Imaging Si nanoparticles embedded in SiO(2) layers by (S)TEM-EELS

Fabrication of systems in which Si nanoparticles are embedded in a thin silica layer is today mature for non-volatile memory and opto-electronics applications. The control of the different parameters (position, size and density) of the nanoparticles population is a key point to optimize the properties of such systems. A review of dedicated transmission electron microscopy (TEM) methods, which can be used to measure these parameters, is presented with an emphasis on those relying on electron energy-loss spectroscopy (EELS). Defocused bright-field imaging can be used in order to determine topographic information of a whole assembly of nanoparticles, but it is not efficient for looking at individual nanoparticles. High-resolution electron imaging or dark-field imaging can be of help in the case of crystalline particles but they always provide underestimated values of the nanocrystals population. EELS imaging in the low-energy-loss domain around the Si plasmon peak, which gives rise to strong signals, is the only way to visualize all Si nanoparticles within a silica film and to perform reliable size and density measurements. Two complementary types of experiments are investigated and discussed more extensively: direct imaging with a transmission electron microscope equipped with an imaging filter (EFTEM) and indirect imaging from spectrum-imaging data acquired with a scanning transmission electron microscope equipped with a spectrometer (STEM-PEELS). The direct image (EFTEM) and indirect set of spectra (STEM-PEELS) are processed in order to deliver images where the contribution of the silica matrix is minimized. The contrast of the resulting images can be enhanced with adapted numerical filters for further morphometric analysis. The two methods give equivalent results, with an easier access for EFTEM and the possibility of a more detailed study of the EELS signatures in the case of STEM-PEELS. Irradiation damage in such systems is also discussed.     

The wear rate of n-type Si(100)

Single-crystal Si(100) (n type) was scratched at room temperature by a single-point 90° pyramidal diamond in each of the following fluids: reagent-grade absolute ethanol, methanol, acetone and deionized water. The wear rate in each case was determined from a measurement of the cross-sectional areas of circular multiscratch grooves and the increase in this area with scratching time. These areas vary as the contact force on the diamond and the fluid covering the silicon surface during the scratching test vary. As expected, the wear rate depended on the force (dead-weight load) on the diamond (the wear rate increased as the force was increased) but fluids also had a significant effect on the wear. The wear rate of silicon scratched in ethanol is twice that in deionized water when the dead-weight load on the diamond is 0.49 N and all other experimental variables are held constant. These results were compared with two models of abrasive wear of ceramic materials.     

一种测量Si/SiO2界面残余应力的微结构应变计

借鉴工程力学中测量残余应力的盲孔法,给出了一种测量半导体氧化工艺中形成的硅-二氧化硅界面残余应力的微结构应变计,并对其测量结果作了讨论.     

基于薄膜退火的MoS_2/SiO_2/Si异质结太阳能电池光伏性能提高

为了制备高效的MoSi/SiO_2/Si异质结太阳能电池,利用磁控溅射技术制备MoS_2薄膜,并在硫气氛下对MoS_2薄膜进行退火处理。分别用退火和未退火的MoS_2薄膜制备MoS_2/SiO_2/Si异质结太阳能电池,研究了退火对MoS_2薄膜的微观结构和MoS_2/SiO_2/Si异质结太阳能电池光电性能的影响。实验结果显示,相比于未退火的,经过退火处理的MoS_2薄膜的拉曼峰半高宽(FWHM)变窄,峰强增强,显微荧光光谱中也出现明显的激子发光峰。由此表明,退火处理使MoS_2薄膜由非晶向晶态转变,薄膜的体缺陷减少,异质结太阳能电池的开路电压和填充因子得到提升,器件转换效率从0.94%提高到1.66%。不同光照强度下的J-V测量和暗态的J-V测量结果表明,经退火处理的MoS_2薄膜的异质结太阳能电池具有较高的收集电压和更接近于1的理想因子,这归因于退火导致MoS_2薄膜的体缺陷的减少,近而降低了MoS_2/SiO_2/Si异质结太阳能电池器件的体缺陷复合。     

Characteristics of Sputter-deposited Gadolinia-doped Ceria Thin Films on Al2O3/SiO2/Si Systems

Metal oxide films prepared by thin film technology have been reported for the potential applications on thin solid electrolyte layers for solid oxide fuel cells(SOFCs). Gadolinia-doped ceria(GDC) thin films and Al2O3 layers on SiO2/Si substrates are successively deposited by RF reactive magnetron sputtering from a cerium-gadolinium (90:10 at.%) alloy target and Al target in O2/Ar gas mixture and then perform post-thermal treatments at 300-700 ℃ and 900 ℃ for 2 h, respectively. Materials characteristics and chemical compositions of GDC films and Al2O3 layers are investigated by X-ray photoelectron spectroscopy(XPS), cross-sectional scanning electron microscopy(SEM), X-ray diffraction(XRD), and atomic force microscopy(AFM). Stoichiometric Al2O3 layers with polycrystalline structures are firstly prepared onto SiO2/Si substrates. A cubic fluorite structure with columnar crystallites of GDC films is successfully deposited on Al2O3/SiO2/Si systems. The chemical composition of 700 ℃-annealed GDC films is (Ce0.91Gd0.09)O1.94 and possesses a higher film density of 7.257 g/cm3. As a result, GDC thin films prepared by RF reactive magnetron sputtering and post-thermal treatments can be used as thin solid electrolyte layers for intermediate temperature SOFCs system as compared to the well-known yttria-stabilized zirconia(YSZ).     

Mean free paths for inelastic electron scattering in silicon and poly(styrene) nanospheres

The mean free paths for inelastic electron scattering, lambda(in), in silicon [Si] and poly(styrene) [PS] have been measured using off-axis electron holography in a field-emission transmission electron microscope (FEG TEM). The holographic imaging method determines both quantitative wave phase information as well as elastic energy-filtered wave amplitude information. Using the energy-filtered amplitude data, two-dimensional t/lambda(in) images are reconstructed. The present work uses spherical nanoparticles as samples, so the sample thickness at any point in a two-dimensional image can be calculated knowing the center and radius of the projected nanosphere. The thickness contribution to t/lambda(in) is removed to obtain quantitative lambda(in) values. This work finds values of lambda(i)Si = 53.8 +/- 5.5 and 88.6 +/- 6.9 nm, and lambda(PS) = 78.1 +/- 3.4 and 113.0 +/- 5.9 nm for 120 and 200 keV incident electron energies, respectively.     

Comparison of the fretting wear of 100Cr6/100Cr6, Si3N4/Si3N4 and Si3N4/100Cr6 contacts in lubricated and dry conditions

The fretting wear behaviour of bearing steel against bearing steel, silicon nitride against silicon nitride, and silicon nitride against bearing steel, was investigated under lubricated and dry conditions. Amplitudes in the intermediate 5 to 50 μm range, and test durations from 10 to 360 min, were studied. Light microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS) were employed to determine the detailed nature of the friction and wear processes. In the silicon nitride against silicon nitride contact, brittle fracture of Si₃N₄ grains, and tribochemical reaction creating an amorphous layer on the mechanically damaged surface, were found. The main mechanism of fretting wear in the case of bearing steel against bearing steel contact was delamination. In the silicon nitride against bearing steel contact, chemical reactions predominated.     

The differential reactivity of octahydridosilsesquioxane on Si(100)-2x1 and Si(111)-7x7: a comparative experimental study

Scanning tunneling microscopy (STM), in conjunction with X-ray photoemission (XPS) and reflection-absorption infrared (RAIRS) spectroscopy, has been used to investigate the reaction of octahydridosilsesquioxane clusters (H(8)Si(8)O(12)) on the Si(100)-2x1 and Si(111)-7x7 surfaces. The clusters exhibit a markedly different reactivity upon exposure to the two clean silicon surfaces. STM data is presented that, in conjunction with XPS and RAIRS data, provides numerous constraints upon possible geometries for the chemisorbed clusters. The sum of the data is consistent with a dissociative reaction mechanism on Si(100)-2x1, resulting in cluster attachment to the surface via a single vertex. Conversely, data of Si(111)-7x7 subject to a saturation exposure of H(8)Si(8)O(12) is presented that is highly suggestive of cluster decomposition on the surface.     

Si(111)和Si(100)衬底上AlN薄膜的激光分子束外延生长特征

采用激光分子束外延技术在Si(111)和Si(100)衬底上制备了AlN薄膜,研究了衬底温度和激光能量对薄膜物相结构和形貌的影响。结果表明:低的激光能量和高的衬底温度有益于薄膜的取向度和表面质量;激光能量为100mJ时,Si(111)衬底上的AlN薄膜呈单一的h-AlN(002)取向,Si(100)衬底上的薄膜在600℃时出现小的h-AlN(100)衍射峰,在700℃时呈微弱的h-AlN(002)取向;在Si(111)衬底上更易生长出取向度高的AlN薄膜。     

The relative importance of multiple inelastic scattering in the quantification of EELS

A comparison is given of energy loss results obtained for the L and K edges of aluminium as a function of specimen thickness, crystallographic orientation and collection angle. It is demonstrated that as the thickness is increased post-loss elastic scattering is generally important in reducing the fraction of electrons collected. The implications for the quantification of EELS data are discussed while a comparison of the Fe/C ratio in cementite demonstrates the improved consistency which can be obtained when comparing K and L losses at lower energy separation than are the losses for aluminium.     

Experimental investigation of flow characteristics of a magnetohydrodynamic (MHD) duct of fan-shaped cross section

Experiments along with numerical calculations are carried out to investigate the effect of the geometry of the cross section on flow characteristics of a MHD propulsion duct. A fan-shaped cross-section MHD thruster duct is chosen for comparison with a previously investigated rectangular cross section. Measurement of the velocity field is made using LDV (Laser Doppler Velocimetry) system with a fiber-optic cable and pressure distribution is measured with static pressure holes at the bottom surface. Comparison with rectangular cross section shows that the velocity profile is significantly influenced by the geometry of cross section while the axial pressure distribution is not so affected.     

100/32t型起重机主梁加强筋的探讨

非标桥式起重机结构设计大都采用传统的设计方法,结构很保守.安全系数较大,致使材料浪费.文中对100/32t型起重机主梁在ANSYS中建立了有限元模型,对其在典型工况下的强度、刚度、可靠性、疲劳强度、稳定牲进行分析探讨,并把主梁T型钢两侧有加强筋时与无加强筋的结果进行了比较,最后得出加强筋可去掉的结论.从而减少主梁的材料,可以减轻主梁重量,降低制造成本,对实际生产有一定的指导意义,并为同类产品设计提供借鉴.     

Nanofretting Behavior of Monocrystalline Silicon (100) Against SiO2 Microsphere in Vacuum

With an atomic force microscopy, the tangential nanofretting between spherical SiO₂ tips and monocrystalline Si(100) surface was carried out at various displacement amplitudes (0.5–250 nm) under vacuum condition. Similar to fretting, the nanofretting of Si(100)/SiO₂ pair could also be divided into stick regime and slip regime upon the transition criterion. However, it was found that the energy ratio corresponding to the transition between two nanofretting regimes varied between 0.32 and 0.64, which was higher than the normal value of 0.2 for the transition criterion to determine the partial slip and gross slip regimes in fretting. One of the reasons may be attributed to the effect of adhesion force, since whose magnitude is at the same scale to the value of the applied normal load in nanofretting. During the nanofretting process of Si(100)/SiO₂ pair, the adhesion force may induce the increase in the maximum static friction force and prevent the contact pair from slipping. The higher the applied load, or the higher the adhesion force, the larger will be the transition displacement amplitude between two regimes in nanofretting. Different from fretting wear, the generation of hillocks was observed on Si(100) surface under the given conditions in nanofretting process. With the increase in the displacement amplitude in slip regime of nanofretting, the height of hillocks first increased and then attained a constant value. Compared to chemical reaction, the mechanical interaction may be the main reason responsible for the formation of silicon hillocks during the nanofretting in vacuum. The results in the research may be helpful to understand the nanofretting failures of components in MEMS/NEMS.     

A method to measure the total scattering cross section and effective beam gas path length in a low‐vacuum SEM

A method is presented to determine the total scattering cross section of imaging gases used in low‐vacuum scanning electron microscopy or environmental scanning electron microscopy. Experimental results are presented for water vapor, nitrogen gas and ambient air for primary beam electron energies between 5 and 30 keV. The measured results are compared and discussed with calculated values. This method allows the effective beam gas path length (BGPL) to be determined. The variations of the effective BGPL with varying chamber pressure are presented. SCANNING 31: 107–113, 2009. © 2009 Wiley Periodicals, Inc.     

Surface roughness modeling in chemically etched polishing of Si (100) using double disk magnetic abrasive finishing

Abstract

The present paper focuses on proposing a new method for determining the surface roughness of chemically etched polishing of Si (100) using double disk magnetic abrasive finishing (DDMAF). Based on chemical etching in KOH solution Vicker’s hardness of Si (100) at different concentration of KOH was determined in context to chemical etching phenomenon. A mathematical relationship was established to relate Vicker’s hardness of Si (100) as a function of the concentration of KOH. The penetration depth of abrasive particle into Si (100) workpiece was determined considering viz; the normal force acting on the abrasive particle under the influence of magnetic flux density and Vicker’s hardness of etched Si (100). The other modeling variables such as wear constant, penetration area of the abrasive particle into Si (100) workpiece which is dependent on the penetration depth of abrasive particle was modified in terms of magnetic flux density and concentration of KOH. The process parameters such as working gap, abrasive mesh number and the rotational speed of the primary magnet were also considered in modeling the surface roughness. The results of surface roughness obtained by the model were also experimentally validated. The theoretical and experimental findings agreed well with each other.     

Status and possibilities of the time-of-flight measurement technique using long scintillation counters with a small cross section (Review)

Results of the analysis of the state-of-the-art time-of-flight measurement technique with the use of long scintillation counters with a small cross section (the length of the counter far exceeds its width in the plane of the hodoscope and thickness along the beam direction), which are used as basic elements of time-of-flight detectors for large physical installations and intended for identifying secondary particles generated during collisions of high-energy particles. The following issues are considered in this review. Various methods for identifying particles are compared, and it is pointed out that the time-of-flight method has certain advantages for secondary particles with momenta higher than ～3–5 GeV/c. Some elements incorporated in scintillation counters and affecting its time resolution are considered: optical fibers, optical contacts in the scintillator-fiber-photodetector system, and high-frequency cables. Their characteristics are presented. The characteristics of all elements of a counter (scintillator, photodetector (PD), and electronics) and the processes occurring in them are discussed. The presented experimental data show that, under the conditions of high counting rates and strong magnetic fields, the working capacity of counters holds at a time resolution of ～100–200 ps. The results of measuring the operating characteristics of counters are analyzed. The dependences of the time resolution on such variables as the coordinate of the particle transit through a counter along its length, the counter length, the light-absorption length in the scintillator, the quality of treatment of the scintillator’s surface, and the energy deposited by a particle in the scintillator substance are considered. The main characteristics of individual time counters and average parameters of time-of-flight detectors in certain physical facilities are presented. Possible ways to improve the time resolution and reduce it to ～50–100 ps are considered.     

A real space investigation of the dimer defect structure of Si(001)-(2times8)

The atomic arrangement of the Si(001)-(2 times 8) surface has been directly imaged in real space by scanning tunnelling microscopy. The superstructure is impurity induced and stablilized by as little as 1% Ni. Clean Si(001) surfaces do not form the (2times8) phase. The two-dimensional Fourier transforms of the STM topographs correspond well to the (2times8) LEED pattern, but the real space images are in fact considerably more complex than previously concluded on the basis of recent diffraction technique measurements. The STM images clearly demonstrate that the (2times8) surface consists of a complex missing dimer structure, namely one and multiple dimer vacancies. Such a dimer defect appears related to the Ni impurity and intimately related to the ordering of the dimer defects probably by third layer dimerization to produce quasi-ordered ‘channels’.     

六方层状结构LixCoO2(0.5＜x≤1)中空位和阳离子的有序化

Layered deintercalamble alkall metal oxides,such as LixCoO2,have been a subject of intense research activities in the past years owing to the technological applications as the battery electrodes and thermoelectric materials[1-2].Vacancy and cation ordering is a notable structural feature in this system.Extensive theoretical and experimental study has been performed concerning this issue in several typical materials[1-2].     

Determination of the inelastic mean free path of electrons in vitrified ice layers for on-line thickness measurements by zero-loss imaging

The inelastic mean free path of 120 keV electrons in vitrified ice layers has been determined in an energy-filtering TEM. From the ratio of the unfiltered and zero-loss-filtered image intensities recorded with a slow-scan CCD camera, the relative sample thickness t/ Λ can be calculated. For calibration, the geometric ice thickness was measured by imaging a tilted view of a cylindrical hole which had been burnt into the ice layer. The total inelastic mean free path was found to be 161 nm, and the partial inelastic mean free path for an acceptance angle of 4.2 mrad was 232 nm. These results were built into a standard protocol for use in cryo-electron microscopy allowing on-line measurements of local ice-layer thicknesses by zero-loss-filtered/unfiltered imaging.     

Scanning tunnelling microscopy studies of heteroepitaxy: CaF2 on Si(111)

We apply scanning tunnelling microscopy and tunnelling spectroscopy to study the initial stages of CaF₂ epitaxy on Si(111)-(7×7) for a range of deposition temperatures. We find that deposition at surface temperatures <700°C leads to CaF₂ clustering. At temperatures between 750 and 800°C two new structures, a 2×3 and a (√3 X √3***)R30°, are observed. Tunnelling spectra and topographs obtained at different energies allow us to measure interface band gaps, and determine the valence state of Ca bonded directly to silicon and the valence state of Ca in the second layer. More importantly, we demonstrate that STM can be used to image thick insulating layers of CaF₂ by tunnelling into the conduction band of the films. One of our goals in this study has been to test the ability of STM to image insulating multilayers. It is generally believed that STM cannot be applied to insulators. We find, however, that despite the large band gap of ～12 eV, the CaF₂ conduction band is accessible, and that insulating films can be imaged by STM.