Five-parameter grain boundary analysis of a grain boundary–engineered austenitic stainless steel

Two different grain boundary engineering processing routes for type 304 austenitic stainless steel have been compared. The processing routes involve the application of a small level of strain (5%) through either cold rolling or uni-axial tensile straining followed by high-temperature annealing. Electron backscatter diffraction and orientation mapping have been used to measure the proportions of Σ3ⁿ boundary types (in coincidence site lattice notation) and degree of random boundary break-up, in order to gain a measure of the success of the two types of grain boundary engineering treatments. The distribution of grain boundary plane crystallography has also been measured and analyzed in detail using the five-parameter stereological method. There were significant differences between the grain boundary population profiles depending on the type of deformation applied.     

Site-specific atomic scale analysis of solute segregation to a coincidence site lattice grain boundary

A site-specific method for measuring solute segregation at grain boundaries in an Aluminum alloy is presented. A Σ7(Σ7=38°〈1 1 1〉) grain boundary (GB) in an aluminum alloy (Zr, Cu as main alloying elements) was evaluated using site-specific Local Electrode Atom Probe (LEAP). A sample containing a Σ7 GB was prepared by combining electron backscatter diffraction (EBSD) and focused ion beam (FIB) milling to locate the GB of interest and extract a specimen. Its composition was determined by LEAP, and compared to a general high angle GB (HAGB). Zr was the only alloying element present in the Σ7 GB, whereas the general HAGB contained both Cu and Zr. This site-specific LEAP method was found to be an accurate method for measuring GB segregation at specific GB misorientations. The method has advantages over other methods of measuring chemistry at GBs, such as spectroscopy, in that GB structure can be assessed in three dimensions.     

'Five-parameter' analysis of grain boundary networks by electron backscatter diffraction

This paper describes state‐of‐the‐art analysis of grain boundary populations by EBSD, with particular emphasis on advanced, nonstandard analysis. Data processing based both on misorientation alone and customised additions which include the boundary planes are reviewed. Although commercial EBSD packages offer comprehensive data processing options for interfaces, it is clear that there is a wealth of more in‐depth data that can be gleaned from further analysis. In particular, determination of all five degrees of freedom of the boundary population provides an exciting opportunity to study grain boundaries by EBSD in a depth that was hitherto impossible. In this presentation we show ‘five‐parameter’ data from 50 000 boundary segments in grain boundary engineered brass. This is the first time that the distribution of boundary planes has been revealed in a grain boundary engineered material.     

Three-dimensional EBSD study on the relationship between triple junctions and columnar grains in electrodeposited Co–Ni films

Electrodeposited nanocrystalline materials are expected to have a homogeneous grain size and a narrow grain size distribution. In Co–Ni electrodeposited films, however, under certain conditions an undesired columnar grain structure is formed. Fully automated three‐dimensional (3D) orientation microscopy, consisting of a combination of precise material removal by focussed ion beam and subsequent electron backscatter diffraction (EBSD) analysis, was applied to fully characterize the grain boundaries of these columnar grains in order to gain further understanding on their formation mechanisms. Two‐dimensional orientation microscopy on these films indicated that the development of columnar grains could be related to the formation of low‐energy triple junctions. 3D EBSD allowed us to verify this suggestion and to determine the boundary planes of these triples. The triplets are formed by grain boundaries of different quality, a coherent twin on the {} plane, an incoherent twin and a large‐angle grain boundary. These three boundaries are related to each other by a rotation about the 〈〉 direction. A second particularity of the columnar grains is the occurrence of characteristic orientation gradients created by regular defects in the grain. Transmission electron microscopy was applied to investigate the character of the defects. For this purpose, a sample was prepared with the focussed ion beam from the last slice of the 3D EBSD investigation. From the TEM and 3D EBSD observations, a growth mechanism of the columnar grains is proposed.     

磷在2.25CrlMo钢中的非平衡晶界偏聚动力学实验

采用2.25Cr1Mo工业用钢,通过俄歇电子能谱分析方法(AES),对磷在1050℃固溶处理、540℃恒温保持过程中的非平衡晶界偏聚浓度进行了测试,获得了磷在钢中的非平衡晶界偏聚动力学曲线,该曲线直接验证了非平衡晶界偏聚动力学理论中的Xu-Song模型。     

Crystallographic analysis of facets using electron backscatter diffraction

Applications of electron backscatter diffraction (EBSD), also known as backscatter Kikuchi diffraction in the scanning electron microscope (SEM) are first and foremost microtexture and grain boundary misorientation analysis on a single polished section in the specimen. A more subtle and revealing approach to analysis of these data is to use EBSD to probe the orientations of planar surfaces, i.e. facets, which bound crystals. These surfaces include: • grain or phase boundaries • fractures • cracks It is of great interest to know the crystallography of such facets since it provides a key to understanding the physical properties of them.
As far as investigation methodology is concerned, surfaces or facets associated with polycrystals are of two types: exposed or unexposed. Exposed facets, such as a fracture surface, can be viewed directly in the SEM, whereas unexposed facets, such as a grain boundary, are usually revealed as an etched trace on a polished surface. Photogrammetric methods can be used to obtain the positional orientation of an exposed facet, and the crystallographic orientation is obtained either directly from the surface or by indirect sectioning. Calibrated sectioning is required to obtain the equivalent parameters for an internal surface. The present paper compares the methods for obtaining and interpreting the crystallography of facets, with illustrations from several materials.     

采用电子背散射衍射技术研究变形温度对压缩后1235铝合金织构的影响

采用电子背散射衍射技术对经不同温度热压缩后1235铝合金的织构进行了研究,分析了在50%变形量、0.1s-1应变速率下,变形温度对该合金晶粒取向、晶界特征及织构组分的影响。结果表明:随着变形温度的升高,织构的取向聚集性弱化,织构相对体积总含量降低,晶粒内小角度晶界更稀疏,大角度晶界更加平直且连通性好,再结晶晶粒长大更充分。     

纳米碳化硅颗粒强化氧化铝基陶瓷材料机理的研究现状

综述和分析了纳米碳化硅颗粒强化氧化铝基陶瓷材料的强韧化机制,认为由沿晶断裂到穿晶断裂的断裂模式的改变不是使复相陶瓷材料强韧化的机制之一,而恰恰是其韧性得不到显著提高的重要原因,并由此提出了有关复相材料新的设计思路。     

化工机械设备地脚螺栓断裂失效分析

某化工设备地脚螺栓在运行过程中发生断裂,通过对断裂螺栓采用化学成分分析、断口形貌分析、金相组织分析、扫描电镜、显微硬度分析等方法分析了其断裂原因。一系列分析表明,正常断裂与异常断裂螺栓在化学成分、显微硬度、金相组织等方面没有明显差异,说明这些均不是造成螺栓异常断裂的主要原因;正常断裂与异常断裂微观断口形貌分析结果表明,螺栓芯部出现偏聚现象,螺栓在调质高温回火的过程中,发生偏聚继而导致了疲劳裂纹的萌生及扩展,最终引发螺栓断裂。     

压缩机2Cr13活塞杆亚温淬火工艺及其弯曲问题的研究

2Cr13活塞杆经过亚温淬火、回火调质后,采用580℃保温3～4h空冷或炉冷的稳定化工艺,基本上可以消除应力,并且没有明显的第二类回火脆性的产生,从而保证了2Cr13活塞杆高频淬火时减小弯曲量,避免感应器放电现象熔化活塞杆。     

Analysis of ceramic materials by electron spectroscopy

The basic principles of X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy are described and their relative advantages as analysis methods for ceramic materials are reviewed. Their application in ceramics technology is illustrated by examples taken from the fields of catalysis and mineralogy. In particular, attention is drawn to recent developments of XPS which make it especially attractive for the study of ceramic materials. These include quantitative application of the X-ray photoelectron diffraction effect to layered, single crystal minerals; the development of higher energy X-ray sources for XPS, and the attendant study of the Sils–KLL Auger parameter as a probe of molecular and crystalline structure; and the analysis of small (?250 μm) surface features by XPS.     

In situ observation of intergranular crack nucleation in a grain boundary controlled austenitic stainless steel

Grain boundary engineering has been proposed to increase the lifetime performance of sensitized austenitic stainless steel in aggressive environments. Increased microstructure resistance is typically associated with higher fractions of twin (Σ3) grain boundaries, but there is uncertainty about the properties and role of other boundaries. To develop predictive models for stress corrosion crack nucleation, more information is required about how grain boundary crystallography and the orientations of the grain boundary plane and its surrounding grains affect crack development. Digital image correlation combined with electron backscatter diffraction has been used to characterize the microstructure and to observe, in situ , the nucleation and propagation of short stress corrosion cracks in thermo-mechanically processed type 304 stainless steel. The crack path and its growth rate have been determined and are found to be influenced by the microstructure.