SYNTHESIS AND CHARACTERIZATION OF POLY(P-ANISIDINE) BY X-RAY DIFFRACTION AND SCANNING ELECTRON MICROSCOPY.

Published in 12/12/2023 - ISBN: 978-65-272-0088-8

Paper Title
SYNTHESIS AND CHARACTERIZATION OF POLY(P-ANISIDINE) BY X-RAY DIFFRACTION AND SCANNING ELECTRON MICROSCOPY.
Authors
  • Diogo de Carvalho Menezes
  • YVONNE PRIMERANO MASCARENHAS
  • Pedro Henrique de Oliveira Santiago
  • EDGAR SANCHES
Modality
Pôster
Subject area
Síntese e caracterização de materiais
Publishing Date
12/12/2023
Country of Publishing
Brasil
Language of Publishing
Inglês
Paper Page
https://www.even3.com.br/anais/workshop-do-ineo-2023/612943-synthesis-and-characterization-of-poly(p-anisidine)-by-x-ray-diffraction-and-scanning-electron-microscopy
ISBN
978-65-272-0088-8
Keywords
methoxianiline, structure, XRD, refinement, SEM
Summary
Introduction Despite electrical, thermal, structural, and morphological properties of ortho– and meta–substituted poly(methoxyaniline) have been widely reported, there are significant lack of systematic research on PPA. Several studies have focused p-anisidine (PPA) monomers, but only few reports have been devoted to investigate the polymerization process and PPA potential applications. Materials and Methods Standard chemical oxidative polymerization of p-anisidine was performed at two different temperatures, i.e., at 4°C and 25°C. In both cases, Solution I was prepared by solubilizing 2.0 g of p-anisidine monomer in HCl 1M (125 mL), and Solution II was obtained by adding 4.0 g of ammonium persulfate also in HCl 1M (125mL). Solution II was incorporated dropwise to Solution I under constant stirring. After 3 hours, the dark powder was vacuum filtered, washed with distilled water, and kept in a desiccator until reach constant weight. The resulting materials were labeled PPA4 and PPA25. X-ray diffraction of both PPAs were obtained from Rigaku RotaFlex diffractometer, with a rotating anode tube, a multilayer mirror monochromator, CuKa radiation, ? = 1.54 Å, 40 kV, and 20 mA. The scan mode was performed with 0.02°/s step, velocity of 5°/min, in the 2? = 3 – 100° interval and identical results were obtained. Whole Powder Pattern Decomposition A tridimensional model for the molecular structure of the monomer was obtained using the program MolView® and hoping that the packaging of the molecules in the crystal might be similar in the semi-crystalline phase of the polymer, several tentative unit cell parameters were obtained from a search of similar molecular structures reported in the Cambridge Crystallographic Data Center (CCDC). The better fitting of the X-ray diffraction (XRD) pattern of PPA25 was obtained from the crystalline structure of end-capped polyaniline single crystals, corresponding to Space Group P1 ¯. Taking into consideration that the repeating unit in the polymer crystal should contain more than one monomer, that unit cell had to be adapted for a tetrameric model and a repeating unit with 2 tetramers per asymmetric unit, cell dimensions equal to a=10.000 Å, b=20.000 Å, c=20.000 Å, alpha=84.00°, beta= 92.00° and gamma= 94.00°. This choice of unit cell also yields good agreement with average value of polymer density. The software package FullProf® was then used to perform the Whole Powder Pattern Decomposition (WPPD) and the least squares refinement of the initial cell parameters using the Le Bail method resulting in final agreement indices of a=10.043 Å, b=20.160 Å, c=17.205 Å, alpha=85.16°, beta= 92.34° and gamma= 95.49°. Scanning Electron Microscopy (SEM) Analysis Powdered samples were placed on a carbon tape and covered with a thin gold layer. SEM images were taken at 25°C on a Carl Zeiss Supra 35 microscope using 4.0 kV showing interesting but complex structures that deserve an in-depth and systematic evaluation. Images shows the surface of PPA basically formed by elongated structures (needles up to a few micrometers in length) arranged on a matrix of undefined morphology. Further Perspectives Other characterizations are in progress with pure and doped PPA with Eu2O3 nanoparticles using (a) ATR-FTIR analyses in order to find out the changes in molecular interactions between the polymer and the nanoparticles and (b) UV-Vis spectroscopy in order to detect changes in the photophysical properties of the polymer due to its interaction with the nanoparticles.
Title of the Event
Workshop do INEO 2023
City of the Event
Nazaré Paulista
Title of the Proceedings of the event
Anais do Workshop INEO 2023
Name of the Publisher
Even3
Means of Dissemination
Meio Digital

How to cite

MENEZES, Diogo de Carvalho et al.. SYNTHESIS AND CHARACTERIZATION OF POLY(P-ANISIDINE) BY X-RAY DIFFRACTION AND SCANNING ELECTRON MICROSCOPY... In: Anais do workshop INEO 2023. Anais...Nazaré Paulista(SP) Hotel Estância Atibainha, 2023. Available in: https//www.even3.com.br/anais/workshop-do-ineo-2023/612943-SYNTHESIS-AND-CHARACTERIZATION-OF-POLY(P-ANISIDINE)-BY-X-RAY-DIFFRACTION-AND-SCANNING-ELECTRON-MICROSCOPY. Access in: 10/11/2024

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