scholarly journals SYNTHESIS AND CHARACTERIZATION OF TOLUENE SULFONIC ACID (TSA)-DOPED POLYPYRROLE NANOPARTICLES: EFFECTS OF DOPANT CONCENTRATIONS

Author(s):  
S. Alva ◽  
R. S. Utami ◽  
L. K. Shyuan ◽  
I. Puspasari ◽  
A. B. Mohammad

<p class="TRANSAffiliation"><span>Nanoparticles of the conducting polymer polypyrrole in toluene sulfonic acid (PPy/TSA) were synthesized and characterized. The polymerization was process carried out in situ using ammonium persulfate (APS) as an oxidant. The particles were synthesized by varying the dopant concentration of <em>para</em>-toluene sulfonic acid over five sulphonic acid concentrations. The main objective of this study was to examine the effect of TSA dopant concentrations on the properties of polypyrrole nanoparticles. Understanding nature and characteristics of polypyrrole/TSA nanoparticles are important in determining whether the nanoparticles have the potential to be a component in the manufacture of fuel cells. The conducting polymer particles synthesized in this study were characterized using a particle analyzer, X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), spectroscopy UV-visible (UV-vis), thermogravimetric analysis (TGA) and electrical conductivity measurement. XRD shows that the particles generated possessed an amorphous structure, as also indicated by SEM images revealing the formation of aggregated and granular composite particles. Furthermore, the FTIR peak between 1273 and 1283cm<sup>-1</sup> indicated that sulfonic acids (SO<sub>3</sub><sup>-</sup>) groups were present in the structure of PPy. The size of the PPy/TSA nanoparticles was determined to be approximately 24-51 nm, and their conductivity measured to be 1.3 x 10<sup>-1</sup> S/cm.</span></p>

2021 ◽  
Author(s):  
Songlin Wang ◽  
Qian Wang ◽  
Yao Kai

Abstract Cellulose nanocrystals (CNC) were first isolated from microcrystalline cellulose (MCC) by p-toluene sulfonic acid (p-TsOH) hydrolysis. Cellulose II nanocrystal (CNC II) and cellulose III nanocrystal (CNC III) were then formed by swelling the obtained cellulose I nanocrystal (CNC I) in concentrated sodium hydroxide solutions and ethylenediamine (EDA) respectively. The properties of CNC I, CNC II and CNC III were subjected to comprehensive characterization by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). The results indicated that CNC I, CNC II and CNC III obtained in this research had high crystallinity index and good thermal stability. The degradation temperatures of the resulted CNC I, CNC II and CNC III were 300 ℃, 275 ℃ and 242 ℃, respectively. No ester bonds were found in the resulted CNC. CNC prepared in this research also had large aspect ratio and high negative zeta potential.


2021 ◽  
Vol 21 (4) ◽  
pp. 79-89
Author(s):  
Muhammed Fatih Kılıçaslan ◽  
Yasin Yılmaz ◽  
Bekir Akgül ◽  
Hakan Karataş ◽  
Can Doğan Vurdu

Abstract Alloys of FeNiSiB soft magnetic materials containing variable Fe and Ni contents (wt.%) have been produced by melt spinning method, a kind of rapid solidification technique. The magnetic and structural properties of FeNiSiB alloys with soft magnetic properties were investigated by increasing the Fe ratio. X-ray diffraction analysis and SEM images shows that the produced alloy ribbons generally have an amorphous structure, together with also partially nanocrystalline regions. It was observed that the structure became much more amorphous together with increasing Fe content in the composition. Among the alloy ribbons, the highest saturation magnetization was obtained as 0.6 emu/g in the specimen with 50 wt.% Fe. In addition, the highest Curie temperature was observed in the sample containing 46 wt.% Fe.


BioResources ◽  
2021 ◽  
Vol 16 (2) ◽  
pp. 3186-3199
Author(s):  
Songlin Wang ◽  
Zongjia Song ◽  
Hui He ◽  
Qian Wang

Poplar wood sawdust was chemically modified and separated into fractions using a mixture of p-toluene sulfonic acid (p-TsOH) and formic acid under different conditions. The optimum conditions of poplar lignin separation were determined by single-factor experiment. The mixed acid lignin (MAL) and the solid residues were subjected to comprehensive structural characterization by Fourier-transform infrared spectroscopy (FTIR), proton nuclear magnetic resonance (1H-NMR), X-ray diffraction (XRD), and scanning electron microscope (SEM). At the mass ratio of 5:1 of p-TsOH and formic acid, temperature of 80 °C, acid concentration of 75%, and reaction time of 20 min, more than 80% of lignin was removed, and almost all of the cellulose was retained in the solid residue. The results indicated that the p-TsOH/formic acid achieved rapid and nearly-complete dissolution of wood lignin below the water boiling temperature by enhancing the cleavage of interunitary bonds in lignin (β-O-4′ bond) and the 4-hydroxy-3-methoxy cinnamic acid structure in the lignin.


2019 ◽  
Vol 2019 ◽  
pp. 1-6
Author(s):  
Wenjuan Zhang ◽  
Wenhong Tian ◽  
Shihua Song ◽  
Xianren Zeng ◽  
Peng Gao ◽  
...  

Cinnamaldehyde- (CMA-) modified coal tar pitches (CTPs) are prepared in the presence of acids. In this paper, the effect of boric acid and p-toluene sulfonic acid on the pyrolysis and graphitization process of CMA-modified CTP was studied. The pyrolysis process was studied by Fourier transform infrared spectroscopy, thermogravimetric analysis and derivative thermogravimetry, and polarized-light microscopy. In addition, the graphitization process was studied by X-ray diffraction and Raman spectroscopy. The results indicate the carbon yield of CMA-modified CTP with boric acid as catalyst (B7C10) is higher than that of CMA-modified CTP with p-toluene sulfonic acid as a catalyst (P7C10). In addition, under the same experimental condition (heated at 400°C and held for 1 h), the mesophase spheres of B7C10 are more regular than those of P7C10 and the largest diameter of the mesophase spheres can reach to 40 um. Further, after the graphitization process, the graphitization degree of B7C10 is higher than that of P7C10. So, it is more effective to modify CTP with boric acid as a catalyst.


2017 ◽  
Vol 25 (7) ◽  
pp. 515-520 ◽  
Author(s):  
Hazira Hussin ◽  
Seng Neon Gan ◽  
Sharifah Mohamad ◽  
Sook Wai Phang

Pure polyaniline (PAni) is insoluble in water. Water-soluble complexes of PAni with different of cellulose derivatives were successfully synthesized by using chemical oxidation polymerization of aniline in aqueous solution of cellulose derivatives. In this study, cellulose derivatives such as methylcellulose (MC), hydroxypropyl cellulose (HPC), and hydroxypropyl methylcellulose (HPMC) had been used as a steric stabilizer, aniline (Ani) as a monomer with hydrogen chloride (HCl) as an acidic dopant, and ammonium persulfate (APS) as an initiator. The chemical structure of PAni complexes were confirmed by using Fourier Transform Infrared Spectroscopy (FTIR). The interactions of PAni and cellulose derivatives were observable through Ultraviolet-Visible Spectroscopy (UV-Vis) in the wavelength range of 300 nm to 900 nm. The Standard Four-Point Probe Method was used for the conductivity measurements. In the electrical conductivity measurement, PAni in toluene was used as a control. The result showed that water-soluble PAni-cellulose derivatives gave higher conductivity value (9.47 × 10−2 – 1.87 × 10−1 S/cm) than the pristine PAni (1.60 × 10−3 S/cm).


2010 ◽  
Vol 96 ◽  
pp. 221-226
Author(s):  
Hong Juan Sun ◽  
Ying Liu ◽  
Tong Jiang Peng ◽  
Hai Feng Liu ◽  
Jin Mei Sun

A series of polyaniline/vermiculite nanocomposites was synthesized. The interlayer space of vermiculite was initially increased by the insertion of dioctadecyl dimethyl ammonium bromide, and then the aniline monomers were inserted into the interlayer space of vermiculite replacing dioctadecyl dimethyl ammonium cations. The polyaniline/vermiculite nanocomposites materials were prepared via in situ polymerization of the aniline monomers in the interlayer space of vermiculite. The as-synthesized polyaniline/vermiculite nanocomposite materials were characterized by X-ray diffraction analysis, infrared spectroscopy, and electrical conductivity measurement. The results indicated that the vermiculite was peeled off into the polyaniline. The introduction of vermiculite nanosheets showed a beneficial effect on the electrical conductivity of polyaniline.


e-Polymers ◽  
2007 ◽  
Vol 7 (1) ◽  
Author(s):  
Wu Yan ◽  
Xing Shuangxi ◽  
Jing Shengyu ◽  
Zhou Teili ◽  
Zhao Chun

AbstractWe reported a chemical approach for the in-situ preparation of conducting polyaniline (PANI)/Fe2O3 composite dispersions using dodecylbenzene sulfonic (DBSA) acid both as dopant and surfactant. The PANI/Fe2O3 composite dispersions were characterized by X-ray diffraction, UV-vis and FT-IR spectra and conductivity measurement. The dispersions showed good stability and existed without precipitate for at least half a year. The gas-sensing behavior of the composite film to 100 ppm of NH3 was studied through monitoring the change of the resistance.


2019 ◽  
Vol 17 (40) ◽  
pp. 67-76
Author(s):  
Ali A-K. Hussain

Optical properties of Rhodamine-B thin film prepared by PLDtechnique have been investigated. The absorption spectra using1064nm and 532 nm laser wavelength of different laser pulseenergies shows that all the curves contain two bands, B band and Qbands with two branches, Q1 and Q2 band and a small shift in thepeaks location toward the long wavelength with increasing laserenergy. FTIR patterns for Rhodamine-B powder and thin film withinshows that the identified peaks were located in the standard valuesthat done in the previous researches. X-ray diffraction patterns ofpowder and prepared Rhodamine-B thin film was display that thepowder has polycrystalline of tetragonal structure, while the thin filmhas an amorphous structure. SEM images for Rhodamine-B, showshomogeneous distributed cauliflower-like nanostructures attachedwith each other. FM diagram shows that the average grain size wasfound to be 68.52 nm and the RMS surface roughness was 1.68 nm.


2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Anurag Krishna ◽  
Amit Kumar ◽  
Rajiv Kumar Singh

Polypyrrole (PPy) nanoparticles were synthesized via microemulsion polymerization technique using sodium dodecyl sulfate as surfactant. Polyvinyl alcohol (PVA) was added as soft template during polymerization to modify the structure and properties of PPy nanoparticles. The synthesized materials namely, PVA-free and PVA added were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and DC electrical conductivity measurements. The sample synthesized in the presence of PVA has longer conjugation length as estimated from FT-IR investigation. Temperature dependence (4.2–300 K) of DC electrical conductivity measurement reveals that the PVA has a strong effect on the polymerization mechanism of PPy giving evidence of H-bonded assistance during polymerization leading to the synthesis of better ordered polymer. A growth mechanism has been proposed which explains the H-bonded assistance of PPy polymerization leading to enhanced structural ordering.


Author(s):  
G. A. Bertero ◽  
W.H. Hofmeister ◽  
N.D. Evans ◽  
J.E. Wittig ◽  
R.J. Bayuzick

Rapid solidification of Ni-Nb alloys promotes the formation of amorphous structure. Preliminary results indicate promising elastic properties and high fracture strength for the metallic glass. Knowledge of the thermal stability of the amorphus alloy and the changes in properties with temperature is therefore of prime importance. In this work rapidly solidified Ni-Nb alloys were analyzed with transmission electron microscopy (TEM) during in-situ heating experiments and after isothermal annealing of bulk samples. Differential thermal analysis (DTA), scanning electron microscopy (SEM) and x-ray diffraction (XRD) techniques were also used to characterize both the solidification and devitrification sequences.Samples of Ni-44 at.% Nb were electromagnetically levitated, melted, and rapidly solidified by splatquenching between two copper chill plates. The resulting samples were 100 to 200 μm thick discs of 2 to 3 cm diameter. TEM specimens were either ion-milled or alternatively electropolished in a methanol-10% sulphuric acid solution at 20 V and −40°C.


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