Thermal stability of several polyaniline/rare earth oxide composites

Polyaniline/rare earth oxide composites (PANI/La₂O₃ and PANI/Sm₂O₃) were synthesized by in situ polymerization at the presence of sulfosalicylic acid (as dopant). The composites obtained were characterized by Fourier transform infrared spectra (FTIR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The thermal stability of the composites was investigated by thermogravimetry (TG) and derivative thermogravimetry (DTG). The electrochemical performance of the composites was investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The results of FTIR, XRD, SEM, CV, and EIS show that the structure of composite has changed greatly when rare earth oxide content is >0.7 g (PANI/La₂O₃[w/w(92.7/7.3)] and PANI/Sm₂O₃[w/w(96.2/3.8)]) and the PANI in the composite has transformed into pernigraniline base (non-conducting state) from emeraldine base (conducting state). TG-DTG analysis indicates that the thermal stability of composite was higher than pure PANI, which is attributed to the interaction between PANI and rare earth oxide.     

Thermal stability and glass transition behavior of PANI/γ-Al2O3 composites

Polyaniline/γ-Al₂O₃ (PANI/γ-Al₂O₃) composites were synthesized by in-situ polymerization at the presence of HCl as dopant by adding γ-Al₂O₃ nanoparticles into aniline solution. The composites were characterized by FTIR and XRD. The thermogravimetry (TG) and modulated differential scanning calorimetry (MDSC) were used to study the thermal stability and glass transition temperature (T _g) of the composites, respectively. The results of FTIR showed that γ-Al₂O₃ nanoparticles connected with the PANI chains and affected the absorption characteristics of the composite through the interaction between PANI and nano-sized γ-Al₂O₃. And the results of XRD indicated that the peaks intensity of the PANI/γ-Al₂O₃ composite were weaker than that of the pure PANI. From TG and derivative thermogravimetry (DTG) curves, it was found that the pure PANI and the PANI/γ-Al₂O₃ composites were all one step degradation. And the PANI/γ-Al₂O₃ composites were more thermal stable than the pure PANI. The MDSC curves showed that the nano-sized γ-Al₂O₃ heightened the glass transition temperature (T _g) of PANI.     

Thermal stability of several polyaniline/rare earth oxide composites (I): polyaniline/CeO<Subscript>2</Subscript> composites

Polyaniline (PANI)/CeO₂ composites were prepared by adding CeO₂ powder into the polymerization reaction mixture of aniline. Fourier transform infrared spectra (FTIR) and X-ray diffraction (XRD) were used to characterize the composites. Thermogravimetry (TG) and derivative thermogravimetry (DTG) were used to study the thermal stability of the composites. IR and XRD results show that interaction exists between PANI and CeO₂. This interaction maybe is hydrogen bonding action between the hydroxyl groups on the surface of the CeO₂ and the imine groups in the PANI molecular chains. TG–DTG analysis indicates that the thermal stability of the composites is higher than that of the pure PANI. The improvement in the thermal stability of the composites is attributed to the interaction between PANI and CeO₂, which restricts the thermal motion of PANI chains and shields the degradation of PANI in the composites.     

Thermal stability and glass transition behavior of PANI/MWNT composites

Polyaniline/multi-walled carbon nanotube (PANI/MWNT) composites were prepared by in situ polymerization. Transmission electron microscope (TEM), X-ray diffraction (XRD) and Fourier transform infrared (FTIR) were used to characterize the PANI/MWNT composites. Thermal stability and glass transition temperature (T _g) were measured by thermogravimetry (TG) and temperature modulated differential scanning calorimetry (TMDSC), respectively. The TG and derivative thermogravimetry (DTG) curves indicated that with augment of MWNTs content, the thermal stability of PANI/MWNT composites increased continuously. While, T _g increased and then decreased with the MWNTs content increasing from 0 to 20 mass%.     

Synthesis,characterization, thermal,electrical and magnetic properties of polyaniline composites with rare earth gadolinium coordination complex

Novel polyaniline/gadolinium (PANI/Gd) composites were successfully synthesized by “in‐situ” polymerization at the presence of rare earth Gd coordination complex and D‐tartaric acid (an a dopant). It is rarely to find the studies on related field to add rare earth Gd coordination complex as fillers. Fourier transform infrared (FTIR) spectra, X‐ray diffraction (XRD) and scanning electron microscope (SEM) were used to examine the structure and surface appearance characterization of materials. The thermal stability performance of composites was investigated by thermogravimetry and derivative thermogravimetry (TG‐DTG). Electrochemical performance was measured by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and galvanostatic charge–discharge test. The magnetic property was investigated by physical property measurement system (PPMS). The structure and surface appearance characterization and the magnetic properties jointly demonstrate the polymerization of rare earth Gd coordination complex and PANI–D‐tartrate (DTA) not only simple physical mixing but also chemical mixing. TG‐DTG analysis suggests that thermal stability of PANI/Gd composites is higher than that of PANI–DTA. Electrochemical performance tests and SEM indicate that the composite (PANI/Gd = 3.3:1,mass ratio) has the most regular morphology and best specific capacitance. The magnetization of the composite (PANI/Gd = 3.3:1,mass ratio)is evidently smaller compared with PANI–DTA and rare earth Gd coordination complex. Copyright © 2016 John Wiley & Sons, Ltd.     

Preparation,characterization and thermal decomposition of phenylenediammonium sulfate salts Part. XVI

Polyaniline/α-Al₂O₃ (PANI/α-Al₂O₃) composites were synthesized by in situ polymerization through ammonium persulfate ((NH₄)₂S₂O₈, APS) oxidized aniline using HCl as dopant. XRD and FTIR were used to characterize the PANI/α-Al₂O₃ composites. The thermal stabilities and glass transition temperature (T _g) of PANI/α-Al₂O₃ composites were tested using thermogravimetric (TG) method and modulated differential scanning calorimetry (MDSC) technique. The results of TG showed that the thermal stability of PANI/α-Al₂O₃ composite increased and then decreased with the increase in α-Al₂O₃ content. The derivative thermogravimetry (DTG) curves showed one step degradation of PANI when the α-Al₂O₃ content was lower than 52.5 mass%, and exhibited two steps degradation when the α-Al₂O₃ content was higher than 63.6 mass%. The MDSC curves showed that the T _g of PANI/α-Al₂O₃ composites increased and then decreased with the augment of α-Al₂O₃ for the interaction between PANI chains and the surface of α-Al₂O₃.     

Effect Nd2O3 content on electrochemical performance of polyaniline/Nd2O3 composites

Polyaniline/neodymium(III) oxide (PANI/Nd₂O₃) composites were synthesized by in situ chemical oxidative polymerization method, and the new electrode materials were used for supercapacitor. The composites were characterized physically by scanning electron microscope (SEM), Fourier transform infrared spectra (FTIR) and X‐ray diffraction (XRD). SEM, IR and XRD results showed the existence of interactions between PANI and Nd₂O₃. The electrochemical capacitance performance of the composites was investigated by cyclic voltammetry, galvanostatic charge–discharge tests and ac impedance spectroscopy with a three‐electrode system in 6 M KOH solution. Cyclic voltammetry and galvanostatic charge/discharge tests proved that the addition of Nd₂O₃ enhanced the capacitance of the composites. However, the conductivity of the composites decreases with increasing the amount of Nd₂O₃. Electrochemical impedance tests manifest that the charge‐transfer resistance of the composites is smaller than that of the pure PANI, which indicates the addition of Nd₂O₃ could lower resistance and facilitate the charge transfer of the active materials. All results support that Nd₂O₃ has a significant contribution to the performance of PANI and makes the composites have more active sites for faradiac reaction and larger specific capacitance than pure PANI. Copyright © 2014 John Wiley & Sons, Ltd.     

Synthesis,Characterization and Electrorheological Properties of Polyaniline/Titanate Core-Shell Composite

In this study, a facile method was developed for the preparation of a new conducting polymer composite with core-shell structure. The surfaces of layered titanate (K₂Ti₄O₉) particles were first modified with 3-aminopropyltriethoxysilane, and then a polyaniline/titanate (PANI/K₂Ti₄O₉) composite was synthesized via chemical oxidative polymerization. The resulting composites were characterized by SEM, XRD, FTIR and TG measurements. The results indicated that the PANI deposited on the surface of K₂Ti₄O₉ particles resulted in the formation of the composite with a core-shell structure. TG analysis showed that the composite containing 28.7 wt% PANI had better thermal stability than that of pure PANI. Further, the PANI/K₂Ti₄O₉ composite particles were adopted as a dispersed phase in silicone oil for electrorheological (ER) investigation. Suspension of the composite particles exhibited typical ER behavior subjected to an external electric field under steady and dynamic oscillatory shear.     

Synthesis, characterization and thermal analysis of polyaniline/ZrO2 composites

Conducting polyaniline-zirconium dioxide (PANI/ZrO₂) composites were synthesized by ‘in situ’ deposition technique in the presence of hydrochloric acid (HCl) as dopant by adding the fine grade powder (average particle size of approximately 20 nm) of ZrO₂ into the polymerization reaction mixture of aniline. The composites obtained were characterized by infrared spectra (IR) and X-ray diffraction (XRD) and thermogravimetric analysis (TGA). TG curves and DTG curves of the composites suggest that the thermal degradation process of PANI/ZrO₂ composites proceeds in two-steps and the composites are more thermally stable than that of the pure PANI. The improvement in the thermal stability for the composites is attributed to the interaction between PANI and ZrO₂, which restricts the thermal motion of PANI chains and shields the degradation of PANI in the composites.     

Synthesis,characterization and thermal analysis of polyaniline (PANI)/Co<Subscript>3</Subscript>O<Subscript>4</Subscript> composites

Conducting polyaniline/Cobaltosic oxide (PANI/Co₃O₄) composites were synthesized for the first time, by in situ deposition technique in the presence of hydrochloric acid (HCl) as a dopant by adding the fine grade powder (an average particle size of approximately 80 nm) of Co₃O₄ into the polymerization reaction mixture of aniline. The composites obtained were characterized by infrared spectra (IR) and X-ray diffraction (XRD). The composition and the thermal stability of the composites were investigated by TG-DTG. The results suggest that the thermal stability of the composites is higher than that of the pure PANI. The improvement in the thermal stability for the composites is attributed to the interaction between PANI and nano-Co₃O₄.     

One-step synthesis of PANI/Mn3O4 nanocomposites and evaluation of their electrochemical properties

In this paper, we have developed a simple, facile, and efficient approach to synthesize polyaniline/Mn₃O₄ (PANI/Mn₃O₄) nanocomposites using aniline as a reducer in the presence of KMnO₄ without any additives or templates. The morphology of the composites is characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results demonstrate that the tetrahedral Mn₃O₄ nanoparticles have uniform sizes and are finely dispersed in the PANI matrix. The crystallinity and chemical constituents of the composites are characterized by powder X-ray diffraction (XRD), Fourier transformation infrared spectroscopy (FTIR) and UV-vis spectrophotometry. Moreover, cyclic voltammetry (CV) measurements are used to characterize the electrochemical properties of PANI/Mn₃O₄ nanocomposites. The developed materials give a pair of redox peaks and have better operation stability, which indicates that the composites show distinct electrochemical performance. So the PANI/Mn₃O₄ nanocomposites would have potential applications in bioanalysis, biodetection and so on.     

FTIR and thermal studies on gel grown neodymium tartrate crystals

The growth of neodymium tartrate crystals was achieved in silica gel by single diffusion method. Optimum conditions were established for the growth of good quality crystals. Fourier transform infrared (FT-IR) spectroscopic study indicates the presence of water molecules and tartrate ligands and suggests that tartrate ions are doubly ionised. The thermal behaviour of the material was studied using thermogravimetry (TG), differential thermal analysis (DTA), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). Thermogravimetric analysis support the suggested chemical formula of the grown crystal to be Nd₂(C₄H₄O₆)₃·7H₂O, and the presence of seven water molecules as water of hydration. It is shown that the material is thermally stable up 45 °C beyond which it decomposes through many stages till the formation of neodymium oxide (Nd₂O₃) at 995 °C. The decomposition pattern is reported to be typical of a hydrated metal tartrate.     

Thermal stability and electrochemical performance of Polyaniline/Pr6O11 composites

In order to describe the influence of Pr₆O₁₁ on thermal and electrochemical performance of polyaniline (PANI), PANI/Pr₆O₁₁ composites were synthesized by in situ polymerization in the presence of sulfosalicylic acid (as dopant). The composites obtained was characterized by scanning electron microscope, Fourier transform infrared spectra, and X‐ray diffraction. The thermal stability of the composites was investigated by thermogravimetry and derivative thermogravimetry. Finally, the comparative analysis on the electrochemical properties of PANI/Pr₆O₁₁ composites electrodes, such as cyclic voltammetry, electrochemical impedance spectroscopy, and constant current charge–discharge test, was conducted under similar conditions. Scanning electron microscope, infrared, and X‐ray diffraction results show that interaction exists between PANI and Pr₆O₁₁, and the composites are more crystalline than pure PANI. Thermogravimetry and derivative thermogravimetry analyses indicate that PANI/Pr₆O₁₁ composites and pure PANI have similar thermal stability. Moreover, the studies regarded to capacitive properties show that the electrochemical performance of the composites is improved greatly when Pr₆O₁₁ is added in small amount. However, with increasing the amount of Pr₆O₁₁, the electrochemical performance of the composites become worse, which indicates a large amount of Pr₆O₁₁ has a negative effect on the capacitance. These results suggest that PANI is still in the conductive form after inserting the Pr₆O₁₁, and the capacitance performance of PANI can be improved only by a low percentage of Pr₆O₁₁. Copyright © 2013 John Wiley & Sons, Ltd.     

Ag/PANI/Fe_2O_3复合纳米粒子的合成与催化性能

借助于PANI的还原性质,PANI/Fe2O3复合载体与AgNO3发生表面氧化还原反应,合成了Ag/PANI/Fe2O3复合纳米粒子。TEM和XRD结果表明,立方晶系纳米银的平均粒径10nm。FTIR结果表明,Ag与PANI及Fe2O3复合载体之间不存在化学键合作用,但由于PANI与Ag之间的电子相互作用,Ag/PANI/Fe2O3复合纳米粒子的FTIR吸收峰发生蓝移。Ag/PANI/Fe2O3复合纳米粒子对于间硝基苯磺酸钠的硼氢化钠还原反应表现出良好的催化活性,30min内间硝基苯磺酸钠的转化率达到86.77%。     

Preparation and Characterization of In-Situ Polymerized Nanocomposites Based on Polyaniline in Presence of MWCNTs

Summary: Polyaniline (PANI) composites were prepared with both unmodified and amine modified MWCNTs with and without BaTiO₃ through in-situ oxidative polymerization. Uniform coating of PANI on the MWCNTs and BaTiO₃ surfaces was found which was evident from the Field Emission Scanning Electron Microscopic (FESEM) and High Resolution Transmission Electron Microscopic (HRTEM) images. The structure of pure and amine modified MWCNTs was identified by Fourier Transform Infrared Spectroscopy (FTIR). The thermal stability of the amine modified composite with BaTiO₃ is higher than that of the unmodified composite because of the better affinity between modified MWCNTs and polymer matrix and due to the higher stability of barium titanate itself. The capacitance of amine modified MWCNTs and BaTiO₃ composites was less than that of the pure MWCNTs composites but the thermal stability increased in amine modified MWCNTs and BaTiO₃ composites with respect to the pure MWCNTs composites. The maximum capacitance and energy density values were found in MWCNT/PANI composites which were equal to 523.20 F/g and 142.83 Wh/kg respectively at a scan rate of 10mv/s. Maximum power density was found to be 5147.70 W/kg in the same composite at a scan rate of 200 mv/s.     

Synthesis and characterization of polyaniline–zirconium dioxide and polyaniline–cerium dioxide composites with enhanced photocatalytic degradation of rhodamine B dye

For the first time, chloroform and 2-butanol were used as solvent systems for the preparation of ZrO₂–PANI and CeO₂–PANI composites. Solubility of the synthesized composites was studied in chloroform, N-methyl-2-pyrrolidinone (NMP), and in mixture of toluene?+?2-propanol (2:1). XRD and cyclic voltammetry data showed that the ZrO₂–PANI and CeO₂–PANI composites possess both crystalline and amorphous domains indicating some sort of conductivity. TGA results showed that ZrO₂–PANI composite have a better thermal stability than pure PANI; however, CeO₂–PANI composite has lower thermal stability than pure PANI. The conjugated unsaturated structure of PANI is responsible for the enhanced photocatalytic properties of ZrO₂–PANI and CeO₂–PANI. Photocatalytic results showed that, at photolysis time of 60 min, rhodamine B (RhB) dye was degraded up to 34 and 35% by ZrO₂–PANI and CeO₂–PANI, respectively. The degradation products of RhB were quantified by LC–MS and GC–MS, and accordingly, a detailed pathway was proposed.     

Synthesis, characterization, and thermal study of polyaniline composite with the photoadduct of potassium hexacyanoferrate (II) involving hexamine ligand

The present paper involves the synthesis of polyaniline (PANI) composite with photoadduct of potassium hexacyanoferrate (II) involving hexamine as a ligand and cobalt chloride as a complexing agent via in situ oxidative polymerization by ammonium persulphate. The photoadduct has been synthesized by photoirradiation followed by substitution with the hexamine ligand. The final product has been isolated by using CoCl₂ as complexing agent. Viscosity average molar mass has been determined by viscosity method using Ostwald’s viscometer. The photoirradiation, substitution, and successful synthesis have been proved by recording pH, UV–visible spectra before and after irradiation, and FTIR of the photoadduct. The composite based on the synthesized photoadduct has been subjected to FTIR, X-ray diffraction, and SEM characterization techniques. Thermal analysis has been done by using TG and DSC technique. FTIR absorption peaks confirm the insertion of photoadduct in the backbone of PANI. SEM of the composite also supports its successful synthesis. The XRD of photoadduct shows crystalline structure, which has remained dominant in the composite, hence proving the successful synthesis of PANI composite with photoadduct. Thermal analysis shows high thermal stability of photoadduct which in turn has improved the thermal stability of PANI composite, therefore, shows the potential of composite for high-temperature application purposes.     

MIL-101/P25复合材料的制备及光催化性能

采用水热法,将MIL-101负载到预处理过的P25表面,制得MIL-101/P25复合光催化材料,通过X射线衍射(XRD)、傅里叶变换红外(FTIR)、低温N2物理吸附-脱附(BET)、热重(TG)、场发射透射电镜(FETEM)和光致发光光谱(PL)等对催化剂进行结构表征,同时考察MIL-101及复合材料的稳定性,并且提出协同因子指标来定量评价复合带来的协同效应。结果表明MIL-101呈片状,与P25部分结合。复合后,MIL-101的稳定性得到提高。在适当的配比下,复合具有协同效应,当Cr(NO3)3·9H2O与P25的物质的量之比为1∶1时,复合材料对罗丹明B的可见光催化活性最高,协同因子达到1.64。复合材料对无色有机污染物水杨酸同样表现出良好的光催化效果。     

Use of derived derivative thermogravimetric curves in the compositional study of two-component oxide systems

Reaction between two oxides leading to the formation of a new compound through a change in weight can be studied by TG methods. However, for catalyst preparations, in most of the cases the starting materials are not oxides. The more common methods of coprecipitation or kneading of the precipitated oxides are employed. In such cases the TG and DTG curve of the composites are of a complex nature for several possible reasons including the formation of new compounds. The interpretation of the conventional DTG curve of such a sample and identification of temperature regions for any new thermal activity thus presents problems. For such studies the use of a derived derivative thermogravimetric curve is suggested as described in this paper. This curve indicates the differences between the experimental thermal behaviour of the composite vis-a-vis theoretical thermal behaviour of the composite computed from the thermal behaviour of its constituents. The regions of a new thermal activity can be readily located and interpretated. Two systems are described, MgO-Cr₂O₃ and MgO-Fe₂O₃.     

Temperature dependent electrical conductivity of polyaniline/Y2O3 composites

Composites of polyaniline with yttrium oxide (Y₂O₃) nanoparticles have been prepared by chemical polymerizations method by increasing the weight percentage of yttrium oxide. X-Ray diffraction (XRD) and Fourier Transform Infrared Spectra (FTIR) were used to characterize the composites. XRD and FTIR pattern indicate that Polyaniline (PANI) is intercalated into the layers of Y₂O₃ nanoparticles successfully by in situ polymerization and therefore the degree of crystallinity increases due to crystalline of yttrium oxide nanoparticles. The scanning electron micrographs (SEM) also confirm the formation of dual phase of platelet as well as of flaky structure in PANI-Y₂O₃. Temperature dependant DC conductivity showed three dimensional variable ranges hopping (3D VRH) model. Activation energy, density of states and hopping length are calculated and found to be influenced by intercalating PANI into the layers of Y₂O₃ clay.