Polycrystalline Alumina Research Articles

Modeling the effects of crystallite alignment on birefringent light scattering in transparent polycrystalline aluminum oxide

Transparent alumina ceramics are known for high toughness and the ability to withstand high temperatures, making them ideal materials for use in extreme environments and high-power optical devices. However, polycrystalline alumina, which has a hexagonal crystal structure, is difficult to make highly transparent due to birefringent scattering loss. Research has shown that birefringent scattering can be reduced by having finer grains and/or aligned grains. Here, we present an analytical birefringence scattering model that can model realistic microstructures, by including chord length distributions and grain orientations, and predict the birefringence scattering loss quantitatively. Our modeled results match well with existing experimental data for transparent fine grained and aligned alumina. This model is derived from first-principles and is applicable to other transparent ceramics.

A hybrid mesoscale-continuum approach to understand and predict melting kinetics of Al powders during laser processing

Abstract Laser interaction with metallic powders during additive manufacturing (AM) leads to fast heating and cooling rates that can affect the quality of the final products due to the formation of defects. One of the first steps towards predicting microstructures generated during AM, therefore, requires an accurate understanding of the laser energy deposition mechanisms that determine the melting kinetics at the level of individual powders. The critical challenge, however, is the availability of computational methods that can model the laser energy absorption, heat transfer, and the related microstructure evolution in individual metal powders at the length and time scales of AM. This manuscript demonstrates the capability of a novel scale-bridging methodology that combines the mesoscale quasi-coarse-grained dynamics (QCGD) simulations with a continuum two-temperature model (TTM) to account for the atomistic mechanisms of laser energy deposition and microstructure evolution and predict the kinetics of melting of individual powders at the experimental time and length scales. The scale-bridging capability of the hybrid QCGD-TTM simulations is demonstrated here by investigating the laser-induced microstructure evolution in aluminum powders with various sizes ranging from 200 nm to 20 µm. The analysis of the evolution of temperature, pressure, phase fraction, and melt fronts suggests the melting mechanism is heterogeneous due to the interaction with a laser, and the melting time is observed to decrease exponentially as the laser intensity increases. The solid-liquid interface velocity can be quantified to identify correlations with interface temperatures, and the predicted values satisfy the theoretically reported limits of crystal stability of metals against homogeneous melting. In addition, the pre-melting is found at the grain boundaries of 20 µm polycrystalline aluminum powder, while a minute contribution to melting is observed. This manuscript demonstrates the capability of the QCGD-TTM method to capture laser-powder interaction and allow the investigation of the kinetics of laser melting.

A molecular dynamics study of the effect of initial pressure on the mechanical resilience of aluminum polycrystalline

Polycrystalline materials are essential in engineering due to their ability to withstand various forces, heat, and environmental conditions. The arrangement of atoms within these crystals significantly affects their mechanical properties. This study used molecular dynamics simulations to explore how initial pressure affects the mechanical resilience of aluminum polycrystals. Aluminum composite materials, known for their strength, flexibility, and environmental sustainability, are the focus of this investigation. We particularly investigated stress-strain reactions at 1, 2, and 3 bar initial pressures. Reduced free volume causes atomic migration to be hampered as pressure increases, therefore affecting mean square displacement and diffusion coefficient. The results show that ultimate strength and Young's modulus of the polycrystalline samples were 30 and 6.64 GPa at 1 bar pressure. Moreover, the results demonstrated a notable decrease in mechanical performance by increasing pressure; the ultimate strength and Young's modulus of the polycrystalline samples diminished to 5.66 GPa and 22.43 GPa, respectively, at 3 bar. Furthermore, the heat flux increased by rising initial pressure in the Al-polycrystalline sample due to the compression of material that reduced atomic distances. This improved atomic arrangement facilitated more efficient heat transfer. These insights are essential for engineering applications, as they establish a foundation for the production of aluminum components that maintain structural integrity in the face of extreme conditions.

Structure, Composition and Electrochemical Properties of Disordered Rock-Salt LiCoO2 Thin Films Prepared by Ion Beam Assisted Deposition

Ion beam assisted deposition is a method used to deposit thin films while irradiating the growing film with an ion beam. This technique is known to be effective in crystallization and orientation control at low temperatures. In this study, LiCoO2 (LCO) thin films were prepared at temperatures below 100 °C using ion beam assisted pulsed laser deposition. The structure, composition, and electrochemical properties of these films were characterized. The results indicated that LCO thin films with a disordered rock salt structure and triaxial orientation were successfully grown on polycrystalline aluminum and quartz glass substrates using ion beam assisted deposition. Furthermore, the diffusion coefficient of Li ions and the charge/discharge capacity were significantly improved compared to LCO thin films with a disordered rock salt structure prepared without the ion beam assisted process.

Influence of forging pretreatments on microstructure evolution and surface roughness of Al 6061 alloy

Achieving ultra-smooth surfaces is the goal of aluminum optical manufacturing. Under certain processing conditions, improving the microstructure of aluminum and understanding its relationship with surface roughness requires systematic study. The grain structure and various types of second-phase particles are of paramount importance. This study analyzed the microstructure of 6061 alloy after undergoing severe plastic deformation under various processing conditions followed by T6 homogenization heat treatment. Utilizing a white light interferometer, a comparative analysis of the surface roughness was conducted on specimens that underwent single-point diamond turning to achieve a mirror finish. The assessment of surface roughness on machined surfaces is solely based on white light interferometry. The analysis and discussion focus on the effects of phases (causing scratches and voids), the grains and grain boundaries. Experimental findings signify: the grain size, grain boundary and residual second phase can both influence the surface quality, the increase in deformation temperature and accumulated strain both facilitate the dissolution and fragmentation of the secondary phases. However, they also contribute to some extent to grain growth, resulting in a minimum secondary phase area fraction of 0.87% and grain sizes reaching 147.8 μm. Subsequent heat treatments, while effective in reducing the negative impact of the phases, reveal noticeable step-like structures affecting the quality of surface roughness, with the lowest obtained Ra value being 0.8 nm. A proposed pretreatment method in cleaner ingot processing with lower alloy element content addresses the trade-off between reducing phases and controlling grain growth, aiming to achieve improved surface roughness, promoting the application of polycrystalline aluminum alloys in the field of optics manufacturing.

Measuring thermal conductivity using H2-O2 flame on ceramic films prepared by atmospheric chemical vapor deposition

Uneven micron-sized pores on the surface of the polycrystalline alumina (Al2O3) substrates can affect their performance as electrical insulating plates. In this study, we investigated the sealing of these pores with amorphous Al2O3 films deposited via atmospheric chemical vapor deposition. Furthermore, we conducted annealing treatments on the samples. The color change of the deposited Al2O3 films was investigated using the Commission Internationale de I’Eclairage color space. Notably, the deposited films initially changed the sample color from white to orange or brown. However, increasing the annealing temperature and duration reversed this discoloration effectively and restored the original white (colorless) appearance of the sample. We measured thermal conductivity using the flame flash method with the H2-O2 flame to assess the influence of sealing. While the unsealed substrate exhibited a thermal conductivity of 4.66 W/mK in the range of 400–500 °C, the annealed and flattened Al2O3 film deposited on the substrate maintained a comparable thermal conductivity of 4.67 W/mK within the same temperature range. This finding demonstrates that our sealing method successfully filled the pores while having minimal influence on thermal conductivity, which is a crucial property for electrical insulation applications.

Synthesis, thermal X-ray, neutron diffraction, Mössbauer spectroscopy and magnetic properties investigation of Al doped barium hexaferrite BaFe11AlO19

Polycrystalline aluminum substituted barium hexaferrite BaFe11AlO19 synthesized by the ceramic technique. The results of energy dispersive X-ray analysis, thermal X-ray diffraction (XRD), neutron diffraction, Mössbauer spectroscopy, magnet properties measurements were measured. XRD analysis demonstrated P63/mmc hexagonal structure of BaFe11AlO19. The magnetic sublattice of barium hexaferrite BaFe11AlO19 was obtained using neutron diffraction data. The distribution of aluminum in barium hexaferrite matrix at positions 2a and 12k was obtained with Mössbauer spectroscopy. A comparison of the calculated intensities of the neutronograms and the actual ones allowed us to establish that in position 2a the aluminum ion occupied a position with the coordinate (1;1;0), and the position of the substituent ion in position 12k (0.83333; 0.66667; 0.10810). According to neutron diffraction data, it was found that the actual Curie temperature is lower than that measured by differential scanning calorimetry.

Molecular dynamics simulation of fatigue damage formation in single-crystal/polycrystalline aluminum

The fatigue plasticity mechanisms and local defect characteristics of engineering materials are critical for addressing fatigue damage. This study aims to identify the formation mechanisms of fatigue damage and delineate the microstructural characteristics that resisted or facilitated fatigue-induced plastic accumulation. The fatigue mechanical properties and microstructural evolution processes of single-crystal/polycrystalline aluminum were investigated through strain-controlled fatigue testing, considering three distinct strain amplitudes. The initiation and cumulative occurrence of local plasticity in single-crystal aluminum occur at the intersections of slip planes, which serve as sources of dislocations. The cumulative formation of irreversible surface steps results in local stress concentration, ultimately leading to fatigue damage at the free surface. Polycrystalline aluminum undergoes grain rotation and merging during cyclic loading, leading to a gradual increase in grain size during plastic deformation. The initiation and cumulative occurrence of local plasticity occur at grain boundaries, ultimately leading to fatigue damage at the grain boundaries.

Effect of the third element on the wetting of alumina by TiAl-X (X = Fe, Ni) alloys at 1500 °C

In this work we show how the addition of a third element, namely Fe or Ni, influences the interfacial behaviour of liquid TiAl alloys on polycrystalline alumina. Wetting of these alloys was studied by the sessile drop method at 1500 °C and the interfacial microstructures were characterised to determine the relation between the contact angle and the interfacial reaction with the aid of the relevant phase diagrams. The equiatomic TiAl intermetallic wetted the alumina substrate forming a contact angle of 60°. On the other hand, increasing concentrations of Fe and Ni were found to improve the wetting behaviour of ternary TiAl-X alloys: for third-element atomic concentrations of 5 at. %, contact angles decreased to 32° and 29° by adding Fe and Ni, respectively. Neither reactive-formed interlayers nor newly formed phases were observed for any binary or ternary composition as confirmed by thermodynamic calculations. A slight dissolution of the ceramic occurred during liquid/solid contact and became more evident with the increase of concentration of the third element. The introduction of oxygen into the melt provided by the dissolution of alumina improved the wetting behaviour.

Discrete model for discontinuous dynamic recrystallisation applied to grain structure evolution inside adiabatic shear bands

Discontinuous dynamic recrystallisation (DDRX) is a well-known phenomenon playing a significant role in the high-temperature processing of metals, including industrial forming and severe plastic deformations. The ongoing discussion on the Zener–Hollomon (Z–H) parameter as a descriptor of materials’ propensity to DDRX and a measure of microstructure homogeneity leaves more questions than answers and prevents its practical application. Most of the existing DDRX models are continuous, and so the geometry and topology of real grain microstructures cannot be considered. The present study uses a fully discrete representation of polycrystalline aluminium alloys as 2D/3D Voronoi space tessellations corresponding to EBSD maps. Such tessellations are geometric realisations of combinatorial structures referred to as polytopal cell complexes. Combining discrete models with FEM LS-Dyna simulations of shock-wave propagation in AA1050 and AW5083 aluminium alloys makes it possible to estimate for the first time the contribution of DDRX to the final material microstructure inside adiabatic shear bands. It is shown that the increase of the initial fraction of high-angle grain boundaries, caused by preliminary deformation, significantly increases the spatial homogeneity and decreases the clustering of DDRX grains. The obtained results contradict the conventional assumption that the microstructures obtained by severe plastic deformation under quasi-static and dynamic deformation conditions are similar due to the similar value of the Z–H parameter: competition between the two recrystallisation mechanisms leads to almost unpredictable final grain structures inside share bands that require further comprehensive experimental studies. This agrees with experimental evidence for high material sensitivity to the Z–H parameter.

A diamond anvil microassembly for Joule heating and electrical measurements up to 150 GPa and 4000 K

When diamond anvil cell (DAC) sample chambers are outfitted with both thermal insulation and electrodes, two cutting-edge experimental methods are enabled: Joule heating with spectroradiometric temperature measurement and electrical resistance measurements of samples heated to thousands of kelvin. The accuracy of temperature and resistance measurements, however, often suffers from poor control of the shape and location of the sample, electrodes, and thermal insulation. Here, we present a recipe for the reproducible and precise fabrication of DAC sample, electrodes, and thermal insulation using a three-layer microassembly. The microassembly contains two potassium chloride thermal insulation layers, four electrical leads, a sample, and a buttressing layer made of polycrystalline alumina. The sample, innermost electrodes, and buttress layer are fabricated by focused-ion-beam milling. Three iron samples are presented as proof of concept. Each is successfully compressed and pulsed Joule heated while maintaining a four-point probe configuration. The highest pressure-temperature condition achieved is ∼150 GPa and 4000 K.

Nonlinear optical effects in polycrystalline transparent Al2O3 ceramics using femtosecond laser pulses—supercontinuum generation and laser damage

Nonlinear optical properties play a key role in technologies such as broadband laser light sources and ultrafast laser machining. With the emergence of transparent nanocrystalline Al2O3 ceramics as an alternative to single crystal alumina (sapphire), it is critical to understand their nonlinear optical behavior. Here, we report the demonstration of supercontinuum generation in polycrystalline alumina ceramics. Substantial broadening was observed when a focused 515 nm pulsed (260 fs) laser propagated through the ceramic sample. The broadening increased with increasing laser power and displayed stokes/anti-stokes asymmetries. At higher incident power, permanent damage was observed. Our results show that transparent nanocrystalline Al2O3 ceramics have a higher material removal rate than single crystal alumina. These results have interesting implications for laser machining as well as integrated photonics.

The onset of anelastic behavior in fine-grained synthetic dunite

Micromechanical models suggest that the onset of anelastic relaxation in polycrystalline olivine, critical to interpretation of the seismic wave attenuation and dispersion in the upper mantle, should be a mild dissipation peak caused by elastically accommodated grain-boundary sliding. Such behavior has been tentatively invoked to explain both a short-period shear modulus deficit and a dissipation plateau poorly resolved at 900–700 °C in previous forced-oscillation experiments on fine-grained dunite tested within mild-steel jackets. However, these observations may have been complicated by the austenite to ferrite plus cementite phase transition in the jacket material, compliance associated with interfacial Ni70Fe30 foils, and modeling of the mechanical properties of polycrystalline alumina as control specimen. To investigate the influence of these complications within the experimental setup and provide forced-oscillation data of better quality especially at moderate temperatures, we have conducted further forced-oscillation tests for which we removed the interfacial foils, employed single-crystal sapphire as reference sample, and used alternative jacket materials (stainless steel or copper) which experience no phase transition during the staged cooling. The newly acquired forced-oscillation data, although broadly consistent with the previous results, differ significantly especially in temperature sensitivity, and allow refinement of an appropriate Burgers creep-function model. A mild dissipation peak superimposed on monotonic dissipation background during the onset of anelastic relaxation in dry, melt-free and fine-grained dunite has now been consistently observed at temperatures of ∼950–1050 °C and seismic periods of 1–1000 s. Such a dissipation peak with relaxation strength 0.02 ± 0.01 is attributed to elastically accommodated grain-boundary sliding. The high activation energy (> 600 kJ/mol) of viscoelastic behavior involving both dissipation and related dispersion suggests that grain-boundary diffusion may be limited by interfacial reaction within grain boundaries. The reduced relaxation strength makes it difficult to attribute the oceanic lithosphere-asthenosphere boundary to water-mediated elastically accommodated grain-boundary sliding.

Structural analysis of nanocrystals by pair distribution function combining electron diffraction with crystal tilting.

As an important characterization method, pair distribution function (PDF) has been extensively used in structural analysis of nanomaterials, providing key insights into the degree of crystallinity, atomic structure, local disorder etc. The collection of scattering signals with good statistics is necessary for a reliable structural analysis. However, current conventional electron diffraction experiments using PDF (ePDF) are limited in their ability to acquire continuous diffraction rings for large nanoparticles. Herein, a new method - tilt-ePDF - is proposed to improve the data quality and compatibility of ePDF by a combination of electron diffraction and specimen tilting. In the present work, a tilt-series of electron diffraction patterns was collected from gold nanoparticles with three different sizes and a standard sample polycrystalline aluminium film for ePDF analysis. The results show that tilt-ePDF can not only enhance the continuity of diffraction rings, but can also improve the signal-to-noise ratio in the high scattering angle range. As a result, compared with conventional ePDF data, tilt-ePDF data provide structure parameters with a better accuracy and lower residual factors in the refinement against the crystal structure. This method provides a new way of utilizing ePDF to obtain accurate local structure information from nanoparticles.

Crystallography and anisotropy of crystals shape in dense aluminum titanate ceramics

This study investigates the anisotropic grain growth of Fe-doped aluminum titanate ceramics using Electron Backscatter Diffraction (EBSD). Three grades of materials exhibiting various grain size distributions were prepared on the basis of different sintering conditions. The crystal structure of the raw powder was first refined using X-ray diffraction. Then the microstructure variation of sintered polycrystalline aluminum titanate associated to anisotropic grain coarsening was accurately studied. Due to the orthorhombic structure of β-Al2TiO5, the crystal shape is prismatic and elongated along the [100] direction. This specific grain shape is analyzed in relation with crystallographic axes in the frame work of the Wulff approach. The obtained results provide valuable information regarding the microstructure of such flexible ceramics made off anisotropic grains.

A Comparative Assessment of the Bonding Characteristics of Three-Dimensional Custom-Printed Polycrystalline Alumina Brackets and Conventional Brackets

Objective: The objective was to compare the shear bond strength (SBS) and the adhesive remnant index (ARI) amongst six orthodontic bracket groups. Materials and Methods: Three-dimensional printed polycrystalline alumina brackets (3DBs), ceramic brackets (CBs), and metal brackets (MBs), divided into six groups, were bonded to bovine incisors using different bonding procedures. The SBSs were obtained using a universal testing machine, and the ARIs were assessed with a stereomicroscope. The statistical analyses included one-way analysis of variance (ANOVA) for SBS differences and Fisher’s exact test to show ARI differences amongst the groups (p < 0.05). Results: No significant differences (p > 0.05) were measured amongst the SBSs of the 3DB groups (12.3 MPa, 12.6 MPa, 12.3 MPa, 11.0 MPa, respectively). The latter four groups generally had significantly lower SBSs (p < 0.001) than the conventional bracket groups, CB and MB (16.9 MPa and 19.3 MPa, respectively). Also, there was no significant difference in SBSs for the CB and MB groups (p > 0.05). A high ARI for CBs and MBs (2) indicated that more than 50% of the adhesive remained on the enamel surface. The four 3DB groups had no residual adhesive or less than 50% adhesive on the enamel surface after debonding (ARI scores 0 and 1). A significant difference in ARI levels existed across the types of brackets (p < 0.05). Conclusion: Three-dimensional printed polycrystalline alumina brackets exhibited adequate SBS values for successful bonding. However, the values were lower compared to those for conventional ceramic and metal brackets. The majority of the adhesive remnant for the 3D-printed brackets was mainly located on the bracket base.

High entropy oxide as interfacial material for toughened textured alumina

AbstractTextured alumina ceramics with brick‐and‐mortar microstructures exhibit surprisingly high values of strength and toughness as compared to traditional ceramics. However, in full ceramic systems, pressure‐assisted sintering restricts their shaping potential, and the study of interfacial materials is still insufficient. Here, we fabricate textured alumina exhibiting elevated indentation fracture toughness using a high entropy oxide (HEO) (MgAlSiTiZr)O as the mortar. The HEO undergoes a single‐phase transformation at 1600°C, resulting in a crystallographic structure identical to that of ZrO2. Our HEO mortar is tough and has a high wetting behavior to alumina platelets used in the green body, which promotes densification via liquid phase sintering. Textured alumina ceramics with HEO mortar at concentrations varying from 0 to 90 wt% were fabricated using magnetically assisted slip casting and pressureless sintering through the templated grain growth process. A trade‐off between density and grain anisotropy led to the highest mechanical properties. Textured alumina with 10 wt% HEO exhibited over 95% relative density, an elastic modulus of 244 ± 29 GPa, a flexural strength of 329 ± 27 MPa, and an indentation fracture toughness of 6.80 ± 0.65 MPa∙m0.5, which is more than 1.9 times that of the usual polycrystalline alumina. Thanks to the mineral nature of HEO, the simplicity of the process, and the mechanical properties, the textured alumina with HEO mortar can be produced in complex shapes and could find applications in stringent environments.

Shear bond strength of metal brackets and ceramic brackets with monocrystalline and polycrystalline alumina bonded to provisional polymethyl methacrylate crowns

This study aimed to assess how the material and base design of orthodontic brackets affect the shear bond strength (SBS) when bonded to a provisional polymethyl methacrylate PMMA crown.

SrTiO3 Thin Films on Dielectric Substrates for Microwave Applications

Thin films of strontium titanate, which have nonlinear properties that are promising for microwave applications, were grown on a polycrystalline aluminum oxide substrate using magnetron sputtering and high-temperature annealing. It was shown that the improvement of the film structure with an increase in the deposition temperature was clearly correlated with both an increase in nonlinearity and an improvement in the loss level. A capacitor based on an SrTiO3 film deposited at a deposition temperature of 900 °C and subjected to annealing demonstrated a tunability of 46% with a loss tangent of 0.009–0.014 at a frequency of 2 GHz. This was the first successful attempt to form a planar SrTiO3 capacitor on an alumina substrate, which exhibited a commutation quality factor of above 3000 in the microwave range.

Dimensional accuracy, mechanical property, and optical stability of zirconia orthodontic bracket according to yttria proportions

This in vitro study evaluated comprehensively the performances of zirconia brackets with varying yttria proportions in manufacturing advanced orthodontic brackets. Three experimental groups of zirconia brackets were fabricated using yttria-stabilized zirconia (YSZ) materials with different yttria proportions—3 mol% yttria (3Y-YSZ), 4 mol% yttria (4Y-YSZ), and 5 mol% yttria (5Y-YSZ) (Tosoh Ceramic, Japan). A polycrystalline alumina ceramic bracket (3M™ Clarity™ Advanced, MBT 0.022-in. slot) was employed as the control group. Morphological properties, including slot surface structure and dimensions, were examined using scanning electron microscopy and surface profiler analysis. Manufacturing accuracy was assessed with root mean square calculations of trueness and precision. Mechanical properties were tested, encompassing static and kinetic frictional resistance (FR) and fracture strength. Optical stability was evaluated through 20,000 cycles of thermocycling and a 7-day immersion in various coloring agents. Within the limitations of this study, zirconia brackets containing 3 to 5 mol% YSZ presented enhanced reliability in terms of dimensional accuracy and demonstrated favorable optical stability. Notably, owing to its advantageous mechanical properties, the 3Y-YSZ variant showed remarkable potential as an advanced material for fabricating orthodontic brackets.