Dopant distributions in n-MOSFET structure observed by atom probe tomography

The dopant distributions in an n-type metal-oxide-semiconductor field effect transistor (MOSFET) structure were analyzed by atom probe tomography. The dopant distributions of As, P, and B atoms in a MOSFET structure (gate, gate oxide, channel, source/drain extension, and halo) were obtained. P atoms were segregated at the interface between the poly-Si gate and the gate oxide, and on the grain boundaries of the poly-Si gate, which had an elongated grain structure along the gate height direction. The concentration of B atoms was enriched near the edge of the source/drain extension where the As atoms were implanted.     

Low angle boundary migration of shot‐peened pure nickel investigated by electron channeling contrast imaging and electron backscatter diffraction

Study on recrystallization of deformed metal is important for practical industrial applications. Most of studies about recrystallization behavior focused on the migration of the high‐angle grain boundaries, resulting in lack of information of the kinetics of the low angle grain boundary migration. In this study, we focused on the migration of the low angle grain boundaries during recrystallization process. Pure nickel deformed by shot peening which induced plastic deformation at the surface was investigated. The surface of the specimen was prepared by mechanical polishing using diamond slurry and colloidal silica down to 0.02 μm. Sequential heat treatment under a moderate annealing temperature facilitates to observe the migration of low angle grain boundaries. The threshold energy for low angle boundary migration during recrystallization as a function of misorientation angle was evaluated using scanning electron microscopy techniques. A combination of electron channeling contrast imaging and electron backscatter diffraction was used to measure the average dislocation density and a quantitative estimation of the stored energy near the boundary. It was observed that the migration of the low angle grain boundaries during recrystallization was strongly affected by both the stored energy of the deformed matrix and the misorientation angle of the boundary. Through the combination of electron channeling contrast imaging and electron backscatter diffraction, the threshold stored energy for the migration of the low angle grain boundaries was estimated as a function of the boundary misorientation.     

The role of dynamic recrystallization in dry sliding wear

In dry sliding wear dynamic recrystallization gives a better understanding than grain boundary sliding and fatigue of the process near the contact zone. The process explains the low value of the deformation measured by grain thickness reduction and the absence of visible deformation marks in the case of low melting materials. Dynamic recrystallization explains the almost total consumption of the friction energy by the plastic process. It is also possible to compute the geometry of the worn material in a wear test. This phenomenon is proved experimentally using a copper pin sliding against an SAE 1045 steel ring. Pins of both single crystal and polycrystalline copper were used. The structure was observed by examining thin foils of the material taken from near the contact zone in an electron microscope.     

用于热机械微纳加工的掺Al多晶硅加热器

针对热机械式微纳米结构的加工,提出了一种以掺Al多晶硅为材料,集成于微悬臂梁上的加热器.采用Al诱导退火晶化(AIC)方法,在750 K对Al/a-Si∶H复合薄膜低温晶化18 h,制备出掺Al多晶硅.通过低温退火,使复合薄膜的拉曼特征峰由478 cm-1移至520 cm-1,完成由非晶硅向多晶硅的转变;由四探针仪测得...     

904L不锈钢形变奥氏体的亚结构演化及其对宏观流变应力的影响

为了揭示动态再结晶行为的本质及其对流变应力的影响,选取904L奥氏体不锈钢为研究对象,针对奥氏体在不同工艺下的热变形行为以及变形组织和再结晶组织的亚结构进行深入研究。结果表明材料的宏观应力-应变曲线在特定条件下不能准确反映微观尺寸上的动态再结晶行为。EBSD分析表明动态再结晶晶粒中亚结构特征以取向差角小于1°为主,呈周期性分布,且这种特征不会随晶粒自身长大或应变的增加而发生明显改变,即具有较好的稳定性;而变形组织中亚结构的取向差角明显增大,频繁出现大于1°的小角晶界,局部取向差角的分布范围也增大至1°～4°,即几何必需位错密度显著增加。尽管无论何种工艺下晶界均为再结晶的优先形核位置,但形核条件是不同的。对于完全再结晶组织来说,新的再结晶晶粒形核只需晶界出现局部“弓出”或弯曲;而在原始变形组织中,出现再结晶形核的晶界均存在微区高应变。     

采用Cellular automaton法模拟动态再结晶过程的研究

结合金属塑性成形过程的冶金学原理,给出了一种新的模拟动态再结晶过程的元胞自动机(Cellular automaton,CA)模型,用来模拟塑性变形过程中动态再结晶过程。再结晶晶粒的生长速度与再结晶驱动力成正比, 再结晶驱动力取决于晶界能和位错密度。在一个增量步内,根据动态再结晶晶粒生长速度确定与其相邻原胞转变 概率。采用本模型对不同温度、应变速度、应变条件下的动态再结晶过程进行了模拟,模拟结果与试验结果以及 经验公式得到的结果相一致。本模型也可用于再结晶动力学、微观组织和织构变化过程的模拟。     

Evidence of multimicrometric coherent γ′ precipitates in a hot‐forged γ–γ′ nickel‐based superalloy

This paper demonstrates the existence of large γ’ precipitates (several micrometres in diameter) that are coherent with their surrounding matrix grain in a commercial γ–γ’ nickel‐based superalloy. The use of combined energy dispersive X‐ray spectrometry and electron backscattered diffraction (EBSD) analyses allowed for revealing that surprising feature, which was then confirmed by transmission electron microscopy (TEM). Coherency for such large second‐phase particles is supported by a very low crystal lattice misfit between the two phases, which was confirmed thanks to X‐ray diffractograms and TEM selected area electron diffraction patterns. Dynamic recrystallization of polycrystalline γ–γ’ nickel‐based superalloys has been extensively studied in terms of mechanisms and kinetics. As in many materials with low stacking fault energy, under forging conditions, the main softening mechanism is discontinuous dynamic recrystallization. This mechanism occurs with preferential nucleation on the grain boundaries of the deformed matrix. The latter is then being consumed by the growth of the newly formed grains of low energy and by nucleation that keeps generating new grains. In the case of sub‐solvus forging, large γ’ particles usually pin the migrating boundaries and thus limit grain growth to a size which is determined by the distribution of second‐phase particles, in good agreement with the Smith–Zener model. Under particular circumstances, the driving force associated with the difference in stored energy between the growing grains and the matrix can be large enough that the pinning forces can be overcome, and some grains can then reach much larger grain sizes. In the latter exceptional case, some intragranular primary γ’ particles can be observed, although they are almost exclusively located on grain boundaries and triple junctions otherwise. In both cases, primary precipitates have no special orientation relationship with the surrounding matrix grain(s). This paper demonstrates the existence of high fractions of large γ’ precipitate (several micrometres in diameter) that are coherent with their surrounding matrix grain, in a commercial γ–γ’ nickel‐based superalloy. Such a configuration is very surprising, because there is apparently no reason for the coherency of such particles.     

The remote electron beam-induced current analysis of grain boundaries in semiconducting and semi-insulating materials

When no charge collecting p-n junction or Schottky barrier is present in the specimen, but two contacts are applied, conductive mode scanning electron microscope (SEM) observations known as remote electron beam-induced current (REBIC) can be made. It was described as "remote" EBIC because the contacts to the specimen can lie at macroscopic distances from the beam impact point. In recent years, REBIC has been found to be useful not only for studies of grain boundaries in semiconducting silicon and germanium, but also in semi-insulating materials such as the wider bandgap II-VI compounds and electroceramic materials like varistor ZnO and positive temperature coefficient resistor (PTCR) BaTiO3. The principles of this method are outlined. Accounts are given of the five forms of charge collection and resistive contrast that appear at grain boundaries (GBs) in REBIC micrographs. These are (1) terraced contrast due to high resistivity boundary layers, (2) peak and trough (PAT) contrast due to charge on the boundary, (3) reversible contrast seen only under external voltage bias due to the beta-conductive effect in a low conductivity boundary layer, (4) dark contrast due to enhanced recombination, and (5) bright contrast apparently due to reduced recombination. For comparison, the results of the extensive EBIC studies of GBs in Si and Ge are first outlined and then the results of recent REBIC grain boundary studies in both semiconducting and semi-insulating materials are reviewed.     

Process optimization and microstructural development during superplastic-like forming of AA5083

An advanced sheet forming process was utilized by combining hot drawing and blow forming to establish a fast forming technology. As a continuation of the development in superplastic-like forming, this study dealt with the process optimization and evaluation of post-forming properties. Aluminum alloy 5083 (AA5083) parts with near-net shape were successfully fabricated at 400 °C. Thickness uniformity has been improved by optimizing the mechanical preforming (hot drawing) and adopting a strain-rate-control gas forming (blow forming). Fairly uniform microstructure can be achieved with this forming process. To investigate the microstructural information, the annealed and hot deformed samples were characterized using electron backscatter diffraction technique. Fine grains with high-angle grain boundaries occurred near the elongated grains during hot drawing stage as a result of dynamic recrystallization. Subgrain structure was also examined by characterizing the distribution of grain boundary misorientation angles. Grain growth and subgrain boundary migration were two main microstructural features observed during the gas forming stage.     

考虑晶粒变形动态再结晶过程模拟的元胞自动机法

结合金属塑性成形过程的冶金学原理,给出了一种考虑动态再结晶过程晶粒变形的元胞自动机模型.考虑了晶粒变形对再结晶形核的影响,给出了一种与基元形状有关的形核概率计算方法.根据动态再结晶晶粒生长速度和与其相邻基元形状确定转变概率.采用元胞自动机模型对动态再结晶组织的演变进行了模拟,模拟结果与不考虑晶粒变形的结果进行了比较.     

铝合金双面双弧同步立焊工艺特征与接头组织性能分析

采用双面双弧同步立焊工艺方法,对8 mm厚5083铝合金进行自熔试验,I形坡口一次熔透,焊缝成形美观。通过调节两侧电弧热量配比研究熔池成形规律,并从焊接接头的微观组织、力学性能分析其连接机理。研究结果表明,随着热输入的增加,双面双弧同步立焊热量加速集聚,熔深以三次幂函数的速度增大。双面双弧同步立焊接头轮廓呈“双曲线形”,而相同热输入下的单面焊接头则呈“倒马鞍形”。总热输入一定的情况下,双面双弧接头正面熔宽随能量配比系数的增大而增大,反面熔宽随能量配比系数的增大而减小,中间熔宽基本不变,熔化面积随能量配比系数的增大先增大后减小;能量配比系数一定时,随着焊速的增大,接头熔宽和熔化面积均减小。母材组织为条带状纤维织构,热影响区发生静态回复与再结晶,变形组织消失,产生新晶粒,焊缝区主要由α-Al固溶体、β相(Al8Mg5)质点和骨骼状的Mg2Si析出相组成。焊缝的抗拉强度随着能量配比系数的增大而减小,拉伸断裂形式为韧性断裂。热影响区出现软化现象,双弧交汇区硬度低于正面焊缝区。     

基于晶界迁移率与晶界能各向异性的晶粒生长元胞自动机模拟

基于晶粒长大的理论模型,结合曲率机制与概率性转变规则,建立了晶界迁移率与晶界能各向异性条件下的二维元胞自动机模型,利用该模型对晶粒等温条件下的生长过程进行了模拟,分析了晶粒长大的组织演变与动力学特征、晶粒尺寸和晶粒边数的分布,对比了晶界迁移率各向异性、晶界能各向异性对晶粒生长的影响。结果表明:晶界迁移率与晶界能各向异性条件下晶粒形态演变遵循晶粒正常长大的规律,相对晶粒尺寸偏离正态分布,晶粒边数分布不具有时间不变性特点,小角度取向差三叉晶界平衡角偏离120°;与各向同性相比,晶界迁移率与晶界能各向异性条件下晶粒的生长速率明显减慢,单独考虑晶界迁移率各向异性对晶粒生长的影响不大,晶界能各向异性对晶粒生长的影响大于晶界迁移率各向异性的影响;模拟结果符合晶粒生长动力学理论和相关文献的结论。     

First combined electron backscatter diffraction and transmission electron microscopy study of grain boundary structure of deformed quartzite

The structures of boundaries in a deformed and dynamically recovered and recrystallized quartz polycrystal (mylonite) were characterized by transmission electron microscopy, after the misorientation angles across the same grain boundaries had been analysed using electron backscatter diffraction in a scanning electron microscope. In this new approach, a specific sample area is mapped with electron backscatter diffraction, and the mapped area is then attached to a foil, and by the ion beam thinned for transmission electron microscopy analysis. Dislocations in grain boundaries were recognized as periodic and parallel fringes. The fringes associated with dislocations are observed in boundaries with misorientations less than 9°, whereas such fringes cannot be seen in the boundaries with misorientations larger than 17°. Some boundaries with misorientations between 9° and 17° generally have no structures associated with dislocation. One segment of a boundary with a misorientation of 13.5° has structures associated with dislocations. It is likely that the transition from low‐angle to high‐angle boundaries occurs at misorientations ranging from approximately 9° to 14°. Change in the grain boundary structure presumably influences the mobility of the boundaries. In the studied deformed quartz vein, a relative dearth of boundaries between misorientation angles of θ = 2° and θ = 15° has previously been reported, and high‐angle boundaries form cusps where they intersect low‐angle boundaries, suggesting substantial mobility of high‐angle boundaries.     

Static recrystallization simulations starting from predicted deformation microstructure by coupling multi-phase-field method and finite element method based on crystal plasticity

We have developed a numerical model of recrystallization taking the inhomogeneities of the plastic deformation of a polycrystalline metal into account. Here, the plastic deformation of the polycrystalline metal is simulated by the finite element method based on crystal plasticity theory and the microstructure evolution during recrystallization is simulated by the multi-phase-field method. In primary recrystallization simulations, nucleation is the most difficult problem. In the present model, the deformation microstructure is predicted from the results of a crystal plasticity finite element simulation, and spontaneous nucleation is achieved through abnormal grain growth that is enabled by introducing the misorientation dependences of grain boundary energy and mobility. As a result of simulations under three different compression strains, it is confirmed that primary recrystallization simulations depending on the amount of deformation and taking the inhomogeneities of the plastic deformation of a polycrystalline metal into consideration can be successfully performed by employing the proposed model.     

基于非均匀储存能场的低碳钢静态再结晶CA模拟

采用元胞自动机方法,基于亚晶异常长大形核机制,在非均匀储存能场条件下,建立了低碳钢静态再结晶模型,并模拟了不同变形条件下的静态再结晶过程。结果表明:储存能越大,再结晶临界形核半径越小;变形程度较小时,再结晶晶核优先在晶界和小晶粒处形成;随着变形程度的增大,再结晶晶核的分布趋于均匀,孕育期及再结晶时间缩短,再结晶完成时晶粒较为细小;模拟结果与试验结果一致。     

EBSD coupled to SEM in situ annealing for assessing recrystallization and grain growth mechanisms in pure tantalum

An in situ annealing stage has been developed in‐house and integrated in the chamber of a Scanning Electron Microscope equipped with an Electron BackScattered Diffraction system. Based on the Joule effect, this device can reach the temperature of 1200°C at heating rates up to 100°C/s, avoiding microstructural evolutions during heating. A high‐purity tantalum deformed sample has been annealed at variable temperature in the range 750°C–1030°C, and classical mechanisms of microstructural evolutions such as recrystallization and grain coarsening phenomena have been observed. Quantitative measurements of grain growth rates provide an estimate of the mean grain boundary mobility, which is consistent with the value estimated from physical parameters reported for that material. In situ annealing therefore appears to be suited for complementing bulk measurements at relatively high temperatures, in the context of recrystallization and grain growth in such a single‐phase material.     

Transmission electron microscope observations of the wear tracks of nickel and nickel-based alloys tested in a simulated face seal

The fine structural details of the wear tracks of nickel, nickel-chromium and nickel-molybdenum alloys tested in a simulated face seal apparatus have been observed using transmission electron microscopy. The structures are complex and varied; there are regions of extremely high dislocation density and in all materials recrystallization is prevalent, with a very fine grain size (0.1 μm or less). The nickel-molybdenum alloys had been heat-treated to develop either an ordered or a disordered structure and changes in this due to the wear process showed that in some cases the local interface temperature exceeded 900 °C.     

3-D analysis of semiconductor dopant distributions in a patterned structure using LEAP

This work presents the first 3-D analysis of lateral dopant diffusion in a patterned structure using a pulsed laser-assisted local electrode atom probe (LEAP). A structure similar to a device channel was created for this work by performing a 3 keV, 1×10¹⁵ cm⁻² As⁺ implant on a poly-Si line patterned wafer with 70 nm line width and 200 nm line pitch. The wafer was subsequently annealed at 950 °C for 1 s. LEAP samples were made using a site-selective in-situ focused ion beam (FIB) process. The results from LEAP analysis were then compared with high-resolution transmission electron microscopy (HRTEM) and Florida object-oriented process simulator (FLOOPS) results. Good structural agreement was found between the LEAP and HRTEM results. Several 1-D As concentration profiles extracted from the LEAP data were also found to be in good agreement with FLOOPS process simulation results. These profiles also represent for the first time that results from a 3-D process simulator have been able to be confirmed experimentally using a single sample.     

Shaping the lens of the atom probe: fabrication of site specific, oriented specimens and application to grain boundary analysis

The random sampling provided by classical atom probe sample preparation methods is one of the major factors limiting the types of problems that can be addressed using this powerful technique. A focused ion beam enables not only site-specific preparation, but can also be used to give the specimen, which acts as the lens in an atom probe experiment, a specific shape. In this paper we present a technique that uses low accelerating voltages (10 and 5 kV) in the focused ion beam (FIB) to reproducibly produce specimens with selected grain boundaries <100 nm from the tip at any desired orientation. These tips have a high rate of successfully running in the atom probe and no Ga contamination within the region of interest.This technique is applied to the analysis of grain boundaries in a high purity iron wire and a strip-cast steel. Lattice resolution is achieved around the boundary in certain areas. Reconstruction of these datasets reveals the distribution of light and heavy elements around the boundary. Issues surrounding the uneven distribution of certain solute elements as a result of field-induced diffusion are discussed.     

Monte Carlo simulation of grain growth of single-phase systems with anisotropic boundary energies

The grain growth in single-phase systems with various anisotropic boundary energies is simulated using a modified two-dimensional (2D) Monte Carlo algorithm. Structural self-similarity both in the grain shape distributions and the grain boundary configurations is found regardless of the degree and type of anisotropy. Parabolic evolution kinetics is observed in most cases. The growth rate represented by the time rate of average grain area change is found to be a function of the grain boundary properties. In some cases, the normalized grain size distributions are not time-invariant, and therefore, current grain growth theories cannot explain conclusively the occurrence of the parabolic kinetics in these cases. The effect of anisotropy on the grain growth kinetics is discussed.