X-ray Photoelectron Spectroscopic Study of Petroleum Fuel Cokes

Mateos, Jesús; Fierro, J.L.G.

doi:10.1002/(sici)1096-9918(199604)24:4<223::aid-sia105>3.0.co;2-m

Cited by 85 publications

(17 citation statements)

References 72 publications

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“…We assume here, that the N1 to N4 nitrogen species that are identified from the peak fitting shown in Figures 4b and 4c are the same in nature in both of the annealed materials. Indeed, the N1 to N4 binding energies for both of the annealed materials are, respectively, quite close to each other, and the differences observed (Figures 4b and 4c) lie in the range of those reported in the literature for those kinds of nitrogen sites on different nitrogen-doped carbon nanomaterials [24,25]. Based on the numerous literature related to nitrogen functionalities studied by N1s core level XPS analysis in carbon-based materials [23][24][25][26][27], N1 is attributed to N-Pyridinic, N2 to N-Pyrrole, and N3 and N4 to N-Graphitics, referred as center N-Graphitic and valley N-Graphitic, respectively.…”

Section: Synthesis and Characterization Of The As Formed And Annealed Materialssupporting

confidence: 78%

“…It seems reasonable to draw a parallel between our results and those recorded by XPS, when carbon is thermally treated with ammonia [17][18][19][20][21][22][23]. This literature reports that many different kinds of nitrogen functionalities can be formed in such conditions, among them, functionalities grafted at the edges of graphene planes, such as amine, imine, amide, and nitrile ones, which cover the wide N1s core level binding energy range [24]. These binding energies overlap with those recorded for the nitrogen species directly grafted in the graphene planes, such as of pyridine, pyrrole, and so-called graphitic N-sites.…”

Section: Synthesis and Characterization Of The As Formed And Annealed Materialssupporting

confidence: 76%

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Highly Active, High Specific Surface Area Fe/C/N ORR Electrocatalyst from Liquid Precursors by Combination of CO2 Laser Pyrolysis and Single NH3 Thermal Post-Treatment

Pérez

Jorda

Vigneron

et al. 2019

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This paper reports original results on the synthesis and characterization of Fe/C/N ORR electrocatalysts obtained by a combination of CO2 laser pyrolysis and thermal post-treatment. The precursor liquid media, consisting in a 14 g·L−1 iron III acetylacetonate solution in toluene, was aerosolized and then exposed to a CO2 laser beam for pyrolysis in continuous flow. Ammonia was used in the pyrolysis process, both as the laser wavelength absorbing gas (i.e., energy transfer agent) and as the sole source of nitrogen. After the laser pyrolysis step, the material was submitted to thermal post-treatment under argon on the one hand, and ammonia on another hand. The three materials—one as-prepared, one thermally treated under argon, and one thermally treated under ammonia—were characterized, in particular, through specific surface area determination, XPS analysis, and ORR measurement. It was found that both kinds of thermal treatment significantly improved the ORR performances, which were evaluated on porous electrodes. Indeed, while the as-prepared material showed an ORR onset potential at ≈790 mV vs. the standard hydrogen electrode (SHE) in HClO4 1M, the argon treatment increased the latter to ≈820 mV, and the ammonia treatment led to a very high value of ≈910 mV. Selectivities of 3.65 and 3.93 were measured for the argon and ammonia treated materials, respectively. The outstanding ORR performance resulting from the ammonia treatment is probably related to the very high BET specific surface area measured at 1130 m2·g−1, which was notably obtained without using any templating or sacrificial component in the precursor media.

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Section: Synthesis and Characterization Of The As Formed And Annealed Materialssupporting

confidence: 78%

Section: Synthesis and Characterization Of The As Formed And Annealed Materialssupporting

confidence: 76%

Highly Active, High Specific Surface Area Fe/C/N ORR Electrocatalyst from Liquid Precursors by Combination of CO2 Laser Pyrolysis and Single NH3 Thermal Post-Treatment

Pérez

Jorda

Vigneron

et al. 2019

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“…Pristine PB-PEDOT demonstrates peaks at 398.5 and 400.3 eV, which are pyridinic-type nitrogen and pyrrolic-type nitrogen, respectively. After the pyrolysis, part of the structure was transferred to cyanide and quaternary-type nitrogen at 399.4 and 401.4 eV, respectively. − Quaternary-type nitrogen increased the limiting current density; it was proposed that this type of nitrogen structure reduces the carbon band gap energy, which actually influenced the ORR ability. − While pyridinic-type nitrogen converted the ORR to the ideal process of four-electron, improving the onset potential, it claimed that the nitrogen structure modified the band structure of carbon, raised the density of π states near the Fermi level, and reduced the work function. − FeCN-S-800 has much higher pyridinic-type and quaternary-type nitrogen content. Additionally, only FeCN-S-1000 displays the cyan groups content compared to others.…”

Section: Results and Discussionmentioning

confidence: 99%

Nanostructured Cementite/Ferrous Sulfide Encapsulated Carbon with Heteroatoms for Oxygen Reduction in Alkaline Environment

Huang

Wang

et al. 2019

ACS Sustainable Chem. Eng.

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Nonprecious metal catalysts of the oxygen reduction reaction (ORR) are highly preferred in anion exchange membrane fuel cells (AEMFCs) because of the high stability and low cost. Here, a novel pyrolyzed poly(3,4ethylene dioxythiophene) hydrate (PEDOT)-Prussian blue (PB) catalyst (FeCN-S) for the ORR in an AEMFC cathode demonstrated high catalytic performance. After pyrolysis at 800 °C, the templated PB-PEDOT formed the nanostructured Fe 3 C/FeS encapsulated carbon with heteroatom contribution, which exhibited optimized ORR activity with a direct fourelectron transfer pathway for AEMFC applications. This improvement in activity is attributed to the specific structure, the heteroatom contribution, and the coordination structure.

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“…In this study, the S 2p spectra were measured to compare the sulfur form distribution in SO 2 -activated cokes. Based on previous information reported by other researchers, the binding energy of sulfur species can be arranged in increasing order as follows: metal sulfide < thiols < elemental sulfur < organic sulfide < thiophene < sulfoxide < sulfone < sulfonate < sulfate. − Furthermore, there are overlaps between certain sulfur forms such as thiophene and elemental sulfur, and extreme caution should be exercised to distinguish them. The XPS spectrum of S 2p for raw petroleum coke can be found in Figure S1.…”

Section: Results and Discussionmentioning

confidence: 99%

Impact of Nonoxidized Sulfur Species on Elemental Mercury Removal by SO₂ Activated Petroleum Cokes

et al. 2020

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High-sulfur petroleum coke is potentially one of the most promising materials for developing efficient and low-cost sorbents for Hg0 removal from flue gas. In this study, three distinct SO2-activated high-sulfur petroleum cokes were prepared at 650–850 °C via different sulfurization protocols, including SO2-impregnated petroleum coke (PC-S), SO2-impregnated coke produced with an additional reductive heat-treatment process in N2 (PC-NS), and SO2-impregnated coke prepared with the presence of SO2 in the gas during the cooling process (PC-SC). The SO2-activated cokes were characterized with nitrogen adsorption/desorption measurements, X-ray photoelectron spectroscopy, thermogravimetric analysis, and their mercury removal performances were investigated in a fixed-bed reactor at 80–200 °C with an initial mercury concentration of 35–120 μg/m3. To explore the influence of nonoxidized sulfur species on Hg0 removal, particular focus was given to the comparison of the reduced sulfur, sulfide sulfur, and elemental sulfur formed during different sulfurization processes, as well as the consequent differences in Hg0 adsorption characteristics. It found that the sulfur incorporated into the carbon matrix of PC-S by interaction with SO2 at 650 °C was dominantly organic sulfide. Thermal treatment in N2 at 800 °C led to an addition of reduced sulfur in PC-NS. An increment of 0.74 at. % elemental sulfur was observed in PC-SC after exposure to SO2 during the cooling step. The Hg0 adsorption capacity of PC-SC at low temperatures was significantly enhanced, yielding a mercury capacity of 622 μg/g at 80 °C. However, elemental sulfur suffered from severe temperature sensitivity for mercury binding. The sample PC-NS which contained more reduced sulfur showed the highest Hg0 adsorption capacity at elevated temperatures above 160 °C. Furthermore, the increment in inlet mercury concentration would lead to higher adsorption capacities and faster adsorption rates. According to the R L obtained from Langmuir isotherms, the Hg0 adsorption reactivity can be arranged as follows: PC-NS > PC-S > PC-SC. The mercury temperature-programmed desorption results suggested that sulfur species not only had an effect on Hg0 adsorption capacity but also played an essential role in the thermal stability of the adsorbed mercury compounds. Mercury was principally associated with elemental sulfur in the form of metacinnabar and combined with thermal-stable organic sulfide in cinnabar or organomercuric compounds Hg–SR.

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X-ray Photoelectron Spectroscopic Study of Petroleum Fuel Cokes

Cited by 85 publications

References 72 publications

Highly Active, High Specific Surface Area Fe/C/N ORR Electrocatalyst from Liquid Precursors by Combination of CO2 Laser Pyrolysis and Single NH3 Thermal Post-Treatment

Highly Active, High Specific Surface Area Fe/C/N ORR Electrocatalyst from Liquid Precursors by Combination of CO2 Laser Pyrolysis and Single NH3 Thermal Post-Treatment

Nanostructured Cementite/Ferrous Sulfide Encapsulated Carbon with Heteroatoms for Oxygen Reduction in Alkaline Environment

Impact of Nonoxidized Sulfur Species on Elemental Mercury Removal by SO₂ Activated Petroleum Cokes

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X-ray Photoelectron Spectroscopic Study of Petroleum Fuel Cokes

Cited by 85 publications

References 72 publications

Highly Active, High Specific Surface Area Fe/C/N ORR Electrocatalyst from Liquid Precursors by Combination of CO2 Laser Pyrolysis and Single NH3 Thermal Post-Treatment

Highly Active, High Specific Surface Area Fe/C/N ORR Electrocatalyst from Liquid Precursors by Combination of CO2 Laser Pyrolysis and Single NH3 Thermal Post-Treatment

Nanostructured Cementite/Ferrous Sulfide Encapsulated Carbon with Heteroatoms for Oxygen Reduction in Alkaline Environment

Impact of Nonoxidized Sulfur Species on Elemental Mercury Removal by SO2 Activated Petroleum Cokes

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Impact of Nonoxidized Sulfur Species on Elemental Mercury Removal by SO₂ Activated Petroleum Cokes