X-Ray Photoelectron Spectroscopy Study on Reduction of Graphene Oxide with Hydrazine Hydrate

2011 ◽  
Vol 287-290 ◽  
pp. 539-543 ◽  
Author(s):  
Wen Shi Ma ◽  
Jun Wen Zhou ◽  
Xiao Dan Lin
Keyword(s):  
Graphene Oxide ◽  
Hydrazine Hydrate ◽  
Photoelectron Spectroscopy ◽  
Reduction Rate ◽  
Reduction Reaction ◽  
Chemical Compositions ◽  
Total Oxygen ◽  
Graphene Oxides ◽  
X Ray ◽  
Oxygen Groups

Graphene oxide was prepared through Hummers' method，then different reduced graphenes were prepared via reduction of graphene oxide with hydrazine hydrate for 1h、12h and 24h. X-ray photoelectron spectroscopy (XPS) was used for the characterization of graphene oxide and the reduced graphenes. The variation of the contents of carbon in carbon and oxygen functional groups and chemical compositions of graphene oxides were investigated through analysis the content of different carbon atoms in different reduced graphenes. The results showed that the reduction reaction was very fast in the first 1 h, the content of total oxygen bonded carbon atoms decreased from 83.6% to 22.1%, and then after the reduction rate became very slow. After 12h, the content of total oxygen bonded carbon atom is 19.56%, only 2.54% lower than that of 1h’s. At the same time, C-N was introduced in the graphene oxides; this increased the stereo-hindrance for hydrazine hydrate attacking the C-Oxygen groups, thus reduced the reduction rate. After reduction for 24h, there still exists 16.4% oxygen bonded carbon atoms and the total conversion ratio of graphene approaches 70%.

scholarly journals Characterization of Graphite Oxide and Reduced Graphene Oxide Obtained from Different Graphite Precursors and Oxidized by Different Methods Using Raman Spectroscopy Statistical Analysis

Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 769
Author(s):  
Roksana Muzyka ◽  
Sabina Drewniak ◽  
Tadeusz Pustelny ◽  
Marcin Sajdak ◽  
Łukasz Drewniak
Keyword(s):  
Raman Spectroscopy ◽  
Graphene Oxide ◽  
Statistical Analysis ◽  
Reduced Graphene Oxide ◽  
Graphite Oxide ◽  
Photoelectron Spectroscopy ◽  
Graphene Oxides ◽  
Preparation Methods ◽  
X Ray ◽  
Reduced Graphene

In this paper, various graphite oxide (GO) and reduced graphene oxide (rGO) preparation methods are analyzed. The obtained materials differed in their properties, including (among others) their oxygen contents. The chemical and structural properties of graphite, graphite oxides, and reduced graphene oxides were previously investigated using Raman spectroscopy (RS), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD). In this paper, hierarchical clustering analysis (HCA) and analysis of variance (ANOVA) were used to trace the directions of changes of the selected parameters relative to a preparation method of such oxides. We showed that the oxidation methods affected the physicochemical properties of the final products. The aim of the research was the statistical analysis of the selected properties in order to use this information to design graphene oxide materials with properties relevant for specific applications (i.e., in gas sensors).

scholarly journals Synthesis and Electrochemical Study of Three-Dimensional Graphene-Based Nanomaterials for Energy Applications

Nanomaterials ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 1295
Author(s):  
Antony R. Thiruppathi ◽  
Boopathi Sidhureddy ◽  
Emmanuel Boateng ◽  
Dmitriy V. Soldatov ◽  
Aicheng Chen
Keyword(s):  
Energy Storage ◽  
Energy Conversion ◽  
Photoelectron Spectroscopy ◽  
Electrode Materials ◽  
High Surface ◽  
Three Dimensional ◽  
Reduction Reaction ◽  
Chemical Compositions ◽  
Supercapacitor Electrode ◽  
X Ray

Graphene is an attractive soft material for various applications due to its unique and exclusive properties. The processing and preservation of 2D graphene at large scales is challenging due to its inherent propensity for layer restacking. Three-dimensional graphene-based nanomaterials (3D-GNMs) preserve their structures while improving processability along with providing enhanced characteristics, which exhibit some notable advantages over 2D graphene. This feature article presents recent trends in the fabrication and characterization of 3D-GNMs toward the study of their morphologies, structures, functional groups, and chemical compositions using scanning electron microscopy, X-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. Owing to the attractive properties of 3D-GNMs, which include high surface areas, porous structures, improved electrical conductivity, high mechanical strength, and robust structures, they have generated tremendous interest for various applications such as energy storage, sensors, and energy conversion. This article summarizes the most recent advances in electrochemical applications of 3D-GNMs, pertaining to energy storage, where they can serve as supercapacitor electrode materials and energy conversion as oxygen reduction reaction catalysts, along with an outlook.

scholarly journals X-ray Photoelectron Spectroscopy Analysis of Chitosan–Graphene Oxide-Based Composite Thin Films for Potential Optical Sensing Applications

Polymers ◽  
2021 ◽  
Vol 13 (3) ◽  
pp. 478
Author(s):  
Wan Mohd Ebtisyam Mustaqim Mohd Daniyal ◽  
Yap Wing Fen ◽  
Silvan Saleviter ◽  
Narong Chanlek ◽  
Hideki Nakajima ◽  
...  
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Graphene Oxide ◽  
Photoelectron Spectroscopy ◽  
Functional Group ◽  
Optical Sensing ◽  
Composite Thin Films ◽  
Cobalt Ions ◽  
X Ray ◽  
Sensing Applications

In this study, X-ray photoelectron spectroscopy (XPS) was used to study chitosan–graphene oxide (chitosan–GO) incorporated with 4-(2-pyridylazo)resorcinol (PAR) and cadmium sulfide quantum dot (CdS QD) composite thin films for the potential optical sensing of cobalt ions (Co2+). From the XPS results, it was confirmed that carbon, oxygen, and nitrogen elements existed on the PAR–chitosan–GO thin film, while for CdS QD–chitosan–GO, the existence of carbon, oxygen, cadmium, nitrogen, and sulfur were confirmed. Further deconvolution of each element using the Gaussian–Lorentzian curve fitting program revealed the sub-peak component of each element and hence the corresponding functional group was identified. Next, investigation using surface plasmon resonance (SPR) optical sensor proved that both chitosan–GO-based thin films were able to detect Co2+ as low as 0.01 ppm for both composite thin films, while the PAR had the higher binding affinity. The interaction of the Co2+ with the thin films was characterized again using XPS to confirm the functional group involved during the reaction. The XPS results proved that primary amino in the PAR–chitosan–GO thin film contributed more important role for the reaction with Co2+, as in agreement with the SPR results.

scholarly journals Pore Modification and Phosphorus Doping Effect on Phosphoric Acid-Activated Fe-N-C for Alkaline Oxygen Reduction Reaction

Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1519
Author(s):  
Jong Gyeong Kim ◽  
Sunghoon Han ◽  
Chanho Pak
Keyword(s):  
Phosphoric Acid ◽  
Photoelectron Spectroscopy ◽  
Structural Changes ◽  
Electronic States ◽  
Nitrogen Adsorption ◽  
Reduction Reaction ◽  
Phosphorus Doping ◽  
X Ray ◽  
Precious Metal Catalysts ◽  
Adsorption Desorption

The price and scarcity of platinum has driven up the demand for non-precious metal catalysts such as Fe-N-C. In this study, the effects of phosphoric acid (PA) activation and phosphorus doping were investigated using Fe-N-C catalysts prepared using SBA-15 as a sacrificial template. The physical and structural changes caused by the addition of PA were analyzed by nitrogen adsorption/desorption and X-ray diffraction. Analysis of the electronic states of Fe, N, and P were conducted by X-ray photoelectron spectroscopy. The amount and size of micropores varied depending on the PA content, with changes in pore structure observed using 0.066 g of PA. The electronic states of Fe and N did not change significantly after treatment with PA, and P was mainly found in states bonded to oxygen or carbon. When 0.135 g of PA was introduced per 1 g of silica, a catalytic activity which was increased slightly by 10 mV at −3 mA/cm2 was observed. A change in Fe-N-C stability was also observed through the introduction of PA.

scholarly journals Structure and Characterization of TiC/GLC Multilayered Films with Various Bilayers Periods

Coatings ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 787
Author(s):  
Weiqi Wang ◽  
Xiaoming Ling ◽  
Rui Wang ◽  
Wenhao Nie ◽  
Li Ji ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Chemical Compositions ◽  
Closed Field ◽  
Multilayered Structures ◽  
Multilayered Films ◽  
Sputtering Deposition ◽  
X Ray ◽  
Mechanical And Tribological Properties ◽  
Self Organizing

The spontaneously self-organizing multilayered graphite-like carbon (denoted as GLC) /TiC films with various bilayer periods in the range of 13.3–17.5 nm were deposited on silicon and 1Cr18Mn8Ni5N stainless steel substrates using closed field magnetron sputtering deposition facility. The microstructures and chemical compositions of the prepared multilayered films were characterized by scanning electron microscopy, high resolution transmission electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy respectively. The self-organizing multilayered structures in all of the films consisted of titanium carbide layers and sp2-rich carbon layers periodically alternate arrangement. The TiC contents and bilayer periods of the multilayered films can be controlled by means of adjusting of sputtering current of graphite target. Furthermore, the mechanical and tribological performances of the prepared films were appraised by nano-indentor, scratch measures, and ball-on-plate tribometer respectively. The results indicated that multilayer structure endowed the as-deposited TiC/GLC films outstanding mechanical and tribological properties, especially the multilayer film with 15.9 nm bilayer period deposited at 10 A sputtering current showed the excellent adhesion strength and hardness; Simultaneously it also exhibited the lowest average friction coefficient in the humid environment owing to its high content of sp2 hybrid carbon.

scholarly journals Analysis of Reduced Graphene Oxides by X-ray Photoelectron Spectroscopy and Electrochemical Capacitance

2013 ◽  
Vol 42 (8) ◽  
pp. 924-926 ◽  
Author(s):  
Michio Koinuma ◽  
Hikaru Tateishi ◽  
Kazuto Hatakeyama ◽  
Shinsuke Miyamoto ◽  
Chikako Ogata ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Graphene Oxides ◽  
Electrochemical Capacitance ◽  
X Ray ◽  
Reduced Graphene ◽  
Reduced Graphene Oxides

Well-Aligned Graphene Oxide Nanosheets Decorated with Zinc Oxide Nanocrystals for High Performance Photocatalytic Application

2015 ◽  
Vol 14 (03) ◽  
pp. 1550007 ◽  
Author(s):  
K. Kaviyarasu ◽  
C. Maria Magdalane ◽  
E. Manikandan ◽  
M. Jayachandran ◽  
R. Ladchumananandasivam ◽  
...  
Keyword(s):  
Zinc Oxide ◽  
Graphene Oxide ◽  
High Performance ◽  
Chemical Reduction ◽  
Visible Region ◽  
Single Layer ◽  
Single Layer Graphene ◽  
Graphene Oxides ◽  
X Ray ◽  
Nanoscale Structures

Graphene oxide (GO) nanosheets modified with zinc oxide nanocrystals were achieved by a green wet-chemical approach. As-obtained products were characterized by XRD, Raman spectra, XPS, HR-TEM, EDS, PL and Photocatalytic studies. XRD studies indicate that the GO nanosheet have the same crystal structure found in hexagonal form of ZnO . The enhanced Raman spectrum of 2D bands confirmed formation of single layer graphene oxides. The gradual photocatalytic reduction of the GO nanosheet in the GO : ZnO suspension of ethanol was studied by using X-ray photoelectron (XPS) spectroscopy. The nanoscale structures were observed and confirmed using high resolution transmission electron microscopy (HR-TEM). The evolution of the elemental composition, especially the various numbers of layers were determined from energy dispersive X-ray spectra (EDS). PL properties of GO : ZnO nanosheet were found to be dependent on the growth condition and the resultant morphology revealed that GO nanosheet were highly transparent in the visible region. The photocatalytic performance of GO : ZnO nanocomposites was performed under UV irradiation. Therefore, the ZnO nanocrystals in the GO : ZnO composite could be applied in gradual chemical reduction and consequently tuning the electrical conductivity of the graphene oxide nanosheet.

Ternary Composite of Molybdenum Disulfide-Graphene Oxide-Polyaniline for Supercapacitor

2021 ◽  
Author(s):  
Ke Qu ◽  
Yuqi Bai ◽  
Miao Deng
Keyword(s):  
Graphene Oxide ◽  
Molybdenum Disulfide ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Light Emitting Diode ◽  
Rate Capability ◽  
Energy Storage And Conversion ◽  
Carbon Paper ◽  
Power Sources ◽  
X Ray

Abstract The ever-increasing need for small and lightweight power sources for use in portable or wearable electronic devices has spurred the development of supercapacitors as a promising energy storage and conversion system. In this work, a simple, facile and easy-to-practice method has been developed to employ carbon paper (CP) as the support to coat molybdenum disulfide (MoS2) and graphene oxide (GO), followed by electrodeposition of polyaniline (PANI) to render CP/MoS2-GO-PANI. The preparation parameters, such as amounts of MoS2, GO and number of aniline electropolymerization cycles, have been optimized to render CP/MoS2-GO-PANI the best capacitive performance. The as-prepared optimal CP/MoS2-GO-PANI is characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive spectroscopy, and X-ray photoelectron spectroscopy. The supercapacitive properties of CP/MoS2-GO-PANI as an electrode have been evaluated electrochemically via cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectroscopy testing. CP/MoS2-GO-PANI delivers a specific capacitance of 255.1 F/g at 1.0 A/g and exhibits excellent rate capability under larger current densities. Moreover, a symmetrical supercapacitor is assembled and three are connected in series to power a light-emitting diode for ~15 minutes, demonstrating the promising application potential of CP/MoS2-GO-PANI-based supercapacitor.

Characterization of X-ray irradiated graphene oxide coatings using X-ray diffraction, X-ray photoelectron spectroscopy, and atomic force microscopy

2013 ◽  
Vol 28 (2) ◽  
pp. 68-71 ◽  
Author(s):  
Thomas N. Blanton ◽  
Debasis Majumdar
Keyword(s):  
Atomic Force Microscopy ◽  
Graphene Oxide ◽  
Photoelectron Spectroscopy ◽  
High Energy ◽  
X Ray Diffraction ◽  
Carbon Phase ◽  
X Ray ◽  
Force Microscopy ◽  
Atomic Force ◽  
Before And After

In an effort to study an alternative approach to make graphene from graphene oxide (GO), exposure of GO to high-energy X-ray radiation has been performed. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM) have been used to characterize GO before and after irradiation. Results indicate that GO exposed to high-energy radiation is converted to an amorphous carbon phase that is conductive.

scholarly journals Mechanisms of Two-Electron and Four-Electron Electrochemical Oxygen Reduction Reactions at Nitrogen-Doped Reduced Graphene Oxide

2019 ◽  
Author(s):  
Hyo Won Kim ◽  
Vanessa Jane Bukas ◽  
Hun Park ◽  
Sojung Park ◽  
Kyle M. Diederichsen ◽  
...  
Keyword(s):  
Oxygen Reduction ◽  
Photoelectron Spectroscopy ◽  
Active Sites ◽  
Isotope Effects ◽  
Underlying Mechanism ◽  
Reduction Reaction ◽  
Graphene Oxides ◽  
Nitrogen Doped ◽  
General Chemical ◽  
Reduced Graphene

Doped carbon-based systems have been extensively studied over the past decade as active electrocatalysts for both the two-electron (2e-) and four-electron (4e-) oxygen reduction reaction (ORR). However, the mechanisms for ORR are generally poorly understood. Here we report an extensive experimental and first-principles theoretical study of the ORR at nitrogen-doped reduced graphene oxides (NrGO). We synthesize three distinct NrGO catalysts and investigate their chemical and structural properties in detail via X-ray photoelectron spectroscopy, infrared and Raman spectroscopy, high-resolution transmission electron microscopy and thin-film electrical conductivity. ORR experiments include the pH dependences of 2e- versus 4e- ORR selectivity, ORR onset potentials, Tafel slopes and H/D kinetic isotope effects. These experiments show very different ORR behavior for the three catalysts, both in terms of selectivity and the underlying mechanism which proceeds either via coupled proton-electron transfers (CPETs) or non-CPETs. Reasonable structural models developed from DFT rationalize this behavior. The key determinant between CPET vs. non-CPET mechanisms is the electron density at the Fermi level under operating ORR conditions. Regardless of the reaction mechanism or electrolyte pH, however, we identify the ORR active sites as sp2 carbons that are located next to oxide regions. This assignment highlights the importance of oxygen functional groups, while details of (modest) N-doping may still affect the overall catalytic activity, and likely also the selectivity, by modifying the general chemical environment around the active site.

Sign in / Sign up

Export Citation Format

Share Document