scholarly journals Experimental Investigation on the Mass Diffusion Behaviors of Calcium Oxide and Carbon in the Solid-State Synthesis of Calcium Carbide by Microwave Heating

Molecules ◽  
2021 ◽  
Vol 26 (9) ◽  
pp. 2568
Author(s):  
Miao Li ◽  
Siyuan Chen ◽  
Huan Dai ◽  
Hong Zhao ◽  
Biao Jiang
Keyword(s):  
Solid State ◽  
Microwave Heating ◽  
Calcium Oxide ◽  
Photoelectron Spectroscopy ◽  
Inductively Coupled Plasma ◽  
Calcium Carbide ◽  
Solid State Synthesis ◽  
Carbide Formation ◽  
X Ray ◽  
Diffusion Behaviors

Microwave (MW) heating was proven to efficiently solid-synthesize calcium carbide at 1750 °C, which was about 400 °C lower than electric heating. This study focused on the investigation of the diffusion behaviors of graphite and calcium oxide during the solid-state synthesis of calcium carbide by microwave heating and compared them with these heated by the conventional method. The phase compositions and morphologies of CaO and C pellets before and after heating were carefully characterized by inductively coupled plasma spectrograph (ICP), thermo gravimetric (TG) analyses, X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). The experimental results showed that in both thermal fields, Ca and C inter-diffused at a lower temperature, but at a higher temperature, the formed calcium carbide crystals would have a negative effect on Ca diffusion to carbon. The significant enhancement of MW heating on carbon diffusion, thus on the more efficient synthesis of calcium carbide, manifested that MW heating would be a promising way for calcium carbide production, and that a sufficient enough carbon material, instead of CaO, was beneficial for calcium carbide formation in MW reactors.

scholarly journals Intercalation of calcein into layered silicate magadiite and their optical properties

2017 ◽  
Vol 4 (11) ◽  
pp. 171258 ◽  
Author(s):  
Shengnan Gao ◽  
Jiang Zhu ◽  
Yifu Zhang ◽  
Qiushi Wang ◽  
Xuyang Jing ◽  
...  
Keyword(s):  
Solid State ◽  
Photoelectron Spectroscopy ◽  
Inductively Coupled Plasma ◽  
Thermo Gravimetric Analysis ◽  
Layered Silicate ◽  
Atomic Emission ◽  
Fluorescence Properties ◽  
Gravimetric Analysis ◽  
X Ray ◽  
Metal Organic

Calcein–Ca (II), Zn (II) and Al (III) complexes were successfully intercalated into interlayer surfaces of layered silicate magadiite and fluorescence properties of organic metal-chelates in the confined spaces were investigated. Structures, compositions and morphologies of the intercalated magadiites were adequately studied by tests, including X-ray diffraction, energy-dispersive X-ray spectrometer, elemental mapping, X-ray photoelectron spectroscopy, inductively coupled plasma atomic emission spectroscopy, Fourier-transform infrared spectra, ultraviolet–visible spectroscopy, thermo-gravimetric analysis, differential thermal analysis and scanning electron microscopy. Results confirmed that metal–organic chelate species were immobilized onto the silicate sheets via solid-state interaction. Basal spacings between silicate layers decreased by exchanged metal ions and increased after intercalation of calcein into the interlayer spaces of cation-exchanged magadiites. The encapsulation was obtained by a flexible solid–solid reaction, and the present reaction and products had a potential of application to industrial uses. A speculative mechanism was proposed for reaction by solid-state intercalation. Furthermore, it was found that the complexes in the interlayer space also exhibited special fluorescence properties. The significance of this current work was that it provided a possible route for synthesizing metal–organic complexes that encapsulated in phyllosilicate.

Solid state synthesis of LiFePO4 studied by in situ high energy X-ray diffraction

2011 ◽  
Vol 21 (15) ◽  
pp. 5604 ◽  
Author(s):  
Zonghai Chen ◽  
Yang Ren ◽  
Yan Qin ◽  
Huiming Wu ◽  
Shengqian Ma ◽  
...  
Keyword(s):  
Solid State ◽  
High Energy ◽  
Solid State Synthesis ◽  
X Ray Diffraction ◽  
X Ray

29Si NMR and XPS Investigation of the Structure of Silicon Oxycarbide Glasses Derived from Polysiloxane Precursors

1994 ◽  
Vol 346 ◽  
Author(s):  
R.J.P. Corriu ◽  
D. Leclercq ◽  
P.H. Mutin ◽  
A. Vioux
Keyword(s):  
Solid State ◽  
Photoelectron Spectroscopy ◽  
Solid State Nmr ◽  
Random Distribution ◽  
Silicon Oxycarbide ◽  
29Si Nmr ◽  
Xps Spectra ◽  
Excess Carbon ◽  
X Ray ◽  
Silicon Oxycarbide Glasses

ABSTRACTTwo silicon oxycarbide glasses with different compositions (O/Si ratio 1.2 and 1.8) were prepared by pyrolysis at moderate temperature (900 °C) of polysiloxane precursors. Their structure was investigated using quantitative 29Si solid-state NMR and X-ray photoelectron spectroscopy (XPS). The environment of the silicon atoms in the oxycarbide phase corresponded to a purely random distribution of Si-O and Si-C bonds depending on the O/Si ratio of the glass only and not on the structure of the precursors. At the light of the NMR results, the Si2p XPS spectra of the glasses may be interpreted using the contribution of the five possible SiOxC4-x tetrahedra. The Cls spectra of these glasses indicated the presence of oxycarbide carbon in CSi4 tetrahedra, similar to carbide carbon, and graphitic-like excess carbon.

Structural and Catalytic Properties of the Alkali Metal Ion-Exchanged Y-Zeolites by 29Si and 27Al Solid-State NMR and FT-IR Spectroscopy

2005 ◽  
Vol 277-279 ◽  
pp. 708-719
Author(s):  
Chang Seop Lee ◽  
Hee Jung Lee ◽  
Sung Woo Choi ◽  
Jahun Kwak ◽  
Charles H.F. Peden
Keyword(s):  
Solid State ◽  
Alkali Metal ◽  
Photoelectron Spectroscopy ◽  
Metal Ion ◽  
Nmr Spectra ◽  
Catalytic Properties ◽  
Nox Reduction ◽  
29Si Nmr ◽  
Y Zeolites ◽  
X Ray

A series of cation exchanged Y-zeolites were prepared by exchanging cations with various alkali (M+, M= Li, Na, K, Cs) metals. The structural and catalytic properties of the alkali metal exchanged Y-zeolites have been investigated by a number of analytical techniques. Comparative elemental analyses were determined by an Energy Dispersive Spectroscopy X-ray (EDS), X-ray Photoelectron Spectroscopy (XPS), Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) and X-ray Fluorescence (XRF) before and after cation substitution. The framework and non-framework Al coordination and the Si/Al ratios of the Y-zeolites were investigated by MAS Solid-State Nuclear Magnetic Resonance (NMR) spectroscopy. The Al NMR spectra were characterized by two 27Al resonance signals at 12 and 59 ppm, indicating the presence of the non-framework and framework Al respectively. The intensities of these resonances were used to monitor the amount of the framework and non-framework Al species in the series of exchanged zeolites. The 29Si NMR spectra were characterized by four resonance signals at -79, -84, -90, and -95 ppm. Changing the alkali metal cations in the exchanged Y-zeolites significantly altered the extent of the octahedral/tetrahedral coordination and the Si/Al ratio. The Fourier Transform Infrared spectra of the CO2 adsorbed on to the exchanged Y-zeolites showed a low frequency shift, as the atomic number of the exchanged alkali metal increased. In addition, the catalytic activity of these samples for NOx reduction were tested in combination with a non-thermal plasma technique and interpreted based on the above structural and spectroscopic information.

X-ray scintillator Gd2O2S:Tb3+ materials obtained by a rapid and cost-effective microwave-assisted solid-state synthesis

2019 ◽  
Vol 777 ◽  
pp. 638-645 ◽  
Author(s):  
Ian Pompermayer Machado ◽  
Verônica Carvalho Teixeira ◽  
Cássio Cardoso Santos Pedroso ◽  
Hermi Felinto Brito ◽  
Lucas Carvalho Veloso Rodrigues
Keyword(s):  
Solid State ◽  
Cost Effective ◽  
Solid State Synthesis ◽  
X Ray ◽  
Microwave Assisted

scholarly journals The effect of cobalt on morphology, structure, and ORR activity of electrospun carbon fibre mats in aqueous alkaline environments

2021 ◽  
Vol 12 ◽  
pp. 1173-1186
Author(s):  
Markus Gehring ◽  
Tobias Kutsch ◽  
Osmane Camara ◽  
Alexandre Merlen ◽  
Hermann Tempel ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Inductively Coupled Plasma ◽  
Elevated Temperatures ◽  
Current Collector ◽  
Alkaline Media ◽  
Emission Spectrometry ◽  
Free Standing ◽  
X Ray ◽  
Turbostratic Carbon ◽  
Current Densities

An innovative approach for the design of air electrodes for metal–air batteries are free-standing scaffolds made of electrospun polyacrylonitrile fibres. In this study, cobalt-decorated fibres are prepared, and the influence of carbonisation temperature on the resulting particle decoration, as well as on fibre structure and morphology is discussed. Scanning electron microscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, elemental analysis, and inductively coupled plasma optical emission spectrometry are used for characterisation. The modified fibre system is compared to a benchmark system without cobalt additives. Cobalt is known to catalyse the formation of graphite in carbonaceous materials at elevated temperatures. As a result of cobalt migration in the material the resulting overall morphology is that of turbostratic carbon. Nitrogen removal and nitrogen-type distribution are enhanced by the cobalt additives. At lower carbonisation temperatures cobalt is distributed over the surface of the fibres, whereas at high carbonisation temperatures it forms particles with diameters up to 300 nm. Free-standing, current-collector-free electrodes assembled from carbonised cobalt-decorated fibre mats display promising performance for the oxygen reduction reaction in aqueous alkaline media. High current densities at an overpotential of 100 mV and low overpotentials at current densities of 333 μA·cm−2 were found for all electrodes made from cobalt-decorated fibre mats carbonised at temperatures between 800 and 1000 °C.

scholarly journals Towards chemically neutral carbon cleaning processes: plasma cleaning of Ni, Rh and Al reflective optical coatings and thin Al filters for free-electron lasers and synchrotron beamline applications

2018 ◽  
Vol 25 (6) ◽  
pp. 1642-1649 ◽  
Author(s):  
Harol Moreno Fernández ◽  
Marco Zangrando ◽  
Guillaume Sauthier ◽  
Alejandro R. Goñi ◽  
Vincent Carlino ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Free Electron ◽  
Inductively Coupled Plasma ◽  
High Performance ◽  
Extreme Ultraviolet ◽  
Filter Material ◽  
Gas Mixture ◽  
Carbon Contamination ◽  
X Ray ◽  
Chemical Surface

The choice of a reflective optical coating or filter material has to be adapted to the intended field of application. This is mainly determined by the required photon energy range or by the required reflection angle. Among various materials, nickel and rhodium are common materials used as reflective coatings for (soft) X-ray mirrors. Similarly, aluminium is one of the most commonly used materials for extreme ultraviolet and soft X-ray transmission filters. However, both of these types of optics are subject to carbon contamination, which can be increasingly problematic for the operation of the high-performance free-electron laser and synchrotron beamlines. As an attempt to remove this type of contamination, an inductively coupled plasma source has been used in conjunction with N2/O2/H2 and N2/H2 feedstock gas plasmas. Results from the chemical surface analysis of the above materials before and after plasma treatment using X-ray photoelectron spectroscopy are reported. It is concluded that a favorable combination of an N2/H2 plasma feedstock gas mixture leads to the best chemical surface preservation of Ni, Rh and Al while removing the carbon contamination. However, this feedstock gas mixture does not remove C contamination as rapidly as, for example, an N2/O2/H2 plasma which induces the surface formation of NiO and NiOOH in Ni and RhOOH in Rh foils. As an applied case, the successful carbon removal from ultrathin Al filters previously used at the FERMI FEL1 using an N2/H2 plasma is demonstrated.

Surface Characterization of W/Ni/Al2O3 Catalysts

1997 ◽  
Vol 497 ◽  
Author(s):  
M. H. Jordão ◽  
J. M. Assaf ◽  
P. A. P. Nascente
Keyword(s):  
Photoelectron Spectroscopy ◽  
Inductively Coupled Plasma ◽  
Surface Characterization ◽  
Nickel Content ◽  
Stable Phase ◽  
Preparation Methods ◽  
X Ray ◽  
Inductively Coupled ◽  
Temperature Programmed ◽  
Two Phases

ABSTRACTCatalysts containing tungsten and nickel oxides are important in hydrodesulfurization (HDS), hydrogénation (HY), and steam reforming of hydrocarbons. A series of W/Ni/Al2O3 catalysts was prepared by two different methods: (1) coprecipitation of nickel and aluminium hydroxicarbonate from their nitrates, followed by calcination and impregnation of tungsten; (2) precipitation of boehmite from aluminium nitrate, followed by impregnations of nickel, firstly, and tungsten. The nickel content was kept constant, while the amount of tungsten varied from 2.5 to 15.5 wt-%. The resulting oxides were characterized by inductively coupled plasma spectroscopy (ICP), atomic absorption spectroscopy (AAS), X-ray diffraction (XRD), temperature programmed reduction (TPR), and X-ray photoelectron spectroscopy (XPS). ICP and AAS were used to determine the W, Ni, and Al concentrations. XRD detected two phases: NiO and NiAl2O4 (no phase containing metallic tungsten was detected). Increasing the amount of W, the quantity of NiAl2O4 rose, the quantity of NiO decreased, and the particle size of NiO enlarged. The TPR profiles presented three peaks: one at about 1000 °C, associated to a very stable phase; for the samples prepared by coprecipitation, the other two peaks corresponded to “free NiO” and a nonstoichiometric aluminate. For the samples prepared by impregnation, those peaks corresponded to NiO and NiAl2O4. XPS identified Al2O3, NiAl2O4, and Al2(WO4)3 for both preparation methods. Increasing the amount of tungsten in the impregnated samples, NiWO4 was also observed.

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