Interpretation of Auger depth profiles of thin SiC layers on Si

Silicon carbide thin films, prepared by carbonization of Si-wafers are analysed by Auger depth profiling. The influence of atomic mixing is simulated with a Monte Carlo model. By using mixing simulations the dependence of the two mixing parameters (width of the mixing zone and recoil depth) on ion beam energy, incidence angle and ion mass can be calculated. For comparison of the simulated data with Auger measurements an Auger electron escape depth correction is necessary. The simulated and -corrected data of several layer structures show good qualitative agreement with Auger depth profiles of thin carbonized SiC-layers.Dedicated to Professor Dr. rer. nat. Dr. h.c. Hubertus Nickel on the occasion of his 65th birthday     

Initial formation of contact layers on Ni/SiC samples studied by XPS

This study deals with the quantitative assessment of the coverage and thickness of Ni silicide films formed during annealing of SiC substrates with sputtered thin films of Ni. The analytical approach involves the use of XPS and depth profiling by means of successive ion etchings and XPS analyses. For either 3 or 6 nm initial Ni film thickness, a 10 nm Ni₂Si product is formed. On top of this product, the C released is accumulated in a very thin (1–2 nm) film. In neither case, the Ni₂Si covers the whole surface, although the coverage is almost complete (～90%) in the latter case. For the greater initial Ni‐film thickness of 17 nm, the thickness of the Ni₂Si product corresponds well to the value of 25 nm expected from the Ni/Ni₂Si stoichiometric relationship. This thickness is significantly greater than a critical level and the film covers the whole surface. Carbon is similarly accumulated in a very thin layer on the top surface, although the major part of C (～70%) is found inside the main reaction product layer. Copyright © 2008 John Wiley & Sons, Ltd.     

Ion‐beam synthesis of 3C‐SiC surface layers on silicon

The attempt to grow 3C‐SiC thin films on silicon substrates has become an area of significant scientific interest, largely as a consequence of the impressive electrical properties that this polytype displays. In this paper, we have utilized low‐energy (20 keV) high‐fluence carbon implantation and a subsequent annealing step to form layers of 3C‐SiC directly on a silicon surface, and have investigated the effect of implantation fluence on the resultant materials properties. The quality of the Si/SiC interface is shown to be highly fluence‐dependent, with the formation of voids decreasing significantly with increased fluence. The conversion of carbon into 3C‐SiC is found to be most efficient at near‐stoichiometric concentrations, while at higher implantation fluences clusters of excess carbon are discovered to form within the silicon and to diffuse to the surface of the grown 3C‐SiC layer upon annealing. Copyright © 2011 John Wiley & Sons, Ltd.     

用透射电子显微技术研究Si3N4/纳米SiC复相陶瓷的微观结构与力学性能

利用透射电子显微镜,观察了Si3N4/纳米SiC复相陶瓷材料的显微结构特点、分析比较了纳米复相陶瓷与单相Si3N4陶瓷的显微结构差异、讨论了复相陶瓷材料的力学性能与其微观结构的关系,并提出在材料中引入纳米SiC粒子后,可以起到抑制Si3N4晶体长大,使材料的力学性能得到显著提高.     

SiC表面Ni沉积超疏水膜层的形成机理

前期采用环境友好方法制备的改性碳化硅颗粒,经较长时间放置,发现其由亲水性转变为超疏水性,接触角为156°。为解释这一新的现象,采用扫描电子显微镜、能谱、(高分辨)透射电子显微镜、X射线光电子能谱(XPS)对原粉碳化硅、改性后碳化硅及久置碳化硅进行了测试与分析。结果显示：改性后碳化硅经较长时间放置,表面胞状颗粒增大并出现凸起物,粗糙度增加,存在类似于荷叶的微纳米结构。改性后颗粒的主要成分为Ni、Si、O,其中凸起处Ni、O元素的含量明显高于凹陷处。Ni颗粒表面出现清晰的膜层,膜层厚度为2～3 nm,但结晶度偏低。XPS测试结果显示金属镍的特征峰正向移动近4 eV,与镍的氧化态特征峰相一致,从而解释了颗粒表面形态发生细小改变,自发形成超疏水膜层的机理。     

SiC表面Ni沉积超疏水膜层的形成机理

前期采用环境友好方法制备的改性碳化硅颗粒,经较长时间放置,发现其由亲水性转变为超疏水性,接触角为156°。为解释这一新的现象,采用扫描电子显微镜、能谱、(高分辨)透射电子显微镜、X射线光电子能谱(XPS)对原粉碳化硅、改性后碳化硅及久置碳化硅进行了测试与分析。结果显示：改性后碳化硅经较长时间放置,表面胞状颗粒增大并出现凸起物,粗糙度增加,存在类似于荷叶的微纳米结构。改性后颗粒的主要成分为Ni、Si、O,其中凸起处Ni、O元素的含量明显高于凹陷处。Ni颗粒表面出现清晰的膜层,膜层厚度为2~3 nm,但结晶度偏低。XPS测试结果显示金属镍的特征峰正向移动近4eV,与镍的氧化态特征峰相一致,从而解释了颗粒表面形态发生细小改变,自发形成超疏水膜层的机理。     

碳源对MoO_3/Al_2O_3碳化过程的影响

利用几种常见的液态烃作为碳源对MoO3/Al2O3进行了程序升温碳化(TPC),通过在线质谱(MS)的跟踪分析以及对所得催化剂的XRD表征,研究了这些烃在TPC过程中对MoO3/Al2O3物相转变的影响以及这些烃在不断转化催化剂表面的化学行为.结果显示在不同温度范围内这些烃具有不同的碳化活性,对MoO3/Al2O3的完全碳化来说,正己烷表现出了最好的活性.TPC-MS的分析结果也见证了MoO3/Al2O3碳化时的中间物相及其对链烃的脱氢芳构化作用,这对于不同用途的钼基碳化物催化剂制备时合适碳源的选择极具参考意义.     

熔盐电解SiO2/C直接制备SiC纳米线

采用纳米SiO₂和酚醛树脂为原料制备酚醛树脂裂解碳纳米SiO₂复合阴极(硅碳物质的量的比为1:1),直接电解PFC/SiO₂复合阴极,在900℃熔融盐CaCl₂中,恒槽压2.0V下电解,制备出碳化硅纳米线。采用场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)及其附带的能谱仪、X射线分析衍射仪(XRD)和拉曼光谱(Raman)对产物的组成、形貌、微观结构等进行了表征。结果表明:碳化硅纳米线呈立方晶体结构,其直径为4~13nm,长可达数微米;室温下该纳米线在415nm和534nm附近有宽的发光峰。最后,讨论了碳化硅纳米线的生成机制。     

熔盐电解SiO2/C直接制备SiC纳米线

采用纳米SiO₂和酚醛树脂为原料制备酚醛树脂裂解碳纳米SiO₂复合阴极(硅碳物质的量的比为1∶1),直接电解PFC/SiO₂复合阴极,在900 ℃熔融盐CaCl₂中,恒槽压2.0 V下电解,制备出碳化硅纳米线。采用场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)及其附带的能谱仪、X射线分析衍射仪(XRD)和拉曼光谱(Raman)对产物的组成、形貌、微观结构等进行了表征。结果表明：碳化硅纳米线呈立方晶体结构,其直径为4~13 nm,长可达数微米;室温下该纳米线在415 nm和534 nm附近有宽的发光峰。最后,讨论了碳化硅纳米线的生成机制。     

Chemical surface passivation of 3C‐SiC nanocrystals: A first‐principle study

The effect of the chemical surface passivation, with hydrogen atoms, on the energy band gap of porous cubic silicon carbide (PSiC) was investigated. The pores are modeled by means of the supercell technique, in which columns of Si and/or C atoms are removed along the [001] direction. Within this supercell model, morphology effects can be analyzed in detail. The electronic band structure is performed using the density functional theory based on the generalized gradient approximation. Two types of pores are studied: C‐rich and Si‐rich pores surface. The enlargement of energy band gap is greater in the C‐rich than Si‐rich pores surface. This supercell model emphasizes the interconnection between 3C‐SiC nanocrystals, delocalizing the electronic states. However, the results show a clear quantum confinement signature, which is contrasted with that of nanowire systems. The calculation shows a significant response to changes in surface passivation with hydrogen. The chemical tuning of the band gap opens the possibility plenty applications in nanotechnology. © 2010 Wiley Periodicals, Inc. Int J Quantum Chem 110:2455–2461, 2010     

近化学计量比碳化硅的制备及其结构表征

近化学计量比碳化硅的制备及其结构表征;聚碳硅烷;聚甲基硅烷;聚环硼氮烷     

Investigation of various SiC materials by means of EPMA/WDS techniques

The microstructure and compositions of SiC materials from different sources and processing routes were investigated by means of EPMA/WDS and image analysis techniques. The influence of various sources of errors like carbon contamination and spectrometers defocusing on the analysis has been assessed.The presence of dissolved sintering aids, or impurities, and their distributions were investigated by EPMA/WDS. In addition, inhomogeneities, porosity agglomerations and heterogeneous inclusions were found in almost all the SiC materials, which are known to influence the corrosion and mechanical behavior of the material.Quantification of secondary phase contents was performed by means of image analysis, EPMA and, when possible, by density measurement. All methods are affected by errors of difficult assessment. In particular, the EPMA/WDS technique has to handle the problem of non homogeneous volumes of analysis. Two quantitative approaches were attempted, both based on the averaging of many points. In the first, the beam was highly focused. In the second approach, large areas (from 10 to 50 m in diameter) were illuminated. The errors and limits of these methods are discussed and the results compared.     

硅钼蓝光度法测定碳化硅中二氧化硅的含量

采用氯化钠-盐酸-氢氟酸溶解碳化硅样品,加钼酸铵使硅酸离子形成硅钼杂多酸,然后用1-氨基-2-萘酚-4-磺酸还原剂将其还原成硅钼蓝,在700nm波长处测定其吸光度,从而测得碳化硅中的二氧化硅含量。考察了称样量、水浴温度、水浴加热时间、样品储存容器、显色反应时间等因素对测定结果的影响,优化了测试条件。二氧化硅的质量浓度在0．25-12．5mg／（100mL）的范围内与吸光度呈良好的线性关系,线性相关系数r=0．99986。加标回收率为99．2％～100．9％,测定结果的相对标准偏差为0．76％（n=6）。     

Ti-Si-N films prepared by plasma-enhanced chemical vapor deposition

Ti-Si-N thin films were deposited on HSS substrates at 560°C using plasmaenhanced chemical vapor deposition. Feed gases used were TiCl₄, SiCl₄, N₂, and H₂. The composition of the films could be controlled well through adjustment of the mixing ratio of the chlorides in the feed gases. The Si content in the film varied in the range of O to 40 at. %. It was jbund that a small addition of Si to a TiN film improved the morphology significantlv, showing dense and glasslike structure. Also a much smootherand more homogeneous interface between thefilm and the substrate was obtained. The Ti-Si- N films containing 10–15 at. % Si showed the maximal microhardness value of about 6350 kgf/mm², much higher than that of TiN films.     

Infrared reflection studies of ceramics: characterization of SiC layers on graphite substrates

Summary Technical CVD-grown silicon carbide (-SiC) layers on graphite substrates have been studied by infrared spectroscopy. Specular reflectance spectra were measured at oblique incidence, and for the same experimental conditions such spectra were simulated starting from oscillator parameters which basically determine the optical behaviour of the material. Both the roughness of the surface and the roughness of the interface within the coated material, have considerable influence on the spectra. Modelling these zones as gradient layers on the basis of effective-medium approximations, convincing agreement between experiment and simulation can be obtained. In this way the effective dielectric function of the layer, as well as its thickness, are derived. Certain features within the reststrahlen band can be assigned to the excitation of surface phonons which strongly depend on the morphology of the layer.     

高频红外碳硫分析仪测定含碳化硅耐火材料中碳化硅含量

采用对试样进行灼烧预处理的方法,除去游离碳,用锡粒、纯铁、钨粒作为助熔剂,并以钢铁标准样品校正仪器,高频燃烧红外吸收法测定含碳化硅耐火材料中的碳化硅含量,测定结果的相对标准偏差为1.07%(n=6),该法与化学法的测定结果较接近,精密度和准确度均满足化学分析的要求。     

铝含量对含铝碳化硅陶瓷先驱体结构和性能的影响

采用不同比例的乙酰丙酮铝[Al(AcAc)3]与聚硅碳硅烷(PSCS)反应制备含铝碳化硅陶瓷的先驱体聚铝碳硅烷(PACS). 采用气相凝胶色谱(GPC)、化学分析和红外等手段对不同铝含量的PACS组成和结构进行了表征, 研究了铝含量对PACS结构和性能的影响. 结果表明, 随着铝含量的增加, PACS的氧含量增加, 分子量分布变宽, 主要活性基团Si—H键的含量降低, PACS的可纺性降低. 当Al(AcAc)3/PSCS(质量比)大于20%以后, PACS不可纺. 热重-差热分析(TG-DTA)的研究表明: 当制备PACS的Al(AcAc)3/PSCS(质量比)大于4%, PACS在N2中400～560 ℃之间的失重明显降低. 铝含量在0.4～0.7 wt%的PACS, 制备的Si-Al-C-O纤维抗张强度最高. Al(AcAc)3/PSCS＝6 wt%时制备的PACS, 烧结的SiC(Al)纤维最致密.     

Growth and Chemical Thermodynamics Analysis of SiC Film on Si Substrate by Heating Polystyrene/Silica Bilayer Method

SiC films were prepared by modified heating polystyrene/silica bilayer method on Si (111) substrate in normal pressure flowing Ar ambient at 1300 o C. The films were investigated by Fourier transform infrared absorption, X-ray diffraction, and scanning electron microscopy measurements. The chemical thermodynamics process is discussed. The whole reaction can be separated into four steps. The carburizing of SiO is the key step of whole reaction. The main reaction-sequence is figured out based on Gibbs free energy and equilibrium constant. Flowing Ar is necessary to continue the progress of whole reaction by means of carrying out accumulating gaseous resultants. The film is very useful for application in a variety of MOS-based devices for its silica/SiC/Si(111) structure, in which the silica layer can be removed thoroughly by the standard RCA cleaning process.     

Investigations on Chemical Vapour Transport of Intermetallic Phases in the System Co/Fe/Si

The ternary phases existing on the quasi binary section CoSi/FeSi and CoSi₂/β‐FeSi₂ have been investigated by solid state reactions and chemical transport. The solid solution serie Co_xFe_1‐xSi can be described as a regular solution. The transport behaviour calculated is in good agreement with the experiments. The phases have been characterized by X‐ray powder diffraction, EDX and ICP‐OES. The temperature dependence of the resistivity has been measured from 20 K up to room temperature on single crystals.     

多孔SiC纳米片的原位合成及光催化性能

以可膨胀石墨作为原材料,通过高温膨化和机械砂磨得到石墨薄片,再以石墨薄片作为模板合成了不同比表面积的碳化硅纳米片(SiCNSs)。探究了比表面积对SiCNSs光催化制氢性能的影响。结果表明,SiCNSs的比表面积对其产氢性能影响显著,提高光催化剂的比表面积有利于增强其产氢活性。SiCNSs的最大比表面积可达149 m²·g^-1,其光解水产氢速率为51.0μL·g^-1·h^-1。在对石墨薄片和SiCNSs结构、形貌分析的基础上,提出了以石墨薄片为模板原位生成SiCNSs的形成机理,该过程主要遵循气固反应机制。高温下,气态的SiO和Si与石墨薄片反应生成SiCNSs,产物较好地继承了石墨薄片的片状结构。大尺寸石墨片上未反应部分除碳之后留下了大量纳米尺寸穿孔,使得所生成SiC的比表面积反而比小尺寸石墨片产物的高。