Influence of pyrrole feeding ratios on physicochemical characteristics of high-performance multilayered PPy/PVC/PDA@FG-NH2 nanocomposites

2019 ◽  
Vol 33 (10) ◽  
pp. 1358-1382
Author(s):  
Asima Naz ◽  
Rabia Sattar ◽  
Muhammad Siddiq ◽  
Muhammad Abid Zia

Nanocomposites of conjugated polymers polypyrrole (PPy) and polyvinyl chloride (PVC) as matrices and 1,4-phenylenediamine (PDA) as a linker with amine functional graphite (FG-NH2) as filler have been efficiently fabricated using in situ oxidative polymerization, and the effect of various mass ratios on physicochemical characteristics of prepared nanocomposite was investigated. The layer-by-layer oxidative polymerization of various matrices on host filler surface is confirmed by Fourier transform infrared, energy dispersive X-ray, and X-ray photoelectron spectroscopy examinations. Field emission scanning electron microscopy revealed fibrillary morphology of obtained nanocomposites. Thermal stability, glass transition temperature, and melting and crystallization temperature of the nanocomposites were increased with the incorporation of modified graphite. Brunauer–Emmett–Teller analysis explored the improved adsorption capacity (128 cm3 g−1) of the nanocomposite with higher feeding ratio of pyrrole. The influence of FG-NH2 and pyrrole on electrical conductivity performance of composites was also investigated. Functionalized graphite in the resultant PPy/PVC/PDA@FG-NH2 nanocomposites played an important role in forming conducting network in PPy matrix indicating synergistic effect between PPy and FG-NH2.

2014 ◽  
Vol 34 (5) ◽  
pp. 415-429 ◽  
Author(s):  
Rozina Ashraf ◽  
Ayesha Kausar ◽  
Muhammad Siddiq

Abstract Compared to conventional materials, nanocomposites of conjugated polymers are found to have excellent performance due to a larger exposed surface area. In this study, polyaniline (PANi), polypyrrole (PPy), polythiophene (PTh) and polyazopyridine (PAP)/nanodiamonds (NDs) composites were efficiently synthesized by in situ oxidative polymerization. Physical characteristics of fabricated nanocomposites were explored using Fourier transform infrared spectroscopy (FTIR), energy dispersive X-ray (EDX) spectroscopy, field emission scanning electron microscopy (FESEM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). FTIR indicated layer-by-layer oxidative polymerization of various matrices on functional ND (F-ND) surfaces. FESEM revealed the fibrillar (web-like) morphology of multilayered nanocomposites having a granular arrangement of NDs. TGA of multilayered F-NDs/PAP/PANi/PTh showed 10% degradation at an enhanced temperature of 482°C compared with F-NDs/PANi/PPy/PTh (471°C). Improvement in glass transition of layered material was observed from 99°C (NDs/PANi/PPy/PTh) to 121°C (NDs/PAP/PANi/PTh). Functional filler also contributed towards the enhancement in the conductivity of NDs/PAP/PANi/PTh (5.7 S cm-1) relative to NDs/PANi/PPy/PTh (3.7 S cm-1) systems. New conducting composites are potentially important in various applications, including polymer lithium-ion batteries.


Polymers ◽  
2021 ◽  
Vol 13 (21) ◽  
pp. 3657
Author(s):  
Andrey V. Orlov ◽  
Svetlana G. Kiseleva ◽  
Galina P. Karpacheva ◽  
Dmitriy G. Muratov

New oxidative polymerization monomers—diarylaminodichlorobenzoquinones were synthesised by alkylating aniline, m-phenylenediamine and methanilic acid with chloranil. Oxidative polymerization of diarylaminodichlorobenzoquinones was studied for the first time in relation to the concentration of the monomer, acid, and oxidant/monomer ratio. It was found that the synthesized monomers are highly active in the polymerization reaction, and the oxidation rate grows with the increase in the acid concentration. Only one arylamine group is involved in the polymerization reaction. The optimal oxidant/monomer ratio is stoichiometric for one arylamine group, despite the bifunctionality of the monomers. It was shown that the type of the substituent in the aniline ring (electron donor or electron acceptor) determines the growth of the polymer chain and the structure of the resulting conjugated polymers. A mechanism for the formation of active polymerization centers for diarylaminodichlorobenzoquinones was proposed. FTIR-, NMR-, X-ray photoelectron spectroscopy, and SEM were used to identify the structure of the synthesized monomers and polymers. The obtained polymers have an amorphous structure and a loose globular morphology. The frequency dependence of the electrical conductivity was studied.


NANO ◽  
2020 ◽  
Vol 15 (05) ◽  
pp. 2050058
Author(s):  
Yuhua Huang ◽  
Weiwei Li ◽  
Bingchu Mei ◽  
Yu Yang ◽  
Zuodong Liu

In this paper, the effects of etching temperature and concentrations of hydrochloric acid (HCl) on the exfoliating process and the electrochemical performance of LIBs were systematically explored. The transformation from Ti3AlC2 to Ti3C2 was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and Raman spectra. The suitable conditions of preparing Ti3C2 MXene though HCl and lithium fluoride (LiF) were obtained. Besides, the in-situ oxidation conditions of Ti3C2 during the etching process were studied. The TiO2/Ti3C2 was beneficial to improve the specific capacity from 125[Formula: see text]mAh[Formula: see text]g[Formula: see text] to 150[Formula: see text]mAh[Formula: see text]g[Formula: see text] at 1 C.


2006 ◽  
Vol 527-529 ◽  
pp. 1075-1078 ◽  
Author(s):  
Carey M. Tanner ◽  
Jun Lu ◽  
Hans Olof Blom ◽  
Jane P. Chang

The material properties of HfO2 thin films were studied to evaluate their potential as a high-κ gate dielectric in 4H-SiC power metal-oxide-semiconductor field effect transistors. Stoichiometric HfO2 films were deposited on n-type 4H-SiC (0001) by atomic layer deposition (ALD) at substrate temperatures of 250-450°C. No significant interfacial layer formation was observed by in-situ X-ray photoelectron spectroscopy (XPS) and an abrupt interface was confirmed by high-resolution transmission electron microscopy (HRTEM). A temperature-dependent transition from amorphous layer-by-layer growth to crystalline three-dimensional island growth was identified by in-situ reflection high-energy electron diffraction (RHEED) and ex-situ atomic force microscopy (AFM). X-ray diffraction (XRD) confirmed the presence of monoclinic HfO2 domains in crystallized films.


2006 ◽  
Vol 21 (1) ◽  
pp. 112-118 ◽  
Author(s):  
A. Vadivel Murugan ◽  
Mathieu Quintin ◽  
Marie-Helene Delville ◽  
Guy Campet ◽  
Annamraju Kasi Viswanath ◽  
...  

Here we demonstrate the synthesis of a new type of layered poly(3,4-ethylenedioxy- thiophene) (PEDOT)/MoS2 nanocomposite via flocculation of delaminated MoS2 with subsequent in situ oxidative polymerization of 3,4-ethylenedioxythiophene. The resulting nanocomposite was characterized by Fourier transform infrared spectroscopy, powder x-ray diffraction, x-ray photoelectron spectroscopy, thermal analysis, transmission electron microscopy, and four-probe electrical conductivity measurements with respect to temperature. X-ray diffraction results indicated that the exfoliated MoS2 and PEDOT are restacked to produce a novel nanoscale composite material containing alternate nanoribbons of PEDOT in between MoS2 with a basal distance of ∼1.38 nm. The nanocomposite, which could be used as a cathode material for small power rechargeable lithium batteries, has also been demonstrated by the electrochemical insertion of lithium into the PEDOT/MoS2 nanocomposite, where a significant enhancement in the discharge capacity is observed, compared to that of respective pristine molybdenum disulfide.


2010 ◽  
Vol 123-125 ◽  
pp. 189-192
Author(s):  
Hong Wei Shi ◽  
Li Zhang ◽  
Cong Wang ◽  
Ke Ying Zhang

Nanocomposite films containing Au nanoparticles were fabricated by alternating adsorption of poly(diallydimethyl ammonium chloride) (PDDA) and HAuCl4 using layer-by-layer self-assembly technique and subsequent in situ electrochemical reduction of the AuCl4- ions. The composition and properties of the composite films were characterized by ultraviolet-visible spectroscopy (UV-vis), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV).The UV-vis characteristic absorbances of PDDA and Au increase almost linearly with the number of bilayers, which suggests a progressive deposition with almost an equal amount of the PDDA and Au in each cycle. X-ray photoelectron spectroscopy further confirms the presence of the main components (such as PDDA and Au) of the nanocomposite films. Furthermore, the nanocomposite films also exhibit good electrocatalytic activity for the oxidation of ascorbic acid (AA), which may be used in electrochemical biosensors.


Minerals ◽  
2020 ◽  
Vol 10 (10) ◽  
pp. 884
Author(s):  
Soyoung Min ◽  
Yeongkyoo Kim

The synthesis methods used to produce todorokite (10 Å manganate, OMS-1) and birnessite (7 Å manganate), which are abundant in marine manganese nodules, have been studied to confirm whether pure mineral phases can be obtained and to compare their physicochemical characteristics. The physicochemical characteristics of todorokite and its precursor Na–birnessite can vary widely based on the precursors used during their synthesis. Birnessite can be synthesized via three mechanisms, i.e., the oxidation of Mn2+, a redox reaction between Mn2+ and MnO4−, or the reduction of MnO4−. Herein, four precursors are used to synthesize birnessite using different methods before being transformed into todorokite. The characteristics of the birnessite and todorokite synthesized using different methods are investigated via X-ray diffraction (XRD), chemical analysis, Brunauer–Emmett–Teller (BET), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and field emission scanning electron microscopy (SEM). Based on the method used, birnessite and todorokite exhibit distinct physicochemical features, including crystallinity, crystal structure, specific surface area, oxidation state of manganese, thermal stability, and morphology. Thus, the characteristics of birnessite and todorokite are closely correlated, indicating the importance of designing suitable methods to synthesize them for specific applications.


2010 ◽  
Vol 89-91 ◽  
pp. 91-96
Author(s):  
G.R. Chang ◽  
Fei Ma ◽  
B. Ma ◽  
Ke Wei Xu

An in-situ investigation was performed on the stress relaxation of sandwiched Si3N4/Al/Si3N4 thin films by using multi-beam optical stress sensor (MOSS), a developed technique for substrate curvature measurement. Furthermore, the microstructures of the thin films were characterized by several analyzing techniques, such as X-ray Photoelectron Spectroscopy (XPS), Field Emission Scanning Electron Microscope (FE-SEM) and X-ray energy dispersive spectroscopy (EDS). The results indicated sharp rise and drop of the residual stress due to the cracks of Si3N4 surface layer or the separation of Al particles during annealing process. An appropriate model was suggested to interpret this phenomenon.


Catalysts ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 916 ◽  
Author(s):  
Yu ◽  
Kiwi ◽  
Wang ◽  
Pulgarin ◽  
Rtimi

This study presents the first evidence for the photocatalytic performance of ZnO/CuxO hexagonal nanowires leading to sulfamethazine (SMT) degradation. The chemical composition of the nanowires was determined by X-ray fluorescence (XRF). The sample with the composition ZnO/Cux = 1.25O led to faster SMT-degradation kinetics. The SMT-degradation kinetics were monitored by high performance liquid chromatography (HPLC). The morphology of the hexagonal nanowires was determined by scanning electron microscopy (SEM) and mapped by EDX. The redox reactions during SMT degradation were followed by X-ray photoelectron spectroscopy (XPS). The interfacial potential between the catalyst surface and SMT was followed in situ under solar and indoor visible light irradiation. SMT-degradation was mediated by reactive oxidative species (ROS). The interfacial charge transfer (IFCT) between ZnO and CuxO is shown to depend on the type of light used (solar or visible light). This later process was found to be iso-energetic due to the potential energy positions of ZnO and CuxO conduction bands (cb). The intervention of surface plasmon resonance (LSPR) species in the SMT degradation is discussed.


1993 ◽  
Vol 312 ◽  
Author(s):  
J. D. Denlinger ◽  
Eli Rotenberg ◽  
U. Hessingert ◽  
M. Leskovar ◽  
Marjorie A. Olmstead

AbstractThin (0.5 to 8 triple layer) CaF2 on Si(111) films were grown using molecular beam epitaxy (MBE) and characterized using an in situ combination of x-ray photoelectron spectroscopy (XPS) and componentresolved x-ray photoelectron diffraction (XPD). We identified surface, bulk-like, and interface F and Ca core-level shifts and used the XPS shifts and XPD modulations to identify the growth modes as a function of the kinetic parameters of CaF2 flux and Si temperature. We identify 3 distinct regimes: (i) for high temperatures and flux we find a complete reacted F-Ca-Si layer, overlaid by 2 layer high islands which coalesce, followed by layer-by-layer growth, (ii) for high temperature and low flux, we find the reacted F-Ca-Si layer to be partially covered with thick islands, and (iii) for low temperatures we find an incompletely occupied F-Ca-Si layer followed by layer-by-layer growth. In all cases we find the buried interface to be structurally identical to the unburied F-Ca-Si layer


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