Using transmission Kikuchi diffraction to characterise α variants in an α+β titanium alloy

Two phase titanium alloys are important for high‐performance engineering components, such as aeroengine discs. The microstructures of these alloys are tailored during thermomechanical processing to precisely control phase fractions, morphology and crystallographic orientations. In bimodal two phase (α + β) Ti‐6Al‐2Sn‐4Zr‐2Mo (Ti‐6242) alloys there are often three microstructural lengthscales to consider: large (～10 μm) equiaxed primary α; >200 nm thick plate α with a basketweave morphology; and very fine scaled (<50 nm plate thickness) secondary α that grows between the larger α plates surrounded by retained β. In this work, we utilise high spatial resolution transmission Kikuchi diffraction (TKD, also known as transmission‐based electron backscatter diffraction, t‐EBSD) and scanning electron microscopy (SEM)‐based forward scattering electron imaging to resolve the structures and orientations of basketweave and secondary α in Ti‐6242. We analyse the α variants formed within one prior β grain, and test whether existing theories of habit planes of the phase transformation are upheld. Our analysis is important in understanding both the thermomechanical processing strategy of new bimodal two‐phase titanium alloys, as well as the ultimate performance of these alloys in complex loading regimes such as dwell fatigue. Our paper champions the significant increase in spatial resolution afforded using transmission techniques, combined with the ease of SEM‐based analysis using conventional electron backscatter diffraction (EBSD) systems and forescatter detector (FSD) imaging, to study the nanostructure of real‐world engineering alloys.     

Effect of heat treatment and number of passes on the microstructure and mechanical properties of friction stir processed AZ91C magnesium alloy

In this paper, the effect of heat treatment and number of passes on microstructure and mechanical properties of friction stir processed AZ91C magnesium alloy samples were investigated. From six samples of as-cast AZ91C magnesium alloy, three plates were pre-heated at temperature of 375°C for 3 hours, and then were treated at temperature of 415°C for 18 hours and finally were cooled down in air. Three plates were relinquished without heat treatment. 8 mm thick as-cast AZ91C magnesium alloy plates were friction stir processed at constant traverse speed of 40 mm/min and tool rotation speed of 1250 rpm. After process, microstructural characterization of samples was analyzed using optical microscopy and tensile and Vickers hardness tests were performed. It was found that heat treated samples had finer grains, higher hardness, improved tensile strength and elongation relative to non-heat treated ones. As the number of passes increased, higher UTS and TE were achieved due to finer grains and more dissolution of β phase (Mg₁₇Al₁₂). The micro-hardness characteristics and tensile improvement of the friction stir processed samples depend significantly on grain size, removal of voids and porosities and dissolution of β phase in the stir zone.

     

电子束熔丝增材制造TC11钛合金组织及力学性能

采用电子束熔丝增材工艺制造了直径260 mm的试环。分析了不同热处理状态的增材制造TC11钛合金微观组织和室/高温拉伸性能及其各向异性。并测试分析了锻件基体晶粒2次热处理和锻件基体与增材界面处的组织和性能。结果表明：沉积态微观组织为沿<001>β方向生长的柱状晶。晶界存在连续α相，晶体内部由集束和网篮α相组成的片层组织。经950℃/2h/空冷+530℃/6h/空冷的热处理后晶界连续α相破碎，晶内α相宽度从1.1μm增加至1.8μm。并形成具有二次α相的双片层组织。锻件与增材过渡区锻件一侧，等轴初生α相转变为“雪花”状初生α相。锻件基体2次热处理后等轴初生α相轮廓光滑，转变β相比例增加，并形成大量细小的针状二次α相。沉积态室温及500℃高温拉伸性能均具有明显的各向异性。经过热处理后室/高温拉伸性能均获得改善并高于锻件要求且各向异性明显降低。与沉积态相比，热处理态室温抗拉强度和断后伸长率各向异性分别从4.4%和27.1%降低至1.6%和5.4%。柱状晶及其晶界连续α相是引起塑性各向异性的原因。锻件+增材界面处热处理后其室/高温拉伸性能均满足锻件要求。     

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.     

Energy dispersive spectroscopy analysis of aluminium segregation in silicon carbide grain boundaries

The aluminium distribution in polycrystalline SiC hot‐pressed with aluminium, boron and carbon additives was studied using X‐ray energy‐dispersive spectroscopy (EDS) and transmission electron microscopy (TEM). The Al excess in homophase SiC grain boundary films was determined, taking into account dissolved Al in the SiC lattice. In the spot‐EDS analysis, an electron beam probe with a calibrated diameter was formed, and the total beam–specimen interaction volume was defined, taking the beam spreading through crystalline TEM foil into consideration. EDS spectra were collected from regions containing intergranular films and adjacent matrix grains, respectively. A theoretical treatment was presented and experimental errors were estimated, with a further discussion about the effects of foil thickness. Experimental examples are given, followed by statistical EDS analyses for grain boundary films in SiC samples hot‐pressed with increased amounts of Al additions. The results demonstrated a substantial Al segregation in the nanometer‐wide intergranular films in all samples. Al additions higher than 3 wt% saturated the Al concentrations in SiC grains and in grain boundary films. The effect of foil thickness, and the parameters for determining the optimum incident beam diameter in the EDS analysis are discussed.     

On the orientations of abnormally grown grains in nanocrystalline Ni and Ni–Fe

The scanning electron microscopy–based electron backscatter diffraction technique has been used to determine grain orientations of abnormally grown grains upon annealing in nanocrystalline Ni and Ni–20 at.% Fe electrodeposits. The results show that in nanocrystalline Ni and Ni–Fe, the first grown grains that can be detected are 〈411〉 oriented with respect to the normal direction (〈411〉//ND). Upon annealing, further grain growth occurs and the dominant orientation of the abnormally growing grains changes from 〈411〉//ND to 〈111〉//ND. Twinning is found to be the mechanism responsible for the orientation change and is for the first time described in connection with abnormal grain growth in nanocrystalline materials. This means that well‐known models for the formation of annealing twins (initially introduced in connection with recrystallization) also seem to apply in nanocrystalline materials.     

Effect of friction stir processing parameters on the microstructural and electrical properties of copper

Friction stir processing (FSP) is an innovative technology, based on friction stir welding (FSW) operative principles, which can be used for changing locally the microstructure and the mechanical properties of conventional materials. In this work, the copper alloy C12200 was friction stir processed using two distinct tools, i.e. a scrolled and a conical shoulder tool, in order to promote different thermomechanical conditions inside the stirred volume, and consequently, varied post-processed microstructures. The influence of the tool geometry and tool rotation and traverse speeds on the microstructural and electrical properties of the processed copper alloy was analysed. The processing conditions were found to have an important influence on the electrical conductivity of the processed material. The differences in electrical conductivity were explained based on dislocations density effects. The effect of the dislocations density on electrical conductivity of the processed material was found to prevail over the effect of the grain boundaries.     

Transmission electron microscopy of fluorapatite–gelatine composite particles prepared using focused ion beam milling

In this paper, synthetic fluorapatite–gelatine composite particles are prepared for transmission electron microscopy (TEM) studies using two methods based on focused ion beam (FIB) milling. TEM studies on the FIB‐prepared specimens are compared with TEM observations on samples prepared using an ultramicrotome. The results show that ultramicrotome slicing causes significant cracking of the apatite, whereas the ion beam can be used to make high‐quality, crack‐free specimens with no apparent ion beam‐induced damage. The TEM observations on the FIB‐prepared samples confirm that the fluorapatite composite particles are composed of elongated, preferentially orientated grains and reveal that the grain boundaries contain many small interstices filled with an amorphous phase.     

搅拌摩擦加工次数对AZ91D镁合金组织的影响

研究了搅拌摩擦加工(FSP)次数对AZ91D镁合金组织的影响.结果表明:加工次数对搅拌摩擦区晶粒大小影响不大;但加工次数多可增加搅拌摩擦区组织的面积,并使组织均匀化;使热机械影响区组织向搅拌摩擦区组织发生转变;增大轴肩下压区细晶组织面积,进一步细化轴肩下压区的晶粒.     

Microstructural characterization of nitrided Timetal 834

The microstructure of Timetal 834, in as‐received condition and after nitriding under glow discharge has been examined by light microscopy and analytical transmission electorn microscopy (TEM) methods (SAED, EDS, EELS and EFTEM). The microstructure of the as‐received alloy consists of the α phase and a small amount of the β phase. Silicide precipitates (Zr₅Si₄) are present both inside the grains and at the grain boundaries. TEM investigations of cross‐sectional thin foils allow for detailed analysis of the nitrided layer microstructure. It was found that the nitrided layer exhibits a graded character with continuously varying nitrogen content. The outermost sublayer consists of nanocrystals of δ‐TiN. The following sublayers consist mainly of δ′‐Ti₂N and ?‐Ti₂N grains. The last sublayer, closest to the substrate, is identified as a nitrogen‐rich α(N) solid solution containing up to 14 at% of nitrogen.     

Influence of substrate orientation on the morphologyand orientation of LaNiO3 thin films

LaNiO₃ thin films were successfully prepared by a chemical method from citrate precursors. The LNO precursor solution was spin‐coated onto Si (100) and Si (111) substrates. To obtain epitaxial or highly oriented films, the deposited layers were slowly heated in a gradient thermal field, with a heating rate of 1° min^?1, and annealed at 700°C. The influence of different substrate orientations on the thin film morphology was investigated using atomic force microscopy and X‐ray diffraction analysis. Well‐crystallized films with grains aligned along a certain direction were obtained on both substrates. Films deposited on both substrates were very smooth, but with a different grain size and shape depending on the crystal orientation. Films deposited on Si (100) grew in the (110) direction and had elongated grains, whereas those on Si (111) grew in the (211) direction and had a quasi‐square grain shape.     

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.     

Ti600/TC17钛合金惯性摩擦焊接头组织与力学性能研究

采用惯性摩擦焊方法对TC17和Ti600钛合金进行了连接,着重分析接头焊态和热处理条件下的组织特征与力学性能。接头焊态TC17一侧：在热力影响区原始β晶粒发生破碎,晶界以及晶内α相扭曲变形;在再结晶区β晶粒发生动态再结晶形成细小的等轴晶粒,晶内为亚稳态的β相;接头Ti600一侧：在热力影响区片层组织随着金属流动发生变形;在再结晶区,α片层团簇发生再结晶形成大量细小的α片层团簇片层。经过热处理后,TC17钛合金一侧亚稳态β相析出细小的层片状α相,Ti600钛合金一侧层状α相长大,但是不明显。热处理使接头的显微硬度升高,TC17钛合金焊缝一侧显微硬度增加明显。接头抗拉强度与Ti600母材相当,断裂发生在Ti600钛合金一侧,断口为典型的杯锥状断口。     

Investigation of fatigue crack initiation facets in Ti‐6Al‐4V using focused ion beam milling and electron backscatter diffraction

In the very high cycle fatigue regime, internal crack initiation can occur in Ti‐6Al‐4V because of the formation of facets, which are α grains that have fractured in a transcrystalline and planar manner. Because this crack initiation phase occupies most of the fatigue life, it is essential to understand which mechanisms lead to facet formation. Fatigue tests have been performed on drawn and heat‐treated Ti‐6Al‐4V wires, and the facets at internal crack initiation sites have been analysed in detail in terms of their appearance, their spatial orientation and their crystallographic orientation. The facets were not smooth, but showed surface markings at the nanoscale. In nearly all cases, these markings followed a linear pattern. One anomalous facet, in a sample with the largest grain size, contained a fan‐shaped pattern. The facets were at relatively steep angles, mostly between 50° and 70°. Cross‐sections of the fracture surfaces have been made by focused ion beam milling and were used to measure the crystallographic orientation of facets by electron backscatter diffraction. Most facet planes coincided with a prismatic lattice plane, and the linear markings were parallel to the prismatic slip direction, which is a strong indication that prismatic slip and slip band formation led to crack initiation. However, the anomalous facet had a near‐basal orientation, which points to a possible cleavage mechanism. The cross‐sections also exposed secondary cracks, which had formed on prismatic lattice planes, and in some cases early stage facet formation and short crack growth phenomena. The latter observations show that facets can extend through more than one grain, and that there is crack coalescence between facets. The fact that drawn wires have a specific crystallographic texture has led to a different facet formation behaviour compared to what has been suggested in the literature.     

Combining quantitative 2D and 3D image analysis in the serial block face SEM: application to secretory organelles of pancreatic islet cells

A combination of two‐dimensional (2D) and three‐dimensional (3D) analyses of tissue volume ultrastructure acquired by serial block face scanning electron microscopy can greatly shorten the time required to obtain quantitative information from big data sets that contain many billions of voxels. Thus, to analyse the number of organelles of a specific type, or the total volume enclosed by a population of organelles within a cell, it is possible to estimate the number density or volume fraction of that organelle using a stereological approach to analyse randomly selected 2D block face views through the cells, and to combine such estimates with precise measurement of 3D cell volumes by delineating the plasma membrane in successive block face images. The validity of such an approach can be easily tested since the entire 3D tissue volume is available in the serial block face scanning electron microscopy data set. We have applied this hybrid 3D/2D technique to determine the number of secretory granules in the endocrine α and β cells of mouse pancreatic islets of Langerhans, and have been able to estimate the total insulin content of a β cell.     

Crystal orientation mapping of NiO grown on cube textured Ni tapes

Samples of cube textured Ni tapes were oxidized in flowing oxygen at different temperatures. Crystal orientation maps (COMs) of the resulting oxide layers were produced by electron backscatter diffraction. The oxide layers were also analysed by X‐ray diffraction (XRD), scanning electron microscopy and atomic force microscopy (AFM). The oxide grain size of a sample oxidized at 600 °C was similar to that of the substrate and the oxide was highly textured, both indicating epitaxial growth. The orientation relationship between the substrate and the oxide was directly observed from XRD to be (111)_NiO//(001)_Ni, [01]_NiO//[110]_Ni with four, equivalent, in‐plane variants. In each variant, the oxide has both <110>‐ and <211>‐type directions parallel to the Ni <110> directions. Differences in oxide thickness and surface roughness on neighbouring grains were revealed by AFM and these were attributed to the existence of a range of oxide growth conditions resulting from small differences in the orientation of each substrate grain. Similar macrotexture and microstructure were observed on a sample oxidized at 1300 °C, but additional, facetted oxide crystals had formed at the oxide grain boundaries. COMs showed that these crystals were either cube or 45° rotated cube orientated, a texture different to that of the large oxide grains. The grain boundary crystals were thought to form by inward diffusion of oxygen at defects in the growing oxide scale.     

Effect of Ca addition on the microstructure and mechanical properties of as‐cast Mg–Sm alloys

This study investigated the effect of Ca addition on the microstructure and mechanical properties of as‐cast Mg–4Sm alloys. The addition of 1.0 wt% Ca led to a significant grain refinement of Mg–4.0Sm alloys owing to the formation of rod‐like Mg2Ca phases that acted as active nucleates for the Mg matrix. The as‐cast Mg–4.0Sm–1.0Ca alloy showed the smallest grain size at 45 μm. Furthermore, the Mg–4.0Sm–1.0Ca alloy exhibited greater hardness, higher tensile strength, and higher yield tensile strength and elongation than the other two alloys with different Ca contents. These results were attributed to the grain refinement and precipitation strengthening of the Mg2Ca and Mg41Sm5 phases. Microsc. Res. Tech. 79:707–711, 2016. © 2016 Wiley Periodicals, Inc.     

Fine structure characterization of martensite/austenite constituent in low‐carbon low‐alloy steel by transmission electron forward scatter diffraction

Transmission electron forward scatter diffraction and other characterization techniques were used to investigate the fine structure and the variant relationship of the martensite/austenite (M/A) constituent of the granular bainite in low‐carbon low‐alloy steel. The results demonstrated that the M/A constituents were distributed in clusters throughout the bainitic ferrite. Lath martensite was the main component of the M/A constituent, where the relationship between the martensite variants was consistent with the Nishiyama–Wassermann orientation relationship and only three variants were found in the M/A constituent, suggesting that the variants had formed in the M/A constituent according to a specific mechanism. Furthermore, the Σ3 boundaries in the M/A constituent were much longer than their counterparts in the bainitic ferrite region. The results indicate that transmission electron forward scatter diffraction is an effective method of crystallographic analysis for nanolaths in M/A constituents.     

On the role of cooling and tool rotational direction on microstructure and mechanical properties of friction stir processed AZ91

This paper deals with an experimental investigation focused on the effects of water cooling treatment, friction stir processing pass number, and tool rotational direction on the microstructure and mechanical properties of friction stir processed AZ91 magnesium alloy. Specimens were produced using different combinations of process parameters. Parallel to increasing the amount of oxide particles in the processed area, water cooling was found to reduce the final grain size and enhance their hardness and strength. Changing the rotational direction in each pass reduces the grain size severely (from 150 to ~4?μm) and increases the hardness (from 63 to 98?HV) and strength (from ~130 to ~250?MPa). However, no significant difference was found in wear resistance of the specimens produced with different process parameters.     

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.