Addendum to: Fabrication and characterization of graphene derived from SiC

<正>Addendum to:Science China:Physics,MechanicsAstronomy,2013,56(12):2386–2394doi:10.1007/s11433-013-5348-2The legends of the following Figures should be as follows:Figure 3 AFM morphologies and Raman spectra of a EG on a 2 inch SiC(0001)measured at five representative regions.(a)AFM Morphology reproduced from ref.[14]with permission from Science China Press and Springer publishing,(b)Raman spectra.Figure 6 SEM images of the VAGS.(a)Cross-section image of the VAGS;(b)and(c)are the top view images of the as-grown VAGS and the VAGS after top graphene layer removed reproduced from ref.[16]with permission from Wiley-VCH publishing.     

Fabrication and characterization of graphene oxide/zinc oxide nanorods hybrid

This work presented a hybrid architecture of graphene oxide (GO)/ZnO nanorods (ZNs) with ZNs attached parallel onto GO sheets. ZNs were synthesized by refluxing zinc acetate dehydrate in methanol solution under basic conditions followed by surface modification of 3-aminopropyl triethoxysilane (ATS), and then the preformed ZNs were attached onto GO sheets by reaction of the amino groups on the outer wall of ZNs with the carboxyl groups on the GO surface. Transmission electron microscopy (TEM) image of the as-prepared hybrid reveals the morphology of the architecture of GO/ZNs hybrid. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) ultraviolet-visible (UV-vis) and fluorescence spectroscopy were also performed to characterize the structure and properties of the GO/ZNs hybrid. It was shown that ZNs maintained their initial morphology and crystallinity in the hybrid and the luminescence quenching of yellow-green emission of ZNs confirmed the electron transfer from excited ZnO to GO sheets.     

Nano-sized patterns derived from a SiCN preceramic polymer: Fabrication and their characterization

A microfabrication of ceramic materials with a low shrinkage has created inevitable demands in the fields of micro total analysis systems (μ-TAS) and microfluidic devices with thermal, chemical, and mechanical stability. In this study, nano-sized patterns were prepared using a soft lithographic technique, followed by the UV and thermal curation of a non-oxide SiCN preceramic polymer. The characterization of the thermal and mechanical properties of the cured preceramic polymer revealed that it becomes ceramic-like after the heat treatment at higher temperature than 600 °C. The heat-treated nano-sized patterns showed a low linear shrinkage as well as good chemical stability and optical properties. The results showed the feasibility of enormous potentials of the cured preceramic polymer because of the low shrinkage, the high optical transparency, and the thermal and chemical stability.     

Fabrication of ionic polymer actuator with graphene nanocomposite electrodes and its characterization

In the present study, a novel ionic polymer actuator employing a graphene nanocomposite (GN) as its electrodes was fabricated. By a conventional solvent mixing of a graphene nanopowder and polystyrene, a GN solution was prepared. The solution was then utilized in a dip coating process of an ionic polymer membrane, forming a thin liquid GN layer on the surfaces of the ionic polymer membrane. After removing the solvent from the coated film, the solidified conducting GN layer could be obtained, which was used as the electrodes in the ionic polymer actuator. An electrical property of the GN layer formed by the present method was characterized, confirming the possibility of the present GN in the actuator applications. Simple and reverse bending motions of the fabricated actuator were also investigated, verifying the usefulness of both the GN layer and the present simple fabrication method.     

Growth protocols and characterization of epitaxial graphene on SiC elaborated in a graphite enclosure

The epitaxial growth of graphene by the sublimation of Si-terminated silicon carbide (SiC) is studied inside a graphite enclosure in a radio-frequency furnace by comparing different in situ processes involving hydrogen etching or not and different growth conditions. For the growth under vacuum, even with the surface preparation of hydrogen etching, the morphology of the synthesized graphene is found full of voids and defects in the form of a multilayer graphene film. For the growth under Ar, the hydrogen etching plays a vital role to improve the graphene quality in terms of surface roughness, the number of graphene layers and the domain size. For the graphene samples grown with the proposed protocol, the original combination of micro-probe Raman spectroscopy and simultaneous optical transmission and reflection measurements reveals a detailed spatially resolved image of the graphene domains with monolayer domain size of ~5×5 µm² on about 2/3 of the total sample surface. The magnetotransport data yield charge-carrier mobilities up to 2900 cm²/Vs as found for high quality graphene on the Si-face of SiC. The observed magnetoquantum oscillations in the magnetoresistance confirm the expected behavior of single-layer graphene.     

石墨烯纳米结构的制备及带隙调控研究

石墨烯在未来微电子学领域有极大的应用前景,但是其零带隙的特点阻碍了石墨烯在半导体领域的应用.研究发现,打开室温下可用的石墨烯带隙所需要的石墨烯纳米结构尺度在10 nm以下,这一尺度的纳米结构一方面制备比较困难,另一方面器件可承载的驱动电流较小.因此,如何实现亚10 nm石墨烯纳米结构的有效加工以及如何在有效调控带隙的基础上增大石墨烯器件可承载的驱动电流,还需要进一步的研究.本文首先研究了利用聚甲基丙烯酸甲酯/铬(PMMA/Cr)双层结构工艺,通过刻蚀时间的控制,利用电子束曝光及刻蚀工艺实现了亚10 nm石墨烯纳米结构的可控制备.同时设计并制备了单排孔石墨烯条带结构,该结构打开的带隙远大于相同特征宽度石墨烯纳米带所能打开带隙的大小.该结构在有效打开石墨烯带隙的同时,增加了石墨烯纳米结构可以承载的驱动电流,有利于石墨烯在未来微电子领域的应用.     

石墨烯纳米带的制备与电学特性调控

石墨烯由于其独特的晶体结构展现出了特殊的电学特性,其导带与价带相交于第一布里渊区的六个顶点处,形成带隙为零的半金属材料,具有优异的电子传输特性的同时也限制了其在电子学器件中的使用.因而科研人员尝试各种方法来打开其带隙并调控其能带特性,主要有利用缺陷、应力、掺杂、表面吸附、结构调控等手段.其中石墨烯纳米带由于量子边界效应和限制效应,存在带隙.本综述主要介绍了制备各类石墨烯纳米带的方法,并通过精确调控其细微结构,从而对其进行精确的能带调控,改变其电学特性,为其在电子学器件中的应用提供一些可行的方向.     

Ab initio study of graphene on SiC

Employing density-functional calculations we study single and double graphene layers on Si- and C-terminated 1x1-6H-SiC surfaces. We show that, in contrast with earlier assumptions, the first carbon layer is covalently bonded to the substrate and cannot be responsible for the graphene-type electronic spectrum observed experimentally. The characteristic spectrum of freestanding graphene appears with the second carbon layer, which exhibits a weak van der Waals bonding to the underlying structure. For Si-terminated substrate, the interface is metallic, whereas on C face it is semiconducting or semimetallic for single or double graphene coverage, respectively.     

碳化硅凸非球面反射镜的加工与检测

为了满足凸非球面反射镜加工中的全频段质量控制及光学参数的高精度检验,提出了应用双摆轴极坐标快速非球面加工技术及测杆法控制Hindle法检测光学参数。首先,描述了双摆轴极坐标快速非球面加工技术及设备;然后,介绍了应用测杆法控制Hindle检测法中标准球面镜顶点分别与被检非球面镜顶点及其焦点的光学间隔,并对其控制精度进行了分析;最后,针对Φ158mm的凸非球面,给出了双摆轴加工的检验结果,并对检测精度进行了分析。实验结果表明：应用双摆轴加工工艺在使低频误差快速收敛的同时,可以有效抑制中频误差,其低频误差的控制精度可以稳定地达到λ/30（λ=633 nm）;应用测杆装调Hindle检测光路的控制极限误差为±0.065 mm,两个光学间隔参数的公差分别为±0.22 mm和±0.30 mm。应用双摆轴加工技术实现了凸非球面的快速加工与全频段质量控制,采用Hindle检测凸非球面得到面形精度为0.022λ（RMS,@633 nm）,满足光学设计技术指标要求。     

Phonons of graphene and graphitic materials derived from the empirical potential LCBOPII

We present the interatomic force constants and phonon dispersions of graphite and graphene from the LCBOPII empirical bond order potential. We find a good agreement with experimental results, particularly in comparison to other bond order potentials. From the flexural mode we determine the bending rigidity of graphene to be 0.69 eV at zero temperature. We discuss the large increase of this constant with temperature and argue that derivation of force constants from experimental values should take this feature into account. We examine also other graphitic systems, including multilayer graphene for which we show that the splitting of the flexural mode can provide a tool for characterization.     

Fabrication of ultrasound-mediated tunable graphene oxide nanoscrolls

In this work, a cost-effective and facile method was adopted for the fabrication of graphene oxide nanoscrolls (GONS) by low frequency (20 kHz) ultrasonication with tunable dimensions. The graphene oxide (GO) was synthesized by modified Hummer’s method using synthetic graphite as a base material. Later, GO suspension (0.05 g L⁻¹) were made using methanol as solvent and subjected to different ultrasonication conditions. It was found that GO sheets curls themselves into nanoscrolls by overcoming the energy barrier for scrolling with the help of bubble cavitation energy provided by ultrasonication. Also, the effect of ultrasonication power (100–150 W) for irradiation time (0.5–3 h) over the GONS dimensions were investigated. The spiral wounded GONS structures were shown using electron microscopy. Raman Spectroscopy, Thin-film X-Ray Diffraction, Energy Dispersive X-Ray, FT Infrared Spectroscopic analysis were also done to endorse GONS formation. Factors affecting GONS formation such as sonication power and solvent selection were studied as scrolling of GO sheets are strongly dependent on sonication parameters and solvent characteristics. It was found that GONS length varies inversely with irradiation time for identical power density. Also, a solvent with relatively large Hansen solubility parameter, lower dipole movement and less negative value of zeta potential support GONS formation of longer length. Raman analysis overlays the rapid oxygen-defect site cleavage mechanism. The obtained GONS unlocks further developments in various engineering applications like adsorption, drug delivery and filtration membrane.     

Fabrication of graphene nanostructures by probe nanoablation

We present the results of the study of graphene nanoablation under mechanical stress of an ultrasharp (the rounding radius is ～2 nm) tip of a scanning probe microscope (SPM)). It was found that the SPM probe contact with graphene results in average removal of 7 · 10^?3?5 · 10^?2 nm of film per scan, i.e., only a few carbon atoms or clusters, in the impact area. The capability of this precision nanoablation process was shown in developing graphene nanoislands and nanoribbons ～1 µm long and ～10 nm wide.     

Fabrication of suspended graphene devices and their electronic properties

Suspended graphene devices are successfully fabricated by using a novel PMMA/MMA/PMMA tri-layer resist technique. The gap between graphene and dielectric substrate can be easily controlled by the thickness of the bottom PMMA layer, and no wet-etching with hazardous hydrofluoric acid is involved in our fabrication process. Electrical characterizations on suspended graphene devices are performed in vacuum when in-situ current annealing directly leads to a significant improvement on transport properties of graphene, i.e., the increase of carrier mobility with the reduction of width of Dirac peak. Our results make a new opportunity to study intrinsic properties of graphene.     

Epitaxial graphene perfection vs. SiC substrate quality

Polytype instability of SiC epitaxial films was the main focus of attention in the experiment performed since this factor has a decisive influence on graphene growth, which was the second stage of the experiment. Layers deposited in various initial C/Si ratios were analyzed.     

A torsional potential for graphene derived from fitting to DFT results

We present a simple torsional potential for graphene to accurately describe its out-of-plane deformations. The parameters of the potential are derived through appropriate fitting with suitable DFT calculations regarding the deformation energy of graphene sheets folded around two different folding axes, along an armchair or along a zig-zag direction. Removing the energetic contribution of bending angles, using a previously introduced angle bending potential, we isolate the purely torsional deformation energy, which is then fitted to simple torsional force fields. The presented out-of-plane torsional potential can accurately fit the deformation energy for relatively large torsional angles up to 0.5 rad. To test our proposed potential, we apply it to the problem of the vertical displacement of a single carbon atom out of the graphene plane and compare the obtained deformation energy with corresponding DFT calculations. The dependence of the deformation energy on the vertical displacement of the pulled carbon atom is indistinguishable in these two cases, for displacements up to about 0.5 Å. The presented potential is applicable to other sp² carbon structures.     

Fabrication of functionalized nitrogen-doped graphene for supercapacitor electrodes

A unique and convenient one-step hydrothermal process for synthesizing functionalized nitrogen-doped graphene (FGN) via ethylenediamine, hydroquinone, and graphene oxide (GO) is described. The graphene sheets of FGN provide a large surface area for hydroquinone molecules to be anchored on, which can greatly enhance the contribution of pseudocapacitance. X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectroscopy, and electrochemical workstation are used to characterize the materials. The nitrogen content exhibited in FGN can be up to 9.83 at.%, and the as-produced graphene material shows an impressive specific capacitance of 364.6 F g^?1 at a scan rate of 10 mV s^?1, almost triple that of the graphene (GN)-based one (127.5 F g^?1). Furthermore, the FGN electrodes show excellent electrochemical cycle stability with 94.4 % of its initial capacitance retained after 500 charge/discharge cycles at the current density of 3 A g^?1.     

锯齿形石墨烯反点网络加工与输运性质研究

具有特定边界的石墨烯纳米结构在纳电子学、自旋电子学等研究领域表现出良好的应用前景.然而石墨烯加工成纳米结构时,无序的边界不可避免地会降低其载流子迁移率.氢等离子体各向异性刻蚀技术是加工具备完美边界石墨烯微纳结构的一项关键技术,刻蚀后的石墨烯呈现出规则的近原子级平整的锯齿形边界.本文研究了氮化硼上锯齿形边界石墨烯反点网络的磁输运性质,低磁场下可以观测到载流子围绕着一个空位缺陷运动时的公度振荡磁阻峰.随着磁场的增大,朗道能级简并度逐渐增大,载流子的磁输运行为从Shubnikov-de Haas振荡逐渐向量子霍尔效应转变.在零磁场附近可以观测到反点网络周期性空位缺陷的边界散射所导致的弱局域效应.研究结果表明,在氮化硼衬底上利用氢等离子体刻蚀技术加工锯齿形边界石墨烯反点网络,其样品质量会明显提高,这种简单易行的方法为后续高质量石墨烯反点网络的输运研究提供了新思路.     

微米光栅加速度计的加工与性能研究

介绍了一种以微米衍射光栅为敏感元件的微机电加速度计敏感头的加工和性能。硅质量块底部加工有铝反射膜,透明玻璃基底上制作有金微米光栅,中间为空气腔,经硅玻璃阳极键合,构成敏感头的核心敏感部件。光源透过透明基底,照射在光栅上,在反射场内会产生一系列衍射级次,且各级次衍射光强与外界加速度之间呈函数关系。完成了微米光栅加速度计敏感头的加工,搭建了实验测试平台,完成了加速度计的灵敏度以及静电驱动性能测试。为未来新型集成式微米光栅加速度计设计和加工提供参考。