Determination of surface structure and the depth profile of silica glass by infrared spectroscopy

1Introduction Thesurfacestructureandphysicalproper tiesofcondensedmaterandthinfilmsarediffer entfromthoseofbulk.Thegradientinmicro structurecanextendtomicrometerdepth,de pendingonthepreparationprocessesandchemi calspecies[12].Theformationofsurfacelayersis duetothecorrosionreactions,diffusions,ion implantationandfilmdeposition,exhibitingthe depthprofileinbothmicrostructureandchemi calcomposition.Ithaslongbeenobservedthat attheBrewsterangleofincidenceonthepolishedglasssurface,thereflectedelectr…     

飞行时间二次离子质谱在生物材料和生命科学中的应用(下)

随着仪器性能的不断提高,飞行时间二次离子质谱(TOF-SIMS)在材料表面化学分析中起着越来越重要的作用。TOF-SIMS的主要测试功能包括表面质谱、化学成像及深度剖析,本工作对TOF-SIMS的化学成像及深度剖析2种功能在生物材料和生命科学中的应用做了简单综述,重点介绍了TOF-SIMS成像技术在生物芯片制备工艺中的应用和TOF-SIMS成像和深度剖析技术对生物分子在细胞和生物体组织上空间分布的表征方法;另外,对生物样品的低温制备方法,样品表面添加基质以增强信号强度的实验手段,使用团簇一次离子源提高分子二次离子产额和利用对样品损伤小的C60离子源为轰击源做深度剖析等实验做了简单的介绍;最后,对TOF-SIMS在生物生命材料领域的应用做了展望。     

Charge contrast imaging of material growth and defects in environmental scanning electron miscroscopy--linking electron emission and cathodoluminescence

An electron-based technique for the imaging of crystal defect distribution such as material growth histories in non- and poorly conductive materials has been identified in the variable pressure or environmental scanning electron microscope. Variations in lattice coherence at the meso-scale can be imaged in suitable materials. Termed charge contrast imaging (CCI), the technique provides images that correlate exactly with emitted light or cathodoluminescence in suitable materials. This correlation links cathodoluminescence and an electron emission. The specific operating conditions for observation of these images reflect a complex interaction between the electron beam, the positive ions generated by electron-gas interactions in the chamber, a biased detector, and the sample. The net result appears to be the suppression of all but very near surface electron emission from the sample, probably from of the order of a few nanometres. Consequently, CCI are also sensitive to very low levels of surface contaminants. Successful imaging of internal structures in a diverse range of materials indicate that the technique will become an important research tool.     

氦离子显微镜：技术和应用进展

氦离子显微镜能够提供所有扫描射线法中最高空间分辨率的表面图像,以及极高的表面灵敏度。这些因素结合起来,能提供纳米级的无与伦比的样品信息。结合这种工具独特的充电控制技术,一些应用问题可以得到解决。本文介绍了一些近期的结果。例如,生命科学影像往往依赖于研究高度绝缘的轻型有机材料的表面形貌。氦离子显微镜无需导电涂层就可以提供极好的成像。诸如生物工程学研究之类的应用,可同时受益于充电控制和氦离子成像可避免电子束辐射造成损伤的优点。可以使用氦离子显微镜进行离子散射能谱分析,从而将这项灵敏度最高的表面技术应用于同时要求具有空间分辨率的分析任务中。氦离子显微镜也用于表面和材料的图形化。这对于创建和表征纳米级的新特性是至关重要的。     

深亚微米IC超浅结的SIMS表征

Secondary ion mass spectrometry (SIMS) is a standard technique for characterization of dopant distribution in semiconductor industry. In the ultra-shallow junction (USJ) application, the interested depth scale was extended into the surface transient area of SIMS. There is several improved approach reviewed in this paper that can meet the requirements for the USJ characterization. Sputtering with a low energy primary ion beam incident at a large angle respect to the simple surface normal can effectively minimize the depth of the surface transient area, as well as the length of the profile tail. Oxygen leak can reduce the transient ion yield change, but induces lower depth resolution. Quadrupole SIMS can be used in B profile. As and P profiles, however, need magnetic analyzer with higher mass resolution.     

Polycrystal orientation maps from TEM

Determination of topography of crystallite orientations is an important technique of investigation of polycrystalline materials. A system for creating orientation maps using transmission electron microscope (TEM) Kikuchi patterns and Convergent beam electron diffraction patterns is presented. The orientation maps are obtained using a step-by-step beam scan on a computer-controlled TEM equipped with a CCD camera. At each step, acquired diffraction patterns are indexed and orientations are determined. Although, the approach used is similar to that applied in SEM/electron back scattered diffraction (EBSD) orientation imaging setups, the TEM-based system considerably differs from its SEM counterpart. The main differences appear due to specific features of TEM and SEM diffraction patterns. Also, the resulting maps are not equivalent. On these generated by TEM, the accuracy of orientation determination can be better than 0.1 degrees. The spatial resolution is estimated to be about 10nm. The latter feature makes the TEM orientation mapping system an important tool for studies at fine scale unreachable by SEM/EBSD systems. The automatic orientation mapping is expected to be a useful complement of the conventional TEM contrast images. The new technique will be essential for characterization of fine structure materials. To illustrate that, example maps of an aluminum sample produced by severe plastic deformation are included.     

A surface work function measurement technique utilizing constant deflected grazing electron trajectories: oxygen uptake on Cu(001)

We report on the application of a novel nondestructive in-vacuum technique for relative work function measurements, employing a grazing incidence electron deflection above a sample with a planar surface. Two deflected electron beam detectors are used as a position sensitive detector to control feedback to the sample potential as the sample work function changes. With feedback the sample potential exactly follows the surface sample-size averaged work function variation, so that the deflected beam trajectory remains stable. We also discuss methods to optimize the initial electron trajectories for this method, so as to minimize unwanted effects such as from uncontrolled external magnetic fields. As the electron beam does not impinge on the surface in this new technique electron induced desorption, ionization, dissociation, and/or decomposition is not induced at the interface. Importantly also the technique allows for free access to the surfaces enabling simultaneous deposition/evaporation and/or application of other surface characterization methods. We demonstrate its application in concurrent measurements of helium atom reflectivity and work function changes taking place during molecular oxygen exposure of a Cu(001) surface. A work function measurement sensitivity and stability is demonstrated at ～10?mV at a sampling rate of 1 Hz and after application of an ～7?s smoothing routine. In comparison to the helium atom reflectivity measurements, the work function measurements are more sensitive to the initial O uptake, and less so to the final coverage variations and possible surface reordering at higher O coverages.     

五坐标高压水束加工技术的研究

采用高压水束这一特种加工方法来加工,确定了高压水束加工的技术参数,建立了高压水束切割时工件和载荷的理论模型,并将理论模拟分析与实际试验结果进行了比较。研究了不同高压泵压力作用下高压水束的速度及作用范围。实验结果表明,利用高压水束方法加工上述材料能够满足其加工部位的质量要求。     

Two beam surface fluctuation specular reflection spectroscopy

In surface fluctuation specular reflection spectroscopy (SFSRS) deflections of a specularly reflected laser beam are used to characterize thermally excited surface waves. Here we report on a new two beam version of SFSRS in which the deflections of two reflected laser beams from separate locations on a surface are correlated. We demonstrate that this new two beam SFSRS technique can be used to determine directly the power spectrum of height fluctuation of thermally excited surface waves over a large range of both frequencies and wavevectors. In addition, we show that the technique is well suited for materials ranging from simple liquids to complex liquids and soft solids, including turbid materials.     

Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination

We have developed a new fast electron diffractometer working with high dynamic range and linearity for crystal structure determinations. Electron diffraction (ED) patterns can be scanned serially in front of a Faraday cage detector; the total measurement time for several hundred ED reflections can be tens of seconds having high statistical accuracy for all measured intensities (1-2%). This new tool can be installed to any type of TEM without any column modification and is linked to a specially developed electron beam precession "Spinning Star" system. Precession of the electron beam (Vincent-Midgley technique) reduces dynamical effects allowing also use of accurate intensities for crystal structure analysis. We describe the technical characteristics of this new tool together with the first experimental results. Accurate measurement of electron diffraction intensities by electron diffractometer opens new possibilities not only for revealing unknown structures, but also for electrostatic potential determination and chemical bonding investigation. As an example, we present detailed atomic bonding information of CaF(2) as revealed for the first time by precise electron diffractometry.     

应用免穿丝型电火花线切割机床加工汽车连杆裂解槽实验研究

为了研究免穿丝型电火花线切割机床加工连杆大头孔内表面双侧裂解槽的质量及效率问题,以新一代免穿丝型电火花线切割机床为实验设备,分别进行单工位加工实验与双工位加工实验,其中双工位加工实验分为不同型号和同型号连杆裂解槽双工位加工实验。实验证明：单工位加工时实验样品槽深H随运丝频率的增大呈现先减少后增大,槽宽W受脉冲周期影响显著;同型号双工位加工时实验样品裂解槽槽深H受电源电压影响显著,左工位实验样品裂解槽槽宽W在脉宽30～40μs变化明显,右工位实验样品槽宽W随电压上升而增大。大部分实验组均能在20 s内达到连杆裂解槽加工要求,具有良好的应用前景。     

Electron-beam-generated carrier distributions in semiconductor multilayer structures

The electron beam of a scanning electron microscope causes carrier generation in a semiconductor and these carriers are the probe for various types of image. In particular, the electron-beam-induced current mode gives images which reveal electrically active near-surface defects in a semiconductor sample. Since semiconductor multilayer structures are now very common, one needs to know how the multilayer structure modifies the shape of the generation volume. The Monte Carlo technique for modelling beam electron trajectories inside the sample is used and gives a detailed insight into the shape of such a generated carrier generation distribution. Additionally, a simpler analytical method is developed for constructing a one-dimensional depth distribution for multilayer structures, starting from known depth dose distributions for bulk materials. The analytical method is validated by comparison with Monte Carlo results.     

Site-specific structural investigations of oxidized nickel samples modified by plasma erosion processes

A focused ion beam was employed for local target preparation for EBSD analysis. The volume of the ion‐solid interaction is well below 50 nm at glancing incidence for metallic and transition metal oxide samples. Therefore, focused ion beam can successfully be used for electron backscatter diffraction (EBSD) sample preparation. The sample investigated consists of Ni covered with a NiO layer of ～5 μm thickness. Focused ion beam cross‐sectioning of these layers and subsequent electron imaging in addition to EBSD maps shows a bimodal structure of the oxide layer. In order to test the potential of such oxidized samples as electrode materials, single spark erosion experiments were performed. The erosion craters have diameters up to 40 μm and have a depth corresponding to the thickness of the oxide layer. In addition, a deformation zone produced by thermoshock accompanies the formation of the crater. This deformation zone was further investigated by EBSD analysis using a new way of sample preparation employing the focused ion beam technology. This target preparation routine is called Volume of Interest Transfer and has the potential of providing a full three‐dimensional characterization.     

Microstructural analysis of a FeAl/quasicrystal-based composite prepared using a focused ion beam miller

A composite consisting of a brittle multiphase matrix containing both an Al-based quasicrystalline phase (ψ) and an ordered body centred cubic phase (β) and a relatively ductile ordered body centred cubic intermetallic FeAl phase has been developed as an abrasive wear-resistant coating material. It is applied as a 500 μm thick layer onto stainless steel substrates through plasma spray processing. The microstructure of such materials can be readily examined by optical and scanning electron microscopy, but the inherent difficulty of preparing transmission electron microscope (TEM) samples has inhibited higher resolution studies. However, the relatively recent development of the focused ion beam (FIB) miller as a tool in materials science provides a method ideal for the preparation of TEM specimens of these materials. In this study a coating consisting of a mixture of an Al–Cu–Fe based quasicrystal and FeAl+Cr was deposited on to a 304 stainless steel substrate. TEM specimens were prepared using a FIB and subjected to detailed microstructural characterization. The structure consisted of elongated bands of a FeAl phase about 100 nm in width and several micrometres in length, which enclosed more equiaxed regions about 1 μm in diameter that consisted of fine mixtures of quasicrystal and two Al-Fe-Cu phases isostructurally related to FeAl.     

A study on the effect of tool-edge radius on critical machining characteristics in ultra-precision milling of tungsten carbide

A crack-free surface can be finished on brittle materials by a specialized but traditional machining technique known as ductile-mode machining. In ductile-mode machining of brittle material, crack propagation is suppressed by selecting a suitable combination of tool and machining parameters leading to the removal of material through plastic deformation enabled by dislocation motion. In ductile-mode machining, the tool–workpiece interaction is of critical significance for the capability of the cutting process to finish a crack-free surface on a brittle material. This interaction is largely dictated by the cutting-edge radius of the tool when the undeformed chip thickness is comparable to the edge radius as is the case of ductile-mode machining. This paper presents the experimental results of ductile-mode milling of tungsten carbide to investigate the effect of cutting-edge radius on certain critical machining characteristics associated with the ductile–brittle transition specific to milling process of brittle material. The experimental results have established that an increase in the cutting-edge radius within a certain range increases the critical feed per edge leading to the improvement of material removal rate in ductile-mode milling. An increasingly negative effective rake angle is desired during milling with larger edge-radiused tool to suppress the crack propagation in the cutting zone to achieve ductile-mode machining. The results also identify the effect of the edge radius on certain other parameters such as critical specific cutting energy, plowing effect and subsurface damage depth to comprehend the ductile–brittle transition phenomenon in ductile-mode milling.     

Depth profiling by secondary ion mass spectrometry

The principles and applications of depth profiling by secondary ion mass spectrometry (SIMS) are reviewed. Discussed are the basic physical processes and instrumental factors which influence the shape of depth profiles and which have to be understood or controlled for successful experimental measurements. Microroughness caused by sputtering, atomic mixing by primary beam knock-on, and sample consumption limit the depth resolution which can be achieved while the chemical effect of ion yield enhancement by reactive species, matrix effects, and preferential sputtering can strongly affect the secondary ion signal. Instrumental effects to be controlled include beam uniformity, sample charging, and beam, and residual gas contamination. High depth resolution and sensitivity are the reasons for a wide variety of applications for SIMS depth profiling. Reviewed are measurements of the range distribution of ions implanted into semiconductors and their redistribution by subsequent annealing, studies of thin films and of oxide layers, diffusion measurements in metals, semiconductors, and minerals, measurements of elemental surface enhancements in airborne particles, and lunar glass spherules, and the search for solar wind implanted ions in lunar crystals.     

Maximum entropy reconstruction of compositional depth profiles from electron probe microanalysis data

Electron probe microanalysis (EPMA) is a powerful method for the quantitative determination of the elemental composition of micro-regions of a sample surface. Here, we report on the development of a method of reconstructing compositional depth profiles in thin films from EPMA data measured over a range of electron beam energies, using maximum entropy data processing. The method gives quantitative information on film compositions up to approximately 1 μm in depth, with a lateral spatial resolution of approximately 1 μm. The method is tested using both simulated data and measured experimental data from well-characterized model sample structures.     

Image quality evaluation for FIB-SEM images

Focused ion beam scanning electron microscopy (FIB-SEM) tomography is a serial sectioning technique where an FIB mills off slices from the material sample that is being analysed. After every slicing, an SEM image is taken showing the newly exposed layer of the sample. By combining all slices in a stack, a 3D image of the material is generated. However, specific artefacts caused by the imaging technique distort the images, hampering the morphological analysis of the structure. Typical quality problems in microscopy imaging are noise and lack of contrast or focus. Moreover, specific artefacts are caused by the FIB milling, namely, curtaining and charging artefacts. We propose quality indices for the evaluation of the quality of FIB-SEM data sets. The indices are validated on real and experimental data of different structures and materials.     

Simple technique for high‐throughput marking of distinguishable micro‐areas for microscopy

Today's (nano)‐functional materials, usually exhibiting complex physical properties require local investigation with different microscopy techniques covering different physical aspects such as dipolar and magnetic structure. However, often these must be employed on the very same sample position to be able to truly correlate those different information and corresponding properties. This can be very challenging if not impossible especially when samples lack prominent features for orientation. Here, we present a simple but effective method to mark hundreds of approximately 15×15 μm sample areas at one time by using a commercial transmission electron microscopy grid as shadow mask in combination with thin‐film deposition. Areas can be easily distinguished when using a reference or finder grid structure as shadow mask. We show that the method is suitable to combine many techniques such as light microscopy, scanning probe microscopy and scanning electron microscopy. Furthermore, we find that best results are achieved when depositing aluminium on a flat sample surface using electron‐beam evaporation which ensures good line‐of‐sight deposition. This inexpensive high‐throughput method has several advantageous over other marking techniques such as focused ion‐beam processing especially when batch processing or marking of many areas is required. Nevertheless, the technique could be particularly valuable, when used in junction with, for example focused ion‐beam sectioning to obtain a thin lamellar of a particular pre‐selected area.     

Towards the imaging of Weibel–Palade body biogenesis by serial block face‐scanning electron microscopy

Electron microscopy is used in biological research to study the ultrastructure at high resolution to obtain information on specific cellular processes. Serial block face‐scanning electron microscopy is a relatively novel electron microscopy imaging technique that allows three‐dimensional characterization of the ultrastructure in both tissues and cells by measuring volumes of thousands of cubic micrometres yet at nanometre‐scale resolution. In the scanning electron microscope, repeatedly an image is acquired followed by the removal of a thin layer resin embedded biological material by either a microtome or a focused ion beam. In this way, each recorded image contains novel structural information which can be used for three‐dimensional analysis. Here, we explore focused ion beam facilitated serial block face‐scanning electron microscopy to study the endothelial cell–specific storage organelles, the Weibel–Palade bodies, during their biogenesis at the Golgi apparatus. Weibel–Palade bodies predominantly contain the coagulation protein Von Willebrand factor which is secreted by the cell upon vascular damage. Using focused ion beam facilitated serial block face‐scanning electron microscopy we show that the technique has the sensitivity to clearly reveal subcellular details like mitochondrial cristae and small vesicles with a diameter of about 50 nm. Also, we reveal numerous associations between Weibel–Palade bodies and Golgi stacks which became conceivable in large‐scale three‐dimensional data. We demonstrate that serial block face‐scanning electron microscopy is a promising tool that offers an alternative for electron tomography to study subcellular organelle interactions in the context of a complete cell.