scholarly journals In situ polymerization monitoring of a diacrylate in an electrically conducting mesoporous nanoparticle scaffold

2022 ◽  
Author(s):  
Ron Hoffmann ◽  
Hendrik Naatz ◽  
Andreas Hartwig
Keyword(s):  
Indium Tin Oxide ◽  
In Situ Polymerization ◽  
Uv Light ◽  
Reaction Rates ◽  
Polymerization Process ◽  
Polymerization Reaction ◽  
Radical Initiation ◽  
Electrically Conducting ◽  
Ft Ir ◽  
Ito Nanoparticles

AbstractThe properties of nanoparticle–polymer composites strongly depend on the network structure of the polymer matrix. By introducing nanoparticles into a monomer (solution) and subsequently polymerizing it, the formation of the polymer phase influences the mechanical and physicochemical properties of the composite. In this study, semi-conducting indium tin oxide (ITO) nanoparticles were prepared to form a rigid nanoparticle scaffold in which 1,6-hexanediol diacrylate (HDDA), together with an initiator for photo-polymerization, was infiltrated and subsequently polymerized by UV light. During this process, the polymerization reaction was characterized using rapid scan Kubelka–Munk FT-IR spectroscopy and compared to bulk HDDA. The conductivity change of the ITO nanoparticles was monitored and correlated with the polymerization process. It was revealed that the reaction rates of the radical initiation and chain propagation are reduced when cured inside the voids of the nanoparticle scaffold. The degree of conversion is lower for HDDA infiltrated into the mesoporous ITO nanoparticle scaffold compared to purely bulk-polymerized HDDA. Graphical abstract

Study on the Synthesis and Characterization of PANi/Nano-CeO2 Composites

2007 ◽  
Vol 124-126 ◽  
pp. 287-290 ◽  
Author(s):  
Fei Liu ◽  
Yong Jun He ◽  
Jeung Soo Huh
Keyword(s):  
In Situ Polymerization ◽  
Solid Phase ◽  
Polymerization Reaction ◽  
Solid Phase Reaction ◽  
Phase Reaction ◽  
Vis Spectroscopy ◽  
Ft Ir ◽  
Average Size

The nano-CeO2 was synthesized by two-step solid-phase reaction. The image of TEM showed that nano-CeO2 with an average size of about 70 nm. The series of polyaniline/nano-CeO2 composites with different PANi: CeO2 ratios were prepared by in-situ polymerization in the presence of hydrochloric acid (HCl) as dopant by adding nano-CeO2 into the polymerization reaction mixture of aniline. The composites obtained were characterized by FT-IR and UV-vis spectroscopy analysis. The FT-IR spectra of nanocomposites indicate different blue-shifts, attributed to C–N stretching mode for benzenoid unit. The UV-vis spectra of nanocomposites display einstein-shifts compared with PANi at 620nm. The conductivity properties of the composites are also changed compare to the pure PANi. These results suggest that the interactions between the polymer matrix and nanoparticles take place in polyaniline/nano- CeO2 composites.

scholarly journals Synthesis and Characterizations of Poly(3-hexylthiophene) and Modified Carbon Nanotube Composites

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Mohammad Rezaul Karim
Keyword(s):  
Carbon Nanotube ◽  
In Situ Polymerization ◽  
Polymerization Process ◽  
Multiwall Carbon Nanotube ◽  
X Ray Diffraction ◽  
Nanotube Composites ◽  
Ft Ir ◽  
Carbon Nanotube Composites ◽  
Fourier Transfer Infrared Spectroscopy

Poly(3-hexylthiophene) and modified (functionalized and silanized) multiwall carbon nanotube (MWNT) nanocomposites have been prepared through in situ polymerization process in chloroform medium with FeCl3oxidant at room temperature. The composites are characterized through Fourier transfer infrared spectroscopy (FT-IR), Raman, and X-ray diffraction (XRD) measurements to probe the nature of interaction between the moieties. Optical properties of the composites are measured from ultraviolet-visible (UV-Vis) and photoluminescence (PL) spectroscopy. Conductivity of the composites is followed by four probe techniques to understand the conduction mechanism. The change (if any) in C=C symmetric and antisymmetric stretching frequencies in FT-IR, the shift in G band frequencies in Raman, any alterations inλmaxof UV-Vis, and PL spectroscopic measurements are monitored with modified MWNT loading in the polymer matrix.

scholarly journals Synthesis and Characterization of BaTiO3/Polypyrrole Composites with Exceptional Dielectric Behaviour

Polymers ◽  
2018 ◽  
Vol 10 (11) ◽  
pp. 1273 ◽  
Author(s):  
Khalil Ahmed ◽  
Farah Kanwal ◽  
Shahid Ramay ◽  
Shahid Atiq ◽  
Rabia Rehman ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Dielectric Constant ◽  
In Situ Polymerization ◽  
Weight Ratio ◽  
Aqueous Dispersion ◽  
Polymerization Process ◽  
Dielectric Parameters ◽  
Host Matrix ◽  
Ft Ir ◽  
Tga Analysis

Higher concentrations of ceramic fillers induce brittleness in the ceramic/polymer hybrids which restrict their applications to limited fields especially when such hybrids are prepared for their use as dielectrics. We have synthesized and characterized different BaTiO3-polypyrrole (PPy) composites by changing the concentration of BaTiO3 from 1% by weight of PPy taken to 5 wt % to explore its effect on the dielectric parameters of the final product and found that the BaTiO3-polypyrrole composite with weight ratio of 0.05:1 exhibited highest dielectric constant, lowest dielectric loss and thermally most stable. All the composites were prepared using in-situ polymerization of pyrrole in an aqueous dispersion of low content of BaTiO3 in the presence of small amount of Hydrochloric acid. These composites were characterized for their microstructure and crystallinity by X-ray diffractometer (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM) while thermal stability by thermo gravimetric (TGA) analysis. An impedance analyser (LCR meter) was utilized to investigate the dielectric parameters. FT-IR data confirmed the presence of the two phases and their interaction, inferred from the shifting of normal PPy peaks. The data obtained from XRD confirmed the presence of crystallites of 2.8 to 5 nm with dominant crystallinity of the filler, TGA analysis (25 to 600 °C) confirmed the higher thermal stability induced on successive addition of the filler into the prepared composites as compared to that of pure PPy in a wide temperature range which is unusual for such a low % age addition of the filler. The SEM analysis together with XRD results reveal that the successive introduction of BaTiO3 particles produced crystallites of 2 to 5 nm size which bonded together and changed the hemispherical shaped larger grains of the matrix to regular shaped smaller grains. The dielectric constant of the composites was enhanced with filler contents from 178 to 522 at 1 MHz for 1 wt % and 5 wt % BaTiO3 respectively. It was concluded that the introduction of BaTiO3 into the polymer matrix with this new procedure has greatly affected the polymerization process, thermal stability, morphology and dielectric properties of the host matrix and has resulted in a novel series of the composites which may have broad applications.

scholarly journals Synthesis and characterization of indium tin oxide nanoparticles via reflux method

2018 ◽  
Vol 35 (4) ◽  
pp. 799-805 ◽  
Author(s):  
Sahebali Manafi ◽  
Simin Tazikeh ◽  
Sedigheh Joughehdoust
Keyword(s):  
Tin Oxide ◽  
Indium Tin Oxide ◽  
Oxide Nanoparticles ◽  
Hydroxyl Groups ◽  
Sem Images ◽  
Tin Chloride ◽  
Ft Ir ◽  
Tin Oxide Nanoparticles ◽  
Ito Nanoparticles ◽  
Indium Tin Oxide Nanoparticles

Abstract Synthesis of indium tin oxide (ITO) nanoparticles by reflux method without chlorine contamination at different pHs, temperatures, solvents and concentrations has been studied. Indium chloride, tin chloride, water, ethanol and Triton X-100 were used as starting materials. Structure, size, surface morphology and transparency of indium tin oxide nanoparticles were studied by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and UV-Vis spectrophotometry. XRD patterns showed that 400 °C is the lowest temperature for synthesis of ITO nanoparticles because metal hydroxide does not transform to metal oxide in lower temperature. FT-IR results showed the transformation of hydroxyl groups to oxide. SEM images showed that pH is the most important factor affecting the nanoparticles size. The smallest nanoparticles (40 nm) were obtained at pH = 8.8. The size of crystallites was decreased by lowering of concentration (0.025 M).

scholarly journals Optical and Structural Properties of Prepared Polyaniline – Graphene (PANI/GN) Nanocomposite

2021 ◽  
pp. 138-146
Author(s):  
Najlaa J. Abdullah ◽  
Abbas F. Essa ◽  
Salma M. Hasan
Keyword(s):  
Active Sites ◽  
Energy Gap ◽  
Chemical Oxidation ◽  
Polymerization Process ◽  
Polymerization Reaction ◽  
Wave Numbers ◽  
Ft Ir ◽  
Nano Graphene ◽  
Poly Aniline ◽  
Pani Sample

Polyaniline (PANI) polymer was successfully prepared by the chemical oxidation method at 0 oC. Polyaniline-nano grapheme (GN) powder nanocomposites were prepared by the addition of GN with different weight ratios (0.1, 1, 5, and 10 g wt. %) during the polymerization of PANI. It was found that the polymerization reaction of poly-aniline was exothermic.  The effect of adding nano-graphene powder during polymerization process on the time and temperature of the reaction was studied. The resulting polymer was diagnosed using several methods, including Fourier transform infrared spectroscopy (FT-IR) and UV-VIS spectrophotometry. The results of FTIR demonstrated a shift to higher wave numbers in the peaks of nanocomposites, due to PANI peaks, in addition to the matching between the groups of active sites of the polymer with its chemical composition. The results of the optical properties showed a decrease in the energy gap of the nanocomposite compared with that of the pure PANI sample. The morphology of the samples was studied using Scanning Electron Microscope (SEM). The increase in the concentration of GN led to a change in the surface morphology of the composites. The results predict that the PANI/GN nano-composites can be used in many applications, such as those of sensors.

Ultrasonic Assisted Dynamic Inverse Emulsion: A Novel Polymerization Technique to Prepare Conductive Polyaniline/Palygorskite Composite

2013 ◽  
Vol 873 ◽  
pp. 507-513
Author(s):  
Zhe Zhang ◽  
Xiao Liang Wang ◽  
Jian Xu ◽  
Heng Chang Ma ◽  
Zi Qiang Lei
Keyword(s):  
Weight Ratio ◽  
Polymerization Process ◽  
Ammonium Bromide ◽  
Dodecylbenzenesulfonic Acid ◽  
Inverse Emulsion ◽  
Electrically Conducting ◽  
Ultrasonic Assisted ◽  
Ft Ir ◽  
Conductive Polyaniline ◽  
Dynamic Inverse

The present work describes an ultrasonic assisted in-situ dynamic inverse emulsion polymerization process of aniline (ANI) in the presence of organic palygorskite (OPGS) in toluene. Core-shell structure of electrically conducting polymerized ANI (PANI) combined with OPGS was prepared by utilizing the method. Dodecylbenzenesulfonic acid (DBSA) was used as the dopant and emulsifier. The OPGS was obtained via the chemical reaction of pretreated palygorskite with hexadecyltrimethyl ammonium bromide (HTAB). The prepared PANI/OPGS composite was characterized by FT-IR, UV-Vis, XRD, TGA and SEM. In addition, the conductivity was evaluated at different ANI/OPGS weight ratio. When the ANI/OPGS weight ratio increased to 2:7, the conductivity of the composite still remained at 10 S/m at room temperature. The results demonstrated that ultrasonic assisted dynamic inverse emulsion would be an excellent polymerization technique to increase the conductivity and the polymerization rate.

SO3H-functionalized Zeolite-Y as an Efficient Nanocatalyst for the Synthesis of Nbenzimidazole- 2-aryl-4-thiazolidinones and tri-substituted Imidazoles

2020 ◽  
Vol 17 (2) ◽  
pp. 117-130 ◽  
Author(s):  
Mehdi Kalhor ◽  
Zohre Zarnegar ◽  
Zahra Seyedzade ◽  
Soodabeh Banibairami
Keyword(s):  
Zeolite Y ◽  
Internal Standard ◽  
Acid Catalyst ◽  
Aromatic Aldehydes ◽  
Reaction Rates ◽  
Ambient Conditions ◽  
Catalytic Method ◽  
Efficient Catalyst ◽  
Bet Analysis ◽  
Ft Ir

Background: SO3H-functionalized zeolite-Y was prepared and used as a catalyst for the synthesis of 2-aryl-N-benzimidazole-4-thiazolidinones and tri-substituted imidazoles at ambient conditions. Objective: The goals of this catalytic method include excellent yields and high purity, inexpensive procedure and ease of product isolation, the use of nontoxic and heterogeneous acid catalyst, shorter reaction times and milder conditions. Materials and Methods: NMR spectra were recorded on Brucker spectrophotometer using Me4Si as internal standard. Mass spectra were recorded on an Agilent Technology 5975C VL MSD with tripe-axis detector. FTIR spectra were obtained with KBr disc on a galaxy series FT-IR 5000 spectrometer. The surface morphology of nanostructures was analyzed by FE-SEM (EVO LS 10, Zeiss, Carl Zeiss, Germany). BET analysis were measured at 196 °C by a Japan Belsorb II system after the samples were vacuum dried at 150°C overnight. Results: The NSZ was characterized by FT-IR, FESEM, EDX, XRF, and BET. The catalytic activity of NSZ was investigated for synthesis of 1,3-tiazolidin-4-ones in H2O/Acetone at room temperature. Moreover, NSZ was used for synthesis of tri-substituted imidazoles at 60 °C via solvent-free condensation. Different kinds of aromatic aldehydes were converted to the corresponding of products with good to excellent yields. Conclusion: Sulfonated zeolite-Y was as an efficient catalyst for the preparation of N-benzimidazole-2-aryl-1,3- thiazolidin-4-ones and 2,4,5-triaryl-1H-imidazoles. High reaction rates, elimination toxic solvent, simple experimental procedure and reusability of the catalyst are the important features of this protocol.

scholarly journals Room-Temperature Solution-Processed 0D/1D Bilayer Electrodes for Translucent CsPbBr3 Perovskite Photovoltaics

Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1489
Author(s):  
Bhaskar Parida ◽  
Saemon Yoon ◽  
Dong-Won Kang
Keyword(s):  
Solar Cells ◽  
Indium Tin Oxide ◽  
High Performance ◽  
Room Temperature ◽  
Low Cost ◽  
Perovskite Solar Cells ◽  
Ambient Air ◽  
Plasma Damage ◽  
Temperature Solution ◽  
Ito Nanoparticles

Materials and processing of transparent electrodes (TEs) are key factors to creating high-performance translucent perovskite solar cells. To date, sputtered indium tin oxide (ITO) has been a general option for a rear TE of translucent solar cells. However, it requires a rather high cost due to vacuum process and also typically causes plasma damage to the underlying layer. Therefore, we introduced TE based on ITO nanoparticles (ITO-NPs) by solution processing in ambient air without any heat treatment. As it reveals insufficient conductivity, Ag nanowires (Ag-NWs) are additionally coated. The ITO-NPs/Ag-NW (0D/1D) bilayer TE exhibits a better figure of merit than sputtered ITO. After constructing CsPbBr3 perovskite solar cells, the device with 0D/1D TE offers similar average visible transmission with the cells with sputtered ITO. More interestingly, the power conversion efficiency of 0D/1D TE device was 5.64%, which outperforms the cell (4.14%) made with sputtered-ITO. These impressive findings could open up a new pathway for the development of low-cost, translucent solar cells with quick processing under ambient air at room temperature.

scholarly journals Synthesis of poly (n-butyl acrylate) with tempo by nitroxide mediated polymerization method

2021 ◽  
pp. 096739112110245
Author(s):  
Amrita Sharma ◽  
PP Pande
Keyword(s):  
Butyl Acrylate ◽  
Low Cost ◽  
Polymerization Process ◽  
Polymerization Reaction ◽  
High Concentration ◽  
Acrylate Monomer ◽  
Controlled Polymerization ◽  
Acrylate Monomers ◽  
Nitroxide Mediated Polymerization ◽  
Polymerization Method

It has been observed that acrylate monomers are very difficult to polymerize with the low cost nitroxide catalyst 2,2,6,6-tetramethylpiperidinyl-1-oxyl (TEMPO). Therefore, costly acyclic nitroxides such as N-tert-butyl-N-(1-diethylphosphono-2,2-dimethyl)-N-oxyl, (SG1), 2,2,5-Trimethyl-4-phenyl-3-azahexane-3-nitroxide (TIPNO) and TIPNO derivatives have to be used for the polymerization of the acrylic acid derivatives. There are very few reports on the use of TEMPO-derivatives toward the polymerization of n-butyl acrylate. Generally different reducing agents viz. glucose, ascorbic acid, hydroxyacetone etc. have been used to destroy excess TEMPO during the polymerization reaction. The acrylate polymerizations fail in the presence of TEMPO due to the strong C–O bond formed between the acrylate chain end and nitroxide. To the best of our knowledge, no literature report is available on the use of TEMPO without reducing agent or high temperature initiators, toward the polymerization of n-butyl acrylate. The present study has been carried out with a view to re-examine the application of low cost nitroxide TEMPO, so that it can be utilized towards the polymerization of acrylate monomers (e.g. n-butyl acrylate). We have been able to polymerize n-butyl acrylate using the nitroxide TEMPO as initiator (via a macroinitiator). In this synthesis, a polystyrene macroinitiator was synthesized in the first step from TEMPO, after this TEMPO end-capped styrene macroinitiator (PSt-TEMPO) is used to polymerize n-butyl acrylate monomer. The amount of macroinitiator taken was varied from 0.05% to 50% by weight of n-butyl acrylate monomer. The polymerization was carried out at 120°C by bulk polymerization method. The experimental findings showed a gradual increase in molecular weight of the polymer formed and decrease in the polydispersity index (PDI) with increase in amount of PSt-TEMPO macroinitiator taken. In all experiments conversion was more than 80%. These results indicate that the polymerization takes place through controlled polymerization process. Effect of different solvents on polymerization has also been investigated. In the following experiments TEMPO capped styrene has been used as macroinitiator leading to the successful synthesis of poly n-Butyl acrylate. It has been found that styrene macroinitiator is highly efficient for the nitroxide mediated polymerization, even in very small concentration for the synthesis of poly n-butyl acrylate. High concentration of macroinitiator results in the formation of block copolymers of polystyrene and poly ( n-butyl acrylate) viz. polystyrene-block-poly-( n-butyl acrylate). The use of TEMPO toward controlled polymerization is of much importance, because it is the nitroxide commercially available at the lowest cost.

scholarly journals Zirconium-Doped Chromium IV Oxide Nanocomposites: Synthesis, Characterization, and Photocatalysis towards the Degradation of Organic Dyes

Catalysts ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 117
Author(s):  
Zahir Muhammad ◽  
Farman Ali ◽  
Muhammad Sajjad ◽  
Nisar Ali ◽  
Muhammad Bilal ◽  
...  
Keyword(s):  
Methylene Blue ◽  
Photocatalytic Activity ◽  
Methyl Orange ◽  
Solid State ◽  
Room Temperature ◽  
Organic Dyes ◽  
Uv Light ◽  
Heterogeneous Photocatalysis ◽  
Ft Ir ◽  
Complete Mineralization

Degradation of organic dyes and their byproducts by heterogeneous photocatalysts is an essential process, as these dyes can be potentially discharged in wastewater and threaten aquatic and xerophyte life. Therefore, their complete mineralization into nontoxic components (water and salt) is necessary through the process of heterogeneous photocatalysis. In this study, Zr/CrO2 (Zirconium-doped chromium IV oxide) nanocomposite-based photocatalysts with different compositions (1, 3, 5, 7 & 9 wt.%) were prepared by an environmentally friendly, solid-state reaction at room temperature. The as-prepared samples were calcined under air at 450 °C in a furnace for a specific period of time. The synthesis of Zr/CrO2 photocatalysts was confirmed by various techniques, including XRD, SEM, EDX, FT-IR, UV-Vis, and BET. The photocatalytic properties of all samples were tested towards the degradation of methylene blue and methyl orange organic dyes under UV light. The results revealed a concentration-dependent photocatalytic activity of photocatalysts, which increased the amount of dopant (up to 5 wt.%). However, the degradation efficiency of the catalysts decreased upon further increasing the amount of dopant due to the recombination of holes and photoexcited electrons.

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