Chemical vapor deposition growth behavior of graphene

The optimized growth parameters of graphene with different morphologies,such as dendrites,rectangle,and hexagon,have been obtained by low-pressure chemical vapor deposition on polycrystalline copper substrates.The evolution of fractal graphene,which grew on the polycrystalline copper substrate,has also been observed.When the equilibrium growth state of graphene is disrupted,its intrinsic hexagonal symmetry structure will change into a non-hexagonal symmetry structure.Then,we present a systematic and comprehensive study of the evolution of graphene with different morphologies grown on solid copper as a function of the volume ratio of methane to hydrogen in a controllable manner.Moreover,the phenomena of stitching snow-like graphene together and stacking graphene with different angles was also observed.     

铜基石墨烯的CVD法制备工艺参数研究

采用乙炔作为碳源,分析了碳源浓度、生长时间等参数对铜基石墨烯成核密度、生长速率及单层覆盖率的影响,通过热氧化法系统展示了石墨烯形核、长大、生长结束的全过程.研究发现;碳源浓度较小时成核密度较低,所得石墨烯晶粒更大,但单个多层点的面积较大,且多以双层为主;在石墨烯生长过程中,氢气既可辅助碳氢化合物分解,同时也会刻蚀部分成核点,从而促进石墨烯质量的提高;基于单层率与晶粒尺寸之间的平衡,采用乙炔与氢氩混合气(体积比为1∶9)流速比为5∶100作为生长石墨烯的气体工艺参数,获得了透过率约为97.1%,缺陷较少且以单层为主的大面积石墨烯.     

合成参数对MOCVD法生长氧化锌纳米针的影响

使用脉冲液滴注入式MOCVD,在金膜裹覆的MgO(100)衬底上于500℃合成氧化锌纳米针.纳米针为晶态并且在XRD谱线上主要呈现ZnO的4个衍射强峰(100)、(002)、(101)及(004).金没有起到催化剂的作用,在较薄(2.4nm)金膜上生长的纳米针密度较高且直径较小.500℃是ZnO纳米针较佳的合成温度,在温度不低于550℃时合成的是片状ZnO.每周期前驱体的注入剂量对纳米针的形貌有显著影响.充足的注入剂量(6.8mg/周期)能够保证纳米针合成,而较低的注入剂量(3.4mg/周期)将会合成较短且直径较小的纳米针.     

玻璃陶瓷基板上铜薄膜的化学气相沉积

使用低介电常数基板和高电导率、高抗电迁移的金属Cu进行布线,可以提高高密度电子封装的传输速度和可靠性。采用乙酰丙酮铜作为前驱体,在常压下利用化学气相沉积技术对玻璃陶瓷基板进行Cu薄膜金属化。利用热重分析、X射线衍射和扫描电子显微镜等技术对前驱体、Cu薄膜进行分析观察。结果表明:影响Cu导体的电阻的主要因素是沉积温度。在温度为290～310℃,N2气流量为200～350mL/min和H2气流量为450～600mL/min的条件下,获得了致密的Cu薄膜,Cu导体方块电阻为25mΩ。     

Fabrication of copper nanorods by low-temperature metal organic chemical vapor deposition

Copper nanorods have been synthe-sized in mesoporous SBA-15 by a low-temperature metal organic chemical vapor deposition (MOCVD) employing copper (II) acetylacetonate, Cu(acac)2, and hydrogen as a precursor and reactant gas, re- spectively. The hydrogen plays an important role in chemical reduction of oganometallic precursor which enhances mass transfer in the interior of the SBA-15 porous substrate. Such copper nanostructures are of great potentials in the semiconductor due to their unusual optical, magnetic and electronic properties. In addition, it has been found that chemically modi- fying the substrate surface by carbon deposition is crucial to such synthesis of copper nanostructures in the interior of the SBA-15, which is able to change the surface properties of SBA-15 from hydrophilic to hydrophobic to promote the adsorption of organic cupric precursor. It has also been found that the copper nanoparticles deposited on the external sur- face are almost eliminated and the copper nanorods are more distinct while the product was treated with ammonia. This approach could be achieved under a mild condition: a low temperature (400℃) and vac-uum (2 kPa) which is extremely milder than the con- ventional method. It actually sounds as a foundation which is the first time to synthesize a copper nanorod at a mild condition of a low reaction temperature and pressure.     

Effects of the flow rate of hydrogen on the growth of graphene

Graphene samples with different morphologies were fabricated on the inside of copper enclosures by low pressure chemical vapor deposition and tuning the flow rate of hydrogen. It is found that the flow rate of hydrogen greatly influences the growth of graphene. Thermodynamic analysis indicates that a higher flow rate of hydrogen is favorable to the formation of good quality graphene with regular morphology. However, the mass-transfer process of methane dominates the growth driving force. At very low pressure, mass-transfer proceeds by Knudsen diffusion, and the mass-transfer flux of methane decreases as the flow rate of hydrogen increases, leading to a decrease in the growth driving force. At a higher pressure, mass-transfer proceeds by Fick's diffusion, and the mass-transfer flux of methane is dominated by the gas velocity, whose variation determines the growth driving force variation of graphene.     

Catalyst enhanced chemical vapor deposition of nano-particle nickel films on teflon surface

Films formed with nanosized nickel particles on teflon surface were prepared by means of catalyst enhanced chemical vapor deposition (CECVD) with Ni(dmg)₂, Ni(acac)₂, Ni(hfac)₂, Ni(TMHD)₂, and Ni(cp)₂ as precursors, and complexes Pd(hfac)₂, PdCl₂ and Pd(η ³-2-methylallyl)acac as catalyst under carrier gas (H₂). The film growth rate depends on the precursors and substrate temperature. The chemical value, purity and surface morphology of the Ni particle films were characterized by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The films obtained were shiny with silvery color, and consisted of grains with a particle size of 50–140 nm. The Ni was metallic of which the purity was about 90%–95% from XPS analysis. SEM micrograph showed that the film had good morphology.      

单源化学气相沉积法制备In2O3纳米线

以乙酰丙酮合铟[In（acac）3]（acac=acetylacetonate）作为单源前驱体,Au为催化剂,采用化学气相沉积法,于较低温度（550℃）下成功制得了In2O3纳米线．用X射线粉末衍射（XRD）、扫描电镜（SEM）、透射电镜（TEM）和能量分散光谱（EDS）对In2O3纳米线进行了表征;制得的In2O3纳米线具有单晶结构,平均直径约为80nm,长度达十几微米,其生长服从气一液一固机理．光致发光研究发现,In2O3纳米线在483nm处有一个强的发射峰,这可归因于氧空位的存在．     

Synthesis of nano onion-like fullerenes by using Fe/Al2O3 as catalyst by chemical vapor deposition

Nano-carbon materials were synthesized by the catalytic decomposition of acetylene at 400℃ by using Fe/Al₂O₃ as catalyst. The product was refluxed in 36% concentrated HCl at 60℃ for 48 h in order to remove the catalyst support. The samples were examined by scanning and high resolution transmission electron microscopy, energy dispersive spectroscopy and X-ray diffraction. The results show that nano onion-like fullerenes encapsulating a Fe₃C core were obtained. These had a structure of stacked graphitic fragments, with diameters ranging from 15―50 nm. When the product was further heat- treated at 1100℃ for 2 h, nano onion-like fullerenes with a clear concentric graphitic layer structure were obtained. The growth mechanism of nano onion-like fullerenes encapsulating metal cores is suggested to follow a vapor-solid growth model.     

Well-aligned carbon nanotube array membrane synthesized in porous alumina template by chemical vapor deposition

A new simple approach was devetoped for preparing wetl-aligned and monodispersed carbon nanotube (CNT) array membrane within the cylindrical pores of anodic aluminum oxide (AAO) template by chemical vapor deposition (CVD). Acetylene and hydrogen were used in the CVD process with Fe-catalyzer at 700°C under 250 Pa. Scanning etectron microscope (SEM) and transmission etectron microscope (TEM) were employed to characterize the resulting highly-oriented uniform hollow tube array which had a diameter of about 250 nm, a tube density of 5.3x10⁸ cm² and a length of about 60 μm. The length and diameter of the tubes depend on the thickness and pore diameter of the template. The growth properties of the CNT array film can be achieved by controlling the structure of the template, the particle size of Fe-catalyzer, the temperature in the reactor, the flow ratio and the deposition time. The highly-oriented and uniform CNT array membrane fabricated by this simple method is very much useful in a variety of applications.     

Controllable synthesis of Ni-catalyzed tetragonal tungsten nanowires via chemical vapor deposition

Controllable synthesis of Ni-catalyzed tetragonal tungsten nanowires via chemical vapor deposition     

Synthesis of graphene on a Ni film by radio-frequency plasma-enhanced chemical vapor deposition

Large-area single-or multilayer graphene of high quality is synthesized on Ni films by radio-frequency plasma-enhanced chemical vapor deposition (RF-PECVD) at a relatively low temperature (650℃).In the deposition process,a trace amount of CH4 gas (2-8 sccm (sccm denotes standard cubic centimeter per minute at STP)) is introduced into the PECVD chamber and only a short deposition time (30-60 s) is used.Single-or multilayer graphene is obtained because carbon atoms from the discharging CH4 diffuse into the Ni film and then segregate out at its surface.The layer number of the obtained graphene increases when the deposition time or CH4 gas flow rate is increased.This investigation shows that PECVD is a simple,low-cost,and effective technique to synthesize large-area single-or multilayer graphene,which has potential for application as electronic devices.     

Pulsed metal organic chemical vapor deposition of InAlN-based heterostructures and its application in electronic devices

As a promising group III-nitride semiconductor material, InAlN ternary alloy has been attracted increasing interest and widespread research efforts for optoelectronic and electronic applications in the last 5 years. Following a literature survey of current status and progress of InAlN- related studies, this paper provides a brief review of some recent developments in InAlN-related III-nitride research in Xidian University, which focuses on innovation of the material growth approach and device structure for electronic applications. A novel pulsed metal organic chemical vapor deposition （PMOCVD） was first adopted to epitaxy of InAlN-related heterostructures, and excellent crystalline and electrical properties were obtained. Furthermore, the first domestic InAlN-based high-electron mobility transistor （HEMT） was fabricated. Relying on the PMOCVD in combination with special GaN channel growth approach, high-quality InAlN/GaN double-channel HEMTs were successfully achieved for the first time. Additionally, other potentiality regarding to AlGaN channel was demonstrated through the successful realization of nearly lattice-matched InAlN/AlGaN heterostructures suitable for high-voltage switching applications. Finally, some advanced device structures and technologies including excellent work from several research groups around the world are summarized based on recent publications, showing the promising prospect of InAlN alloy to push group III-nitride electronic device performance even further.     

放电电流对热阴极等离子体化学气相沉积金刚石膜影响

建立了快速沉积高品质金刚石膜的热阴极辉光放电等离子体化学气相沉积新方法. 相对于常规冷阴极辉光放电而言,热阴极辉光放电是一种新型放电形式,具有许多新的特性,其中重要一点是具有较高的放电电流(6.0～10.0 A). 较高的放电电流既是热阴极辉光放电本身的突出特点,同时对于化学气相沉积金刚石膜工艺也产生重要影响. 实验研究了放电电流于金刚石膜沉积速率、表面形貌和热导率的影响,发现由于放电电流影响辉光放电的等离子体区和阳极区,进而对金刚石膜的沉积速率和品质有很大影响. 特别是通过放电电流的提高,可以有效地提高金刚石膜的品质,这对于制备优质金刚石膜产品有重大意义.     

石墨烯薄膜的化学气相法制备及光、电特性研究

利用化学气相沉积方法制备了石墨烯薄膜,并研究了其光电特性。以乙醇做反应原料、氩气作为携载气体,在873 K、973 K、1 073 K的温度下合成石墨烯薄膜。应用光学显微镜观察,发现在1 073 K时能够制备大面积均匀、平整光滑的石墨烯薄膜。纳曼光谱分析结果表明:制备的石墨烯薄膜出现2 650 cm-1的石墨烯的特征峰-D强峰,同时该峰强度随温度的升高而迅速增强,说明低温不能使沉积的碳原子有效的石墨化为石墨烯,而较高的温度有助于乙醇分解并石墨化为石墨烯薄膜。在1 073 K时沉积的石墨烯薄膜具有良好的光、电特性,其电子迁移率可以达到104 cm2.(V.s)-1,光透射率达97%,因此,可用于制备石墨烯晶体管、太阳能电池等光电子器件。     

采用热丝化学气相沉积法制备SiCN薄膜的研究

采用热丝化学气相沉积(HFCVD)系统,在单晶Si衬底上制备SiCN薄膜。所采用的源气体为高纯的SiH4,CH4和N2。用原子力显微镜(AFM)、X线衍射谱(XRD)和X线光电子能谱(XPS)对样品进行表征与分析。研究结果表明:SiCN薄膜表面由许多粒径不均匀、聚集紧密的SiCN颗粒组成;薄膜虽然已经晶化,但晶化并不充分,存在着微晶和非晶成分,通过Jade软件拟合计算出薄膜的结晶度为48.72%;SiCN薄膜不是SiC和Si3N4的简单混合,薄膜中Si,C和N这3种元素之间存在多种结合态,主要的化学结合状态为Si—N,Si—N—C,C—N,N=C和N—Si—C键,但是,没有观察到Si—C键,说明所制备的薄膜形成了复杂的网络结构。     

Synthesis of carbon nanotube array using corona discharge plasma-enhanced chemical vapor deposition

A corona discharge phasma-enhanced chemical vapor deposition with the features of atmospheric pressure and low temperature has been developed to synthesize the carbon nanotube array ,The array was synthesized from methane and hydrogen mixture in anodic aluminum oxide template channels in that cobalt was electrodeposited at the bottom.The characterization results by the scanning electron microscopy,transmission electron microscopy,energy dispersive X-ray spectroscopy and Raman spectroscopy indicate that the array consists of carbon nanotubes with the diameter of about 40 nm and the length of more than 4 μm, and the carbon anotubes are mainly restrained within the channels of templates.     

环氧树脂上激光诱导局部化学沉铜

用激光诱导化学沉积方法在非导体环氧树脂基体上实现微区局部、快速化学沉铜，并用卢瑟福背散射和扫描电镜方法对镀层的形貌、性质进行了观测和分析。激光的输出功率密度及照射时间决定了镀斑的面积和厚度。所得镀层比传统方法所得的化学镀层更致密。同时，由于激光照射引起的短时局部高温，使界面的金属原子向光照区基体内部扩散，得到的铜镀层与基体有较好的结合力。     

Synthesis of carbon nanotube array using corona discharge plasma-enhanced chemical vapor deposition

Carbon nanotube array plays an important role in the area of nanomaterials due to its potential applications, e.g. as field emitter in flat panel display[1,2] and as template for synthesizing arrays of other important nanomaterials[3]. Anodic aluminum oxide (AAO) template possesses an ordered porous structure that is formed through self-or- ganization during anodization[4,5], and is widely used to synthesize one-dimensional nanomaterial arrays[6]. Carbon nanotubes are usually assembled into t…     

Growth behavior of polycrystalline silicon thin films deposited by RTCVD on quartz substrates

Polycrystalline silicon (poly-Si) thin films were prepared on quartz substrates by rapid thermal chemical vapor deposition (RTCVD) system, and their structures were studied by XRD, SEM and TEM, respectively. XRD spectra exhibit a single strong (220) diffraction peak, which indicates that the poly-Si films are preferentially <110> oriented. Plane-view SEM images show that the surface of the poly-Si films is composed of large numbers of polygonal pyramid grains with different sizes, and cross-section SEM images further indicate that they are columnar grains with growth direction perpendicular to substrate surface. TEM observation results demonstrate that there are a lot of twin crystals including one-order, two-order and high-order (≥3) twin crystals in the poly-Si films. The above experimental results can not be elucidated by the conventional opinion on growth behavior of poly-Si films prepared by atmosphere pressure chemical vapor deposition (APCVD), but can be explained by the Ino’s multiply twinned particles (MTPs) model found in the face centered cubic metal films. According to the above experimental results and Ino’s model, we tend to think that nucleation and grain growth of poly-Si films deposited by RTCVD on quartz substrates are based on the formation of MTPs, and then these MTPs form the continuous films in an island growth mode.