Structure and role of the interfacial layers in VC-rich WC-Co cermets

The microstructure of WC-Co composites sintered with VC or with a mixture of VC and Cr₃C₂ is investigated by several techniques in order to understand the grain growth inhibition process. In this work, using the high-resolution transmission electron microscopy and high-resolution energy-filtering electron microscopy, we are able to study on the atomic scale the microstructure and composition of the phases present in the alloys. A thin (VW)C _x layer less than 1 nm thick covering all surfaces of WC grains and thin (VW)C _x platelets embedded in the WC grains are evidenced. Microsteps are observed at the interface between Co and WC along the ?11amp;2macr;0?_WC directions. Small (VW)C _x precipitates lie on the (0001)_WC and {10amp;1macr;0} facets of these steps. On the (0001) surface of WC grains, other stacking sequences of the metal planes are sometimes observed and, in particular, the occurrence of the compound (VW)₂C is shown. Owing to these observations a grain growth inhibition mechanism is proposed.     

Control of grain boundary microstructures in molybdenum polycrystals by thermomechanical processing of single crystals

The formation of grain structures and grain boundary microstructures in polycrystalline molybdenum, produced by thermomechanical processing from cylindrical single crystals with different initial surface normal orientations of ?110?, ?111? and ?112?, were investigated with the objective of controlling grain boundary microstructures. The polycrystalline specimens displayed different microstructures depending on the initial orientation of the single crystal and the deformed microstructure. The recrystallized microstructure was composed of some oriented-grain clusters, in which grains possessing a similar orientation were assembled. The frequency of low-angle boundaries was very high in the oriented-grain clusters. A close relationship also existed between the grain boundary character distribution (GBCD) and the triple junction distribution. Grain boundary microstructures were compared of bcc molybdenum and fcc polycrystalline materials with reference to path-dependent percolation resistance.     

Twinning structure of M23C6 carbide precipitated at twin-related grain boundaries in Alloy 600

The microstructure features of carbides precipitated at twin boundary and Σ9 grain boundary (GB) in nickel-based Alloy 600 after aging at 715?°C for different time were investigated by high-resolution transmission electron microscopy. The carbides precipitated at incoherent twin boundary and Σ9 GB were identified as M₂₃C₆. The bar-like carbides grow parallel to each other and into each side of grain nearby incoherent twin boundary, while only growth into one side nearby Σ9 GB is observed. The carbides precipitated at incoherent twin and Σ9 GBs contain twins. The carbides have (1?1?1) _matrix // (1?1?1) _M23C6 orientation relationship with the nearby matrix. Based on the experimental results, the formation of twinning microstructure features in the M₂₃C₆ is discussed.     

Accommodation of the Lattice Mismatch at the VCx-WC Interface

A VC doped WC-Co alloy is investigated using high resolution transmission electron microscopy. The VC grain growth inhibitor induces the presence of a thin layer on the surfaces of the WC grains in contact with Co and precipitates in the corners of Co pockets. These (VW)C_x compounds adopt an epitaxial orientation relationship with regards to the (0001) base facets of the WC crystals. Due to the small difference in lattice parameters, misfit dislocations are expected in the interfaces. Unlike the thin layers where no defects are observed, two kinds of dislocations are pointed out for larger precipitates. 1/6〈112〉_VC interfacial dislocations are sometimes present while more often 1/2〈1¯10〉_VC dislocations lying above the interface in the (VW)C_x phase are visible.     

Ordering and grain growth of FePt thin films by annealing

Microstructure variation of FePt thin film upon annealing at elevated temperatures was investigated by transmission electron microscopy (TEM). A special shape aperture was employed to observe the ordered L1₀ phase in the dark-field TEM images. With increasing the annealing temperature, crystal grains formed clusters with gathering of neighboring grains, and crystal grain growth proceeded within the cluster. L1₀ ordered crystal grains were preferentially formed near the grain boundaries, and their sizes grew with increasing the annealing temperature.     

The deformation of B4C particle in the B4C/2024Al composites after high velocity impact

In the present work, B₄C/2024Al composites with volume fraction of 45% were prepared by a pressure infiltration method. The microstructure of the crater bottom of B₄C/2024Al composite after impact was characterized by transmission electron microscope (TEM), which indicated that recovery and dynamic recrystallization generated in Al matrix, and the grain size distribution was about from dozens of nanometer to 200 nm. Furthermore, the plastic deformation was observed in B₄C ceramic, which led to the transformation from monocrystal to polycrystal ceramic grains. The boundary observed in this work was high-angle grain boundary and the two grains at the boundary had an orientation difference of 30°.     

The formation of α at triple junctions of parent β phase in titanium alloys

We have examined the formation of α phase at grain boundary triple junctions of parent β in a metastable β titanium alloy with orientation imaging microscopy based on electron backscattered diffraction (EBSD). As in the case of α formed at grain boundaries of parent β grains, α at a triple junction also forms with the Burgers orientation relationship with one of the three neighbouring β grains. The experimental results are analyzed in terms of the deviation of the 36 possible α variants that can form at a triple junction from the Burgers orientation relationship with neighbouring grains.     

Structure of ultradisperse diamonds

The structure of crystallites (regions of coherent scattering — RCS), which comprise the grains of ultradisperse diamond (UDD) powder, was investigated by x-ray crystallography and coordination-sphere diffractometry. It was established that the RCS have an average size $\bar L = 42 \pm 2{\AA}$ and that these regions are themselves UDD grains with the structure of a diamond lattice and a negligible content of clusters of carbon atoms distributed throughout the volume that do not form a lattice and are mainly located at interatomic distances ～1.5 Å. The clusters of carbon atoms, for which the distribution of interatomic distances is close to Gaussian, which may indicate an amorphous structure of the boundary layers, lie along grain boundaries.     

Analysis of slip activity and heterogeneous deformation in tension and tension-creep of Ti–5Al–2.5Sn (wt %) using in-situ SEM experiments

The deformation behavior of a Ti–5Al–2.5Sn (wt %) near-α alloy was investigated during in-situ deformation inside a scanning electron microscope. Tensile experiments were performed at 296?K and 728?K (≈0.4?T _m), while tensile-creep experiments were performed at 728?K and 763?K. Active deformation systems were identified using electron backscattered diffraction-based slip trace analysis. Both basal and prismatic slip systems were active during the tensile experiments. Basal slip was observed for grains clustered around high Schmid factor orientations, while prismatic slip exhibited less dependence on the crystallographic orientation. The tension-creep experiments revealed less slip but more development of grain boundary ledges than in the higher strain rate tensile experiments. Some of the grain boundary ledges evolved into grain boundary cracks, and grain boundaries oriented nearly perpendicular to the tensile axis formed ledges earlier in the deformation process. Grain boundaries with high misorientations also tended to form ledges earlier than those with lower misorientations. Most of the grain boundary cracks formed in association with grains displaying hard orientations, where the c-axis was nearly perpendicular to the tensile direction. For the tension-creep experiments, pronounced basal slip was observed in the lower-stress creep regime and the activity of prismatic slip increased with increasing creep stress and temperature.     

掺杂立方氮化硼对金刚石聚晶致密化和显微结构的影响

 以小于0.5 μm的金刚石和氮化硼（以下简称cBN）微粉为原料,在6.0 GPa和1 450～1 480 ℃保温30 min的工艺条件下,成功地烧结出晶粒尺寸小于1 μm、以WC/Co硬质合金为衬底的金刚石聚晶。研究了cBN掺杂对金刚石基质密实化和显微结构的影响。研究表明,cBN可以有效地抑制金刚石异常长大。细晶而且致密的金刚石聚晶有优异的力学性能。     

Grain Boundary Junctions in Microstructure Generated by Multiple Twinning

The microstructure of a Cu-Ni alloy after static recrystallization was investigated using electron backscatter diffraction in a scanning electron microscope and the existence of orientationally related clusters of crystallites formed by multiple twinning has been established. Grain boundary and triple junction character within the clusters are analyzed. While the outer boundaries of the cluster are crystallographically random, all the inner boundaries have 3 ⁿ misorientations. A newly developed crystallographic theory of triple junctions and multicrystallite ensembles consisting of CSL boundaries is used to describe the structure of the cluster. The presence of an 1 triple junction is confirmed. Apparently, the microstructure of recrystallized materials susceptible to annealing twinning consists of multiple-twinned clusters. The cluster size cannot be reduced to the grain size excluding twins.     

Effect of microstructure on the coercivity of HDDR Nd-Fe-B permanent magnetic alloy

The effect of the grain boundary microstructure on the anisotropy and coercivity was investigated in an HDDR Nd-Fe-B permanent magnetic alloy. Considering the special microstructure of its magnetic powder grain, an anisotropic theoretical model influenced simultaneously by the structure defect at the grain boundary and the exchange coupling interaction was put forward. The variations of the structure defect factors based on the nucleation and pinning mechanism with 2r ₀/lex (where r ₀ and lex are the defect thickness and the length of exchange coupling, respectively) were calculated. The results show that the coercivity mechanism of an HDDR Nd-Fe-B permanent magnetic alloy is greatly related to its microstructure defect at the grain boundary. For a fixed lex, when 2r ₀/lex < 1.67, the coercivity is controlled by the pinning mechanism; when 2r ₀/lex > 1.67, it is determined by the nucleation mechanism. The coercivity reaches the maximum when 2r ₀/lex = 1.67. The calculation result is consistent well with the experimental result given by Morimoto et al. Supported by the National Natural Science Foundation of China (Grant No. 50671055)     

Nanoparticle dispersion effect of laser-surface melting in ZrB<Subscript>2p</Subscript>/6061Al composites

Zirconium diboride (ZrB_2p, 15 vol%)/6061 aluminum (Al) composites were fabricated via in situ reaction. The existence, morphologies, and dispersion degree of the in situ ZrB₂ particles with size from tens to hundreds of nanometers were studied by X-ray diffractometry, energy-dispersive X-ray spectroscopy, field-emission scanning electron microscopy, and high-resolution transmission electron microscopy. As the particle-settlement effect becomes dominant during the composite fabrication process, ZrB₂ nanoparticles agglomerate to a certain extent in some areas of the as-cast composites. A laser-surface melting (LSM) strategy was applied to disperse agglomerated ZrB₂ nanoparticles in as-cast composites, and the ZrB₂ nanoparticle dispersion is affected visibly by LSM. After LSM, nanoparticles tend to distribute along the grain boundary. Particle clusters were dispersed in an explosive orientation and the particle diffusion distance varied in terms of its radius and melt-viscosity vicinity. High-resolution transmission electron microscopy showed the existence of a subgrain structure near the ZrB₂–Al interface after LSM. This may increase the yield strength when a dislocation tangle forms.     

Structural study of Mn-doped ZnO films by TEM

The structural study of diluted magnetic semiconductors is important for interpreting the ferromagnetic behavior associated with the materials. In the present work, a series of low concentration Mn-doped ZnO thin films synthesized by pulsed laser deposition was studied by electron microscopy. All films show the wurtzite structure with (001) preferred growth orientation on the Si substrate. Electron diffraction experiments indicate the deterioration of the growth orientation in some areas of the films with increasing Mn concentration, and the existence of a secondary phase, of Mn₂O₃-type, in the films with larger Mn concentrations. High-resolution electron microscopy images confirm the existence of the secondary phase in the grain boundary of the Mn-doped ZnO phase. The magnetic properties of Mn-doped ZnO are discussed in relation to the structures of the films.     

Abnormal grain growth of WC with small amount of cobalt

Abnormal grain growth (AGG) often appears in the synthesis of cemented tungsten carbide (WC), especially where ultra-fine powder is used. In this study, it was observed that AGG was strongly affected by the amount of Co. The obvious AGG was found to occur when the amount of Co was between 0.2 and 0.9 wt%. Careful examination of the etched samples found crack-like defects in abnormal grains, which were indications of grain boundaries in these large grains. Therefore, it is suggested that the considerable AGG of WC at lower Co concentrations be attributed to a grain boundary re-entrant edge (GBRE)-assisted two-dimensional nucleation process. Grain coalescence during sintering was the source of the grain boundaries. Due to the selective wetting of (0001) WC planes with the Co liquid, those grain boundaries were parallel to the (0001) planes resulting in platelet-like large grains with high aspect ratio. The amount of Co would affect the number of the wetted (0001) planes and the probability of grain boundary formation, and hence affect the AGG. The correspondence of the calculated weight percentage of Co required surrounding all the planes of WC grains and the experimental upper limit of the range supported this mechanism.     

Structural investigation of YBCO films and bicrystal grain boundary junctions

Summary We present a structural analysis of YBCO superconducting thin films fabricatedin situ by Inverted Cylindrical Magnetron (ICM) sputtering on commercial SrTiO₃ single-crystal and bicrystal substrates. A detailed structural characterization of the superconductor films was performed by using single-crystal X-ray diffractometry confirming that YBCO films have a strongc-axis orientation of the grains with a small mosaic spread. In the films grown on bicrystal substrates we observed a strong correlation with the lattice structure of the substrate. In addition, a surface analysis of the region across the grain boundary edge has been performed by using scanning electron microscopy. Paper presented at the ?VII Congresso SATT?, Torino, 4–7 October 1994.     

Microstructures of grain boundaries in (001)-oriented strontium bismuth tantalate thin films grown by pulsed laser deposition

(001)-oriented strontium bismuth tantalate thin films have been grown on Pt/TiO₂/SiO₂/Si (100) substrates by pulsed laser deposition. The room-temperature current–electric field dependence of the films has been investigated, which revealed a space-charge-limited conduction mechanism. The microstructures of grain boundaries and structural defects in these films were also examined by transmission electron microscopy and high-resolution transmission electron microscopy, respectively. The grains of the films deposited at 550 °C exhibited polyhedral morphologies, and the average grain size was about 50 nm in length and 35 nm in width. At a small misorientation angle (8.2°) tilt boundary, a regular array of edge dislocations with about 3-nm periodic distance was observed, and localized strain contrast near the dislocation cores was also observed. The Burgers vector b of the edge dislocation was determined to be [110]. At a high misorientation angle (39.0°) tilt grain boundary lattice strain contrast associated with the distortion of lattice planes was observed, and the mismatching lattice images occurred at about 2 nm along the boundary. The relationship between microstructural defects at grain boundaries and leakage currents of these films is also discussed. Received: 8 September 2000 / Accepted: 18 December 2000 / Published online: 28 February 2001     

High pressure infiltration sintering behavior of WC-Co alloys

In this paper, two average tungsten carbide particle sizes of 2, 0.5?μm are placed respectively, in contact with a WC-16Co substrate, pressed at the pressure of 4.5–5.5?GPa, and heated to temperatures ranging from 1350°C to 1500°C in a large-volume cubic press. During the process Co was forced out of the WC-16Co substrate into the compressed powder. The resulting infiltrated samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), Vickers hardness and cutting performance tests. The results of XRD confirmed that the sintered bulks have WC and Co phases. The scanning electron microscopy (SEM) analysis reveals that the WC grains in well-sintered alloys are round in shape and cobalt with lower content is uniformly dispersed in the WC grain boundaries. The sintered sub-micron WC-Co alloy with a cobalt content of 3.8?wt% exhibits a prominent combination of high hardness value of 23.1?GPa and a large fracture toughness value of 8.6?MPa?m^½. The high-speed cutting tests indicating its cutting performance is significantly superior to the commercial YG6X (WC-6?wt%Co with WC grain size of 0.5?μm).     

Preparation and characterization of molybdenum diselenide thin films

MoSe₂ layers, synthesized by annealing a molybdenum foil under selenium pressure, have been investigated by scanning electron microscopy, X-ray analysis, electron spectroscopy (XPS) and electrical resistance measurements. It has been found that stoichiometric layers are obtained after appropriate processing. The films crystallize in the hexagonal structure. The crystallites develop preferentially along the c axis. The binding energies deduced from the XPS lines were found to be in good agreement with those of the reference powder. The electrical resistance is governed by hopping conduction in the low temperature range (80–250 K) and by grain boundary scattering mechanisms at higher temperatures.     

Dependence of grain boundary character distribution on the initial grain size of 304 austenitic stainless steel

Abstract

In order to study the dependence of the grain boundary character distributions (GBCD) on the grain size, annealing treatment was carried out on 304 austenitic stainless steel with different initial grain sizes. The evolution of the GBCD was analysed by electron backscatter diffraction. The experimental results showed that abnormal grain growth (AGG) occurred when grain size was small. With a smaller initial grain size, the number density of abnormally large grains and the fraction of low-Σ CSL boundaries increased but the size of abnormally large grains decreased and the random boundaries presented a continuous network. With a larger initial grain size, the fraction of low-Σ CSL boundaries also increased as well as the size of abnormally large grains but the number density of abnormally large grains decreased and the connectivity of random boundary network was disrupted by low-Σ CSL boundaries, especially Σ3ⁿ (n = 1, 2, 3) boundaries. However, with a very large initial grain size, normal grain growth (NGG) occurred, which had no effect on the fraction of low-Σ CSL boundaries and the connectivity of random boundary network.