Effect of base‐deposited graphene oxide on the thermal stabilization of poly(vinyl chloride)

Graphene oxide was deposited in a base solution to form base‐deposited graphene oxide (bd‐GO) particles. The structure and properties of the bd‐GO particles were evaluated using transmission electron microscopy, powder X‐ray diffraction and X‐ray photoelectron, Fourier transform infrared, UV‐visible and fluorescence spectroscopies. The effect of the bd‐GO particles on the thermal stabilization of poly(vinyl chloride) (PVC) was investigated using the Congo red test and thermogravimetric analysis. The results showed that the thermal stability of PVC was greatly improved by the bd‐GO particles. Furthermore, this stabilization mechanism was investigated using UV‐visible spectroscopy and nitrogen adsorption–desorption isotherm analysis. It was found that the improvement of thermal stability was mainly related to the deactivation of thermally labile structural defects in the PVC chains by the carboxylate and alkoxide moieties of the basic groups in the bd‐GO particles, and the highly efficient adsorption of the bd‐GO particles with hydrogen chloride produced during PVC degradation. © 2015 Society of Chemical Industry     

Controlled synthesis of few-layered graphene sheets on a large scale using chemical exfoliation

The synthesis of few-layered graphene sheets with controlled number of layers (3-4) on a large scale was developed using chemical exfoliation by simply controlling the oxidation and exfoliation procedure. The obtained Few-layered Graphene Oxide (FGO) was characterized by atomic force microscopy, X-ray diffraction, thermal gravimetric analysis and Ultraviolet-visible spectroscopy. It is found that the FGO, which contains less functional groups than single-layered graphene oxide (GO), also has excellent water dispersion. Moreover, after reduction treatments under the same conditions as that used for GO, reduced FGO show a much better electrical conductivity of 108 S/cm, two-orders higher than reduced GO.     

Reduction of functionalized graphite oxides by trioctylphosphine in non-polar organic solvents

Graphene, functionalized with oleylamine (OA) and soluble in non-polar organic solvents, was produced on a large scale with a high yield by combining the Hummers process for graphite oxidation, an amine-coupling process to make OA-functionalized graphite oxide (OA-GO), and a novel reduction process using trioctylphosphine (TOP). TOP acts as both a reducing agent and an aggregation-prevention surfactant in the reduction of OA-GO in 1,2-dichlorobenzene (DCB). The reduction of OA-GO is confirmed by X-ray photoelectron spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, thermogravimetric analysis, and Raman spectroscopy. The exfoliation of GO, OA-GO, and OA-functionalized graphene (OA-G) is verified by atomic force microscopy. The conductivity of TOP-reduced OA-G, which is deduced from the current-voltage characteristics of a vacuum-filtered thin film, shows that the reduction of functionalized GO by TOP is as effective as the reduction of GO by hydrazine.     

Facile and safe graphene preparation on solution based platform

Graphene has attracted increasing attention because of its interesting properties. In this study, graphene was prepared from graphite by a very simple and easy process. The two-step protocol involves conversion of graphite to graphene oxide (GO) by oxidation, and subsequent reduction of GO to graphene. The structures and properties of the obtained GO and graphene were characterized via X-ray diffraction, and Raman, NMR, UV–vis absorption, and X-ray photoelectron spectroscopic techniques. The morphologies of these products were observed via field emission scanning electron microscopy. The preparation protocol is simple, easy, environmental friendly, i.e., nontoxic, and the yield of graphene is high.     

高可见光活性的棒状钒酸铋/氧化石墨烯复合光催化剂的制备

通过水热法制备了棒状钒酸铋/氧化石墨烯（BiVO4/GO）复合可见光光催化剂。用扫描电子显微镜、X射线衍射、Raman光谱和紫外–可见漫反射光谱表征了所制备的样品。在可见光（λ≥420nm）光照下光催化降解亚甲基蓝水溶液来检测样品的活性。结果表明：氧化石墨烯的加入有效地提高了BiVO4的可见光光催化活性,含1%（质量分数）的氧化石墨烯的复合光催化剂活性最好。BiVO4/GO活性增强的原因是氧化石墨烯能快速捕获并转移光生电子,有效提高BiVO4光生载流子的分离效率,从而提高其光催化活性。     

Furfuryl alcohol functionalized graphene nanosheets for synthesis of high carbon yield novolak composites

Graphene oxide and furfuryl alcohol modified graphene nanosheets (G‐FA) were used to prepare graphene/novolak composites. Effect of graphene compatibilization on the properties of the composites especially carbon yield value is evaluated. Both types of graphene nanosheets were dispersed uniquely in the novolak matrix as proved by X‐ray diffraction analysis. However, modification of graphene sheets by furfuryl alcohol results in more improved dispersions. Thermogravimetric analysis confirms the elevated thermal stability of the nanocomposites in comparison with the neat novolak. In addition, G‐FA containing composites have higher carbon yield values. A shift in the wave number of characteristic bonds of graphene after oxidation and modification with furfuryl alcohol, O? H, C?O, and C? O bonds, are seen in the Fourier transform infrared spectroscopy spectra. Raman results and scanning electron microscopy images show that graphene nanosheets reduced in size and wrinkled by oxidation and functionalization. Transmission electron microscopy image of the composite with 0.2 wt % of G‐FA reveals the presence of nanosheets with curvature. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40273.     

氧化石墨烯杂化分子印迹复合膜制备及性能研究

采用改进的Hummers法,通过冷冻干燥制备了氧化石墨烯(GO)。以辛弗林盐酸盐为模板分子,水溶性的丙烯酰胺为功能单体,离子液体(溴代1-丁基-3-甲基咪唑)为致孔剂,把GO加入聚合液中,制备了GO杂化的分子印迹复合膜(GO-MIM)。利用透射电镜、扫描电镜、X射线衍射和红外光谱等方法对GO及GO-MIM进行了表征。通过将分子印迹膜技术与GO相结合,明显提高了分子印迹膜的力学性能。吸附及渗透实验表明,GO-MIM可在纯水溶剂体系,对辛弗林盐酸盐具有很好的选择性吸附能力和优先透过能力,体现了明显的分子印迹效果。     

Modification of bismaleimide resin by using γ-aminopropyl triethoxysilane functionalised graphene oxide

In this paper, γ-aminopropyl triethoxysilane (APTES) was first used to covalent functionalised graphene oxide (GO). The resulting APTES functionalised GO (APTES-f-GO) was then incorporated into the bismaleimide (BMI) resin to improve its mechanical properties. Fourier transform infrared spectroscopy, X-ray photoelectron spectra and Raman spectroscopy were used to characterise APTES-f-GO. The study showed that the APTES-f-GO/BMI nanocomposites presented higher impact strength, flexural strength, tensile strength and elastic modulus than the neat BMI resin. The maximum increment of impact strength, flexural strength, tensile strength and elastic modulus of APTES-f-GO/BMI nanocomposites were 84.3, 54.5, 31.4 and 35.6%, respectively. The scanning electron microscopy photographs show that the fracture morphology of APTES-f-GO/BMI composite is entirely different from that of BMI resin, which exhibits typical ductile fracture features.     

Edge‐functionalized graphene nanoplatelets with polystyrene by atom transfer radical polymerization: grafting through carboxyl groups

The surface modifier 3‐((4‐hydroxybutoxy)dimethylsilyl)propyl methacrylate (CD), which contains a double bond and a hydroxyl group, was synthesized through a coupling reaction of 1,4‐butanediol and (3‐methacryloxypropyl)dimethylchlorosilane. Subsequently, graphene oxide (GO) was functionalized with different amounts of CD from its edge carboxyl groups. Then, grafting through atom transfer radical polymerization of styrene in the presence of various amounts of the edge‐functionalized GO was carried out to evaluate the effect of graphene loading along with graft density. A peak at 3.8 ppm in the ¹H NMR spectrum of CD associated with the methylene adjacent to the Si–O group indicated a successful coupling reaction. Attachment of CD on the edges of GO was evaluated using X‐ray photoelectron and Fourier transform infrared spectroscopies. Expansion of GO interlayer spacing by functionalization was evaluated using X‐ray diffraction. The ordered and disordered crystal structure of carbon was studied using Raman spectroscopy. The close I_D/I_G values for GO and various kinds of functionalized graphenes show the preserved graphitic crystallite size. Relaxation behaviour of polystyrene chains in the presence of graphene nanoplatelets and also the effect of graft content on chain confinement were studied using differential scanning calorimetry. High‐graft‐density nanocomposites show higher glass transition temperatures. Morphology of graphene nanoplatelets was studied using scanning electron and transmission electron microscopies. The flat and smooth morphology of graphene nanoplatelets is disturbed and also the transparency of the nanoplatelets decreases during the oxidation and functionalization processes. © 2014 Society of Chemical Industry     

A green approach for the reduction of graphene oxide by wild carrot root

A green approach for the reduction of graphene oxide (GO) using wild carrot root is reported in this work. It avoids the use of toxic and environmentally harmful reducing agents commonly used in the chemical reduction of GO to obtain graphene. The endophytic microorganisms present in the carrot root, reduces exfoliated GO to graphene at room temperature in an aqueous medium. Transmission electron microscopy and atomic force microscopy images provide clear evidence for the formation of few layer graphene. Characterization of the resulting carrot reduced GO by Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy shows partial reduction of GO to graphene. Raman spectroscopy data also indicates the partial removal of oxygen-containing functional groups from the surface of GO and formation of graphene with defects.     

Chemically modified graphene oxide/polybenzimidazobenzophenanthroline nanocomposites with improved electrical conductivity

Graphene/polybenzimidazobenzophenanthroline nanocomposites were prepared through the liquid-phase exfoliation of graphene oxide (GO) and reduced graphene oxide (rGO) in methanesulfonic acid with subsequent solution mixing. Various chemical and combined chemical-thermal methods were examined to be effective for producing rGO with highly graphitic structure and excellent electrical conductivity. Raman and X-ray photoelectron spectroscopy showed higher degree of reduction of the GO with the combined chemical-thermal method compared to other chemical reduction processes. Structural characterization of the nanocomposites by X-ray diffraction, scanning electron microscopy and transmission electron microscopy showed good exfoliation and dispersion of both GO and rGO fillers in the polymer matrix. The thermogravimetric analysis found that the nanocomposites with rGO have higher onset and maximum weight loss temperatures than those with GO. Compared with the pure polymer, the electrical conductivity of the nanocomposites containing 10 wt% GO and GO reduced by the combined chemical-thermal treatment showed a remarkable increase by four and seven orders of magnitude, respectively. Long-term in-situ thermal reduction was performed to further improve the conductivities of the nanocomposites.     

Preparation of polyester resin/graphene oxide nanocomposite with improved mechanical strength

Graphene oxide (GO) has attracted huge scientific interest due to its unique physical and chemical properties as well as its wide‐scale applicability including facile synthesis and high yield. Here, we report preparation of nanocomposites based on GO and unsaturated polyester resin (PE). The synthesized samples were characterized by Fourier transform infrared spectroscopy, X‐ray diffraction, scanning electron microscopy, thermogravimetric analysis, and tensile strength measurements. A good dispersion of the GO sheets within the resin matrix was observed from the morphological analysis. A significant enhancement in mechanical properties of the PE/GO composites is obtained at low graphene loading. Around 76% improvement of tensile strength and 41% increase of Young's modulus of the composites are achieved at 3 wt % loading of GO. Thermal analysis of the composite showed a noticeable improvement in thermal stability in comparison to neat PE. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Effect of octa(aminopropyl) polyhedral oligomeric silsesquioxane (OapPOSS) functionalized graphene oxide on the mechanical,thermal, and hydrophobic properties of waterborne polyurethane composites

A novel graphene nanomaterial functionalized by octa(aminopropyl) polyhedral oligomeric silsesquioxane (OapPOSS) was synthesized and then confirmed by Fourier transform infrared spectroscopy, thermogravimetric analysis (TGA), Raman spectroscopy, X‐ray photoelectron spectroscopy, transmission electron microscopy, scanning electron microscopy with energy‐dispersive X‐ray spectroscopy (SEM EDX), atomic force microscopy, and X‐ray diffraction. The obtained functionalized graphene (OapPOSS‐GO) was used to reinforce waterborne polyurethane (WPU) to obtain OapPOSS‐GO/WPU nanocomposites by in situ polymerization. The thermal, mechanical, and hydrophobic properties of nanocomposites as well as the dispersion behavior of OapPOSS‐GO in the polymer were investigated by TGA, a tensile testing machine, water contact angle tests, and field emission SEM, respectively. Compared with GO/WPU and OapPOSS/WPU composites, the strong interfacial interaction between OapPOSS‐GO and the WPU matrix facilitates a much better dispersion and load transfer from the WPU matrix to the OapPOSS‐GO. It was found that the tensile strength of the OapPOSS‐GO/WPU composite film with 0.20 wt % OapPOSS‐GO exhibited a 2.5‐fold increase in tensile strength, compared with neat WPU. Better thermal stability and hydrophobicity of nanocomposites were also achieved by the addition of OapPOSS‐GO. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44440.     

Synthesis of click‐coupled graphene sheets with hyperbranched polyurethane: Effective exfoliation and enhancement of nanocomposite properties

Graphene oxide (GO) was functionalized with hyperbranched polyurethane (HBPU) via click coupling between azide‐functionalized HBPU and alkynyl‐decorated GO. HBPU‐functionalized GO composites of various compositions were prepared. The azide‐containing HBPU was characterized using Fourier‐transform infrared (FT‐IR) spectroscopy and ¹H‐nuclear magnetic resonance spectroscopy. The HBPU‐functionalized GO composites were characterized using transmission electron microscopy and FT‐IR spectroscopy. The functionalized GO showed excellent dispersion in the HBPU matrix, giving composites with enhanced mechanical and thermal properties. The material properties were effectively regulated by click‐coupled exfoliation of GO with HBPU, enabling the production of high‐performance materials. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44631.     

氧化石墨烯的制备及其封堵龙马溪组泥页岩机理研究

孔隙压力传递是泥页岩井壁失稳的重要机理之一，纳微米尺度氧化石墨烯的研究为泥页岩孔隙封堵提供了新的途径。针对四川龙马溪组泥页岩，基于扫描电镜（SEM）、氮气吸附等方法表征了其孔隙结构；以改性Hummers法制备了厚度约为1.2 nm，平均片层尺寸分布范围为197 nm - 969.9 nm的氧化石墨烯（GO），并通过压力传递实验评价了其封堵性能；基于封堵后泥页岩的 SEM 及 X 射线能量色散谱（EDS）测试，探讨了GO封堵泥页岩岩心的主要机理。结果表明，片层尺寸为969.9 nm、质量分数为0.1%的GO阻缓压力传递效果最明显，其1 MPa压差传递时间为1000 s，而蒸馏水传递时间为30 s；GO呈半透明絮状膜堆叠、覆盖在岩心表面，对岩心纳微米孔隙进行了充填与封堵。     

Graphene‐based composite with microwave absorption property prepared by in situ reduction

Binary composite of graphene/poly(ethylene oxide) (PEO) with microwave absorption property is prepared by in situ reduction process. Graphite oxide (GO) is prepared from flake graphite by modified Hummers' method and further dispersed in distilled water to get GO solution. Then, PEO powder is slowly added into GO solution to get GO/PEO solution, and graphene/PEO composites is prepared via a facile and quick reduction process in GO/PEO solution. PEO and graphene/PEO composites are characterized by scanning electron microscopy, atomic force microscopy, thermo gravimetric analysis, and vector network analyzer. The results show that graphene is uniformly dispersed in PEO matrix because GO and PEO can be uniformly dispersed at molecular level due to their water‐solubility and the agglomeration of graphene can be prevented by PEO macromolecular chains during in situ reduction process. Graphene/PEO composite has better thermal stability than PEO, which can be explained by the graphene restoration of sp² bonded carbon structure. Meanwhile, graphene/PEO composite shows excellent microwave absorption property at low grapheme content. The minimum reflection loss of graphene/PEO composite is up to −20.0 dB when the content of graphene is only 1 wt%. POLYM. COMPOS., 35:461–467, 2014. © 2013 Society of Plastics Engineers     

Utilization of multiple graphene nanosheets in fuel cells: 2. The effect of oxidation process on the characteristics of graphene nanosheets

Structural properties of graphene nanosheets that will be used as electrode material in fuel cells were investigated at different oxidation times. As the oxidation time was increased, the strong bonding between graphene layers in graphite was reduced and graphene layers started to exfoliate forming clusters with a few number of graphene layers. The variations in interplanar spacings, layer number and percent crystallinity indicated how stepwise chemical procedure influenced the morphology of graphite. It was possible to produce relatively flat graphene clusters with definite number of layers by controlling the oxidation time. Graphene nanosheets were characterized in detail by scanning electron microscopy, atomic force microscopy, X-ray diffraction, Raman spectroscopy, and thermal gravimetric analyzer.     

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach

Graphene nanoplate-MnO(2) composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO(2) nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material.     

Effect of ball milling speed on the quality of Al2O3 stripped graphene in a wet milling medium

Graphene nanosheets (GNSs)/Al₂O₃ composites were synthesized by wet milling. In this study, the effects of wet milling speed on the layer distribution, quality and conversion efficiency of graphene in GNSs/Al₂O₃ composites were studied using scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), raman spectroscopy, fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The results show that the intensity of graphite peak decreases and the conversion efficiency of graphene increases with the increase of rotational speed in the range of 200–300 rpm, and a small amount of graphene coated Al₂O₃ nanoparticles were found in GNSs/Al₂O₃ composites. The number of layers (≤10 layers) of GNSs gradually increases with the increase of ball milling speed. When the rotational speed is 300 rpm, the graphene conversion efficiency is the highest. At different rotational speeds, graphene defects were the least influential marginal defects. There was no characteristic peak of graphene oxide (GO) appeared in the composite, indicating a small oxidation degree of graphene.     

One‐Step Sonochemical Synthesis of Reduced Graphene Oxide/Pt/Sn Hybrid Materials and Their Electrochemical Properties

Low frequency ultrasound (20 kHz) was used for the reduction of graphene oxide (GO), Pt and Sn precursors with simultaneous loading of Pt and Sn monometallic and Pt–Sn bimetallic nanoparticles on the surface of reduced GO (rGO). The physicochemical characterizations of the catalysts were carried out using transmission electron microscopy (TEM), X‐ray photoelectron spectroscopy (XPS), energy dispersive X‐ray spectroscopy (EDX), and selected area electron diffraction (SAED) techniques. The reduced monometallic and bimetallic nanoparticles were spherical in shape with diameters around 2–6 nm, uniformly embedded on rGO sheets of few layers thickness. The electrocatalytic activities of the synthesized materials were evaluated by cyclic voltammetric studies.