Imaging of a single atomic column in silicon grain boundary

Atomic resolution high voltage electron microscopy was applied in investigations of the atomic structure of [112] sigma3 CSL grain boundary of silicon. Images of the grain boundary, viewed in the < 110 > direction, showed two types of dark spots. One type was rod shaped, which represented an atomic pair aligned in the < 111 > direction. The other was a small round spot, which represented a single atomic column in the grain boundary. The atomic structure of [112] sigma3 CSL grain boundary was directly shown from the atomic-structure image.     

SBT材料微结构的TEM研究

本文利用透射电子显微术(TEM)对 SrBi2Ta2O9 (SBT) 材料(单晶、陶瓷及薄膜)的微结构进行了研究. 在(001)取向的SBT单晶材料及多晶陶瓷中观察到90°铁电畴结构.在SBT晶体中观察到大量的条带状四度反相畴界结构和少量的三度反相畴界结构,利用TaO6氧八面体的扭转和四态自旋结构模型,对反相畴界结构的实验观测结果进行了解释.在(001)取向的SBT铁电薄膜中,观察到小角晶界(倾角为8 2°)的位错分解现象,导致不全位错和层错的出现.利用平衡状态下两个不全位错之间的排斥力等于层错的吸引力,估算了小角晶界处的层错能量,大小为0 27～0 29 J/m2.小角晶界位错的分解对(001)取向的SBT铁电薄膜漏电流及耐疲劳特性具有重要的影响.     

N元素偏聚对2205双相不锈钢微观组织结构的影响

采用金相、SEM、XRD和EBSD等分析方法,对双相不锈钢管N元素偏聚区域组织进行成分及结构的分析.结果表明:双相不锈钢管有100μm宽的带状N元素偏聚区,中心开裂,该区域基本为奥氏体单相组织,内部晶粒粗大且为等轴晶,以Σ3重位点阵(CSL)晶界为主,出现频率约为40%.而远离偏聚区中,铁素体奥氏体双相组织的相比例正常,奥氏体晶粒细小呈条状,也以Σ3晶界为主,出现频率降为27%.N偏聚区奥氏体与正常区奥氏体组织均可形成<111>∥RD及<110>∥ND方向的织构,但偏聚区奥氏体织构强度较之正常区域弱.     

Transmission electron microscopy and x-ray topography study of mercury-cadmium-telluride

The fault structure of MCT crystals was studied by means of X-ray topography and transmission electron microscopy. Subgrain boundaries were revealed and identified by both techniques, and their tilt angle was calculated to be of the order of 10^-3 rad. The dislocations which form the subgrain boundaries were identified by TEM to have Burger‘s vectors parallel to the <110> directions. Twins in large numbers were observed by TEM. The twins were identified to have a {111} habit plane.     

Grain growth simulation of [001] textured YBCO films grown on (001) substrates with large lattice misfit: Prediction of misorientations of the remaining boundaries

We study the effects of (1) the variation of grain boundary energy with misorientation and (2) the large lattice misfit (>3%) between the films and substrates on grain growth in films by method of Monte Carlo simulations. The results from the grain growth simulation in YBa₂Cu₃O_7-x (YBCO) films was found to concur with previous experimental observation of preferred grain orientations for YBCO films deposited on various substrates such as (001) magnesium oxide (MgO) and (001) yttria stabilized zirconia (YSZ). The simulation has helped us to identify three factors influencing the competition of these [001] tilt boundaries. They are: (1) the relative depths of local minima in the boundary energy vs. misorientation curve, (2) the number of combinations of coincidence epitaxy (CE) orientations contributing to the exact misorientation for each of the high-angle-but-low-energy (HABLE) boundaries, and (3) the number of combinations of CE orientations within the angular ranges bracketing each of the exact HABLE boundaries. Hence, these factors can be applied to clarify the origin of special misorientations observed experimentally.     

Grain boundary segregation in multicrystalline silicon: correlative characterization by EBSD,EBIC, and atom probe tomography

This study aims to better understand the influence of crystallographic structure and impurity decoration on the recombination activity at grain boundaries in multicrystalline silicon. A sample of the upper part of a multicrystalline silicon ingot with intentional addition of iron and copper has been investigated. Correlative electron‐beam‐induced current, electron backscatter diffraction, and atom probe tomography data for different types of grain boundaries are presented. For a symmetric coherent Σ3 twin boundary, with very low recombination activity, no impurities are detected. In case of a non‐coherent (random) high‐angle grain boundary and higher order twins with pronounced recombination activity, carbon and oxygen impurities are observed to decorate the interface. Copper contamination is detected for the boundary with the highest recombination activity in this study, a random high‐angle grain boundary located in the vicinity of a triple junction. The 3D atom probe tomography study presented here is the first direct atomic scale identification and quantification of impurities decorating grain boundaries in multicrystalline silicon. The observed deviations in chemical decoration and induced current could be directly linked with different crystallographic structures of silicon grain boundaries. Hence, the current work establishes a direct correlation between grain boundary structure, atomic scale segregation information, and electrical activity. It can help to identify interface–property relationships for silicon interfaces that enable grain boundary engineering in multicrystalline silicon. Copyright © 2015 John Wiley & Sons, Ltd.     

Connection structures between type-I and type-II defects in neutron irradiated beta-Si3N4

High-resolution electron microscopy (HREM) observation clarified that various types of interstitial dislocations were induced into beta-Si3N4 by high-dose neutron irradiation, and two of them have been analysed and reported in our previous papers. These two defective structures are called type-I and type-II. They are interstitial dislocation loops introduced into [100] and [110] planes, respectively. In this study, it was found that some of these dislocation loops connected with each other. The connections of type-I-L2-type-II-B and type-I-R2-type-II-A dislocations were observed by HREM. Tetrahedral arrangements of the connected parts are proposed, based on the simplified crystal structure model of beta-Si3N4. In addition, a new type of defect, type-III, was found. Type-III is an interstitial dislocation loop introduced into [100] planes. It was also found that type-I-A and type-III dislocations connected with each other.     

利用EBSD技术对690合金不同类型晶界处碳化物形貌的研究

利用扫描电子显微镜（SEM）、电子背散射衍射（EBSD）技术和取向成像显微（OIM）软件研究了Ni基690合金中不同类型晶界处碳化物的形貌。不同类型晶界处析出碳化物的形貌有很大区别,在孪晶的非共格界面（Σ3i）附近,棒状碳化物向两侧晶粒内部生长,而类似的棒状碳化物只向Σ9晶界一侧的晶粒内部生长。Σ3i与Σ9晶界附近的棒状碳化物的生长方向与基体晶粒的{111}面平行。晶界上析出的碳化物尺寸随着Σ值的升高而明显增大。在相同的腐蚀条件下,晶间腐蚀的痕迹随着Σ值的升高变得严重。     

大马士革铜互连线织构的研究

采用EBSD研究了不同线宽和退火前后Cu互连线的织构和晶界特征分布.Cu互连线均具有多重织构,其中(111)织构强度最高.沉积态样品在室温下发生了自退火现象,并出现了一些异常长大的晶粒.随高宽比降低和退火处理,Cu互连线晶粒尺寸变大,(111)织构得到加强,而具有较低应变程度的织构与(111)织构强度的比例下降.沉积态样品出现了(111)<112>和(111)<231>织构组分.退火后,出现了(111)<110>组分,而且(111)<112>和(111)<231>组分得到增强.Cu互连线以大角度晶界为主,其中具有55°～60°错配角的晶界和∑3晶界比例最高,35°～40°的错配角和∑9晶界次之.随高宽比增加和退火处理,∑3晶界比例逐渐升高,∑9晶界比例下降.     

Local textures and grain boundaries in voided copper interconnects

We have characterized grain boundary structures and local textures in stress voided copper lines. Grain boundary misorientations as well as the tilt and twist character of boundaries were measured using electron backscatter diffraction in the scanning electron microscope in conjunction with focused ion beam images. We have summarized data for a number of boundaries immediately adjacent to voids and made comparisons to boundaries from regions that remained intact. These data were acquired from the same lines, and so represent measurements from material with identical histories. Significant local variations in microstructure were observed. Local <111> textures of grains near voids were of lower strength than those away from voids. Grain boundaries intersecting voids were of higher angle character and had significant twist components. These results suggest that local regions associated with more favorable kinetics are more susceptible to void formation and growth.     

Electron transport behaviour in Nb-doped SrTiO3 bicrystals

In order to elucidate the relationship between electron transport behaviour and defect chemistry, grain boundary structure and current-voltage characteristics across the boundary were investigated for Nb-doped SrTiO3 bicrystals. Two kinds of boundaries, i.e. small angle and random boundaries, were prepared for 0.2at% and 1.0at% Nb-doped SrTiO3. The bicrystals were prepared by joining two single crystals at 1400 degrees C for 10 h under a pressure of 0.4 MPa in air. High-resolution transmission electron microscopy (HRTEM) study revealed that all of the joined boundaries are free from any secondary phases or amorphous films. On the other hand, it was found that non-linearity in current-voltage dependence becomes remarkable by reduction of cooling rate after joining in small angle boundaries of 0.2at% Nb-doped SrTiO3 bicrystal. In addition, the random boundary of 1.0at% Nb-doped SrTiO3 bicrystal exhibits clear alpha = 2 I-V relation, which appears across a contact of semiconductor-insulator-semiconductor (n-i-n). From the results of HRTEM study and I-V behaviours, it could be concluded that the electron transport mechanism is controlled mainly by defect chemistry and not by the grain boundary structure.     

Identification of crack path of inter- and transgranular fractures in sintered silicon nitride by in situ TEM

Inter- and/or transgranular crack paths in sintered silicon nitride (Si3N4) during fracture were investigated by in situ straining experiments in a transmission electron microscope at room temperature, using a high-precision micro-indenter. By this technique, cracks introduced in an in situ manner were observed to propagate in the grain interior and along grain boundaries. High-resolution electron microscopy (HREM) observation revealed that the crack propagation takes place at an interface between Si3N4 grains and an intergranular glassy film (IGF) in the case of intergranular fractures. According to the results by previous molecular dynamics simulations, a number of dangling bonds are present at the Si3N4/IGF interface, which should result in the observed fracture behavior at the interface. On the other hand, the crack path introduced during transgranular fracture of Si3N4 grains was found to be sharp and straight. The observed crack propagated towards [1120] inside the Si3N4 grain with the crack surface parallel to the (1100) plane. The HREM observations of crack walls revealed them to be atomically flat. The atomic termination of the crack walls was identified in combination with image simulations based on atomic models of the cleaved crack walls.     

Effect of film thickness on the evolution of annealing texture in sputtered copper films

Microstructural evolution during elevated temperature annealing of sputter deposited copper (Cu) films was investigated by electron backscatter diffraction (EBSD). Analysis of films was performed both in situ using a heating stage, and by ex-situ observation of microstructural evolution. It was noted that not only is the Cu film texture and grain size a function of film thickness, but also that the fraction of twin boundaries present in the material is strongly dependent upon film thickness. This is explained by means of a simple model that considers the energy of the system. Surface and interface energies, as well as grain boundary energies for random high angle boundaries and for twin boundaries (both coherent and incoherent planes) are used in the determination. The model was shown to accurately predict the twin boundary size in self-annealed films. This type of analysis also results in a texture map similar to that presented by Thompson,¹² but incorporates the development and effect of twin boundaries, so that additional texture components (in addition to 111 and 100 fibers) are included.     

Raney合金中NiAl3相在脱铝过程中结构的转变

ａｎｅｙ催化剂由纳米级镍晶粒、未转变的ＮｉＡｌ３和Ｎｉ２Ａｌ３母相以及包围着它们的界面区组成。Ｘ射线衍射和高分辨电子显微镜观察发现，在脱铝过程中，ＮｉＡｌ３晶粒碎裂为纳米级尺寸，而Ｎｉ２Ａｌ３相则不出现这现象。     

Suppression of twin formation in CdTe(111)B epilayers grown by molecular beam epitaxy on misoriented Si(001)

CdTe(lll)B layers have been grown on misoriented Si(001). Twin formation inside CdTe(lll)B layer is very sensitive to the substrate tilt direction. When Si(001) is tilted toward [110] or [100], a fully twinned layer is obtained. When Si(001) is tilted toward a direction significantly away from [110], a twin-free layer is obtained. Microtwins inside the CdTe(111)B layers are overwhelmingly dominated by the lamellar twins. CdTe(111)B layers always start with heavily lamellar twinning. For twin-free layers, the lamellar twins are gradually suppressed and give way to twin-free CdTe(111)B layer. The major driving forces for suppressing the lamellar twinning are the preferential orientation of CdTe[11-2] along Si[1-10] and lattice relaxation. Such preferential orientation is found to exist for the CdTe(111)B layers grown on Si(001) tilted toward a direction between [110] and [100].     

EBSD研究取向硅钢晶粒取向和晶界结构

采用扫描电镜结合EBSD技术分析了取向硅钢初次再结晶晶粒的取向和晶界结构。初次再结晶晶粒中以30°～55°的大角晶界为主,Goss取向晶粒含量小于5%,且经常生长在（111）〈112〉取向的晶粒周围。同时测定了二次再结晶晶粒的实际取向,并计算出与Goss取向的取向差关系。     

Performance dependence of CMOS on silicon substrate orientation for ultrathin oxynitride and HfO/sub 2/ gate dielectrics

Dependence of CMOS performance on silicon crystal orientation of [100], [111], and [110] has been investigated with the equivalent gate dielectric thickness less than 3 nm. Hole mobility enhancement of /spl ges/160% has been observed for both oxynitride and HfO/sub 2/ gate dielectrics on [110] surfaces compared with [100]. CMOS drive current is nearly symmetric on [110] orientation without any degradation of subthreshold slope. For HfO/sub 2/ gate dielectrics, an approximately 68% enhancement of pMOSFET drive current has been demonstrated on [110] substrates at L/sub poly/=0.12 /spl mu/m, while current reduction in nMOS is around 26%.     

低维纳米材料中五次孪晶结构的透射电镜研究

本文对Ag纳米线中的五次孪晶结构进行了深入系统的透射电镜研究。首次获得了Ag纳米线截面的五次孪晶结构的高分辨图像和电子衍射花样;研究了单根孪晶Ag纳米线中五次孪晶的结构特性。结果表明:Ag纳米线沿着[110]方向生长,具有显著的五次孪晶结构特点,其中五次孪晶是由五个{111}晶体旋转组成。并针对五重旋转孪晶产生7°20′本征间隙的这一典型结构问题,进行了统计实验分析,提出了纳米线中五次孪晶的新的结构模型。电子能量损失谱(EELS)研究表明:五次孪晶的中心部位相对于Ag单晶,其Ag M4,5峰向低能量方向有轻微漂移。单根纳米线的选区电子衍射或者是由[112]和[110]方向,或者是由[110]和[111]方向叠加产生的。对五次孪晶纳米线高温动态行为的透射电镜原位观察将有利于了解纳米线的生长机理。     

Ordering in InGaAs/InAlAs layers

The structure of InCaAs/InAlAs layers lattice matched to an InP substrate, grown on either (100) or on (110) with a 4° tilt toward [111] at 500 and 300°C has been investigated by transmission electron microscopy. High perfection resulted for the layers grown on [001] oriented substrates whereas growth on the near [110] substrates resulted in compositional nonuniformities, macrosteps formation, and ordering of the group III elements. This difference in structural perfection between the two sets of samples was also reflected in differences in electrical properties.     

原子探针层析方法研究690合金晶界偏聚的初步结果

利用脉冲电解抛光的方法制备了含有晶界的三维原子探针（3DAP）针尖样品,用原子探针层析方法（APT）研究了杂质原子在690合金晶界附近的偏聚情况。结果表明：样品经过固溶处理并在500℃～0.5 h时效后,碳化物仅在部分有利于形核的晶界位错纠结处析出,大小为5～10 nm。用三维原子探针可观察到晶界处杂质原子的偏聚现象,C主要偏聚在晶界附近1个原子层内,Si和P偏聚在晶界附近约2个原子层的厚度内。根据这些元素的偏聚数据,讨论了它们发生偏聚时的规律。