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Graphene, as strict two-dimensional material, exhibits exceptionally good electronic properties. In this paper, graphene was prepared on SiC substrates at different temperature based on two types of pre-treated surface. The surface morphology was characterized by atomic force microscopy (AFM) and scanning electronic microscopy (SEM). The results on SiC surface pre-treatment showed that chemical mechanical polishing (CMP) was an effective surface treatment method for reproducible and controlled growth of graphene. Images of the Si-surface revealed that the thickness of graphitic layers increased with annealing temperature. Meanwhile, a mesh-like network of wrinkles tended to tent-like features with the increase of temperature. The residual stresses, average crystallite size and number of graphene layers were analyzed by Raman spectroscopy. Little shift of 2D-band indicated the presence of certain stresses. Results among four samples showed that graphene layers grown on MP C-surface substrates had the thickest layers，contained the smallest average crystallite size La and exhibited no stresses. While graphene layers grown on Si-surface under 1600°C built upon compressive stresses, exhibited largest La and least number of graphene layers, indicating perfect quality.

MXene films are attractive for advanced supercapacitor electrodes requiring high volumetric energy density due to their high redox capacitance combined with extremely high packing density. However, the self‐restacking of MXene flakes unavoidably decreases the volumetric performance, mass loading, and rate capability. Herein, a simple strategy is developed to prepare a flexible and free‐standing modified MXene/holey graphene film by filtration of the alkalized MXene and holey graphene oxide dispersions, followed by a mild annealing treatment. After terminal groups (—F/—OH) are removed, the increased proportion of Ti atoms enables more pseudocapacitive reaction. Meanwhile, the embedded holey graphene effectively prevents the self‐restacking of MXene and forms a high nanopore connectivity network, which is able to immensely accelerate the ion transport and shorten transport pathways for both ion and electron. When applied as electrode materials for supercapacitors, it can deliver an ultrahigh volumetric capacitance (1445 F cm−3) at 2 mV s−1, excellent rate capability, and high mass loading. In addition, the assembled symmetric supercapacitor demonstrates a fantastic volumetric energy density (38.6 Wh L−1), which is the highest value reported for MXene‐based electrodes in aqueous electrolytes. This work opens a new avenue for the further exploration of MXene materials in energy storage devices.

In this research, the influence of anionic surfactant sodium dodecyl sulfate (SDS), pH, substrate finishing, and annealing temperature on the surface morphology and hardness of the electroless nickel phosphorus (ENi–P) coatings were studied. Taguchi’s experimental design method was used. Parameters selected in three levels and L9 from orthogonal robust array design were employed. Surface roughnesses of the deposits were measured using a stylus instrument. Scanning electron microscope and x-ray diffraction analysis were implemented to study surface morphologies and phase composition, respectively. Microhardness of the ENi–P deposits was measured using a microhardness tester at three trials per sample. The results showed that addition of the SDS increases the microhardness and improves surface morphology. Finally, optimum condition was achieved as, surfactant concentration equal to 1.5 g/L, pH 5.5, substrate finishing provided with emery paper no. 2000, and annealing temperature equal to 400°C.

The thermal transport properties of graphene are strongly influenced by its contact environment and the strength of such interactions can be used to tailor these properties. Here we find that annealing suppresses the basal plane thermal conductivity (κ) of graphene supported on silicon dioxide, due to the increased conformity of graphene to the nanoscale asperities of the substrate after annealing. Intriguingly, increasing the polycrystallinity of graphene, grown by chemical vapor deposition on copper, increases the severity of this suppression after annealing, revealing the role of grain boundaries and associated defects in aiding phonon scattering by the substrate. In highly polycrystalline graphene, the value of κ after annealing is comparable to that after significant fluorination of an identical unannealed sample. Our experiments employ the suspended micro-bridge platform for basal plane thermal conductivity measurements. Using xenon difluoride gas for the final release also enables the investigation of thermal transport in graphene in contact with polymers. We find evidence for weaker phonon scattering in graphene, due to a 10 nm thick polymer layer on top compared to the pre-existing silicon dioxide substrate, which is a promising result for flexible electronics applications of graphene.

Cryogenic treatments are increasingly used to improve the wear resistance of various steel alloys by means of transformation of retained austenite, deformation of virgin martensite and carbide refinement. In this work the nanotribological behavior and mechanical properties at the nano-scale of cryogenically and conventionally treated AISI 420 martensitic stainless steel were evaluated. Conventionally treated specimens were subjected to quenching and annealing, while the deep cryogenically treated samples were quenched, soaked in liquid nitrogen for 2 h and annealed. The elastic–plastic parameters of the materials were assessed by nanoindentation tests under displacement control, while the friction behavior and wear rate were evaluated by a nanoscratch testing methodology that it is used for the first time in steels. It was found that cryogenic treatments increased both hardness and elastic limit of a low-carbon martensitic stainless steel, while its tribological performance was enhanced marginally. Fil: Prieto, Germán. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Bahía Blanca; Argentina. Universidad Nacional del Sur. Departamento de Ingeniería; Argentina Fil: Bakoglidis, Konstantinos D.. Linköping University; Suecia Fil: Tuckart, Walter Roberto. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Bahía Blanca; Argentina. Universidad Nacional del Sur. Departamento de Ingeniería; Argentina Fil: Broitman, Esteban. Linköping University; Suecia

Since graphene and their composites play significant roles in the catalysts, energy storage, electronics and other fields, where electron transport is highly critical, here, we introduce reduced graphene oxide (RGO) interfaces in the carbon fiber (CF) networks for preparing a novel lightweight carbon fiber/reduced graphene oxide/nickel (CF-RGO-Ni) composite textile. Upon the charaterizations on the microscopic morphologies, electrical and magnetic properties, and density, the presence of RGO nanosheets and nickel nanoparticles would substantially influence the related physical properties in the resulting composite textiles. Furthermore, the key parameters, including RGO loading, deposition time, current density and annealing temperature of carbon matrices, have been studied to understand their effects on the electrochemical deposition of nickel nanoparticles. Implication of the results suggests that the RGO interface is a unique medium for essentially promoting the electrochemical deposition kinetics and active sites for growing nickel nanoparticles, which indicates a universal approach for preparing advanced lightweight composites with the presence of graphene naonstructures.

Thin films with high thermal conductivity are urgently needed as heat dissipation materials for electronic devices. In this study, we developed a readily scalable roller coating method followed by ultra-high temperature annealing to prepare large-sized, free-standing, and flexible reduced graphene oxide (rGO) films with high thermal conductivity. The in-plane thermal conductivity measured by a laser flash method for the sample annealed at 2800 °C was 826.0 W m−1 K−1, which was much higher than that of copper foil. X-ray diffraction, Raman, and SEM analyses indicated that, different from common chemical reduction, heat treatment at high temperature could not only remove O, H, and other impure elements but also develop the in-plane crystal size of graphene and decrease the interlayer spacing of graphene sheets. Meanwhile, tight embedding during annealing and concomitant mechanical impaction was indispensable for retaining the shape and raising the density of the films. Furthermore, molecular dynamics analyses demonstrated that point defects, pentagonal/heptagonal defects, or even large in-plane holes in graphene could be rehabilitated to a great extent during ultra-high temperature annealing. In addition, real-time temperature monitoring demonstrated that the rGO films could act as an excellent thermal dissipation material in LED packages by reducing 10%–15% of the temperature increase.

A novel hybrid cathode interlayer (CIL) consisting of reduced graphene oxide and zinc oxide (ZnO) is realized in the inverted organic solar cells (OSCs). A dual-nozzle spray coating system and facile one-step in situ thermal reduction/annealing (ITR/ITA) method are introduced to precisely control the components of the CIL, assemble ZnO with graphene oxide, and reduce graphene oxide into in situ thermal reduced graphene oxide (IT-RGO), simultaneously. The ZnO:IT-RGO hybrid CIL shows high electric conductivity, interconnecting nanostructure, and matched energy level, which leads to a significant enhancement in the power conversion efficiency from 6.16% to 8.04% for PTB7:PC71BM and from 8.02% to 9.49% for PTB7-Th:PC71BM-based OSCs, respectively. This newly developed spray-coated ZnO:IT-RGO hybrid CIL based on one-step ITR/ITA treatment has the high potential to provide a facile pathway to fabricate the large-scale, fast fabrication, and high performance OSCs.

Wrinkle-free graphene was used to form the source–drain electrodes in thin film transistors based on a zinc tin oxide (ZTO) semiconductor. A 10 nm thick titanium adhesion layer was applied prior to transferring a conductive graphene film on top of it by chemical detachment. The formation of an interlayer oxide between titanium and graphene allows the achievement of uniform surface roughness over the entire substrate area. The resulting devices were thermally treated in ambient air, and a substantial decrease in field effect mobility is observed with increasing annealing temperature. The increase in electrical resistivity of the graphene film at higher annealing temperatures may have some influence, however the growth of the oxide interlayer at the ZTO/Ti boundary is suggested to be most influential, thereby inducing relatively high contact resistance.

WOS: 000461138500012, Three different graphite-based powders (expandable graphite and two different nano-graphite powders) were investigated as starting materials for an effective liquid phase exfoliation process in isopropyl alcohol (IPA). The prepared dispersions were analyzed and compared in terms of their graphene concentration, stability, number of graphene layers and quality, as well as the electrical conductivity of the prepared graphene-based materials. Good quality graphene dispersions (I-D/I-G < 0.3) with a relatively high concentration (similar to 1.1 mg/ml) were prepared in IPA within 90 min sonication time by utilizing a high specific surface area (similar to 175 m(2)/g) nano-graphite powder derived from natural graphite. Transmission electron microscope analyses of this sample revealed mostly folded and scrolled few layer graphene (FLG) sheets (, Anadolu University Scientific Research Projects Commission [1110F155, 1101F005], The financial support for this study by Anadolu University Scientific Research Projects Commission (under the project numbers of 1110F155 and 1101F005) is gratefully acknowledged. The authors also thank to Dr. Pascal Puech (CEMES, Toulouse) for discussions on Raman analyses and to Lucien Datas for TEM analyses which were performed at R. Castaing characterization platform, UMS 3623.

Vanadium oxide films amorphous, nonstoichiometric and highly absorbing in the optical region were deposited on ITO-coated glass and on silicon substrates, by the hot-filament metal oxide deposition technique (HFMOD) and oxidized by ex-situ annealing in a furnace at 200, 300, 400 and 500 ºC, under an atmosphere of argon and rarefied oxygen. X-ray diffraction, Raman and Rutherford backscattering spectroscopy as well as optical transmission were employed to characterize the amorphous and annealed films. When annealed at 200 and 300 ºC the as-deposited opaque films become transparent but still amorphous. Under treatments at 400 and 500 ºC a crystalline nonstoichiometric V2O5 structure is formed. All the annealed films became semiconducting, with their optical absorption coefficients changing with the annealing temperature. An optical gap of 2.25 eV was measured for the films annealed at 400 and 500 ºC. The annealing in rarefied oxygen atmosphere proved to be a useful and simple ex-situ method to modulate the structural and optical properties of vanadium oxide films deposited by HFMOD technique. This technique could be applied to other amorphous and non-absorbing oxide films, replacing the conventional and sometimes expensive method of modulate desirable film properties by controlling the film deposition parameters. Even more, the HFMOD technique can be an inexpensive alternative to deposit metal oxide films.

This work is focused on graphene preparation using the segregation method with Co/SiC structure, the method being a viable low temperature synthesis approach. The graphene preparation was carried out with the cobalt layer of 300 nm thickness; the technological process is based on an optimization of parameters (temperature and duration) of annealing which is a crucial step of the synthesis. 850 °C as an annealing temperature and 10 s as an annealing duration have been found to be the most optimal. The prepared graphene is close to the bi-layer graphene structure with its parameters. Structural parameters of the prepared graphene were determined from spectra obtained by Raman spectroscopy.

Graphene oxide (GO) has been recognized as an important intermediate compound for a potential low-cost large-scale graphene-like film fabrication. In this work, graphene oxide multilayer films deposited on glass substrate were reduced using different thermal reduction methods, including low-temperature annealing, flame-induced and laser reduction, and the corresponding surface morphology and structural properties were investigated. These graphene oxide thermal reduction methods strongly affected surface morphology and differently facilitated structural and chemical transformations of graphene oxide. As evidenced by Raman measurements, thermal annealing and laser reduction of graphene oxide produced more ordered graphene-like structure multilayer films. However, surface morphological differences were observed and attributed to the different de-oxidation mechanisms of GO. This Letter provides an important systematic comparison between the GO reduction methods and thermally-driven structural changes they provide to the reduced GO multilayer films obtained.

We have investigated the effect of annealing of graphene sheets on the electrical properties of Au/graphene/n-type silicon Schottky diode. Large scale graphene sheets were grown by chemical vapor deposition and then annealed at 300, 400, and 500 °C; one sheet was left un-annealed as the control. The diodes were fabricated by transferring the graphene sheets directly onto n-type Si substrates and the current – voltage ( I–V ) and capacitance – voltage ( C–V ) characteristics were evaluated. The average values of the Schottky barrier height (SBH) and ideality factor ( η ) for the as-fabricated Au/graphene/n-type silicon Schottky diode from I–V measurements were determined to be ∼0.8 ± 0.01 eV and ∼1.79 ± 0.05, respectively, whereas the SBH from C–V measurements was ∼0.89 ± 0.01 eV. The electrical transport characteristics measured at room temperature indicated that annealing of graphene sheet prior to the transfer of the graphene onto the n-Si substrates significantly reduces the electric degradation of the Schottky diodes, even though no distinct differences in other electric properties, including ideality factors and SBHs, before or after annealing of the graphene sheets were observed. Thus, by simply annealing the graphene sheets at 500 °C, we found that the Au/graphene/n-type silicon Schottky diode showed an approximately 3.3-fold lower series resistance as compared with the un-annealed Schottky diode under air exposure of up to 7 days. These annealed diodes showed significantly reduced electrical degradation by removing the potentially trapped H 2 O and/or O 2 at the interface between the graphene layer and the n-Si substrate.

Graphene sheets decorated with Au nanodots are synthesized by deposition of Au of three different thicknesses and subsequent annealing at 400 °C. Different thicknesses of Au film for the formation of Au nanodots on graphene are measured using Rutherford backscattering spectrometry and morphology is studied using scanning electron microscopy. Raman spectroscopy indicates 3–6-fold increase in I D / I G ratio depending on the content of Au deposited on graphene. The increase in disorder in Au decorated graphene layers is explained on the basis of interaction of Au atoms with Π bonds of graphene. The splitting and blueshift in G band signifies compressive strain in Au deposited graphene. X-ray diffraction studies using synchrotron radiation source confirm compressive strain in graphene, which increases with increase of Au film thickness.

Optical antennas are devices that efficiently convert the energy of free propagating radiation into localized energy and vice versa. The development of optical antennas can improve the efficiency of sensing, photodetection, light emission, and spectroscopy. Graphene rings are a promising material for advanced optical antennas because their plasmons are more electromagnetically confined than metallic plasmons. In this report, we describe the growth of embedded and protrusive graphene rings by annealing Si-terminated 6H–SiC under Ar gas. We found that the growth of the graphene rings depends on both the annealing temperature and the ambient Ar pressure. A bottom–up fabrication method can preserve intact ring edges unlike electron-beam lithographic methods. Moreover, the growth of protrusive graphene rings without bonding between the ring edge and the SiC substrate is emphasized because the ring edge structures are similar to those of free-standing graphene rings, and this provides a new option for graphene applications on Si-terminated SiC. Copyright © 2014 John Wiley & Sons, Ltd.

The industrial scale application of graphene and other functional materials in the field of electronics has been limited by inherent defects, and the lack of simple deposition methods. A simple spray deposition method is developed that uses a supersonic air jet for a commercially available reduced graphene oxide (r-GO) suspension. The r-GO flakes are used as received, which are pre-annealed and pre-hydrazine-treated, and do not undergo any post-treatment. A part of the considerable kinetic energy of the r-GO flakes entrained by the supersonic jet is used in stretching the flakes upon impact with the substrate. The resulting “frozen elastic strains” heal the defects (topological defects, namely Stone-Wales defect and C2 vacancies) in the r-GO flakes, which is reflected in the reduced ratio of the intensities of the D and G bands in the deposited film. The defects can also be regenerated by annealing.

The mechanism of dense vertically aligned carbon nanotube growth achieved by a recently developed thermal chemical vapor deposition method was studied using synchrotron radiation spectroscopic techniques., The mechanism of the one-order-of-magnitude increase in the density of vertically aligned carbon nanotubes (CNTs) achieved by a recently developed thermal chemical vapor deposition process was studied using synchrotron radiation spectroscopic techniques. In the developed process, a Ti film is used as the underlayer for an Fe catalyst film. A characteristic point of this process is that C2H2 feeding for the catalyst starts at a low temperature of 450°C, whereas conventional feeding temperatures are ∼800°C. Photoemission spectroscopy using soft and hard X-rays revealed that the Ti underlayer reduced the initially oxidized Fe layer at 450°C. A photoemission intensity analysis also suggested that the oxidized Ti layer at 450°C behaved as a support for nanoparticle formation of the reduced Fe, which is required for dense CNT growth. In fact, a CNT growth experiment, where the catalyst chemical state was monitored in situ by X-ray absorption spectroscopy, showed that the reduced Fe yielded a CNT forest at 450°C. Contrarily, an Fe layer without the Ti underlayer did not yield such a CNT forest at 450°C. Photoemission electron microscopy showed that catalyst annealing at the conventional feeding temperature of 800°C caused excess catalyst agglomeration, which should lead to sparse CNTs. In conclusion, in the developed growth process, the low-temperature catalyst activation by the Ti underlayer before the excess Fe agglomeration realised the CNT densification.

Capacitive deionization (CDI) is a competent water desalination technique offering an appropriate route to obtain clean water. However, a rational designed structure of the electrode materials is essentially required for achieving high CDI performance. Here, a novel sponge-templated strategy is developed for the first time to prepare graphene sheets with high specific surface area and suitable pore size distribution. Sponge is used as the support of graphene oxide to prevent the restack of graphene sheets, as well as to suppress the agglomerate during the annealing process. Importantly, the as-fabricated graphene sheets possess high specific surface area of 305 m2 g−1 and wide pore size distribution. Ultrahigh CDI performance, a remarkable electrosorptive capacity of 4.95 mg g−1, and siginificant desorption rate of 25 min, is achieved with the sponge-templated prepared graphene electrodes. This work provides an effective solution for the synthesis of rational graphene architectures for general applications in CDI, energy storage and conversion.

We propose microwave-induced annealing as a rapid, simple, and effective method of controlling surface doping and strain in graphene. Raman spectroscopy was used to confirm that heavy and uniform p-type (1.2 × 1013 cm−2) doping can be achieved within only 5 min without unintended defects by placing graphene onto a substrate with a sufficiently high dielectric constant and exposing graphene and its substrate to microwave irradiation. Further, we showed that ripples are formed in suspended graphene when it is exposed to microwave irradiation. Silicon has a sufficiently high dielectric constant (11.9) and graphene is commonly deposited on silicon-based substrates, so our proposed microwave-induced annealing technique can be used for the rapid manipulation of the properties of graphene at low cost.

We show that interface tailoring is an effective approach towards high performance G/Si Schottky-barrier solar cells. Inserting a thin graphene oxide (GO) interfacial layer can improve the efficiency of graphene/silicon solar cells by >100%. The role of the GO interfacial layer is systematically investigated by varying the annealing temperature and thickness of the GO film. It is found that GO cannot be treated as the common thought, i.e., an insulator. In other words, the G/GO/Si solar cell is not suitable to be treated as a “MIS” cell. In contrast, it should be regarded as a p-doped thin layer. The effects of GO film thickness on device response are also studied and there exists an optimal thickness for device performance. A record 12.3% (device size: 3 × 3 mm2) power conversion efficiency is achieved by further performance optimization (chemical doping graphene and antireflection coating).

High temperature deposition of graphene on Cu by chemical vapor deposition can be used to produce high quality films. However, these films tend to have a non-equilibrium structure, with relatively low graphene adhesion. In this study, samples of graphene grown on copper foils by high temperature CVD were post-deposition annealed at temperatures well below the critical temperature of Cu. Resistance to etching under plasma was examined to assess the mechanical robustness of the graphene on the Cu surface, analyzed using optical and Raman microscopies. We found a correlation between the post-annealing time and etching time for the complete removal of graphene from Cu. Etching rates, minimum etch times, and surface appearance were observed to vary depending on the etching plasma (air, oxygen or nitrogen). Oxygen plasmas were found to be the least aggressive, emphasizing the improved adhesion with post-annealing treatments. Our results imply that the etching of graphene on Cu, and hence the adhesion of graphene, can be controlled by proper annealing and choice of plasma gas.

An effective way of synthesizing graphene-wrapped Li4Ti5O12 particles was developed by solid-state reaction between graphene oxide-wrapped P25 (TiO2) and Li2CO3. Compared to the previously reported graphene/Li4Ti5O12 composites, prior wrapping of TiO2 with subsequent chemical lithiation led to more effectively confined Li4Ti5O12. The Li4Ti5O12 tightly bound by graphene exhibited a remarkable specific capacity of 147 mA h g−1 at a rate of 10 C (1 C = 175 mA g−1) after 100 cycles. This rate capability is one of the highest values among reported Li4Ti5O12 with 150 ± 50 nm grains. The improved rate capability was attributed to the enhanced electronic conductivity of each Li4Ti5O12 grain via uniform graphene wrapping, with single-grain growth during annealing from the initial ∼25 nm TiO2 nanoparticles enclosed by outer graphene sheets. Graphene-eliminated Li4Ti5O12 by thermal decomposition was also directly compared to the graphene-coated sample, to clarify the role of graphene with nearly equivalent particle size/morphology distributions.

Samples of carbon paper containing multiwalled carbon nanotube films are produced by current annealing. A scanning tunneling microscope is used to examine the structure of the modified carbon paper. X-, Y-, and V-shaped nanotubes are found.

The reduced graphene oxide (R-GO) films were first fabricated via the dip coating technique in this experiment with graphene oxide (GO) suspension followed by thermal annealing. The growth process was monitored by UV-vis, and the morphology and structure of the obtained films were investigated by AFM, SEM and XPS. The authors found that GO films can grow uniformly on the quartz slides and the thickness, morphology and microstructure of the films were influenced by the coating cycles and the solid content of GO suspension. An ideal R-GO film was obtained when the solid content of GO suspension is 0·3 mg mL−1 with five coating cycles followed by annealing at 600°C in Ar/H2 atmosphere. The sheet resistance is less than 60 kΩ□−1 and the transmittance is as high as 81% (at 550 nm). The dip coating technique might be a promising approach for fabricating R-GO films or composite films.

This short paper presents an overview of the theoretical and technological under-pinnings of D-Wave quantum annealing systems and surveys some methodological challenges that arise when benchmarking these highly unusual systems.

In this paper we study in detail the post-growth annealing of a copper-containing material deposited with focused electron beam induced deposition (FEBID). The organometallic precursor Cu(II)(hfac)2 was used for deposition and the results were compared to that of compared to earlier experiments with (hfac)Cu(I)(VTMS) and (hfac)Cu(I)(DMB). Transmission electron microscopy revealed the deposition of amorphous material from Cu(II)(hfac)2. In contrast, as-deposited material from (hfac)Cu(I)(VTMS) and (hfac)Cu(I)(DMB) was nano-composite with Cu nanocrystals dispersed in a carbonaceous matrix. After annealing at around 150–200 °C all deposits showed the formation of pure Cu nanocrystals at the outer surface of the initial deposit due to the migration of Cu atoms from the carbonaceous matrix containing the elements carbon, oxygen, and fluorine. Post-irradiation of deposits with 200 keV electrons in a transmission electron microscope favored the formation of Cu nanocrystals within the carbonaceous matrix of freestanding rods and suppressed the formation on their surface. Electrical four-point measurements on FEBID lines from Cu(hfac)2 showed five orders of magnitude improvement in conductivity when being annealed conventionally and by laser-induced heating in the scanning electron microscope chamber., Beilstein Journal of Nanotechnology, 6, ISSN:2190-4286

In recent years, nanotechnology has gained significant interest for applications in the medical field. In this regard, a utilization of the ZnO nanoparticles for the efficient degradation of bilirubin (BR) through photocatalysis was explored. BR is a water insoluble byproduct of the heme catabolism that can cause jaundice when its excretion is impaired. The photocatalytic degradation of BR activated by ZnO nanoparticles through a non-radiative energy transfer pathway can be influenced by the surface defect-states (mainly the oxygen vacancies) of the catalyst nanoparticles. These were modulated by applying a simple annealing in an oxygen-rich atmosphere. The mechanism of the energy transfer process between the ZnO nanoparticles and the BR molecules adsorbed at the surface was studied by using steady-state and picosecond-resolved fluorescence spectroscopy. A correlation of photocatalytic degradation and time-correlated single photon counting studies revealed that the defect-engineered ZnO nanoparticles that were obtained through post-annealing treatments led to an efficient decomposition of BR molecules that was enabled by Förster resonance energy transfer.

Graphene was obtained on Cu foil by thermal decomposition method. A gas mixture of H2 and CH4 and an ambient annealing temperature of 1,000℃ were used during the deposition for 30 Min., and for the transfer onto SiO2/Si and Si substrates. The physical properties of graphene were investigated with regard to the effect ofnitrogen atom doping and the various substrates used. The G/2D ratio decreased when the graphene became monolayer graphene. The graphene grown on SiO2/Si substrate showed a low intensity of the G/2D ratio, because the polarity of the SiO2 layer improved the quality of graphene. The intensity of the G/2D ratio of graphene doped with nitrogen atoms increased with the doping time. The quality of graphene depended on the concentration of the nitrogen doping and chemical properties of substrates. High-quality monolayer graphene was obtained with a low G/2D ratio. The increase in the intensity of the G/2D ratios corresponded to a blue shift in the 2D peaks.

Thermally stable and highly conductive films have been prepared based on thermally reduced graphene oxide and exfoliated α-zirconium phosphate nanoplatelet (ZrP) hybrids. Exfoliated ZrP and graphene oxide (GO) were first mixed in aqueous solution to form a stable dispersion and then cast into free-standing films through flow-directed assembly. Upon annealing at 750 °C in Argon atmosphere, significant amounts of oxidized species were removed from the GO and a noticeable recovery of sp2 structure of the reduced GO sheets was observed. With the incorporation of the inorganic nanoplatelets, the thermal stability and structural integrity of the hybrid films were greatly improved, while the good electrical conductivity of the reduced GO was maintained. Potential applications for graphene-based hybrid films based on the current approach are discussed.

International audience; Graphene was synthesized at 1000 °C by Atmospheric Pressure Chemical Vapor Deposition on copper foil from methane diluted in argon and hydrogen. The influence of the main synthesis parameters was studied on 2 × 2 cm2 foils in order to obtain continuous monolayer graphenewithout crystalline defect. The uniformity, crystal quality and number of layers of graphenewere analyzed by Raman spectroscopy and Scanning Electronic Microscopy. First, an increase of the annealing pre-treatment duration induced an increase of the average size of copper grains, leading to larger graphene flakes of higher crystallinity presenting a lower number of layers. Similar evolutions of graphene characteristics were observed when decreasing the methane concentration to 20 ppm, whereas an increase of run duration led to a loss of graphene quality and to a higher number of graphene layers, confirming that graphene formation is not self-limiting on copper. An optimum hydrogen/methane ratio was found, quite different from other results of the literature, probably due to differences in the copper pre-treatment step. Finally, an optimized three step processwas developed to formmonolayer continuous graphene of high quality, successfully transposed to 7 × 7 cm2 substrates after a reactor scale-up.

A new approach to the production of few-layer hydrogenated graphene, which constitutes a hybrid structure with alternating organic and graphene monolayers, is proposed. This material offers an attractive combination of relatively high carrier mobility and (when used as a channel material in the field-effect transistor) the possibility of modulating current by 3–4 orders of magnitude using the gate voltage. The approach is based on the intercalation of the organic solvent N-methylpyrrolidone into few-layer graphene with consequent annealing at temperatures ranging from 190 to 270°C. The novelty of our approach is to organize interaction between the graphene layers and the intercalant. The material has high potential for use in electronics, especially in the production of field-effect transistors.

The electronic and chemical properties of reduced graphene oxide (RGO) can be modulated by chemical doping foreign atoms and functional moieties. Nitrogen-doped reduced graphene oxide (N-RGO) is a promising candidate for oxygen reduction reaction (ORR) in fuel cells. However, there are still some challenges in further preparation and modification of N-RGO. In this work, a low-cost industrial material, urea, was chosen to modify RGO by a facile, catalyst-free thermal annealing approach in large scale. The obtained N-RGO, as a metal-free catalyst for oxygen reduction was characterized by XRD, XPS, Raman, SEM, TEM, and electrochemical measurements. It was found that the optimum synthesis conditions were a mass ratio of graphene oxide and urea equal to 1:10 and an annealing temperature of 800 °C. Detailed X-ray photoelectron spectrum analysis of the optimum product shows that the atomic percentage of N-RGO samples can be adjusted up to 2.6 %, and the resultant product can act as an efficient metal-free catalyst, exhibiting enhanced electrocatalytic properties for ORR in alkaline electrolytes. This simple, cost-effective, and scalable approach opens up the possibility for the synthesis of other nitrogen doping materials in gram-scale. It can be applied to various carbon materials for the development of other metal-free efficient ORR catalysts for fuel cell applications, and even new catalytic materials for applications beyond fuel cells.

a b s t r a c t The Graphite/Silicon@reGO composite was synthesized via spray drying and subsequent annealing. According to XRD, Raman spectroscopy and FT-IR, graphene was demonstrated to be existed in the composite. Moreover, SEM and TEM were also used to illustrate the morphology of Graphite/Silicon@reGO. Used as anode for lithium-ion battery, it exhibited good cyclability with a high reversible charge capacity of 575.1 mAh g−1 and showed a capacity retention ratio of 73.1% after 50 cycles at a current density of 50 mA g −1 . It also presented good rate capability at different rates of 50–1000 mA g −1 . EIS test showed that the composite electrode had a lower SEI resistance and charge-transfer resistance due to the existence of graphene.

Photocatalytic studies under visible light irradiation using nanosized β-Bi2O3 are reported. β-Bi2O3 nanoparticles are prepared starting from the well-defined bismuth oxido cluster [Bi38O45(OMc)24(DMSO)9]⋅2 DMSO⋅7 H2O (OMc=O2CC3H5) using a straightforward hydrolysis and annealing protocol. Powder X-ray diffraction studies, transmission electron microscopy, diffuse reflectance UV/Vis spectroscopy and nitrogen adsorption measurements (using the Brunauer-Emmett-Teller (BET) theory) are used for the characterization of the as-prepared β-Bi2O3. By time-dependent annealing, the crystallite size can be controlled between (17±2) nm and (45±5) nm with BET surface areas of 7 to 29 m(2) g(-1). The indirect band gap of the as-prepared β-Bi2O3 amounts to (2.15±0.05) eV. The decomposition rates for rhodamine B (RhB) solutions are in the range of 2.46×10(-5) to 4.01×10(-4) s(-1) and depend on the crystallite size, amount of catalyst and concentration of RhB. Photocorrosion experiments have shown the formation of Bi2O2CO3 after several catalytic cycles. However, the catalyst can be recycled to phase-pure β-Bi2O3 nanoparticles by annealing for one hour under argon atmosphere at 380 °C. Furthermore, the photocatalytic activity of as-prepared β-Bi2O3 nanoparticles for the decomposition of phenol, 4-chlorophenol, 2,4-dichlorphenol, 4-nitrophenol, triclosan and ethinyl estradiol is demonstrated.

Molecular doping and detection are at the forefront of graphene research, a topic of great interest in physical and materials science. Molecules adsorb strongly on graphene, leading to a change in electrical conductivity at room temperature. However, a common impediment for practical applications reported by all studies to date is the excessively slow rate of desorption of important reactive gases such as ammonia and nitrogen dioxide. Annealing at high temperatures, or exposure to strong ultraviolet light under vacuum, is employed to facilitate desorption of these gases. In this article, the molecules adsorbed on graphene nanoflakes and on chemically derived graphene-nanomesh flakes are displaced rapidly at room temperature in air by the use of gaseous polar molecules such as water and ethanol. The mechanism for desorption is proposed to arise from the electrostatic forces exerted by the polar molecules, which decouples the overlap between substrate defect states, molecule states, and graphene states near the Fermi level. Using chemiresistors prepared from water-based dispersions of single-layer graphene on mesoporous alumina membranes, the study further shows that the edges of the graphene flakes (showing p-type responses to NO2 and NH3) and the edges of graphene nanomesh structures (showing n-type responses to NO2 and NH3) have enhanced sensitivity. The measured responses towards gases are comparable to or better than those which have been obtained using devices that are more sophisticated. The higher sensitivity and rapid regeneration of the sensor at room temperature provides a clear advancement towards practical molecule detection using graphene-based materials. Molecules bind strongly to graphene and graphene nanomesh edges. Annealing at high temperature or exposure to strong UV light is required for desorption. Alternatively, polar molecules can mediate rapid and complete desorption at room temperature. Electrostatic forces of polar molecules alter the overlap of graphene bands with substrate defect bands and molecule bands near Fermi level and cause desorption. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The growth mode of small Ni clusters evaporated in UHV on HOPG has been investigated by scanning tunnelling microscopy. The size, the size distribution, and the shape of the clusters have been evaluated for different evaporation conditions and annealing temperatures. The total coverage of the surface strongly depends on the evaporation rate and time, whereas the influence of these parameters is low on the cluster size. Subsequent stepwise annealing has been performed. This results in a reduction of the total amount of the Ni clusters accompanied by a decreasing in the overall coverage of the surface. The diameter of the clusters appears to be less influenced by the annealing than is their height. Besides this, the cluster shape is strongly influenced, changing to a quasi-hexagonal geometry after the first annealing step, indicating single-crystal formation. Finally, a reproducible methodology for picking up individual clusters is reported Parts of this work have been presented as oral or poster presentations in several national and international conferences (Meeting of the Physical Society of Japan 2011 and 2012, 6th International Symposium on Surface Science 2012, and ImagineNano 2013)..

We report a simple approach to prepare the nitrogen-modified few-layer graphene (FLG) directly from graphite flakes. With the aid of melamine, graphite flakes can be directly ultrasonicated into FLG in acetone. The subsequent annealing process further transforms the melamine absorbed on the surface of graphene into melon (C 6 N 9 H 3 ) x , which is one type of condensation product of melamine, and simultaneously dopes the graphene with nitrogen. When tested as a supercapacitor electrode, the nitrogen-modified FLG shows a much higher specific capacitance (e.g., 227 F/g at 1A/g) than that of reduced graphene oxide (rGO) (e.g., 133 F/g at 1A/g).

Large area epitaxial graphene (EG) layers are synthesized on 6H-SiC (0001) by annealing at 1500 °C for 5 min in a closed graphite chamber at low vacuum of 10-3 mbar and its 2D band in Raman spectra can be satisfactorily fitted by a single Lorentzian. From Raman spectroscopy, measurements indicate that too high growth temperature is to the disadvantage of the formation of graphene. The results of atomic force microscope (AFM) and field-emission scanning electronic microscope (FE-SEM) reveal the surface morphology of graphene is related with its growth temperature.

We demonstrate a chemical-vapor-deposition (CVD)-based approach for the direct synthesis of graphene on insulator with high-dielectric-constant (high-κ). Rutile titanium dioxide (TiO2), an insulator with reported k value of 80–125, is selected as the growth-initiating layer for graphene. A two-step CVD process is shown to grow graphene directly on TiO2 crystals or exfoliated ultrathin TiO2 nanosheets without using any metal catalyst. Various material characterization techniques confirm the growth of few-to-monolayer of graphene. Annealing of the growth substrate at 1100 °C under atmospheric pressure, prior to the low-pressure CVD process, is needed for activating nucleation sites in subsequent graphene synthesis. Electrical behavior of a field-effect transistor fabricated on the graphene/TiO2 heterostructure shows p-type doping in the CVD-synthesized graphene.

Li 4 Ti 5 O 12 /Reduced Graphene Oxide composite is synthesized with Li 4 Ti 5 O 12 (LTO) and graphene oxide nanosheets by spray-drying and annealing processes. The LTO primary particles aggregate in micro-sized spherical secondary particles, which are wrapped homogeneously and loosely with a Reduced Graphene Oxide (RGO) network .When used as a negative material for lithium ion batteries, the composite presents excellent rate performance and high cyclic stability. The initial discharge capacities are 167.8, 156.6, 135.1, and 106.4 mAh · g − 1 at the rates of 2, 5, 10 and 20 C, respectively. After 300 cycles at 20 C, it still can afford a specific capacity of approximately 100 mAh · g − 1 . This makes the composite an attractive anode material for application in lithium ion batteries.

We report on the conversion of epitaxial monolayer graphene on SiC(0 0 0 1) into decoupled bilayer graphene by performing an annealing step in air. We prove by Raman scattering and photoemission experiments that it has structural and electronic properties that characterize its quasi-free-standing nature. The (6 p 3 · 6 p 3)R30� buffer layer underneath the monolayer graphene loses its covalent bonding to the substrate and is converted into a graphene layer due to the oxidation of the SiC surface. The oxygen reacts with the SiC surface without inducing defects in the topmost carbon layers. The high-quality bilayer graphene obtained after air annealing is p-doped and homogeneous over a large area.

Some metal alloys subjected to irreversible plastic deformation can repair the inflicted damage and/or recover their original shape upon heating. The conventional shape memory effect in metallic alloys relies on collective, or “military” phase transformations. This work demonstrates a new and fundamentally different type of self-healing and shape memory in single crystalline faceted nano and microparticles of pure gold, which are plastically deformed with an atomic force microscope tip. It is shown that annealing of the deformed particles at elevated temperatures leads to nearly full recovery of their initial asymmetric polyhedral shape, which does not correspond to global energy minimum shape. The atomistic molecular dynamic simulations demonstrate that the shape recovery of the particles is controlled by the self-diffusion of gold atoms along the terrace ledges formed during the particles indentation. This ledge-guided diffusion leads to shape recovery by the irreversible diffusion process. A semiquantitative model of healing developed in this work demonstrates a good agreement with the experimental data.

A new method to prepare graphene-based fibers with ultrahigh tensile strength, conductivity, and increased elongation is reported. It includes wet-spinning the mixture of GO aqueous dispersion with phenolic resin solution in a newly developed coagulation bath, followed by annealing. The introduced phenolic carbon increased densification of graphene fibers through reducing defects and increased interfacial interaction among graphene sheets by forming new C–C bonds, thus resulting in the increasing of stiffness, toughness, and conductivity simultaneously.

In this paper, an annealing method with hydrogen sulflde was employed for Sulfur-doping of graphene. Both copper and SiO 2 were used as substrate in the experiment and the results showed that SiO 2 was more proper for S-doping of graphene. Raman and EDS spectra indicated that sulfur atoms are doped into the graphene after annealing. By this way, graphene could be easily S-doped and the S-doping density could be controlled by varying the doping time.

Ultrathin 2D materials such as TiO 2 , WOx, NiO, ZnO, VO 2 and graphene, offer scope for low power, highly dense and ultra-fast electronic devices. Due to their extraordinary physical and electrical/electronic property. In this work, a novel forming free memristor has been realized based on hybrid film of ZnO-rGO. The structure of the device is Metal-Insulator-Metal structure, where the Zinc Oxide- Reduced Graphene Oxide (ZnO-rGO) thin film is sandwiched between Silver (Ag) and Fluorine-doped tin oxide (FTO) coated glass. Free oxygen vacancies were created within the composite film by using high temperature annealing at 500 degrees Celsius. We demonstrate bipolar resistive switching behavior of the new device. Also we show that the variation of the conductance of the device is related to delay time of the applied input voltage sweep.

We employed depth-sensing nanoindentation to produce ordered arrays of indents on the surface of 50 nm-thick Au(Fe) films deposited on sapphire substrates. The maximum depth of the indents was approximately one-half of the film thickness. The indented films were annealed at a temperature of 700 °C in a forming gas atmosphere. While the onset of solid-state dewetting was observed in the unperturbed regions of the film, no holes to the substrate were observed in the indented regions. Instead, the film annealing resulted in the formation of hillocks at the indent locations, followed by their dissipation and the formation of shallow depressions nearby after subsequent annealing treatments. This annealing-induced evolution of nanoindents was interpreted in terms of annihilation of dislocation loops generated during indentation, accompanied by the formation of nanopores at the grain boundaries and their subsequent dissolution. The application of the processes uncovered in this work show great potential for the patterning of thin films.

In this work it is shown how porous graphene aerogels fabricated by an eco-friendly and simple technological process, could be used as electrodes in lithium- ion batteries. The proposed graphene framework exhibited excellent performance including high reversible capacities, superior cycling stability and rate capability. A significantly lower temperature (75 °C) than the one currently utilized in battery manufacturing was utilized for self-assembly hence providing potential significant savings to the industrial production. After annealing at 600 °C, the formation of Sn-C-O bonds between the SnO2 nanoparticles and the reduced graphene sheets will initiate synergistic effect and improve the electrochemical performance. The XPS patterns revealed the formation of Sn-C-O bonds. Both SEM and TEM imaging of the electrode material showed that the three dimensional network of graphene aerogels and the SnO2 particles were distributed homogeneously on graphene sheets. Finally, the electrochemical properties of the samples as active anode materials for lithium-ion batteries were tested and examined by constant current charge–discharge cycling and the finding fully described in this manuscript.

The long range objectives of this research are to develop and demonstrate the use of graphene-nanoparticle composites as a high sensitivity, rapid response electronic nose for gas sensing in energy applications. Graphene based device structures suitable for temperatures as high as 1000 °C are targeted. The scope of work includes: a) development of procedures for controllable nucleation and growth of nanoparticles on graphene surfaces, b) fabrication graphene-nanoparticle composite sensors, c) measurement of electrical properties of graphene-nanoparticle composites, and d) determination of sensor characteristics (selectivity and sensitivity). The graphene films are synthesized on 6H-SiC (0001) surfaces using a halogen based plasma etching followed by rapid thermal annealing in atmospheric pressure Ar or under ultrahigh vacuum conditions. Lithography free methods are then used to produce simple sensor structures consisting of interdigitated fingers. This is followed by the nucleation of either Ag, Au, Pt, or Ir nanoparticles on the graphene surfaces using solution based techniques. Atomic force microscopy is used to characterize the particle size distribution of the nucleated nanoparticles. Electrical properties of the graphene and graphenenanoparticle composites are characterized using two point current-voltage measurements. Gas sensor response as a function of temperature is characterized for H 2 in Ar gas mixtures.

Solution processed, highly conductive films are extremely attractive for a range of electronic devices, especially for printed macroelectronics. For example, replacing heavy, metal-based current collectors with thin, light, flexible, and highly conductive films will further improve the energy density of such devices. Films with two-dimensional building blocks, such as graphene or reduced graphene oxide (RGO) nanosheets, are particularly promising due to their low percolation threshold with a high aspect ratio, excellent flexibility, and low cost. However, the electrical conductivity of these films is low, typically less than 1000 S/cm. In this work, we for the first time report a RGO film with an electrical conductivity of up to 3112 S/cm. We achieve high conductivity in RGO films through an electrical current-induced annealing process at high temperature of up to 2750 K in less than 1 min of anneal time. We studied in detail the unique Joule heating process at ultrahigh temperature. Through a combination of experimental and computational studies, we investigated the fundamental mechanism behind the formation of a highly conductive three-dimensional structure composed of well-connected RGO layers. The highly conductive RGO film with high direct current conductivity, low thickness (∼4 μm) and low sheet resistance (0.8 Ω/sq.) was used as a lightweight current collector in Li-ion batteries.