 have been carried out and found to be in good agreement with the tetrahedral environment of the tin (IV) atom as found from the solid state structure, previously determined by a single crystal X-ray diffraction analysis.


1999 ◽  
Vol 44 (4) ◽  
pp. 14550J ◽  
Author(s):  
Garry S. H. Lee ◽  
Don C. Craig ◽  
G. S. Kamali Kannangara ◽  
Michael Dawson ◽  
Costa Conn ◽  
...  

2021 ◽  
Vol 15 (1) ◽  
pp. 108
Author(s):  
Zhongqi He ◽  
Mingxin Guo ◽  
Chanel Fortier ◽  
Xiaoyan Cao ◽  
Klaus Schmidt-Rohr

Conversion to biochar may be a value-added approach to recycle defatted cottonseed meal, a major byproduct from the cotton industry. In this work, complete slow pyrolysis at seven peak temperatures ranging from 300 to 600°C in batch reactors was implemented to process cottonseed meal into biochar products. Elemental analysis, attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy and quantitative solid state 13C nuclear magnetic resonance (NMR) spectroscopy were applied to characterize raw meal and its derived biochar products. The biochar yield and organic C and total N recoveries decreased as the peak pyrolysis temperatures was elevated. However, most of the mineral elements including P in cottonseed meal were retained during pyrolysis and became enriched in biochar as a result of the decreased mass yield. The spectral data showed that pyrolysis removed the functional groups of biopolymers in cottonseed meal, producing highly aromatic structures in biochars. With increasing pyrolysis temperature, alkyl structures decreased progressively in the biochar products and became negligible at higher temperatures (550 and 600°C). Quantitative analysis of FT IR data revealed that the values of a simple 3-band (1800,1700, and 650 cm-1)-based R reading of the biochars were linearly related to the pyrolysis temperature, and showed strong correlations with decreasing aromaticity and increasing alkyl, aliphatic C-O/N and carbonyl signal intensities in the 13C NMR spectra. Therefore, the cheaper and faster FT-IR measurement could be used as a routine conversion indicator of pyrolysis of lignocellulosic biomass instead of the more expensive and time-consuming NMR spectroscopy.


2020 ◽  
Vol 50 (1) ◽  
pp. 493-520
Author(s):  
Po-Hsiu Chien ◽  
Kent J. Griffith ◽  
Haoyu Liu ◽  
Zhehong Gan ◽  
Yan-Yan Hu

Establishing structure–property correlations is of paramount importance to materials research. The ability to selectively detect observable magnetization from transitions between quantized spin states of nuclei makes nuclear magnetic resonance (NMR) spectroscopy a powerful probe to characterize solids at the atomic level. In this article, we review recent advances in NMR techniques in six areas: spectral resolution, sensitivity, atomic correlations, ion dynamics, materials imaging, and hardware innovation. In particular, we focus on the applications of these techniques to materials research. Specific examples are given following the general introduction of each topic and technique to illustrate how they are applied. In conclusion, we suggest future directions for advanced solid-state NMR spectroscopy and imaging in interdisciplinary research.


Author(s):  
Evgeniy Papulovskiy ◽  
Aleksandr A. Shubin ◽  
Olga B. Lapina

In this work, isolated surface sites of vanadium oxide on alumina surface were modeled and compared to experimental data obtained with ⁵¹V Solid-State Nuclear Magnetic Resonance (SSNMR) spectroscopy. The geometry...


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