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      • KCI등재

        Facile diazonium modification of pomegranate peel biochar: a stupendous derived relationship between thermal and Raman analyses

        Khalil Ahmed M.,Msaadi Radhia,Sassi Wafa,Ghanmi Imen,Pires Rémy,Michely Laurent,Snoussi Youssef,Chevillot-Biraud Alexandre,Lau-Truong Stéphanie,Chehimi Mohamed M. 한국탄소학회 2022 Carbon Letters Vol.32 No.6

        There is an ever growing interest in the development of biochar from a large variety of agrowastes. Herein, the main objective is the conversion of pomegranate peel powder biochar and its post-functionalization by phosphoric acid treatment, followed by arylation organic reaction. The latter was conducted using in situ-generated diazonium salts of 4-aminobenzoic acid (H2N-C6H4-COOH), sulfanilic acid (H2N-C6H4-SO3H) and Azure A dye. The effect of diazonium nature and concentration on the arylation process was monitored using thermal gravimetric analysis (TGA) and Raman spectroscopy, scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). SEM pictures showed micrometer-sized biochar particles with tubular structure having about 10–20 µm-wide channels. SEM studies have shown that arylation did not affect the morphology upon arylation. The porous structure did not collapse and withstood the arylation organic reaction in acid medium did not collapse upon arylation. TGA and Raman indicated gradual changes in the arylation of biochar at initial concentrations 10–5, 10–4 and 10–3 mol L−1 of 4-aminobenzoic acid. The detailed Raman spectra peak fittings indicate that the D/G peak intensity ratio leveled off at 3.35 for 4-aminobenzoic acid initial concentration of 10–4 mol L−1, and no more change was observed, even at higher aryl group mass loading. This is in line with formation of oligoaryl grafts rather than the grafting of new aryl groups directly to the biochar surface. Interestingly, Azure A diazonium salt induced much lower extent of surface modification, likely due to steric hindrance. To the very best of our knowledge, this is the first report on diazonium modification of agrowaste-derived biochar and opens new avenues for arylated biochar and its applications.

      • KCI등재

        Highly Ammonia Sensing Using Direct In Situ Electro-Deposited Polypyrrole-Dodecylbenzene Sulfonic Acid Film on ITO Coated Flexible Substrates

        Fateh Merdj,Ahmed Mekki,Djamil Guettiche,Boualem Mettai,Zakaria Bekkar Djeloul Sayah,Zitouni Safidine,Abderrazak Abdi,Rachid Mahmoud,Mohamed M. Chehimi 한국고분자학회 2018 Macromolecular Research Vol.26 No.6

        Air quality monitoring is of major concern as it is directly linked to public health. It requires the development of high sensitive devices with fast response towards hazardous gas and volatile compounds. Such performances depend on the nature and quality of deposition of the sensing layer. Herein, adherent polypyrroledodecylbenzene sulfonic acid (PPy–DBSA) films were deposited on a N-(3-trimethoxysilylpropyl) pyrrole modified ITO coated polyethylene teraphtalate (PET) flexible substrate by facile direct electrochemical oxidation of pyrrole in an aqueous solution of sulfonic acid. The obtained PPy-DBSA films were subjected to various characterization techniques such as, FTIR, Raman, SEM and conductivity measurements. Chemiresistive gas sensing tests have demonstrated selectivity and sensitivity of films toward ammonia vapors over the other vapors (nitrogen dioxide, carbon dioxide, hydrogen sulfide, acetone, methanol and ethanol) with higher response at 20 ppm, reasonably fast response time of 3 min and reaching detection limit of 3ppm. The response of the sensor can reasonably be related to the strong electrostatic interactions between vapor molecules and the dopant agents within PPy films. In comparison PPy- DBSA films prepared on pristine ITO/PET has exhibited lower response at 20 ppm of ammonia exposure, which highlights the role of surface modification and the contribution from the dopant agent nature for ammonia sensing. Moreover, chemiresistive response performances have been tested in the presence of humidity, under varied temperatures, and finally their behaviors were featured by an impedance spectroscopy in both presence and absence of gas. This work conclusively shows that the sensing performances are not only driven by the molecular interactions between the sensor and the analyte but also by the quality of deposition and adhesion of the former to the transducer. The latter feature can be controlled by appropriate chemical surface modification.

      • KCI등재

        Highly Ammonia Sensing Using Direct In Situ Electro-Deposited Polypyrrole-Dodecylbenzene Sulfonic Acid Film on ITO Coated Flexible Substrates

        Fateh Merdj,Ahmed Mekki,Djamil Guettiche,Boualem Mettai,Zakaria Bekkar Djeloul Sayah,Zitouni Safidine,Abderrazak Abdi,Rachid Mahmoud,Mohamed M. Chehimi 한국고분자학회 2018 Macromolecular Research Vol.25 No.6

        Air quality monitoring is of major concern as it is directly linked to public health. It requires the development of high sensitive devices with fast response towards hazardous gas and volatile compounds. Such performances depend on the nature and quality of deposition of the sensing layer. Herein, adherent polypyrroledodecylbenzene sulfonic acid (PPy–DBSA) films were deposited on a N-(3-trimethoxysilylpropyl) pyrrole modified ITO coated polyethylene teraphtalate (PET) flexible substrate by facile direct electrochemical oxidation of pyrrole in an aqueous solution of sulfonic acid. The obtained PPy-DBSA films were subjected to various characterization techniques such as, FTIR, Raman, SEM and conductivity measurements. Chemiresistive gas sensing tests have demonstrated selectivity and sensitivity of films toward ammonia vapors over the other vapors (nitrogen dioxide, carbon dioxide, hydrogen sulfide, acetone, methanol and ethanol) with higher response at 20 ppm, reasonably fast response time of 3 min and reaching detection limit of 3ppm. The response of the sensor can reasonably be related to the strong electrostatic interactions between vapor molecules and the dopant agents within PPy films. In comparison PPy- DBSA films prepared on pristine ITO/PET has exhibited lower response at 20 ppm of ammonia exposure, which highlights the role of surface modification and the contribution from the dopant agent nature for ammonia sensing. Moreover, chemiresistive response performances have been tested in the presence of humidity, under varied temperatures, and finally their behaviors were featured by an impedance spectroscopy in both presence and absence of gas. This work conclusively shows that the sensing performances are not only driven by the molecular interactions between the sensor and the analyte but also by the quality of deposition and adhesion of the former to the transducer. The latter feature can be controlled by appropriate chemical surface modification.

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