Structural and morphological characterization of Poly(o-ethoxyaniline) Emeraldine-salt form using FTIR, XRD, LeBail Method and SEM

Soares, Juliana Coatrini; Mafud, Ana Carolina; Souza, Sérgio Michielon de; Fernandes, Edson Giuliani Ramos; Mascarenhas, Yvonne P.; Sanches, Edgar Aparecido

doi:10.1016/j.molstruc.2014.04.039

Cited by 27 publications

(8 citation statements)

References 30 publications

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“…Nevertheless it has been used to characterize some polymeric materials [16][17][18][19][20]. In order to be able to estimate R factors related to integrated intensities, Rietveld [21] stated: ''a fair approximation to the observed integrated intensity can be made by separating the peaks according to the calculated values of the integrated intensities, i.e.…”

Section: Le Bail Methodsmentioning

confidence: 99%

Rigid and semi rigid polyurethane resins: A structural investigation using DMA, SAXS and Le Bail method

Trovati

Sanches

Souza

et al. 2014

Journal of Molecular Structure

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Section: Le Bail Methodsmentioning

confidence: 99%

Rigid and semi rigid polyurethane resins: A structural investigation using DMA, SAXS and Le Bail method

Trovati

Sanches

Souza

et al. 2014

Journal of Molecular Structure

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“…[47,48] to obtain structural information from semicrystalline patterns is not very common due to the large overlapped peaks on diffractograms. Nevertheless, it has been used to characterize some conducting polymers as polyaniline and substituted polyanilines [49][50][51]. This process uses iteratively the Rietveld decomposition formula for whole powder pattern decomposition (WPPD) in the FullProf program package [52].…”

Section: X-ray Diffraction and Crystallinity Estimativementioning

confidence: 99%

Nanostructured Polypyrrole Powder: A Structural and Morphological Characterization

Sanches

Alves

Soares

et al. 2015

Journal of Nanomaterials

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Polypyrrole (PPY) powder was chemically synthesized using ferric chloride (FeCl3) and characterized by X-ray diffraction (XRD), Le Bail Method, Fourier Transform Infrared Spectrometry (FTIR), and Scanning Electron Microscopy (SEM). XRD pattern showed a broad scattering of a semicrystalline structure composed of main broad peaks centered at 2θ= 11.4°, 22.1°, and 43.3°. Crystallinity percentage was estimated by the ratio between the sums of the peak areas to the area of amorphous broad halo due to the amorphous phase and showed that PPY has around 20 (1)%. FTIR analysis allowed assigning characteristic absorption bands in the structure of PPY. SEM showed micrometric particles of varying sizes with morphologies similar to cauliflower. Crystal data (monoclinic, space group P 21/c,a=7.1499(2) Å,b=13.9470(2) Å,c=17.3316(2) Å,α=90 Å,β=61.5640(2) Å andγ=90 Å) were obtained using the FullProf package program under the conditions of the method proposed by Le Bail. Molecular relaxation was performed using the density functional theory (DFT) and suggests that tetramer polymer chains are arranged along the “c” direction. Average crystallite size was found in the range of 20 (1) Å. A value of 9.33 × 10−9 S/cm was found for PPY conductivity.

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“…Several parameters influence on the mobility of counter ions along the polymer chains in ICP materials. These factors are mainly related to the (i) synthesis methodology [32][33][34], (ii) regular packing of the polymer chains (or polymer crystallinity), (iii) ring side group at the ortho, meta, or para positions [8,[35][36][37], and (iv) the nature of the doping acid and counter ion size [38], as well as (v) the possible chemical and/or physical interactions between counter ions and ring side groups [39].…”

Section: Electrical Conductivitymentioning

confidence: 99%

“…For this reason, the present study evaluated the crystal structure of POMA maintained at 100 • C (TT 100 ) and 200 • C (TT 200 ) in order to provide a systematic evaluation of the crystalline phase modification. The structural, spectroscopic, and morphological aspects of heat-treated semi-crystalline materials continue to be an interesting topic of research [8][9][10][11][12][13].…”

Section: Introductionmentioning

confidence: 99%

Poly(o-methoxyaniline) Chain Degradation Based on a Heat Treatment (HT) Process: Combined Experimental and Theoretical Evaluation

et al. 2022

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Poly(o-methoxyaniline) emeraldine-salt form (ES-POMA) was chemically synthesized using hydrochloric acid and subjected to a heat treatment (HT) process for 1 h at 100 °C (TT100) and 200 °C (TT200). The HT process promoted a progressive decrease in crystallinity. The Le Bail method revealed a decomposition from tetrameric to trimeric-folded chains after the HT process. The unheated POMA-ES presented a globular vesicular morphology with varied micrometric sizes. The heat treatment promoted a reduction in these globular structures, increasing the non-crystalline phase. The boundary length (S) and connectivity/Euler feature (χ) parameters were calculated from the SEM images, revealing that ES-POMA presented a wide distribution of heights. The TT100 and TT200 presented a narrow boundary distribution, suggesting smoother surfaces with smaller height variations. The UV-VIS analysis revealed that the transition at 343 nm (nonlocal π → π*) was more intense in the TT200 due to the electronic delocalization, which resulted from the reduced polymer chain caused by the HT process. In addition to the loss of conjugation, counter ion withdrawal reduced the ion-chain interaction, decreasing the local electron density. This result shows the influence of the chlorine counter ions on the peaks position related to the HOMO → LUMO transition, since the π → polaron transition occurs due to the creation of the energy states due to the presence of counter ions. Finally, the electrical conductivity decreased after the HT process from 1.4 × 10−4 S.cm−1 to 2.4 × 10−6 S.cm−1 as result of the polymer deprotonation/degradation. Thus, this paper proposed a systematic evaluation of the POMA molecular structure and crystallite size and shape after heat treatment.

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Structural and morphological characterization of Poly(o-ethoxyaniline) Emeraldine-salt form using FTIR, XRD, LeBail Method and SEM

Cited by 27 publications

References 30 publications

Rigid and semi rigid polyurethane resins: A structural investigation using DMA, SAXS and Le Bail method

Rigid and semi rigid polyurethane resins: A structural investigation using DMA, SAXS and Le Bail method

Nanostructured Polypyrrole Powder: A Structural and Morphological Characterization

Poly(o-methoxyaniline) Chain Degradation Based on a Heat Treatment (HT) Process: Combined Experimental and Theoretical Evaluation

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