Origin,characteristics, and suppression of residual nitrogen in MPCVD diamond growth reactor

Unintentional nitrogen incorporation has been observed in a set of microwave plasma chemical vapor deposition (MPCVD)-grown samples. No abnormality has been detected on the apparatus especially the base pressure and feeding gas purity. By a comprehensive investigation including the analysis of the plasma composition, we found that a minor leakage of the system could be significantly magnified by the thermal effect, resulting in a considerable residual nitrogen in the diamond material. Moreover, the doping mechanism of leaked air is different to pure nitrogen doping. The dosage of several ppm of pure nitrogen can lead to efficient nitrogen incorporation in diamond, while at least thousands ppm of leaked air is required for detecting obvious residual nitrogen. The difference of the dosage has been ascribed to the suppression effect of oxygen that consumes nitrogen. As the unintentional impurity is basically detrimental to the controllable fabrication of diamond for electronic application, we have provided an effective way to suppress the residual nitrogen in a slightly leaked system by modifying the susceptor geometry. This study indicates that even if a normal base pressure can be reached, the nitrogen residing in the chamber can be "activated" by the thermal effect and thus be incorporated in diamond material grown by a MPCVD reactor.     

Interaction between plasma and electromagnetic field in ion source of 10 cm ECR ion thruster

Through diagnosing the plasma density and calculating the intensity of microwave electric field, four 10 cm electron cyclotron resonance (ECR) ion sources with different magnetic field structures are studied to reveal the inside interaction between the plasma, magnetic field and microwave electric field. From the diagnosing result it can be found that the plasma density distribution is controlled by the plasma generation and electron loss volumes associated with the magnetic field and microwave power level. Based on the cold plasma hypothesis and diagnosing result, the microwave electric field intensity distribution in the plasma is calculated. The result shows that the plasma will significantly change the distribution of the microwave electric field intensity to form a bow shape. From the boundary region of the shape to the center, the electric field intensity varies from higher to lower and the diagnosed density inversely changes. If the bow and its inside lower electric field intensity region are close to the screen grid, the performance of ion beam extracting will be better. The study can provide useful information for the creating of 10 cm ECR ion source and understanding its mechanism.     

大面积等离子体片密度分布分析

利用空心阴极放电产生了尺寸为60 cm× 60 cm× 2 cm的大面积等离子体面. 在实验室条件下对大面积等离子体片的密度分布进行了测量. 由于高压放电脉冲脉宽较短, 实验中改变了测量方法, 同时, 在中等磁场影响下, 为了得到真实的等离子体密度, 进行了必要的数值修正.在放电电流为1---6 A时, 测量了二维的电子密度分布. 另外, 测量并讨论了其他环境参数对等离子体密度的影响. 电子密度的分布情况对与微波波束切换相当重要. 由空心阴极增强型放电产生的大面积等离子体面具有反射X波段(8---12 GHz) 微波需要的足够稠密的电子密度和足够均匀的密度分布, 这是等离子体面在雷达系统中取代金属面板的有利条件.     

Field emission characteristics of nano-sheet carbon films deposited by quartz-tube microwave plasma chemical vapour deposition

Nano-sheet carbon films are prepared on Si wafers by means of quartz-tube microwave plasma chemical vapour deposition （MPCVD） in a gas mixture of hydrogen and methane. The structure of the fabricated films is investigated by using field emission scanning electron microscope （FESEM） and Raman spectroscopy. These nano~carbon films are possessed of good field emission （FE） characteristics with a low threshold field of 2.6 V/μm and a high current density of 12.6 mA/cm^2 at an electric field of 9 V/μm. As the FE currents tend to be saturated in a high E region, no simple Fowler-Nordheim （F-N） model is applicable. A modified F N model considering statistic effects of FE tip structures and a space-charge-limited-current （SCLC） effect is applied successfully to explaining the FE data observed at low and high electric fields, respectively.     

金刚石膜/多孔硅复合材料的性能表征

提出了一种新颖的多孔硅表面钝化技术,即采用微波等离子体辅助的化学气相沉积（MPCVD）方法在多孔硅上沉积金刚石薄膜。采用原子力显微镜（AFM）、扫描电子显微镜（SEM）、X射线衍射仪（XRD）、拉曼光 谱仪和荧光分光度计对多孔硅及金刚石膜的表面形貌、结构和发光特性进行了表征。结果表明采用微波等离子体化学气相沉积法可在多孔硅基片上形成均匀、致密、性能稳定且对可见光具有全透性的金刚石膜。金刚石膜与多孔硅的复合,大大稳定了多孔硅的发光波长和强度,同时增强了多孔硅的机械强度。     

一氧化碳合成金刚石薄膜的形貌和结构分析

利用微波等离子体化学气相沉积(MPCVD)技术，采用偏压增加成核(BEN)、两步生长的方法在一氧化碳(CO)和氢气(H₂)的环境下制备了金刚石薄膜. 利用扫描电子显微镜(SEM)、Raman光谱仪和透射电子显微镜(TEM)对金刚石薄膜的形貌和结构进行了分析. 研究发现金刚石晶粒在第一步成核及生长的过程中产生了层错和孪晶，而在第二步的生长过程中产生的层错和孪晶很少，最终形成的金刚石晶粒外表面比较光滑，包含有近五次对称或者平行的片状的孪晶，并可以观察到少量的位错. 而在样品的边缘由于等离子体的不均匀产生了比样品中心成核密度低的区域. 在这个区域中，发现了一个新的非金刚石的碳结构.     

金刚石薄膜负偏压形核的边缘效应

 在微波等离子体化学气相沉积装置中，研究了金刚石薄膜在Si (100)面上的负偏压形核行为，结果表明，偏压大小对金刚石的形核均匀性有显著影响，而甲烷浓度主要影响形核时间，对金刚石的最大核密度影响不大。在硅片尺寸小于钼支撑架时，形核行为存在明显的边缘效应，即在偏压值低于-150 V时，硅片边缘金刚石核密度急剧降低，远低于硅片中央；在甲烷浓度比较低时，硅片边缘核密度要高于中间。研究表明，造成这种现象的主要原因是硅片下的钼支撑架发射电子所致，过量的原子H对金刚石的形核是不利的。     

Preparation of few-layer graphene-capped boron nanowires and their field emission properties

Large-area boron nanowire(BNW) films were fabricated on the Si(111) substrate by chemical vapor deposition(CVD). The average diameter of the BNWs is about 20 nm, with lengths of 5–10 μm. Then, graphene-capped boron nanowires(GC-BNWs) were obtained by microwave plasma chemical vapor deposition(MPCVD). Characterization by scanning electron microscopy indicates that few-layer graphene covers the surface of the boron nanowires. Field emission measurements of the BNWs and GC-BNW films show that the GC-BNW films have a lower turn-on electric field than the BNW films.     

类球状微米金刚石聚晶膜场发射的稳定性

在覆盖金属钛层的陶瓷上,利用微波等离子体化学气相沉积(MPCVD)法制备出类球状微米金刚石聚晶膜。通过二极管结构测试了聚晶膜的场致电子发射特性,利用扫描电子显微镜、拉曼光谱、XRD分析了场发射前后薄膜的结构和表面形貌的变化。发现在高场、大电流密度的场发射中,对类球状微米金刚石聚晶薄膜中的金刚石聚晶颗粒影响很小,而对金刚石聚晶颗粒间的非晶碳层影响很大。对类球状微米金刚石聚晶变化机理进行了研究。     

Growth and field emission properties of globe-like diamond microcrystalline-aggregate

The globe-like diamond microcrystalline-aggregates were fabricated by microwave plasma chemical vapor deposition (MPCVD) method. The ceramic with a Ti mental layer was used as substrate. The fabricated diamond was evaluated by Raman scattering spectroscopy, X-ray diffraction spectrum (XRD), and scanning electron microscope (SEM). The field emission properties were tested by using a diode structure in a vacuum. A phosphor-coated indium tin oxide (ITO) anode was used for observing and characterizing the field emission. It was found that the globe-like diamond microcrystalline-aggregates exhibited good electron emission properties. The turn-on field was only 0.55 V/μm, and emission current density as high as 11 mA/cm² was obtained under an applied field of 2.9 V/μm for the first operation. The growth mechanism and field emission properties of the globe-like diamond microcrystalline-aggregates are discussed relating to microstructure and electrical conductivity.     

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在微波化学气相沉积装置上采用微波激发氢气甲烷体系等离子体,通过光学多道分析仪采集等离子的发射光谱.实验表明,甲烷在等离子体中的裂解产物主要以CH,CH-,C2基团的形式存在.这些基团的发射光谱强度主要受放电压强和放电功率的影响.随着微波功率的增加甲烷基团发射光谱强度呈增长的趋势;而随着放电压强的增加则是先增大,后减小.这些实验结果对于理解微波等离子体化学气相沉积(MPCVD)中各种反应过程,调整薄膜制备工艺提供了参考.     

High-temperature pretreatment of Ni nanoparticles enhances the growth of high-density carbon fiber bundles during microwave plasma chemical vapor deposition

This paper presents an experimental study on the effect of the pretreatment procedure of Ni nanoparticles (NPs) on the growth of multiwalled carbon fiber (CNF) bundles by means of microwave plasma chemical vapor deposition (MPCVD). We used atomic force microscopy to investigate a series of pretreated Ni films. The structures and compositions of the CNFs on the via were investigated using scanning electron microscopy, high-resolution transmission electron microscopy, and Raman spectroscopy.The geometric shape of the Ni NPs was identified in terms of their roughness, which decreased upon increasing the pretreatment temperature, resulting subsequently in the synthesis of high-density CNFs. The diameter and shape of the Ni NPs were the dominant factors affecting the size and density of the CNFs bundles. We obtained CNFs that fully filled the via effectively; they might serve as potential interconnects in future nanodevices.     

Ferromagnetism dependence on hole carriers in polycrystalline silicon films co-doped with Mn and B

Polycrystalline Si_0.96Mn_0.04:B films were prepared by cosputtering deposition followed by rapid thermal annealing for crystallization. The films are ferromagnetic with Curie temperatures of about 250 K. Through the approach of microwave plasma enhanced chemical vapor deposition, the films were treated by hydrogen plasma and boron plasma. After the plasma treatments, the structural properties of the films did not change, while both the saturation magnetization and hole concentration in the films changed. The correlation between the magnetic properties and the transport properties of the Si_0.96Mn_0.04:B films suggests that free hole carriers play an important role in Si:Mn diluted magnetic semiconductors.     

电子温度对霍尔推进器等离子体鞘层特性的影响

采用二维粒子模拟方法研究了霍尔推进器通道中电子温度对等离子体鞘层特性的影响, 讨论了不同电子温度下电子数密度、鞘层电势、电场及二次电子发射系数的变化规律. 结果表明: 当电子温度较低时, 鞘层中电子数密度沿径向方向呈指数下降, 在近壁处达到最小值, 鞘层电势降和电场径向分量变化均较大, 壁面电势维持一稳定值不变, 鞘层稳定性好; 当电子温度较高时, 鞘层区内与鞘层边界处电子数密度基本相等, 而在近壁面窄区域内迅速增加, 壁面处达到最大值, 鞘层电势变化缓慢, 电势降和电场径向分量变化均较小, 壁面电势近似维持等幅振荡, 鞘层稳定性降低; 电子温度对电场轴向分量影响较小; 随电子温度的增大, 壁面二次电子发射系数先增大后减少. 关键词： 霍尔推进器 等离子体鞘层 电子温度 粒子模拟     

氢气浓度对MPCVD金刚石膜色度的影响

利用自行设计的直接耦合石英管微波等离子体化学气相沉积装置, 以氢气和甲烷为反应气体, 沉积出八个金刚石膜样品。研究了氢气浓度对所沉积金刚石膜色度的影响。结果表明, 饱和纯度和色纯度随着H2浓度的增大而升高; 当H2浓度达到94.137%时, 饱和纯度和色度纯度达到最大, 分别为8.5%和9.5%; 之后随着H2浓度的进一步升高饱和纯度和色纯度开始下降。     

高功率微波作用下等离子体中的雪崩效应研究

研究高功率微波作用下等离子体中的雪崩效应,对于研究等离子体防护技术具有重要意义.通过采用等离子体流体近似方法,建立等离子体中的波动方程、电子漂移-扩散方程和重物质传递方程,表征电磁波在等离子体中的传播以及等离子体内部带电粒子的变化情况,分析研究了高功率微波作用下雪崩效应的产生过程和变化规律.研究表明,入射电磁波功率决定了雪崩效应的产生;初始电子密度能够影响雪崩效应产生的时间;入射电磁波的激励作用初始表现为集聚效应,当激励能量积累到一定阈值时,雪崩效应才会产生;在雪崩效应产生过程中,等离子体内部电子密度的变化非常迅速并且比较复杂.雪崩效应产生后,等离子体内截止频率会远超过入射波频率,电磁波不能在等离子体中传播,从而起到防护高功率微波的效果.     

Mo离子注入对金刚石涂层附着性能的影响

采用Mo离子注入工艺对YG6硬质合金基体表面进行处理,用微波等离子体CVD(MPCVD)法沉积金刚石涂层,研究了Mo离子注入工艺对金刚石涂层附着性能的影响.结果表明,Mo离子注入后,硬质合金基体表面的化学成分发生了明显变化;采用适当剂量的Mo离子注入基体,可使CVD金刚石涂层的附着性能显著提高. 关键词： 金刚石涂层 Mo离子注入 硬质合金基体 附着性能     

射频击穿等离子体对高功率微波传输特性的影响

利用极化正交的高功率微波合路器,开展了等离子体对于微波传输特性的实验研究.通过改变前级源的功率和脉冲宽度,使得在合路器耦合缝处发生射频击穿,产生等离子体.等离子体扩散进入微波传输主通道,对于高功率微波的传输产生明显的影响,导致微波能量吸收和极化的偏转.初步实验结果表明,等离子体扩散到主通道中心的时间约为3μs,扩散速度约为1μs/cm,等离子体的恢复时间约为5μs.实验测得等离子体导致的微波极化方向最大偏转角度约为4.1?,此时通道内电子个数约为3.7×1015,极化偏转角度与电子数密度以及微波频率相关.     

Synthesis of beta-gallium oxide nanobelts through microwave plasma chemical vapor deposition

Beta-gallium oxide (β-Ga₂O₃) nanobelts were synthesized through microwave plasma chemical vapor deposition (MPCVD) of liquid-phase gallium containing H₂O in Ar atmosphere using silicon as the substrate. Unlike the common microwave plasma method, the H₂O, not mixture of the gas, was employed to synthesize the nanostructures. β-Ga₂O₃ nanobelts prepared by MPCVD have not been reported. The thickness of β-Ga₂O₃ nonobelts was 20–30 nm and length of them was tens to hundreds of microns. The morphology and structure of the products were analyzed by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and X-ray diffraction (XRD). Possible growth mechanisms of the β-Ga₂O₃ nanobelts are briefly discussed.     

Numerical study on the characteristics of nitrogen discharge at high pressure with induced plasma

Based on the fluid theory of plasma, a model is built to study the characteristics of nitrogen discharge at high pressure with induced argon plasma. In the model, species such as electrons, N2+, N4+, Ar+, and two metastable states (N 2(A3∑u+), N2 (a1 ∑u-)) are taken into account. The model includes the particle continuity equation, the electron energy balance equation, and Poisson抯equation. The model is solved with a finite difference method. The numerical results are obtained and used to investigate the effect of time taken to add nitrogen gas and initially-induced argon plasma pressure. It is found that lower speeds of adding the nitrogen gas and varying the gas pressure can induce higher plasma density, and inversely lower electron temperature. At high-pressure discharge, the electron density increases when the proportion of nitrogen component is below 40%, while the electron density will keep constant as the nitrogen component further increases. It is also shown that with the increase of initially-induced argon plasma pressure, the density of charged particles increases, and the electron temperature as well as the electric field decreases.