高能等离子体辅助CVD法新型纳米碳膜的制备及分析

利用自制高能等离子体辅助化学气相沉积设备在1Cr18Ni9Ti衬底上，在离子能量2keV、工作压力2Pa、工作气氛为CH₄/H₂=10%的工艺条件下得到了一种硬度高、导电性能良好、可能具有碳链结构的新型碳膜.工艺研究结果表明，衬底材料对制备该新型纳米碳膜具有关键作用，离子能量、工作压力及气氛等工艺因素也具有重要作用.原子力显微镜分析结果表明，该薄膜晶粒尺寸小于100nm，薄膜光滑、致密、均匀.拉曼光谱分析显示，该薄膜的拉曼光谱特征为中心峰在1580cm ^{关键词： 高能等离子体 CVD法 纳米碳膜 衬底材料}     

AlN thin films prepared by ArF plasma assisted PLD. Role of process conditions on electronic and chemical–morphological properties

Aluminium nitride thin films were deposited on n-Si <100> substrates by RF plasma activated reactive pulsed laser deposition (PLD). An ArF excimer pulsed laser, 10 Hz and 2.5 J/cm² energy fluence, has been used to ablate a pure Al target in a reactive atmosphere of N₂ plasma (generated by a RF source), at varying processing parameters (substrate temperature, time, and N₂ plasma configuration). We studied the dependence and correlation of structural and electronic properties with the experimental conditions. The chemical composition of deposited material has been determined by both Raman and X-ray photoelectron spectroscopy (XPS). Electrical resistivity has been evaluated by the sheet resistance method. Both spectroscopic characterizations (Raman and XPS) show a strong dependence in the formation of AlN on the deposition temperature. At low temperatures, there is little formation of nitride, with a prevalence of aluminium oxide, while at higher temperatures the N uptake increases, with AlN formation. Raman analysis also highlights the formation of nano-structures, for temperatures ≥400^°C. These material characteristics have a fundamental influence on the electronic properties. Indeed, electrical resistivity properties have been found to be strongly dependent on the film structure, nitrogen incorporation, and presence of mixed oxide compounds, closely related to deposition temperature.     

Vacuum arc deposition of carbon thin films in a low pressure ofhydrogen

Results on the vacuum arc deposition (VAD) of thin carbon films on silicon, tungsten, and nickel are presented for different hydrogen pressures in the arc chamber. Raman and Auger electron spectroscopy and SEM analysis show that a large variety of film structures can be obtained. Highly oriented pyrolytic graphite is formed at high hydrogen pressure and low substrate temperature. Vacuum deposition resulted in a diamondlike structure. Evidence of the presence of multicrystalline spheres of diamond in some films is also presented     

Study of nanocrystalline diamond film growth in rf hybrid laser deposition systems in O2, H2 and H2+Ar ambients

Pulsed laser deposition (PLD) and hybrid pulsed laser deposition (HPLD) systems were used for nanocrystalline diamond (NCD) film growth on Si(100) and sapphire(0001) substrates. The PLD system was based on a KrF excimer laser (=248 nm,20 ns), which ablated a graphite target in pure oxygen or hydrogen ambient. The HPLD system was based on a combination of PLD and additional capacitively coupled radio-frequency discharges (13.56 MHz) in argon–hydrogen ambient. Radio-frequency power was applied to two plane parallel electrodes or directly to the substrate holder. The working atmosphere pressure was varied from 1 Pa to 220 Pa and the substrate temperature was varied from 20 °C to 660 °C. X-ray diffraction analysis, Raman spectroscopy and a profilometer were used to study the deposited film properties. A band around 1180 cm^-1, which can be attributed to NCD, occurred in the Raman spectra. A characteristic diamond peak at 1332 cm^-1 was not observed. Films prepared by HPLD showed better compositional homogeneity (from Raman analysis) than films created by PLD. PACS 52.80.Pi; 81.07.Bc; 81.15.Fg     

Low energy repetitive miniature plasma focus device as high deposition rate facility for synthesis of DLC thin films

Diamond-like carbon (DLC) films were deposited on Si (1 0 0) substrate using a low energy (219 J) repetitive (1 Hz) miniature plasma focus device. DLC thin film samples were deposited using 10, 20, 50, 100 and 200 focus shots with hydrogen as filling gas at 0.25 mbar. The deposited samples were analyzed by XRD, Raman Spectroscopy, SEM and XPS. XRD results exhibited the diffraction peaks related to SiO₂, carbon and SiC. Raman studies verified the formation amorphous carbon with D and G peaks. Corresponding variation in the line width (FWHM) of the D and G positions along with change in intensity ratio (I_D/I_G) in DLC films was investigated as a function of number of deposition shots. XPS confirmed the formation sp² (graphite like) and sp³ (diamond like) carbon. The cross-sectional SEM images establish the 220 W repetitive miniature plasma focus device as the high deposition rate facility for DLC with average deposition rate of about 250 nm/min.     

Few-layer graphene growth from polystyrene as solid carbon source utilizing simple APCVD method

This research article presents development of an economical, simple, immune and environment friendly process to grow few-layer graphene by controlling evaporation rate of polystyrene on copper foil as catalyst and substrate utilizing atmospheric pressure chemical vapor deposition (APCVD) method. Evaporation rate of polystyrene depends on molecular structure, amount of used material and temperature. We have found controlling rate of evaporation of polystyrene by controlling the source temperature is easier than controlling the material weight. Atomic force microscopy (AFM) as well as Raman Spectroscopy has been used for characterization of the layers. The frequency of G′ to G band ratio intensity in some samples varied between 0.8 and 1.6 corresponding to few-layer graphene. Topography characterization by atomic force microscopy confirmed Raman results.     

非晶碳氮纳米尖端的微结构和发光机理

利用等离子体增强热丝化学气相沉积系统,用CH₄、H₂和N₂为反应气体,在Si衬底上制备了碳氮纳米尖端。用扫描电子显微镜和显微Raman光谱仪对其进行了表征。在室温下测试了它的发光性能,发光谱由中心约为406 nm和506 nm的两条发光带组成。根据Raman散射谱,对其微结构进行了分析。结合非晶碳氮薄膜的结构和发光机理,分析了它的发光性能。     

Double resonant Raman scattering in nanographite films

Experimental results are presented on Raman scattering in graphite films produced by DC plasmaenhanced chemical vapor deposition from a methane-hydrogen gas mixture. Scanning electron and probe microscopy data show that, depending on substrate material and deposition time, the deposited film is either a mesoporous material consisting of graphite nanocrystallites with basal planes oriented perpendicular to the substrate surface or an atomically flat, nanometer-thick stack of graphene layers parallel to the substrate. A comparative Raman spectroscopy analysis is performed for film samples deposited on nickel and silicon substrates for 5 and 60 min, as well as for highly ordered graphite samples. The Raman spectra of the examined samples correspond to the double resonant scattering mechanism. The behavior of Raman peak position and intensity as functions of excitation wavelength suggests a high degree of structural order in the graphite films deposited on nickel for 5 min. The results obtained are used to show that the thickness of these films is 1.5 ± 0.5 nm.     

Preparation of hydrogenated microcrystalline silicon films with hot-wire-assisted MWECR-CVD system

Intrinsic hydrogenated microcrystalline silicon (\muc-Si:H) films have been prepared by hot-wire-assisted microwave electron-cyclotron-resonance chemical vapour deposition (HW-MWECR-CVD) under different deposition conditions. Fourier-transform infrared spectra and Raman spectra were measured. Optical band gap was determined by Tauc plots, and experiments of photo-induced degradation were performed. It was observed that hydrogen dilution plays a more essential role than substrate temperature in microcrystalline transformation at low temperatures. Crystalline volume fraction and mean grain size in the films increase with the dilution ratio (R=H₂/(H₂+SiH₄)). With the rise of crystallinity in the films, the optical band gap tends to become narrower while the hydrogen content and photo-induced degradation decrease dramatically. The samples, were identified as \mu c-Si:H films, by calculating the optical band gap. It is considered that hydrogen dilution has an effect on reducing the crystallization activation energy of the material, which promotes the heterogeneous solid-state phase transition characterized by the Johnson--Mehl--Avrami (JMA) equation. The films with the needed structure can be prepared by balancing deposition and crystallization through controlling process parameters.     

Temperature‐dependent Raman study of PrFeO3thin film

Low‐temperature Raman study of (001)‐oriented PrFeO₃ thin film of around 200 nm thickness deposited on a LaAlO₃ (001) substrate by using the pulsed‐laser deposition technique is presented. X‐ray diffraction analysis of this film shows an orthorhombic structure with Pbnm space group. The observed substrate‐induced strain is found to be small. In the room temperature Raman spectra, different Raman modes were observed that were classified according to the orthorhombic structure. All the observed modes show a decrease in wavenumber with rise in temperature, except the B_1g mode (624 cm⁻¹) which shows some anomalous behavior. We tried to correlate the variations in linewidth and position with temperature for the observed modes with the octahedral disorder of FeO₆. Many possibilities are presented to explain the observed results. Copyright © 2010 John Wiley & Sons, Ltd.     

Study on structural properties of epitaxial silicon films on annealed double layer porous silicon

In this paper, epitaxial silicon films were grown on annealed double layer porous silicon by LPCVD. The evolvement of the double layer porous silicon before and after thermal annealing was investigated by scanning electron microscope. X-ray diffraction and Raman spectroscopy were used to investigate the structural properties of the epitaxial silicon thin films grown at different temperature and different pressure. The results show that the surface of the low-porosity layer becomes smooth and there are just few silicon-bridges connecting the porous layer and the substrate wafer. The qualities of the epitaxial silicon thin films become better along with increasing deposition temperature. All of the Raman peaks of silicon films with different deposition pressure are situated at 521 cm⁻¹ under the deposition temperature of 1100 °C, and the Raman intensity of the silicon film deposited at 100 Pa is much closer to that of the monocrystalline silicon wafer. The epitaxial silicon films are all (4 0 0)-oriented and (4 0 0) peak of silicon film deposited at 100 Pa is more symmetric.     

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利用微波电子回旋共振等离子体增强型化学气相沉积(ECR-PECVD)采用一步法直接在K9玻璃上低温沉积制备了多晶硅薄膜.研究了不同实验参数对薄膜沉积的影响,采用X射线衍射(XRD)、拉曼光谱、扫描电子显微镜(SEM)等实验分析方法对不同条件下制备的样品进行了晶体结构和表面形貌分析,并讨论了多晶硅薄膜沉积的最佳条件.实验结果表明,玻璃衬底上多晶硅薄膜呈柱状生长,并有一定厚度的非晶孵化层;较高氢气比例和衬底温度有利于结晶,薄膜的结晶率达到了62％;晶粒团簇的最大尺寸约为500nm.     

纳米晶硅薄膜中氢含量及键合模式的红外分析

采用传统射频等离子体化学气相沉积技术在100—350℃的衬底温度下高速沉积氢化硅薄膜. 傅里叶变换红外光谱和Raman谱的研究表明,纳米晶硅薄膜中的氢含量和硅氢键合模式与薄膜的晶化特性有密切关系,当薄膜从非晶相向晶相转变时,氢的含量减少了一半以上,硅氢键合模式以SiH₂为主. 随着衬底温度的升高和晶化率的增加,纳米晶硅薄膜中氢的含量以及其结构因子逐渐减少. 关键词： 氢化纳米晶硅薄膜 红外透射谱 氢含量 硅氢键合模式     

Effects of flow ratios on surface morphology and structure of hydrogenated amorphous carbon films prepared by microwave plasma chemical vapor deposition

A series of hydrogenated amorphous carbon (a-C:H) films were deposited on silicon substrates by microwave plasma chemical vapor deposition technique with a mixture of hydrogen and acetylene. The effects of flow ratio of hydrogen to acetylene on surface morphology and structure of a-C:H films were investigated using surface-enhanced Raman spectroscopy and scanning probe microscope (SPM) in the tapping AFM mode. Raman data imply a transition from graphite-like phase to diamond-like bonding configurations when the flow ratio increases. AFM measurements show that the increase in hydrogen content, to some extent, can smoothen the surface morphology and decrease the RMS roughness. Excessive hydrogen is found to cause the formation of polymeric hydrocarbon clusters in the films and reduce deposition rate.     

Photoluminescence of amorphous carbon films fabricated by layer—by—layer hydrogen plasma chemical annealing method

A method in which nanometre-thick film deposition was alternated with hydrogen plasma annealing (layer-by-layer method) was applied to fabricate hydrogenated amorphous carbon films in a conventional plasma-enhanced chemical vapour deposition system.It was found that the hydrogen plasma treatment could decrease the hydrogen concentration in the films and change the sp^2/sp^3 ratio to some extent by chemical etching.Blue photoluminescence was observed at room temperature,as a result of the reduction of sp^2 clusters in the films.     

沉积温度对含氢非晶碳膜电学性质的影响

用苯作为源气体,使用微波电子回旋共振(ECR)等离子体气相沉积法在不同温度下制备了含 氢非晶碳薄膜,研究了沉积温度对薄膜的直流电阻率、击穿场强的影响,发现它们与沉积速 率密切相关.测量了薄膜的含氢量与Raman谱,利用Angus等人提出的随机共价网络模型对结果 作了分析. 关键词： 非晶碳薄膜 ECR等离子体化学气相沉积 直流电阻     

沉积温度对钛硅共掺杂类金刚石薄膜生长、结构和力学性能的影响

采用中频磁控溅射Ti80Si20复合靶在单晶硅表面制备了共掺杂的类金刚石薄膜.研究了沉积温度对薄膜生长速率、化学成分、结构、表面性质和力学性能的影响.结果表明:随沉积温度升高,薄膜生长速率降低,薄膜Ti和Si原子浓度增加,C原子浓度降低;在高温下沉积的薄膜具有低sp3C含量、低表面接触角、低内应力和高的硬度与弹性模量.基于亚表层注入生长模型分析了沉积温度对薄膜生长和键合结构的影响,从薄膜生长机制和微观结构解释了表面性质和力学性能的变化.     

Optical and electrical properties of hydrogenated yttrium nanoparticles

We studied the effect of hydrogen in yttrium nanoparticles on a quartz substrate, using optical spectroscopy and electrical resistance measurements. Pulsed laser deposition is used to obtain the Y clusters in an UHV environment. We show, that these clusters are highly sensitive to monoatomic H₁ produced from ambient hydrogen gas pressures, ranging from 10^-5 to 50 mbar with our experimental arrangement. The changes of optical and electrical properties due to the chemical reaction within the particles are sufficient to consider this material as a possible sensor for low concentrations of hydrogen. Received 29 November 2000     

Control of wettability of hydrogenated amorphous carbon thin films by laser-assisted micro- and nanostructuring

A flexible and rapid surface functionalization of amorphous carbon films shows a great potential for various application fields such as biological surfaces and tribological systems. For this purpose, the combination of thin film deposition and subsequent laser material processing was investigated. Amorphous carbon layers doped with hydrogen were deposited on silicon wafers by reactive direct-current magnetron sputtering. Films with three different hydrogen contents were synthesized. Subsequent to the thin film deposition process, UV laser material processing at wavelengths of 193 nm or 248 nm was performed with respect to chemical surface modification and surface structuring on micro- and nanometer scale. Depending on structure size and laser-induced chemical surface modification the adjustment of the surface energy and wetting behaviour in a broad range from hydrophobic to hydrophilic was possible. The chemical modification and the ablation mechanisms near the ablation threshold were strongly influenced by the hydrogen content in amorphous carbon thin films.Structural and chemical information of the as-deposited and modified films was obtained by Raman spectroscopy, X-ray photoelectron spectroscopy and contact angle measurements.     

Near infrared to UV dielectric functions of Al doped ZnO films deposited on c-plane sapphire substrate using pulsed laser deposition

Transparent conducting polycrystalline Al-doped ZnO (AZO) films were deposited on sapphire substrates at substrate temperatures ranging from 200 to 300 °C by pulsed laser deposition (PLD). X-ray diffraction measurement shows that the crystalline quality of AZO films was improved with increased substrate temperature. The electrical and optical properties of the AZO films have been systematically studied via various experimental tools. The room-temperature micro-photoluminescence (µ-PL) spectra show a strong ultraviolet (UV) excitonic emission and weak deep-level emission, which indicate low structural defects in the films. A Raman shift of about 11 cm⁻¹ is observed for the first-order longitudinal-optical (LO) phonon peak for AZO films when compared to the LO phonon peak of bulk ZnO. The Raman spectra obtained with UV resonant excitation at room temperature show multi-phonon LO modes up to third order. Optical response due to free electrons of the AZO films was characterized in the photon energy range from 0.6 to 6.5 eV by spectroscopic ellipsometry (SE). The free electron response was expressed by a simple Drude model combined with the Cauchy model are reported.