TEM and HREM study of Al3Zr precipitates in an Al-Mg-Si-Zr alloy

The structure of Al₃Zr precipitates in Al‐1.0Mg‐0.6Si‐0.5Zr (in wt.%) alloy was investigated using conventional transmission electron microscopy (TEM) and high‐resolution TEM (HREM). After annealing of the alloy in the temperature range 450–540 °C, spherical precipitates of metastable L1₂‐Al₃Zr phase appeared nearly homogeneously within the matrix, and elongated particles were found at grain boundaries. L1₂‐structured Al₃Zr were about 20–30 nm in diameter and coherent with the matrix. Inside some of them, planar faults parallel to {100} planes were revealed by use of HREM. Most probably, these faults are an indication of the transition stage of transformation to the stable D0₂₃‐type Al₃Zr phase. The elongated precipitates (about 100 nm) were identified as D0₂₂‐type Al₃Zr. Energy‐dispersive X‐ray analysis showed that they contain, apart from Al, mainly Zr with small amounts of Si. The substitution of Al by Si increased the stability of the D0₂₂‐Al₃Zr as compared with D0₂₃‐Al₃Zr.     

Electron microscopy of crack/particle interactions in Al2O3/SiC nanocomposites

Crack/particle interactions in alumina/silicon carbide nanocomposites have been investigated by scanning electron microscopy and transmission electron microscopy, with cracks induced by Vickers microindentation. Intergranular cracks are frequently deflected into grains by SiC particles on grain boundaries inclined to the average direction of crack propagation. This mechanism is proposed to explain the change in the fracture mode from intergranular fracture for monolithic alumina to predominantly transgranular fracture for the nanocomposites. Neither stress-induced microcracking around SiC particles nor significant crack deflection by intragranular particles was found to occur in the nanocomposites. It is argued that an addition of nanoparticles may not be a promising approach for increasing the toughness of alumina.     

Chemical reactions and morphological stability at the Cu/Al2O3 interface

The microstructures of diffusion‐bonded Cu/(0001)Al₂O₃ bicrystals annealed at 1000 °C at oxygen partial pressures of 0.02 or 32 Pa have been studied with various microscopy techniques ranging from optical microscopy to high‐resolution transmission electron microscopy. The studies revealed that for both oxygen partial pressures a 20–35 nm thick interfacial CuAlO₂ layer formed, which crystallises in the rhombohedral structure. However, the CuAlO₂ layer is not continuous, but interrupted by many pores. In the samples annealed in the higher oxygen partial pressure an additional reaction phase with a needle‐like structure was observed. The needles are several millimetres long, ～10 µm wide and ～1 µm thick. They consist of CuAlO₂ with alternating rhombohedral and hexagonal structures. Solid‐state contact angle measurements were performed to derive values for the work of adhesion. The results show that the adhesion is twice as good for the annealed specimen compared to the as‐bonded sample.     

Structure of electrodeposited graded composite coatings of Ni–Al–Al2O3

The structure of electrodeposited composite coatings of Ni–Al–Al₂O₃, with Ni as the matrix and Al and Al₂O₃ as second-phase particles, was investigated using light microscopy and scanning electron microscopy. Ni coatings with no particles, which were used as reference samples, had progressively coarser structures with increasing current density. Co-deposition with Al resulted in refinement of the Ni matrix structure at high (>10 A dm⁻²) current densities. For single-particle baths, the co-deposition of Al₂O₃ was more strongly affected by current density and bath particle content than was the co-deposition of Al. However, for baths containing both Al and Al₂O₃ the amount of incorporated Al₂O₃ no longer depended on current density. With the choice of appropriate conditions, coatings of Ni with up to 39 vol.% Al₂O₃ were made. Similar experiments with Al yielded a maximum of 17.5 vol.% only. Uniform and graded mixed-particle coatings were also produced. When coatings containing Al were annealed, the reaction of the two elements resulted in the formation of either single-phase γ or two-phase γ–γ' alloys, in agreement with the equilibrium phase diagram.     

Defects formed within hardness indenter interaction zone in Al2O3–ZrO2 composite

The Al₂O₃?10 wt% ZrO₂ composites were subjected to hardness tests using a Vickers diamond indenter up to 98.1 N. The microstructure observation using a transmission electron microscopy technique helped to identify up to four zones differing in defect level and character. The densest dislocation tangles, twins accumulation and frequent presence of three slip systems were found in regions that were in contact with the sides of the diamond pyramid. The second zone, characterized by two, or at least one, active slip systems, started at the bottom of the indentation mark and extended up to a distance comparable with the depth of indentation. In the third zone, with a thickness comparable to that above, only some α‐Al₂O₃ crystallites showed the presence of dislocations, whereas other crystallites were defect free. In the last zone the alumina crystals were left unaffected but the ZrO₂ crystallites showed twinning characteristic of strain‐induced transformation.     

Interface study by dual-beam FIB-TEM in a pressureless infiltrated Al(Mg)–Al2O3 interpenetrating composite

This paper considers the microstructures of an Al(Mg)–Al₂O₃ interpenetrating composite produced by a pressureless infiltration technique. It is well known that the governing principle in pressureless infiltration in Al–Al₂O₃ system is the wettability between the molten metal and the ceramic phase; however, the infiltration mechanism is still not well understood. The objective of this research was to observe the metal–ceramic interface to understand the infiltration mechanism better. The composite was produced using an Al-8 wt% Mg alloy and 15% dense alumina foams at 915°C in a flowing N₂ atmosphere. After infiltration, the composite was characterized by a series of techniques. Thin-film samples, specifically produced across the Al(Mg)–Al₂O₃ interface, were prepared using a dual-beam focussed ion beam and subsequently observed using transmission electron microscopy. XRD scan analysis shows that Mg₃N₂ formed in the foam at the molten alloy–ceramic infiltration front, whereas transmission electron microscopy analysis revealed that fine AlN grains formed at the metal–ceramic interface and MgAl₂O₄ and MgSi₂ grains formed at specific points. It is concluded that it is the reactions between Al, Mg and the N₂ atmosphere that improve the wettability between molten Al and Al₂O₃ and induce spontaneous infiltration.     

Three-dimensional analysis of porous BaTiO3 ceramics using FIB nanotomography

Three‐dimensional (3D) data represent the basis for reliable quantification of complex microstructures. Therefore, the development of high‐resolution tomography techniques is of major importance for many materials science disciplines. In this paper, we present a novel serial sectioning procedure for 3D analysis using a dual‐beam FIB (focused ion beam). A very narrow and reproducible spacing between the individual imaging planes is achieved by using drift correction algorithms in the automated slicing procedure. The spacing between the planes is nearly of the same magnitude as the pixel resolution on scanning electron microscopy images. Consequently, the acquired stack of images can be transformed directly into a 3D data volume with a voxel resolution of 6 × 7 × 17 nm. To demonstrate the capabilities of FIB nanotomography, a BaTiO₃ ceramic with a high volume fraction of fine porosity was investigated using the method as a basis for computational microstructure analysis and the results compared with conventional physical measurements. Significant differences between the particle size distributions as measured by nanotomography and laser granulometry indicate that the latter analysis is skewed by particle agglomeration/aggregation in the raw powder and by uncertainties related to calculation assumptions. Significant differences are also observed between the results from mercury intrusion porosimetry (MIP) and 3D pore space analysis. There is strong evidence that the ink‐bottle effect leads to an overestimation of the frequency of small pores in MIP. FIB nanotomography thus reveals quantitative information of structural features smaller than 100 nm in size which cannot be acquired easily by other methods.     

Wear behaviour of Al/(Al2O3p+SiCp) hybrid composites

In this study, dry sliding metal–metal and metal–abrasive wear behaviours of the aluminium matrix hybrid composites produced by pressure infiltration technique were investigated. These composites were reinforced with 37 vol% Al₂O₃ and 25 vol% SiC particles and contained up to 8 wt% Mg in their matrixes. While matrix hardness and compression strength increased, amount of porosity and impact toughness decreased with increasing Mg content of the matrix. Metal–metal and metal–abrasive wear tests revealed that wear resistance of the composites increased with increasing Mg addition. On the other hand, abrasive resistance decreased with increasing test temperature, especially above 200 °C.     

Fretting wear of carburized titanium alloy against ZrO2 under serum lubrication

Fretting wear of carburized titanium alloys was investigated on the universal multifunctional tester (UMT) with the ball-on-flat fretting style under bovine serum lubrication. The tangential load and friction coefficient during the fretting process were analyzed, and the evolution of fretting log during the fretting process was investigated to understand the wear mechanism of the titanium alloy and carburized titanium alloy. Furthermore, the wear scar was examined using a SEM and three-dimension surface profiler. It was found that the friction coefficient of the titanium alloy increased faster than that of carburized titanium alloy in the first stage under serum lubrication, and then remained steady with a similar value in the second stage. The Ft-D curve indicated that there was wear mechanism transition from gross slip to mixed stick and slip. Finally, it was observed that there was a slight damage of the titanium alloy and carburized titanium alloy showed excellent performance during the fretting wear process under serum lubrication. All of the results suggested that carburized titanium alloy was a potential candidate for the stem material in artificial joints.     

A study of the initial growth of PtxCo(1−x) thin films on Si3N4

Pt _x Co_{(1− x )} thin films where x  =0.24 have been deposited onto Si₃N₄ windows and studied using transmission electron microscopy. The films are used in ultrahigh-density recording studies and it was found that the surface of the substrate had a strong influence on the microstructure, crystallography and magnetic properties of the film. An investigation of the early growth of the film was made by studying films of different thickness between 100 and 300 Å. It was found that the grains were hexagonal in structure with a strong c -axis orientation perpendicular to the surface.     

In situ observation of oxygen deficiency occurring during electron irradiation in high Tc superconductor YBa2Cu3Oy

The decreasing process of oxygen in YBa₂Cu₃O _y is investigated through high resolution electron microscopy (HREM) and convergent beam electron diffraction (CBED). Measurements of the axial length in HREM images show that oxygen content y decreases faster near a twin boundary than at the inner part of a twin lamella. The transformation from an orthorhombic to a tetragonal phase starts at a twin boundary and the transformed region propagates to an inner region of lamella. Lattice strains are observed near boundaries between transformed and non-transformed regions. The transformation is almost complete within 30 s during observation of HREM images at 400 kV and at room temperature. A value of y was quantitatively measured by analysing observed intensities of energy-filtered CBED patterns with the dynamical theory. The value of y decreases from 6.9 to 6.5 when 200 kV electrons are irradiated for 160 s in a microscope at 108 K. More precise analysis of the intensities provides information on charge distribution along the c -axis as well as local oxygen content at a spatial resolution of several nanometres.     

About the role of the various types of secondary electrons (SE1; SE2; SE3) on the performance of LVSEM

The relative weight, δ_Β, of the yield of secondary electrons, SE₂, induced by the backscattered electrons, BSE, with respect to that, δ_P, of secondary electrons, SE₁, induced by the primary electrons, PE, is deduced from simple theoretical considerations. At primary energies E₀ larger than E_M (where the total SE yield δ = δ_P + δ_B is maximum), the dominant role of the backscattering events is established. It is illustrated in SEM by a direct comparison of the contrast between SE images and BSE images obtained at E₀ ～ 5 keV and E₀ ～ 15 keV on a stratified specimen. At energies E₀ less than E_M, the dominant role of SE₁ electrons with respect to SE₂ (and SE₃) is established. It is illustrated by the better practical resolution of diamond images obtained with an in‐lens detection in low voltage SEM E₀ ～ 0.2–1 keV range compared with that obtained with a lateral detector. The present contribution illustrates the improved performance of LVSEM in terms of contrast and of practical resolution as well as the importance of variable voltage methods for subsurface imaging. The common opinion that the practical lateral resolution is given by the incident spot diameter is also reconsidered in LVSEM.     

Electron and light microscopy studies on the domain structures of Zn3B7O13Cl, Zn3B7O13Br and Zn3B7O13I ferroic boracites

The domain structures of Zn₃B₇O₁₃Cl, Zn₃B₇O₁₃Br and Zn₃B₇O₁₃I boracite single crystals were studied by means of polarized light in conjunction with electron microscopy. Single crystals of the three compositions were grown by chemical transport reactions in closed quartz ampoules, at a temperature of 900 °C and were examined by polarizing optical microscopy (PLM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). For both PLM and SEM, the same as‐grown samples were used without having to resort to metallization of the crystal faces. For TEM the single crystals were crushed and mounted on holey carbon films. Comparative electron microscope images were useful for revealing the domain structure of these ferroelectric/ferroelastic materials previously observed between the crossed polars of an optical microscope. X‐ray diffraction analysis of the pulverized crystals was performed for this triad of halogen boracites containing zinc as a common metal.     

Interfacial reactions and silicate formation in highly dispersed Lu2O3– SiO2 system

Solid state interface reactions in highly dispersed Lu₂O₃– SiO₂ binary oxide system were studied at 600–1100 °C with X‐ray powder diffraction (XRD), high‐resolution transmission electron microscopy (HRTEM) and Fourier Transform Infrared spectroscopy (FTIR). The results show that at 600–900 °C an amorphous, nanometer thick Lu‐O‐Si layer covering SiO₂ particles exists in the system. At higher temperatures the breakage of the layer into amorphous islands occurs and crystalline silicates with various structures are formed. In particular, Lu₄[Si₃O₁₀][SiO₄] silicate, analogue of B‐type Dy – Tm disilicates, forms at 1000 °C.     

The preferred CSL misorientation distribution in polycrystalline SrTiO3

Electron backscattered diffraction is used to investigate the preferred CSL (coincidence site lattice) distribution of polycrystalline SrTiO₃ as a function of annealing times (1 h and 16 h). Comparison of the CSL misorientations suggests that the CSL boundary energy plays a role in the preferred grain growth.     

Microstructural analysis of Al alloys dispersed with TiB2 particulate for MMC applications

A dispersion of TiB₂ particulates in an Al alloy matrix was formed via the in-situ reaction between mixtures of K₂TiF₆ (K₂ZrF₆), KBF₄ and molten aluminium. The dispersion of the ceramic phase in the aluminium matrix was also achieved in some experiments by adding exogenous TiB₂ particles to the fluoride melt in contact with molten aluminium.
In this work, we have examined the microstructure of the as-cast metal matrix composites using analytical electron microscopy and X-ray diffraction techniques. The phases formed as a result of the reaction between the molten fluoride flux and liquid aluminium have been identified. These were (Ti, Zr, Al)B₂, Al₃Ti and possibly AlB₁₂ in the Al-matrix, and KAlF₄ and KMgF₃ in the solidified flux. The mechanism of formation of TiB₂ and Al₃Ti is explained. The role of alloying elements is also explained in the context of interfacial chemistry and dispersion.     

Sliding wear characteristics of plasma-sprayed Al2O3 and Cr2O3 coatings against copper alloy under severe conditions

Al₂O₃ and Cr₂O₃ coatings were deposited by atmospheric plasma spraying and their tribological properties dry sliding against copper alloy were evaluated using a block-on-ring configuration at room temperature. It was found that the wear resistance of Al₂O₃ coating was superior to that of the Cr₂O₃ coating under the conditions used in the present study. This mainly attributed to its better thermal conductivity of Al₂O₃ coating, which was considered to effectively facilitate the dissipation of tribological heat and alleviate the reduction of hardness due to the accumulated tribological heat. As for the Al₂O₃ coating, the wear mechanism was plastic deformation along with some micro-abrasion and fatigue-induced brittle fracture, while the failure of Cr₂O₃ coating was predominantly the crack propagation-induced detachment of transferred films and splats spallation.     

Characterization and fabrication of fully metal-coated scanning near-field optical microscopy SiO2 tips

The fabrication of silicon cantilever‐based scanning near‐field optical microscope probes with fully aluminium‐coated quartz tips was optimized to increase production yield. Different cantilever designs for dynamic‐ and contact‐mode force feedback were implemented. Light transmission through the tips was investigated experimentally in terms of the metal coating and the tip cone‐angle. We found that transmittance varies with the skin depth of the metal coating and is inverse to the cone angle, meaning that slender tips showed higher transmission. Near‐field optical images of individual fluorescing molecules showed a resolution < 100 nm. Scanning electron microscopy images of tips before and after scanning near‐field optical microscope imaging, and transmission electron microscopy analysis of tips before and after illumination, together with measurements performed with a miniaturized thermocouple showed no evidence of mechanical defect or orifice formation by thermal effects.     

Optimization of a FIB/SEM slice-and-view study of the 3D distribution of Ni4Ti3 precipitates in Ni–Ti

The 3D morphology and distribution of lenticular Ni₄Ti₃ precipitates in the austenitic B2 matrix of a binary Ni₅₁Ti₄₉ alloy has been investigated by a slice-and-view procedure in a dual-beam focused ion beam/scanning electron microscope system. Due to the weak contrast of the precipitates, proper imaging conditions need to be selected first to allow for semi-automated image treatment. Knowledgeable imaging is further needed to ensure that all variants of the precipitates are observed with equal probability, regardless of sample orientation. Finally, a volume ratio of 10.2% for the Ni₄Ti₃ precipitates could be calculated, summed over all variants, which yields a net composition of Ni_50.27Ti_49.73 for the matrix, leading to an increase of 125 degrees for the martensitic start temperature. Also, the expected relative orientation of the different variants of the precipitates could be confirmed.     

原位反应法制备Al2O3/Cu复合材料的工艺研究

将自蔓延和传统铸造方法相结合,制备原位Al2O3颗粒增强铜基复合材料。研究原料配比、反应温度、预制片成型压力以及混粉时间等参数对复合材料组织的影响。结果表明,最佳的工艺参数为:铝粉与氧化铜粉的质量比为2∶1,铜粉加入量为5%(质量分数);预制片成型压力为12 MPa;浇注温度为1 120℃,混粉时间为30 min。