scholarly journals Chlorination of Carbon Nanotubes Obtained on the Different Metal Catalysts

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Iwona Pełech ◽  
Robert Pełech ◽  
Urszula Narkiewicz ◽  
Dariusz Moszyński ◽  
Anna Jędrzejewska ◽  
...  

In this paper, a chlorination method is proposed for simultaneous purification and functionalization of carbon nanotubes, thus increasing their ability to use. Carbon nanotubes were obtained by CVD method through ethylene decomposition on the nanocrystalline iron or cobalt or bimetallic iron-cobalt catalysts. The effects of temperature (50, 250, and 450°C) in the case of carbon nanotubes obtained on the Fe-Co catalyst and type of catalyst (Fe, Co, Fe/Co) on the effectiveness of the treatment and functionalization were tested. The phase composition of the samples was determined using the X-ray diffraction method. The quantitative analysis of metal impurity content was validated by means of the thermogravimetric analysis. Using X-ray Photoelectron Spectroscopy (XPS), Energy Dispersive Spectroscopy (EDS) analysis, and also Mohr titration method, the presence of chlorine species on the surface of chlorinated samples was confirmed.

2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Durga Sankar Vavilapalli ◽  
Ambrose A. Melvin ◽  
F. Bellarmine ◽  
Ramanjaneyulu Mannam ◽  
Srihari Velaga ◽  
...  

AbstractIdeal sillenite type Bi12FeO20 (BFO) micron sized single crystals have been successfully grown via inexpensive hydrothermal method. The refined single crystal X-ray diffraction data reveals cubic Bi12FeO20 structure with single crystal parameters. Occurrence of rare Fe4+ state is identified via X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS). The lattice parameter (a) and corresponding molar volume (Vm) of Bi12FeO20 have been measured in the temperature range of 30–700 °C by the X-ray diffraction method. The thermal expansion coefficient (α) 3.93 × 10–5 K−1 was calculated from the measured values of the parameters. Electronic structure and density of states are investigated by first principle calculations. Photoelectrochemical measurements on single crystals with bandgap of 2 eV reveal significant photo response. The photoactivity of as grown crystals were further investigated by degrading organic effluents such as Methylene blue (MB) and Congo red (CR) under natural sunlight. BFO showed photodegradation efficiency about 74.23% and 32.10% for degrading MB and CR respectively. Interesting morphology and microstructure of pointed spearhead like BFO crystals provide a new insight in designing and synthesizing multifunctional single crystals.


Nanomaterials ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 1619 ◽  
Author(s):  
Anna Kolanowska ◽  
Anna Wioleta Kuziel ◽  
Rafał Grzegorz Jędrysiak ◽  
Maciej Krzywiecki ◽  
Emil Korczeniewski ◽  
...  

We demonstrate Ullmann-type reactions as novel and advantageous functionalization of carbon nanotubes (CNTs) toward tunable surface chemistry. The functionalization routes comprise O-, N-, and C-arylation of chlorinated CNTs. We confirm the versatility and efficiency of the reaction allowing functionalization degrees up to 3.5 mmol g−1 by applying both various nanotube substrates, i.e., single-wall (SWCNTs) and multi-wall CNTs (MWCNTs) of various chirality, geometry, and morphology as well as diverse Ullmann-type reagents: phenol, aniline, and iodobenzene. The reactivity of nanotubes was correlatable with the nanotube diameter and morphology revealing SWCNTs as the most reactive representatives. We have determined the optimized conditions of this two-step synthetic protocol as: (1) chlorination using iodine trichloride (ICl3), and (2) Ullmann-type reaction in the presence of: copper(I) iodide (CuI), 1,10-phenanthroline as chelating agent and caesium carbonate (Cs2CO3) as base. We have analyzed functionalized CNTs using a variety of techniques, i.e., scanning and transmission electron microscopy, energy dispersive spectroscopy, thermogravimetry, comprehensive Raman spectroscopy, and X-ray photoelectron spectroscopy. The analyses confirmed the purely covalent nature of those modifications at all stages. Eventually, we have proved the elaborated protocol as exceptionally tunable since it enabled us: (a) to synthesize superhydrophilic films from—the intrinsically hydrophobic—vertically aligned MWCNT arrays and (b) to produce printable highly electroconductive pastes of enhanced characteristics—as compared for non-modified and otherwise modified MWCNTs—for textronics.


Nanomaterials ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 355
Author(s):  
Ksenia O. Potapenko ◽  
Anna Yu. Kurenkova ◽  
Andrey V. Bukhtiyarov ◽  
Evgeny Yu. Gerasimov ◽  
Svetlana V. Cherepanova ◽  
...  

A series of solid solutions of cadmium and manganese sulfides, Cd1−xMnxS (x = 0–0.35), and composite photocatalysts, CdS-β-Mn3O4-MnOOH, were synthesized by precipitation with sodium sulfide from soluble cadmium and manganese salts with further hydrothermal treatment at 120 °C. The obtained photocatalysts were studied by the X-ray diffraction method (XRD), UV-vis diffuse reflectance spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and N2 low temperature adsorption. The photocatalysts were tested in hydrogen production using a Na2S/Na2SO3 aqueous solution under visible light (λ = 450 nm). It was shown for the first time that both kinds of photocatalysts possess high activity in hydrogen evolution under visible light. The solid solution Cd0.65Mn0.35S has an enhanced photocatalytic activity due to its valence and conduction band position tuning, whereas the CdS-β-Mn3O4-MnOOH (40–60 at% Mn) samples were active due to ternary heterojunction formation. Further, the composite CdS-β-Mn3O4-MnOOH photocatalyst had much higher stability in comparison to the Cd0.65Mn0.35S solid solution. The highest activity was 600 mmol g−1 h−1, and apparent quantum efficiency of 2.9% (λ = 450 nm) was possessed by the sample of CdS-β-Mn3O4-MnOOH (40 at% Mn).


2019 ◽  
Vol 20 (1) ◽  
pp. 13-17
Author(s):  
O. I. Nakonechna ◽  
M. M. Dashevski ◽  
A. M. Kurylyuk ◽  
N. M. Bilyavyna

Nanoscaled (about 15 nm of size) metastable carbide Co3C was synthesized in a high-energy planetary ball mill by mechanical alloying of a mixture of powder cobalt (75 at. %) and multiwalled carbon nanotubes (CNT, 25 at. %). Phase transformation takes place at reaction milling according to the reaction hcp-Co + CNT ® Co3C (reaction time is 120 - 220 min). The crystal structure of the Co3C carbide formed in the milling products was studied by X-ray diffraction method. It has revealed that the Co3C phase crystallizes in a Fe3C-type structure with a = 0.4982(3) nm, b = 0.6715(6) nm, c = 0.4457(7) nm, Pnma space group. The reliability factor RB is equal to 0.065 for 48 reflections presented at diffraction pattern. It is found that the crystal structure of the Co3C carbide obtained by reaction milling of the Co-CNT charge is significantly internally deformed (distortion degree of the CCo6 octahedron is 3.67 %) and contains the reduced interatomic Co-C distances (up to 0.188 nm). It was shown that the use of carbon nanotubes instead of graphite substantially reduces the duration of the Co3C carbide synthesis.


Materials ◽  
2019 ◽  
Vol 12 (19) ◽  
pp. 3174 ◽  
Author(s):  
Andoni Choya ◽  
Beatriz de Rivas ◽  
Jose Ignacio Gutiérrez-Ortiz ◽  
Juan Ramón González-Velasco ◽  
Rubén López-Fonseca

The present work addresses the influence of the support on the catalytic behavior of Co3O4-based catalysts in the combustion of lean methane present in the exhaust gases from natural gas vehicular engines. Three different supports were selected, namely γ-alumina, magnesia and ceria and the corresponding catalysts were loaded with a nominal cobalt content of 30 wt. %. The samples were characterized by N2 physisorption, wavelength dispersive X-ray fluorescence (WDXRF), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and temperature-programmed reduction with hydrogen and methane. The performance was negatively influenced by a strong cobalt-support interaction, which in turn reduced the amount of active cobalt species as Co3O4. Hence, when alumina or magnesia supports were employed, the formation of CoAl2O4 or Co–Mg mixed oxides, respectively, with a low reducibility was evident, while ceria showed a lower affinity for deposited cobalt and this remained essentially as Co3O4. Furthermore, the observed partial insertion of Ce into the Co3O4 lattice played a beneficial role in promoting the oxygen mobility at low temperatures and consequently the catalytic activity. This catalyst also exhibited a good thermal stability while the presence of water vapor in the feedstream induced a partial inhibition, which was found to be completely reversible.


NANO ◽  
2019 ◽  
Vol 14 (06) ◽  
pp. 1950074 ◽  
Author(s):  
Mingping He ◽  
Jianguang Li ◽  
Wanli Xu ◽  
Zhenqiang Dong ◽  
Yuechao Wu ◽  
...  

Carbon nanotubes (CNTs) were welded on the surface of thermoplastic polypropylene (PP) substrate by laser irradiation and then manganese dioxide (MnO2) was deposited on the surface of CNTs by electrochemical method to prepare CNTs/MnO2 flexible electrodes (L-CM). The microstructure and morphology of CNTs/MnO2 composites were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The results showed that CNTs were welded on the surface of the substrate, adhering to each other to form a porous network structure. In addition, there were distinct small protrusions on the surface of CNTs, indicating that MnO2 had been successfully deposited on the surface of CNTs. Cyclic voltammogram (CV), galvanostatic charge/discharge (GCD) and electrochemical impedance spectroscopy (EIS) techniques were employed to investigate the electrochemical performance of the composites. Compared with CNTs/MnO2 composite prepared via compaction (denoted as C-CM), L-CM composite prepared under the laser power of 0.75[Formula: see text]W (denoted as L-CM75) showed a larger capacitance of 214.6[Formula: see text]F[Formula: see text]g[Formula: see text] at the current density of 0.5[Formula: see text]A[Formula: see text]g[Formula: see text] and displayed excellent bendability, demonstrating capacitance retention of approximately 89.6% after 1000 bending cycles. The excellent performance of L-CM75 may be attributed to the fact that the CNTs welded on the substrate have formed an effective conductive network whose porous structure can facilitate easy access of electrolytes to the electrode, which results in enhancement of the electrochemical performance of L-CM75.


Polymers ◽  
2020 ◽  
Vol 12 (12) ◽  
pp. 2918
Author(s):  
Javed Iqbal ◽  
Mohammad Omaish Ansari ◽  
Arshid Numan ◽  
S. Wageh ◽  
Ahmed Al-Ghamdi ◽  
...  

In this study, ternary composites of polyaniline (PANI) with manganese dioxide (MnO2) nanorods and carbon nanotubes (CNTs) were prepared by employing a hydrothermal methodology and in-situ oxidative polymerization of aniline. The morphological analysis by scanning electron microscopy showed that the MnO2 possessed nanorod like structures in its pristine form, while in the ternary PANI@CNT/MnO2 composite, coating of PANI over CNT/MnO2, rods/tubes were evidently seen. The structural analysis by X-ray diffraction and X-ray photoelectron spectroscopy showed peaks corresponding to MnO2, PANI and CNT, which suggested efficacy of the synthesis methodology. The electrochemical performance in contrast to individual components revealed the enhanced performance of PANI@CNT/MnO2 composite due to the synergistic/additional effect of PANI, CNT and MnO2 compared to pure MnO2, PANI and PANI@CNT. The PANI@CNT/MnO2 ternary composite exhibited an excellent specific capacity of 143.26 C g−1 at a scan rate of 3 mV s−1. The cyclic stability of the supercapattery (PANI@CNT/MnO2/activated carbon)—consisting of a battery type electrode—demonstrated a gradual increase in specific capacity with continuous charge–discharge over ~1000 cycles and showed a cyclic stability of 119% compared to its initial value after 3500 cycles.


2003 ◽  
Vol 780 ◽  
Author(s):  
C. Essary ◽  
V. Craciun ◽  
J. M. Howard ◽  
R. K. Singh

AbstractHf metal thin films were deposited on Si substrates using a pulsed laser deposition technique in vacuum and in ammonia ambients. The films were then oxidized at 400 °C in 300 Torr of O2. Half the samples were oxidized in the presence of ultraviolet (UV) radiation from a Hg lamp array. X-ray photoelectron spectroscopy, atomic force microscopy, and grazing angle X-ray diffraction were used to compare the crystallinity, roughness, and composition of the films. It has been found that UV radiation causes roughening of the films and also promotes crystallization at lower temperatures.Furthermore, increased silicon oxidation at the interface was noted with the UVirradiated samples and was shown to be in the form of a mixed layer using angle-resolved X-ray photoelectron spectroscopy. Incorporation of nitrogen into the film reduces the oxidation of the silicon interface.


Polymers ◽  
2021 ◽  
Vol 13 (4) ◽  
pp. 581
Author(s):  
Gajanan S. Ghodake ◽  
Surendra K. Shinde ◽  
Ganesh D. Saratale ◽  
Rijuta G. Saratale ◽  
Min Kim ◽  
...  

The utilization of waste-paper-biomass for extraction of important α-cellulose biopolymer, and modification of extracted α-cellulose for application in enzyme immobilization can be extremely vital for green circular bio-economy. Thus, in this study, α-cellulose fibers were super-magnetized (Fe3O4), grafted with chitosan (CTNs), and thiol (-SH) modified for laccase immobilization. The developed material was characterized by high-resolution transmission electron microscopy (HR-TEM), HR-TEM energy dispersive X-ray spectroscopy (HR-TEM-EDS), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FT-IR) analyses. Laccase immobilized on α-Cellulose-Fe3O4-CTNs (α-Cellulose-Fe3O4-CTNs-Laccase) gave significant activity recovery (99.16%) and laccase loading potential (169.36 mg/g). The α-Cellulose-Fe3O4-CTNs-Laccase displayed excellent stabilities for temperature, pH, and storage time. The α-Cellulose-Fe3O4-CTNs-Laccase applied in repeated cycles shown remarkable consistency of activity retention for 10 cycles. After the 10th cycle, α-Cellulose-Fe3O4-CTNs possessed 80.65% relative activity. Furthermore, α-Cellulose-Fe3O4-CTNs-Laccase shown excellent degradation of pharmaceutical contaminant sulfamethoxazole (SMX). The SMX degradation by α-Cellulose-Fe3O4-CTNs-Laccase was found optimum at incubation time (20 h), pH (3), temperatures (30 °C), and shaking conditions (200 rpm). Finally, α-Cellulose-Fe3O4-CTNs-Laccase gave repeated degradation of SMX. Thus, this study presents a novel, waste-derived, highly capable, and super-magnetic nanocomposite for enzyme immobilization applications.


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