High-quality liquid phase-pulsed laser ablation graphene synthesis by flexible graphite exfoliation

This work reports a one-pot procedure of laser ablation on a graphite target in a liquid medium, based on the variation of different parameters such as target type, laser wavelength, and ablation medium,to obtain high-quality graphene nanosheets. The morphology of derived products was characterized by the field emission scanning electron microscopy(FE-SEM). Then, the morphology and structure of the optimized sample were characterized by transmission electron microscopy(TEM), X-ray diffraction(XRD), ultraviolet-visible-near infrared(UV–vis-NIR) spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy(XPS). By controlling the laser ablation parameters, we were able to prepare micrometer-sized few-layer graphene nanosheets with mainly less than ten layers. Such synthesized graphene nanosheets were grown at the surface of a flexible graphite target, indicating many potential applications in fundamental research, electrochemical and as hydrophobic surfaces.     

用于超级电容器的纳米氧化镍/石墨薄片/银复合电极材料的超声法合成及性能

通过简单超声法制备了球状NiO纳米颗粒、NiO/石墨薄片(NiO/GNS)和NiO/GNS/Ag纳米复合材料。在NiO/GNS和NiO/GNS/Ag复合材料中,GNS作为NiO和Ag纳米颗粒分散的模板,不仅有效避免了NiO和Ag纳米颗粒的团聚,还改善了复合材料的电化学性能。采用场发射扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线衍射对样品的成分、形貌和结构进行了表征。NiO/GNS/Ag复合材料(GNS质量分数为0.5%,Ag质量分数为3%)电极表现出优异的电化学性能。在1A/g时,其初始比电容为501.66F/g,2000次循环后其比电容衰减为440.45F/g。这表明所制备的复合材料是一种有应用价值的超级电容器电极材料。     

Facile fabrication of functionalized graphene sheets (FGS)/ZnO nanocomposites with photocatalytic property

Functionalized graphene sheets (FGS)/ZnO nanocomposites were fabricated via thermal treatment method, using graphene oxide as a precursor of graphene, Zn(NH(3))(4)CO(3) as a precursor of zinc oxide, and poly(vinyl pyrrolidone) as an intermediate to combine zinc with carbon materials. Thermogravimetric analysis, X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), and scanning electron microscopy (SEM) were used to characterize crystal structure and morphology of FGS/ZnO nanocomposites. It was shown that the well-dispersed ZnO nanoparticles were deposited on FGS homogeneously. The composites exhibited photocatalytic activity to decompose rhodamine 6G efficiently under low-power ultraviolet (UV) light. This facile and low-cost method makes the composite a perfect candidate in applications of catalysis and other areas.     

Synthesis of a carbon-coated NiO/MgO core/shell nanocomposite as a Pd electro-catalyst support for ethanol oxidation

Carbon coated on NiO/MgO in a core/shell nanostructure was synthesized by the single-step RAPET (reaction under autogenic pressure at elevated temperatures) technique, and the obtained formation mechanism of the core/shell nanocomposite was presented. The carbon-coated NiO/MgO and its supported Pd catalyst, Pd/(NiO/MgO@C), were characterized by SEM, HR-TEM, XRD and cyclic voltammetry. The X-ray diffraction patterns confirmed the face-centered cubic crystal structure of NiO/MgO. Raman spectroscopy measurements provided structural evidence for the formation of a NiO/MgO composite and the nature of the coated carbon shell. The high-resolution transmission electron microscopy images showed the core and shell morphologies individually. The electrocatalytic properties of the Pd/(NiO/MgO@C) catalyst for ethanol oxidation were investigated in an alkaline solution. The results indicated that the prepared Pd–NiO/MgO@C catalyst has excellent electrocatalytic activity and stability.     

石墨烯的种类对剑麻纳米纤维素/石墨烯/聚苯胺复合材料电化学性能的影响

基于绿色可再生的剑麻纳米纤维素,采用超声分散方法制备剑麻纳米纤维素/石墨烯(CNF/G)分散液,通过机械共混法制备剑麻纳米纤维素/石墨烯/聚苯胺(CNF/G/PANI)复合材料,采用红外光谱、X射线衍射、拉曼光谱和扫描电镜对复合材料的结构和形态进行表征,采用循环伏安、恒流充放电、交流阻抗等方法研究材料的电化学性能,侧重研究石墨烯的种类对CNF/G/PANI复合材料电化学性能及结构的影响。结果表明,加入石墨烯纳米片(GNS),聚苯胺(PANI)和剑麻纳米纤维素(CNF)穿插于GNS中,产生较多的孔洞,复合材料的比电容最高值达到322.25 F/g,内阻仅为0.77Ω,在5 A/g的电流密度下,循环充放电1000次,复合材料的电容保持率达到76.92%。     

网状纤维结构氧化镍的制备及其气敏性能

p型半导体金属氧化物作为气敏材料具备响应快速、选择性高的特点,用于气体传感器的制备与开发。静电纺丝法可制备具有丰富气体吸附位点的网状结构材料,增强材料的气体敏感特性。以聚乙烯吡咯烷酮(PVP)、四水合乙酸镍为原料,采用静电纺丝法制备具有网状纤维结构的p型半导体氧化镍。通过X射线衍射、扫描电镜、X射线光电子能谱和比表面积测试等分析技术对材料的结构、形貌、组成和比表面等性能进行表征,并对其气敏性能进行测定,考察煅烧温度对材料气敏性能的影响。结果表明:煅烧温度为500℃时获得的氧化镍组装成气体传感器,在工作温度为250℃时,该元件对50mg/L丙酮气体表现出快速响应特性(响应时间为5s)、良好选择性和稳定性。     

液相制备石墨烯/硫复合材料及其在锂硫电池正极中的应用

采用氧化石墨烯(grapheneoxide,GO)作为制备石墨烯的前驱体,通过液相还原自组装过程与硫纳米颗粒进行复合,获得了高性能的还原氧化石墨烯/硫(r GO/S)复合正极材料。利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射仪(XRD)、拉曼光谱、X射线光电子能谱分析(XPS)等对材料微观形貌与结构进行表征。结果表明:硫纳米颗粒均匀分布在石墨烯片层间,并且硫纳米颗粒被石墨烯片层有效地封装,硫在35-r GO/S复合物中的质量分数高达83.6%。该35-r GO/S复合正极在0.2C电流密度下初始放电容量可达1197.3mAh·g^-1,经过200次循环后容量仍保持在730mAh·g^-1左右,表现出优异的循环性能。     

三维石墨烯/苯胺-吡咯共聚复合物的制备及其超级电容性能

以制备的氧化石墨凝胶和苯胺-吡咯共聚物为原料,将二者进行混合超声分散,再以其混合分散液为前驱体,采用一步水热法制得三维石墨烯/苯胺-吡咯共聚复合物(3DAP)。利用X射线衍射(XRD)、拉曼光谱(Raman)、傅里叶变换红外(FT-IR)光谱、扫描电镜(SEM)、透射电镜(TEM)和电化学测试等研究了复合物的结构、形貌及电化学性能。结果表明:3DAP拥有丰富的三维多孔网状结构,并且颗粒状的苯胺-吡咯共聚物能够均匀地分布于孔隙间;作为电极材料,该复合物在0.5A·g~(-1)电流密度下比电容可达628.5F·g~(-1),即使在大电流密度(20A·g~(-1))条件下仍可高达384F·g~(-1),且在1A·g~(-1)电流密度下经过1 000次的充放电循环后比容量保持率高达86.1%,表现出良好的倍率特性和循环稳定性,其超级电容性能远优于单纯的石墨烯以及苯胺-吡咯共聚物。     

新型石墨烯-聚苯胺-银基电极复合材料的制备及性能研究

目的设计一个低成本条件下成熟高效制备石墨烯-聚苯胺-银基复合电极材料的工艺路线。方法研究石墨烯的制备工艺以及石墨烯与聚苯胺、银粒子的复合效果,将石墨烯与苯胺、银粒子通过原位聚合的方法制得石墨烯-聚苯胺-银复合材料。利用扫描电子显微镜(SEM)、傅里叶变换-红外光谱(FT-IR)、X射线衍射(XRD)、循环伏安法(CV)和恒电流充放电法(GCD)对石墨烯和石墨烯-聚苯胺-银复合材料的形貌、结构和电化学性能进行分析研究。结果 SEM、FT-IR、XRD等测试表明,聚苯胺类衍生物、石墨烯以及银粒子在整个复合材料中共存。结论 CV和GCD的测试结果表明复合材料有优良的电化学性能,比电容最高可达到293 F/g。     

MnFe2O4/还原氧化石墨烯纳米复合材料的光学性能

由于纳米尺度的尖晶石结构金属氧化物独特的晶体结构和能带结构,使其具有广阔的应用前景。采用水热法合成了MnFe₂O₄复合还原氧化石墨烯(MnFe₂O₄/rGO)纳米复合材料,采用XRD、高分辨透射电子显微镜(HRTEM)、能量色散X射线光谱仪(EDX)、FTIR、XPS、拉曼光谱(Raman)、光致发光光谱(PL)和紫外-可见光谱漫反射(UV-vis DRS)对样品的晶体结构、形貌、元素分布、结合能和光学性能进行表征。结果表明,制备的MnFe₂O/rGO复合材料为立方尖晶石结构,形貌呈不规则的椭球形,颗粒大小比较均匀。rGO表面所负载的MnFe₂O₄纳米粒子被石墨烯部分包裹,颗粒尺寸小,分散性好。MnFe₂O₄/rGO复合材料的电子-空穴对的再结合效率降低,其中石墨烯具有较多缺陷,无序程度较高,含氧基团被聚乙烯吡咯烷酮(PVP)部分还原,数量大大减少。MnFe₂O₄/rGO复合材料的带隙小于纯MnFe₂O₄带隙,发生了红移现象。      

氮掺杂石墨烯的制备及其电催化氧气还原性能

通过改良Hummers法制备氧化石墨(Graphite oxide,GO),采用爆炸辅助还原法将GO还原剥离并原位掺杂得到氮掺杂石墨烯(Nitrogen-doped graphene,N-RGO)。采用TEM、SEM、FI-IR、XPS、XRD及Raman等分析手段对N-RGO的形貌、组成以及结构进行了表征,利用旋转环盘电极技术测试了其电催化氧气还原活性。TEM和SEM结果表明,爆炸条件下GO被很好地剥离开来,得到只有几层厚度的石墨烯;FI-IR及XPS结果表明,GO中大部分含氧官能团被脱除,C/O原子比达到26.2,是目前所得GO还原程度非常高的方法之一,且氮元素成功掺杂进石墨烯晶格中,掺杂氮的原子质量分数约为2.11%;电化学测试结果显示,氧气还原的极限扩散电流由非氮掺杂石墨烯(Reduced graphene oxide,RGO)的0.24mA提高到N-RGO的0.49 mA,尽管爆炸辅助还原得到的RGO对氧气还原也显示出较好的催化活性,但掺杂之后的N-RGO具有更高的催化活性。     

g-C3N4/MoS2纳米片/氧化石墨烯三元复合催化剂的制备及可见光催化性能

采用球磨法制备 g-C₃N₄/MoS₂纳米片/氧化石墨烯(GO)三元复合催化剂。运用X 射线衍射(XRD)、透射电子显微镜(TEM)、紫外-可见吸收光谱(UV-Vis)和光致激发光谱(PL)等分析手段, 对催化剂的结构、形貌和光学性能进行表征。结果表明: MoS₂纳米片和g-C₃N₄形成异质结结构, 均匀地分散在氧化石墨烯的表面上。以罗丹明B(RhB)为模拟污染物, 研究三元复合催化剂在可见光照射下的光催化特性。结果显示: 三元复合催化剂在120 min内对RhB的降解率达到96%, 其降解动力学常数分别是g-C₃N₄、g-C₃N₄/ MoS₂、g-C₃N₄/GO复合催化剂的3、2.1和2.8倍。根据实验结果及能带结构提出了三元复合催化剂可能的光催化机理。     

NiO/In2O3纳米复合材料的制备及气敏性能研究

采用水热法结合水浴法制备出了NiO/In2O3纳米复合材料,利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线衍射仪(XRD)等对其微观形貌和晶相进行表征分析。表征结果表明,制备所得In2O3纳米微球直径为200~300 nm,其表面均匀包覆厚度约为20 nm的NiO纳米片。气敏测试结果表明,基于NiO/In2O3异质结纳米复合材料的气体传感器对甲醛的最佳工作温度为220℃;在最佳工作温度下,对浓度为1×10^-5的甲醛气体响应可达到20,响应/恢复时间分别为4 s/16 s,且具有较好的重复性和选择性。最后,对分级结构及p-n异质结对其气敏机理进行了探讨。     

Facile preparation and electrochemical characterization of graphene/ZnO nanocomposite for supercapacitor applications

Graphene/ZnO nanocomposites were successfully synthesized by microwave-assisted method. The structure, morphology, optical and composition of the obtained samples were characterized using XRD, FT-IR, laser Raman, UV–Vis spectroscopy and XPS analysis. XRD analysis confirmed the presence of graphene/ZnO nanocomposite. FE-SEM image reveals that the homogenous distribution of ZnO nanoparticles on the graphene nanosheets. The electrochemical properties of the graphene/ZnO electrodes were analyzed by cyclic voltammetry and impedance spectroscopy. The results confirmed that the incorporation of ZnO nanoparticles enhanced the capacitive performance of graphene electrode. Graphene/ZnO nanocomposite electrode showed higher capacitance value of 109 F g⁻¹ at a scan rate of 5 mV s⁻¹ in 1 M KCl solution as compared to the graphene electrodes. These results demonstrated the importance and great potential of graphene based composites in the development of high-performance energy-storage systems.     

Production of graphene nanosheets by supercritical CO2 process coupled with micro-jet exfoliation

A facile and cost-effective method which combines supercritical CO₂ and micro-jet exfoliation has been developed for producing graphene nanosheets with high-quality. CO₂ molecules can intercalate into the interlayer of graphite because of their high diffusivity and small molecule size in supercritical operation. The tensile stress induced by graphite interfacial reflection of compressive waves exert on the graphite flakes, which lead to further exfoliation of graphite. Scanning electron microscope (SEM), transmission electron microscope (TEM), atomic force microscopy (AFM), Raman spectrum and X-ray diffraction (XRD) are used to identify morphology and quality of the exfoliated graphene nanosheets, which reveal that the graphite was successfully exfoliated into graphene and more than 88% of graphene nanosheets are less than three layers. The yield of graphene nanosheets is about 28 wt% under optimum conditions, which can be greatly improved by repeated exfoliation of the graphene sediment. The pure graphene film has a high conductivity of 2.1 × 10⁵ S/m.     

碳包覆NiO纳米颗粒的制备与性能

采用直流电弧放电等离子体技术成功制备了碳包覆NiO(NiO@C)纳米颗粒,并对样品的形貌、晶体结构、粒度、比表面积和孔结构采用高分辨透射电子显微镜、X射线衍射、X射线能量色散分析谱仪、拉曼散射光谱和N_2吸-脱附等测试手段进行了分析。实验结果表明:直流电弧等离子体技术制备的NiO@C纳米颗粒具有典型的核壳结构,内核为面心立方结构的NiO纳米颗粒,外壳为碳层。颗粒形貌主要为立方体结构,粒度均匀,分散性良好,粒径分布在30~70nm范围,平均粒径为50nm,外壳碳层的厚度为5nm。NiO@C纳米颗粒BET比表面积为28m~2/g,等效直径为46nm,与TEM和XRD测得的结果基本一致。Raman光谱说明样品中碳包覆层的石墨化程度较低,发生了红移现象。     

氧化镍/镍/碳微球原位制备及葡萄糖传感性能

以葡萄糖、六水合氯化镍和尿素为原料, 通过水热反应一步制备前驱体Ni(OH)₂/C, 在高纯度氮气中煅烧获得NiO/Ni/C微球三元复合材料。采用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、X射线光谱(EDS)和拉曼(Raman)等手段, 分析NiO/Ni/C微球三元复合材料的形貌结构以及物相组成。结果表明: NiO/Ni/C微球为珊瑚花状结构, 直径约1.7 μm, Ni、NiO呈立方相。通过循环伏安法和计时电流法研究了NiO/Ni/C微球三元复合材料的电化学行为及葡萄糖传感性能。当Ni/NiO摩尔比为0.19时, 形成的NiO/Ni/C三元复合微球具有优异的葡萄糖传感性能, 其灵敏度为241.09 μA·mmol/(L·cm²), 线性响应范围为10 μmol/L~5.05 mmol/L, 最低检测限位10 μmol/L。该传感器具有灵敏度高、抗干扰能力强以及稳定性好等特点。     

Selective laser melting of graphene reinforced titanium matrix composites: Powder preparation and its formability

Graphene is an attractive reinforcement in enhancing performances of titanium matrix composites (TMCs). However, the fabrication of graphene reinforced TMCs components is challenging to conventional manufacturing technologies. Selective laser melting (SLM) shows great potential in fabrication of TMCs components. In this study, SLM was employed to fabricate graphene reinforced TMCs, and the effects of ball milling time on properties of composite powder and resultant SLM formability were investigated. The morphologies, chemical composition, flowability and phase constitute of composite powder were evaluated by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Hall flowmeter and X-ray diffraction (XRD), respectively. The structure of graphene in composite powder was assessed by Raman spectroscopy. The formability of SLM scanning-track using different composite powder was also studied. The results showed that the composite powder, milled for 5 h, possessed good sphericity, good flowability and well-dispersion of graphene. Finally, the SLM-processed graphene reinforced TMCs, using the optimized composite powder, exhibited higher microhardness of 432.03 HV_0.2, higher tensile strength of 1276 MPa and lower coefficient of friction of 0.3453 than that of the SLM-processed TC4, revealing the great improvement in mechanical performance of the SLM-processed TMCs by adding graphene.     

聚醚酰亚胺基炭分子筛膜的形成及其气体分离性能研究

以商用聚醚酰亚胺(PEI)作为前驱体,采用经过ZrO2-Al2O3复合溶胶修饰的陶瓷氧化铝为支撑体,浸渍涂膜制备聚合物膜,在空气中预氧化处理后,经500～800℃不同的炭化温度下制备出气体分离炭分子筛膜。为了考察炭化温度对炭膜结构和气体分离性能的影响,采用热重分析(TG)、拉曼光谱(Raman)、X射线衍射(XRD)、扫描电镜(SEM)和气体渗透等测试手段,对热解过程聚合物膜热稳定性、炭微晶结构及石墨化进程、微观形貌和气体分离性能进行了系统研究。结果表明,不同的炭化温度对所形成炭膜表现出不同物理和化学结构、炭结构和孔结构,最终影响炭分子筛膜的气体渗透性和分离选择性。     

基于三元金属催化剂制备碳纳米管/三维石墨烯复合材料及电容性能

通过均匀沉淀法合成Ni-Mg-Al三元金属氧化物（TMO）,再通过一步化学气相沉积法（CVD）以CH₄为碳源、Ar为保护性气体,在原位还原的Ni上生长碳纳米管（CNTs）,在Mg和Al的金属氧化物上生长石墨烯（GR）,利用水热法刻蚀掉TMO,制备CNTs/三维石墨烯（3DGR）复合材料。基于CNTs与GR两种组分生长动力学的差异,通过控制Ni、Mg和Al三种金属离子的摩尔比、生长温度、生长时间,调控和优化CNTs/3DGR复合材料的结构及电容性能。借助TEM、SEM、EDS、Raman和XRD对CNTs/3DGR复合材料的结构、形貌、组分进行表征。结果表明,CNTs与GR协同作用为CNTs/3DGR复合材料提供了更多电子运输通道,可大幅提高导电性能,实现电容性能的提升,CNTs/3DGR复合材料的比电容最高可达20 F/g。