Formation of nano-twinned 3C-SiC grains in Fe-implanted 6H-SiC after 1500-℃ annealing

A nano-twinned microstructure was found in amorphous SiC after high-temperature annealing. Grazing incidence x-ray diffraction, high-resolution transmission electron microscopy, and electron diffraction were performed to characterize the microstructure and phase transition in the recrystallization layer. After 1500 ℃ or 2-h annealing, 3C-SiC grains and numerous stacking faults on the {111} planes were visible. Some 3C-SiC grains have nano-twinned structure with {011} planes. Between the nano-twinned 3C-SiC grains, there is a stacking fault, indicating that the formation mechanisms of the nano-twinned structure are related to the disorder of Si atoms. The increase in the twin thickness with increasing annealing temperature demonstrates that the nano-twinned structure can sink for lattice defects, in order to improve the radiation tolerance of SiC.     

Al-N共掺杂3C-SiC介电性质的第一性原理计算

采用基于密度泛函理论的第一性原理平面波超软赝势法,建立了未掺杂,Al,N单掺杂和Al-N共掺杂3C-SiC的4种超晶胞模型,并分别对模型进行了几何结构优化,对比研究了其能带结构,态密度分布和介电常数.计算结果表明:Al掺杂会增大SiC的晶格常数,而N对SiC的晶格影响很小.Al掺杂会导致费米能级进入价带,使3C-SiC成为p型半导体,且带隙宽度略为加宽.N掺杂后的SiC其导带和价带均向低能端发生移动,带隙稍有减小.本征3C-SiC几乎不具备微波介电损耗性能.但是可以通过进行Al掺杂或N掺杂加以改善,Al掺杂后的效果尤为突出.计算发现Al-N共掺杂后的3C-SiC材料在8.2—12.4 GHz范围内其微波介电损耗性能急剧下降,与实验结果相符合,并对这一结果进行了讨论分析.     

Crystalline quality of 3C-SiC formed by high-fluence C-implanted Si

Carbon ions at 40 keV were implanted into (1 0 0) high-purity p-type silicon wafers at 400 °C to a fluence of 6.5 × 10¹⁷ ions/cm². Subsequent thermal annealing of the implanted samples was performed in a diffusion furnace at atmospheric pressure with inert nitrogen ambient at 1100 °C. Time-of-flight energy elastic recoil detection analysis (ToF-E ERDA) was used to investigate depth distributions of the implanted ions. Infrared transmittance (IR) and Raman scattering measurements were used to characterize the formation of SiC in the implanted Si substrate. X-ray diffraction analysis (XRD) was used to characterize the crystalline quality in the surface layer of the sample. The formation of 3C-SiC and its crystalline structure obtained from the above mentioned techniques was finally confirmed by transmission electron microscopy (TEM). The results show that 3C-SiC is directly formed during implantation, and that the subsequent high-temperature annealing enhances the quality of the poly-crystalline SiC.     

Spatially resolved Raman spectroscopy evaluation of residual stresses in 3C-SiC layer deposited on Si substrates with different crystallographic orientations

Raman scattering studies were performed on hot-wall chemical vapor deposited (heteroepitaxial) silicon carbide (SiC) films grown on Si substrates with orientations of (1 0 0), (1 1 1), (1 1 0) and (2 1 1), respectively. Raman spectra suggested that good quality cubic SiC single crystals could be obtained on the Si substrate, independent of its crystallographic orientation. Average residual stresses in the epitaxially grown 3C-SiC films were measured with the laser waist focused on the epilayer surface. Tensile and compressive residual stresses were found to be stored within the SiC film and in the Si substrate, respectively. The residual stress exhibited a marked dependence on the orientation of the substrate. The measured stresses were comparable to the thermal stress deduced from elastic deformation theory, which demonstrates that the large lattice mismatch between cubic SiC and Si is effectively relieved by initial carbonization. The confocal configuration of the optical probe enabled a stress evaluation along the cross-section of the sample, which showed maximum tensile stress magnitude at the SiC/Si interface from the SiC side, decreasing away from the interface in varied rate for different crystallographic orientations. Defocusing experiments were used to precisely characterize the geometry of the laser probe in 3C-SiC single crystal. Based on this knowledge, a theoretical convolution of the in-depth stress distribution could be obtained, which showed a satisfactory agreement with stress values obtained by experiments performed on the 3C-SiC surface.     

Experimental evidence for the quantum confinement effect in 3C-SiC nanocrystallites

Using electrochemical etching of a polycrystalline 3C-SiC target and subsequent ultrasonic treatment in water solution, we have fabricated suspensions of 3C-SiC nanocrystallites that luminesce. Transmission electron microscope observations show that the 3C-SiC nanocrystallites, which uniformly disperse in water, have sizes in the range of 1-6 nm. Photoluminescence and photoluminescence excitation spectral examinations show clear evidence for the quantum confinement of 3C-SiC nanocrystallites with the emission band maximum ranging from 440 to 560 nm. Tunable, composite polystyrene/SiC film can be made by adding polystyrene to a toluene suspension of the 3C-SiC nanocrystallites and then coating the resulting solution onto a Si wafer.     

Electron beam-physical vapor deposition of SiC/SiO2 high emissivity thin film

When heated by high-energy electron beam (EB), SiC can decompose into C and Si vapor. Subsequently, Si vapor reacts with metal oxide thin film on substrate surface and formats dense SiO₂ thin film at high substrate temperature. By means of the two reactions, SiC/SiO₂ composite thin film was prepared on the pre-oxidized 316 stainless steel (SS) substrate by electron beam-physical vapor deposition (EB-PVD) only using β-SiC target at 1000 °C. The thin film was examined by energy dispersive spectroscopy (EDS), grazing incidence X-ray asymmetry diffraction (GIAXD), scanning electron microscopy (SEM), atomic force microscopy (AFM), backscattered electron image (BSE), electron probe microanalysis (EPMA), X-ray photoelectron spectroscopy (XPS) and Fourier transformed infra-red (FT-IR) spectroscopy. The analysis results show that the thin film is mainly composed of imperfect nano-crystalline phases of 3C-SiC and SiO₂, especially, SiO₂ phase is nearly amorphous. Moreover, the smooth and dense thin film surface consists of nano-sized particles, and the interface between SiC/SiO₂ composite thin film and SS substrate is perfect. At last, the emissivity of SS substrate is improved by the SiC/SiO₂ composite thin film.     

Uniformity study of wafer-scale InP-to-silicon hybrid integration

β-SiC nanowires were synthesized by a simple carbothermal reduction of carbonaceous silica xerogel. The morphology and structure of the nanowires were investigated by X-ray diffraction, scanning electron microscope and transmission electron microscopy. The results showed that the nanowires were hexagonal prism-shaped hierarchical nanostructures. The typical stacking faults and twin defects of SiC nanowires were also observed. Band-gap characterization and photoluminescence properties of SiC nanowires were investigated by UV-vis absorption spectroscopy and fluorescence photometry, respectively. The results showed the SiC nanowire was an indirect transition semiconductor and the band gap energy for the SiC nanowires was 2.85 eV. The photoluminescence peak value at 470 nm (2.64 eV) originating from the SiC nanowires was a little higher than the value of band-gap energy.     

Electronic structure and the local electroneutrality level of SiC polytypes from quasiparticle calculations within the GW approximation

The most important interband transitions and the local charge neutrality level (CNL) in silicon carbide polytypes 3C-SiC and nH-SiC (n = 2?C8) are calculated using the GW approximation for the self energy of quasiparticles. The calculated values of band gap E _g for various polytypes fall in the range 2.38 eV (3C-SiC)-3.33 eV (2H-SiC) and are very close to the experimental data (2.42?C3.33 eV). The quasiparticle corrections to E _g determined by DFT-LDA calculations (about 1.1 eV) are almost independent of the crystal structure of a polytype. The positions of CNL in various polytypes are found to be almost the same, and the change in CNL correlates weakly with the change in E _g, which increases with the hexagonality of SiC. The calculated value of CNL varies from 1.74 eV in polytype 3C-SiC to 1.81 eV in 4H-SiC.     

Interpretation of initial stage of 3C-SiC growth on Si(1 0 0) using dimethylsilane

The initial stage of cubic silicon carbide (3C-SiC) growth on a Si(0 0 1) surface using dimethylsilane (DMS) as a source gas was observed using scanning tunneling microscopy (STM) and reflection high-energy electron diffraction (RHEED). It was found that the dimer vacancies initially existing on the Si(0 0 1)-(2 × 1) surface were repaired by the Si atoms in DMS molecules, during the formation of the c(4 × 4) surface. From the STM measurement, nucleation of SiC was found to start when the Si surface was covered with the c(4 × 4) structure but before the appearance of SiC spots in the RHEED pattern. The growth mechanism of SiC islands was also discussed based on the results of RHEED, STM and temperature-programmed desorption (TPD).     

Formation of epitaxial SiC nanocrystals

Epitaxial 3C-SiC grains are formed at 1190 °C in the top region of silicon, when Si wafers coated by SiO₂ are annealed in CO atmosphere. The formed SiC grains are 40-50 nm high and 100 nm wide in cross-section and contain only few defects. Main advantage of the method is that the final structure is free of voids.The above method is further developed for the generation of SiC nanocrystals, embedded in SiO₂ on Si, and aligned parallel with the interface. The nanometer-sized SiC grains were grown into SiO₂ close to the Si/SiO₂ interface by a two-step annealing of oxide covered Si: first in a CO, than in a pure O₂ atmosphere. The first (carbonization) step created epitaxial SiC crystallites grown into the Si surface, while the second (oxidation) step moved the interface beyond them. Conventional and high resolution cross-sectional electron microscopy showed pyramidal Si protrusions at the Si/SiO₂ interface under the grains. The size of the grains, as well as their distance from the Si/SiO₂ interface (peak of pyramids) can be controlled by the annealing process parameters. The process can be repeated and SiC nanocrystals (oriented in the same way) can be produced in a multilevel structure.     

Driving force of stacking-fault formation in SiC p-i-n diodes

The driving force of stacking-fault expansion in SiC p-i-n diodes was investigated using optical emission microscopy and transmission electron microscopy. The stacking-fault expansion and properties of the partial dislocations were inconsistent with any stress as the driving force. A thermodynamic free energy difference between the perfect and a faulted structure is suggested as a plausible driving force in the tested diodes, indicating that hexagonal polytypes of silicon carbide are metastable at room temperature.     

Low-temperature epitaxial growth of the quaternary wide band gap semiconductor SiCAlN

Two compounds SiC and AlN, normally insoluble in each other below approximately 2000 degrees C, are synthesized as a single-phase solid-solution thin film by molecular beam epitaxy at 750 degrees C. The growth of epitaxial SiCAlN films with hexagonal structure takes place on 6H-SiC(0001) substrates. Two structural models for the hexagonal SiCAlN films are constructed based on first-principles total-energy density functional theory calculations, each showing agreement with the experimental microstructures observed in cross-sectional transmission electron microscopy images. The predicted fundamental band gap is 3.2 eV for the stoichiometric SiCAlN film.     

Synthesis of the vertically aligned carbon hexagonal nanoprism arrays and their application for field emission

A simple approach is demonstrated for effectively growing large-area vertically aligned carbon hexagonal nanoprism arrays on molybdenum substrates by the catalyst-assisted pulsed laser deposition techniques. The carbon hexagonal nanoprisms have uniform shape and length, almost aligned vertically on the substrate, and the average diameters are about 30 nm. The internal angles of the nanoprisms present 60°. The vertically aligned nanorods have also been obtained for a comparison in the presence of catalyst Fe. The sample with vertically aligned carbon hexagonal nanoprism arrays exhibits better field emission behaviors than that with aligned carbon nanorod arrays.     

Effects of carbonization and substrate temperature on the growth of 3C-SiC on Si(1 1 1) by SSMBE

The growth of 3C-SiC on Si(1 1 1) substrate was performed at different carbonization temperatures and substrate temperatures by solid-source molecular beam epitaxy (SSMBE). The properties of SiC film were analyzed with in situ reflection high energy electron diffraction (RHEED), X-ray diffraction (XRD), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The best carbonization temperature of 810 °C was found to be optimal for the surface carbonization. The quality of SiC film grown on Si at substrate temperature of 1000 °C is best. The worse crystalline quality for the sample grown at higher temperature was attributed to the large mismatch of thermal expansion coefficient between SiC and Si which caused more dislocation when sample was cooled down to room temperature from higher substrate temperature. Furthermore, the larger size of single pit and the total area of the pits make the quality of SiC films grown at higher temperature worse. More Si atoms for the sample grown at lower temperature were responsible for the degradation of crystalline quality for the sample grown at lower temperature.     

Atomically resolved images of I(h) ice single crystals in the solid phase

The morphology and crystal structure of nanoparticles of ice were examined by high-resolution transmission electron microscopy. Two different crystal structures were found and unambiguously assigned to hexagonal (I(h)) and cubic (I(c)) ice crystals. Direct observation of oxygen columns clearly revealed the hexagonal packing of water molecules. Electron energy-loss spectroscopy was used to monitor the electronic excitation in ice, suggesting possible dissociation of water molecules. Dynamic process of phase transition between I(h) and I(c) phases of individual ice nanoparticles under electron beam irradiation was also monitored by in situ transmission electron diffractometry.     

Si(100)衬底上n-3C-SiC/p-Si异质结构研究

利用LPCVD方法在Si(100)衬底上获得了3C-SiC外延膜,扫描电子显微镜(SEM)研究表明3C-SiC/p-Si界面平整、光滑,无明显的坑洞形成。研究了以In和Al为接触电极的3C-SiC/p-Si异质结的I-V,C-V特性及I-V特性的温度依赖关系,比较了In电极的3C-SiC/p-Si异质结构和以SiGe作为缓冲层的3C-SiC/SiGe/p-Si异质结构的I-V特性,实验发现引入SiGe缓冲层后,器件的反向击穿电压由40V提高到70V以上。室温下Al电极3C-SiC/p-Si二极管的最大反向击穿电压接近100V,品质因子为1.95。     

Preparation and characterization of single-phase SiC nanotubes and C-SiC coaxial nanotubes

Preparation conditions of single-phase SiC nanotubes and C-SiC coaxial nanotubes were investigated. The characterization of single-phase SiC nanotubes and C-SiC coaxial nanotubes were carried out. The SiC nanowires, which were made of the catenated SiC grains of 50–200 nm in diameter, were obtained in carbon nanotubes reacted at 1450 °C. The only C-SiC coaxial nanotubes were formed at 1300 °C. A few single-phase SiC nantoubes were synthesized at 1200 °C for 100 h. More than half number of nanotubes reacted at 1200 °C for 100 h were altered to single-phase SiC nantoubes by heat treatment of 600 °C for 1 h in air since the remained carbon was removed. The energy dispersive X-ray spectroscopy analysis revealed that the atomic ratio of Si to C in single-phase SiC nanotubes was almost 1; these single-phase SiC nanotubes consisted of near-stoichiometric SiC grains.     

High-dose carbon implantations into silicon: fundamental studies for new technological tricks

Depending on the implantation temperature, the implantation of carbon ions into silicon at high doses results in the formation of either amorphous SiC_x or crystalline 3C-SiC precipitates. Various aspects of the precipitation behaviour observed, such as the impeded nucleation, the limited growth and the resulting sensitivity to ballistic destruction are attributed to the large interfacial energy between crystalline silicon and 3C-SiC. Periodically arranged amorphous SiC_x nanoclusters, which are formed at lower temperatures, are shown to promote amorphisation by their surrounding stress field and to represent sinks for silicon self-interstitials, which can be activated by annealing at 900 °C. By control of the depth distribution of equally sized, oriented 3C-SiC precipitates formed at higher implantation temperatures, it is possible to establish suitable starting conditions for the formation of buried homogeneous, single-crystalline 3C-SiC layers during a post-implantation anneal. The properties of these ion-beam-synthesised SiC layers are described and attempts to combine them with insulating and metallic layers are reviewed. A survey is given of the emerging applications of ion-beam-synthesised buried SiC layers and microstructures in electronic, optical and micromechanical devices and as large-area SiC pseudosubstrates. Received: 11 November 2002 / Accepted: 12 November 2002 / Published online: 4 April 2003 RID="*" ID="*"Corresponding author. Fax: +49-821/598-3425, E-mail: lindner@physik.uni-augsburg.de     

在双热舟化学气相沉积系统中通过掺In技术生长GaN纳米线和纳米锥

在现有的一台蒸发镀膜机基础上，设计加工了一个双热舟化学气相沉积系统.该系统具有真空度高、升温速度快、源和衬底温度可分别控制等优点，有利于化合物半导体纳米材料的生长.利用该生长系统，通过在生长过程中掺入等电子杂质In作为表面活性剂，分别在Si衬底和3C-SiC/Si衬底上生长出高质量的具有纤锌矿结构的单晶GaN纳米线和纳米尖三棱锥.所得产物通过场发射扫描电子显微镜、高分辨透射电子显微镜、能量色散x射线谱仪、x射线衍射仪，和荧光谱仪进行表征.这里所用的生长方法新颖，生长出的GaN纳米尖三棱锥在场发射和激光方面有潜在的应用价值. 关键词： GaN 纳米结构 透射电子显微镜 光致荧光谱     

3C-SiC薄膜小角晶界附近位错核心的原子组态研究

用LaB₆灯丝200 kV高分辨透射电镜拍摄了有小角晶界的3C-SiC/(001)Si 薄膜的[110]高分辨电子显微像. 用像解卷技术把本不直接反映晶体结构的实验像转化为结构像. 首先, 从完整区的结构像中分辨开间距仅为0.109 nm的Si和C原子柱; 随后按赝弱相位物体近似像衬理论, 分析像衬随晶体厚度的变化规律, 辨认出Si和C原子; 进而在原子水平上得出小角晶界附近两个复合位错的核心结构, 构建了结构模型并计算了模拟像. 实验像与模拟像的一致程度验证了结构模型的正确性. 于是, 在已知完整晶体结构的前提下, 仅从一帧实验高分辨像出发, 推演出原子的种类和位错核心的原子组态. 还讨论了3C-SiC 小角晶界的形成与晶界附近出现复合位错的关系.