Selective laser melting of alumina: A single track study

Ceramics-based additive manufacturing is a complex process and the solidification mechanism and microstructural evolution are currently not fully understood. In this work, Al₂O₃ single tracks were formed using a customised selective laser melting (SLM) system equipped with a high power diode laser. The effects of laser energy density (LED) on geometry, microstructure and micro-mechanical properties of Al₂O₃ tracks were investigated. To better understand the solidification mechanism, a transient three-dimensional thermal model was developed for predicting the thermal behaviour of the melt pool. The results indicated the use of high LED gave rise to decreased viscosity and surface tension of the molten alumina and led to localized melting of the substrate. Both, in turn, enabled the formation of a continuous solidified track. The solidified tracks were primarily composed of columnar dendrite. When relatively high LED (≥?25.7?kJ/m) was applied, equiaxed dendrite appeared along the central line near the track surface. The size of dendritic grains decreased with the decreased LED, attributed to the increased cooling rate at solidification interface. The micro-hardness of the solidified track was found to be inversely proportional to the grain size owning to grain boundary strengthening effect.     

Cracks of alumina ceramics by selective laser melting

Alumina ceramic powders have high melting point and are prone to cracking during the rapid heating and cooling process of selective laser melting (SLM). Research on the crack formation and growth mechanisms forms the basis to developing crack suppression techniques. Variable laser power experiments based on single-track, zigzag, and island scanning strategies are designed to analyse crack morphology, distribution state, formation reasons, and extension mechanisms in alumina (Al₂O₃) SLM specimens. Our experiments show that transverse cracks formed by internal stress and longitudinal cracks formed by solidification shrinkage exist in alumina SLM specimens. The transverse cracks continuously expand in melting tracks, while the longitudinal cracks expand along the centre or the juncture of melting tracks. With increasing laser power, the formation and extension length of cracks decrease. Crystal structures exert important influences on the fracture pattern and crack extension of specimens.     

Comparative investigation of microstructure,mechanical properties and strengthening mechanisms of Al-12Si/TiB2 fabricated by selective laser melting and hot pressing

Near-fully dense Al-12Si matrix composites reinforced with TiB₂ ceramic particles (2?wt%) were successfully fabricated by selective laser melting (SLM) and hot pressing (HP) of powder mixtures. TiB₂ ceramic particles are homogeneously distributed in the Al-12Si matrix at the micrometer-scale owing to a very good wetting between molten Al-12Si alloy and TiB₂ ceramic. The microstructural analysis of the as-fabricated SLM samples show the formation of a supersaturated α-Al phase and the decrease of free residual Si with respect to the hot-pressed ones. Both composites exhibit a fine microstructure with a grain size of ~?5.1?µm and ~?5.8?µm for SLM- and HP-fabricated samples with addition of TiB₂ ceramic particles. The SLM Al-12Si/TiB₂ composite exhibits significantly improved microhardness (~?142?±?6.0 HV_0.05) and yield strength (~247?±?4.0?MPa) compared to the corresponding HP one. Fine cell morphology and nanostructured dispersion strengthening are responsible for the improved mechanical strength of the Al-12Si/TiB₂ composite processed by SLM.     

3D打印成型陶瓷零件坯体及其致密化技术

3D打印技术在陶瓷零件成型方面具有较大应用潜力,被认为是近净尺寸成型高性能复杂结构陶瓷零件的一种新途径。本文比较了陶瓷零件或其坯体的激光选区熔化、薄材叠加制造、熔融沉积造型、光固化、三维打印和激光选区烧结等不同3D打印工艺及其致密化手段的优势和不足,认为较低的相对密度和强度是阻碍3D打印陶瓷零件实现产品应用的主要障碍。本团队近年来采用造粒混合法制备出具有良好流动性的3D打印复合陶瓷粉体,再通过激光选区烧结(SLS)和冷等静压(CIP)技术分别进行坯体成型及均匀致密化处理,制备出了高性能、复杂结构的Al_2O_3致密陶瓷零件。本文回顾了这些工作,并补充介绍了溶解沉淀和溶剂蒸发这两种制备复合陶瓷粉体的新方法,利用SLS/CIP复合工艺进一步制造了ZrO_2、SiC、高白土等其它材质的复杂陶瓷零件,为3D打印陶瓷用于航空航天、医疗、艺术等领域奠定了基础。     

One-step additive manufacturing and microstructure evolution of melt-grown Al2O3/GdAlO3/ZrO2 eutectic ceramics by laser directed energy deposition

Synchronized-powder-feeding-based laser directed energy deposition (LDED) has great application potential for the rapid fabrication of large-scale composite ceramics with complex shapes. In this study, near-full-density Al₂O₃/GdAlO₃/ZrO₂ ternary eutectic ceramics with different shapes and smooth surfaces were directly prepared by using an improved LDED device. Spherical ceramic powders with eutectic composition and good flowability were obtained by centrifugal spray drying. The microstructure characteristics and microstructure evolution of the rapidly solidified 3D-printed eutectic ceramic were systematically elucidated. In particular, the formation mechanism of the observed periodic banded structures was revealed through a unique laser partial remelting technique. The result indicated that the appearance of the banded structure is attributed to the drastic abnormal coarsening of the nanoscale microstructures adjacent to the molten pool. On the basis these results, a physical model was proposed to illustrate the microstructure evolution of the 3D-printed Al₂O₃/GdAlO₃/ZrO₂ eutectic ceramic.     

Direct laser melting of Al2O3 ceramic paste for application in ceramic additive manufacturing

We develop the direct laser melting of ceramic paste technology for application in ceramic additive manufacturing (AM). The Al₂O₃ ceramic paste, which is a homogeneous mixture of DI-water and Al₂O₃ ceramic powders, was deposited on an Al₂O₃ substrate using free-forming extrusion (FFE), and subsequently melted by a CO₂ laser. To better control the laser melting process, the flow behavior of the laser-melted Al₂O₃ was investigated by evaluating the microstructure of the laser-melted Al₂O₃ single tracks. When the laser scanning speed increased from 1 to 3.5 mm/s at a fixed laser power, the permeation of the molten Al₂O₃ into the surrounding porous paste was reduced, resulting in the improvement of the surface uniformity of the laser-melted Al₂O₃ tracks. Through optimizing the laser scanning strategy, a fully-dense Al₂O₃ layer with smooth surface was achieved. The phase composition and density of the laser-melted Al₂O₃ layers were evaluated to study their properties. The thickness of the dense Al₂O₃ layer varied from ～90 μm to ～120 μm periodically due to the line-by-line scanning of the Gaussian laser beam. In addition, the relationship between the melting thickness and the laser scanning speed was also investigated to further improve the controllability of the laser melting process. This direct laser melting of ceramic paste technology is promising for applications in ceramic AM, such as 3D printing of ceramic components and high-temperature ceramic welding.     

Laser deposition of compositionally graded titanium oxide on Ti6Al4V alloy

In this study, a laser cladding process was developed to deposit dense and well-adhered titanium single tracks on the surface of Ti6Al4V alloy with a compositional and microstructural gradient. CuO doped, freeze-dried anatase powder was specially formulated for this process. The addition of CuO resulted in stable melt pool with low viscosity, low surface tension and enhanced wettability with the substrate. Continuous titanium oxide single tracks were formed with a cross-sectional profile that was advantageous for coating deposition by means of multiple overlapping scan tracks. Rapid heating and cooling associated with laser cladding produced unique solidified microstructures with a compositional gradient. No structurally critical fractures were observed in the graded oxide layers, or at the coating/substrate interfaces. Furthermore, a transition zone of oxide/metal mixture was observed at the interface, increasing the effective bonding area between the coating and the substrate.     

Deformation and fracture mechanisms of in situ synthesized TiC reinforced TC4 matrix composites produced by selective laser melting

In this study, TiC/TC4 composites were fabricated using selective laser melting (SLM), and the deformation mechanism and fracture characteristics of the composites with nano-sized TiC particles formed in situ were studied. The experimental results showed that the rapid melting and solidification characteristics of SLM and the Marangoni effect of the liquid pool promoted a considerably homogeneous dispersion of the in situ-formed nanoscale-TiC reinforcement in the TiC/TC4 composites. In particular, an enhanced compressive strength of 1490.2 MPa and a considerable fracture elongation of 21.5% were simultaneously achieved for the TiC/TC4 composites, which could be attributed to the load transfer effect and the formation of denser and more uniformly distributed dimples. Combined with the finite element (FE) analysis, the uneven stress distribution in the shear band of the TiC/TC4 composites led to the fracture. Further, the fracture surface analysis showed that the in situ nanoscale TiC reinforcement promoted the fracture of microbubbles from the α/β interface with the concentrated distribution of the V element to the interface between TiC and the Ti matrix because of the load transfer, which promoted the uniform distribution of the V element in the dimple.     

Effect of scanning speed on the solidification process of Al2O3/GdAlO3/ZrO2 eutectic ceramics in a single track by selective laser melting

Al₂O₃/GdAlO₃/ZrO₂ ternary eutectic ceramics with fine microstructure were directly fabricated from mixed pure ceramic powders by selective laser melting. The specimen forming quality, molten pool morphology and microstructure characteristic were investigated as functions of scanning speed. Solidification defects such as cracks and pores were effectively suppressed when the scanning speed was 12 mm/min. The relative density of the as-solidified eutectic specimens decreased from 98.7% to 95.7% with increasing the scanning speed up to 48 mm/min. The melting in this study was governed by conduction mode, leading to a decrease tendency of both melting width and depth with the increase of the scanning speed. Different from ordinary cognition, the eutectic spacing in top zone of the molten pool first decreased and then increased with increasing the scanning speed from 6 mm/min to 48 mm/min. The transition point appeared at 12 mm/min, where the dominant factor affecting the solidification rate changed from the scanning speed to the value of the angle between microstructure growth direction and laser scanning direction.     

Laser additive manufacturing of melt-grown Al2O3/GdAlO3 eutectic ceramic composite: Powder designs and crack analysis with thermo-mechanical simulation

Directed energy deposition method is an efficient one-step laser additive manufacturing technology to achieve eutectic ceramic composite with high property and ultra-fine microstructures. In this paper, melt grown dense Al₂O₃/GdAlO₃(GAP) eutectic ceramic composites have been directly fabricated from the spherical powder reconstructed by an optimized spray granulation method. Effects of the powder size distribution, feeding rate, and heat treatment on the morphology and microstructure of the as-solidified eutectic ceramic composites have been investigated. Results show that the powder fluidity plays an important role in the heat conduction of the laser process. Finer powder (imperfect spherical powder with diameter less than 10 µm) gives rise to the disturbance of molten pool. Moreover, this powder greatly aggravates the phenomenon of powder’ sticking on surface of the specimen, which subsequently induces the leading growth of coarse dendrite-like GAP primary phases (higher interface temperature of dendrite tip for GAP phase) and sintered eutectic phases at the specimen edge. The finite element modeling (FEM) method is used to analysis the coupled thermal dynamic during the process after verification with infrared thermal image. It shows that longitudinal maximum principal stress exhibits a steep gradient at the edges of the as-solidified ceramic, making the specimen susceptible to cracking along the deposited direction at the first few layers. By optimizing the feedstock powder characteristics and the directed energy deposition process, completely solidified cylindrical and thin-walled Al₂O₃/GAP eutectic ceramic composites with the maximum dimensions of ? 4 × 95 mm³ and 10 × 4 × 44 mm³ have been successfully fabricated. The solidified specimens present smooth glossy surface and fine microstructures with the average eutectic spacing of 0.31 µm. The average micro-hardness and fracture toughness of 15.16 ± 0.29 GPa and 4.3 ± 0.09 MPa·m^1/2 have been obtained, respectively.     

SLM printing of cermet powders: Inhomogeneity from atomic scale to microstructure

It is very challenging for 3D printing based on the selective laser melting (SLM) technology to obtain cermet bulk materials with high density and homogeneous microstructures. In this work, the SLM process of the cermet powders was studied by both simulations and experiments using the WC-Co cemented carbides as an example. The results indicated that the evolution of the ceramic and metallic phases in the cermet particle during the heating, melting and solidification processes were all significantly inhomogeneous from atomic scale to mesoscale microstructures. As a consequence, the microstructural defects were caused intrinsically in the printed bulk material. The formation and growth of the bonding necks between the particles were mainly completed at the later stage of laser heating and the early stage of solidification. Both simulations and experiments demonstrated that thin amorphous layers formed at the ceramics/metal interfaces. This work disclosed the mechanisms for the evolution from the atomic scale to microstructure during the SLM printing of cermet powders, and discovered the origin of the defects in the printed cermet bulk materials.     

Pore formation model for direct laser deposition of Al2O3–ZrO2 ceramic

Pores are some of the most common defects that form during direct laser deposition of ceramic materials. A mathematical model of pore formation for Al₂O₃-ZrO₂ ceramic was developed. The pore formation model, which was developed from the bubble escape factor, reveals the relationship between the movement of the solid-liquid interface of the molten pool and that of the bubbles. In the frontier region of the molten pool, with increasing laser power, the proportion of bubbles that escaped and the area from which bubbles escaped increased. With increasing laser power, the actual and theoretical porosity decreased from 80 % to 40 %. At the central region of the molten pool, the bubble escape factor increased with increasing bubble diameter under the same laser power. The theoretical porosity and the actual porosity decreased with increasing laser power. The pore formation model provides a basis for fabricating high-quality Al₂O₃-ZrO₂ ceramics by direct laser deposition.     

Writing conducting lines into alumina ceramics by a laser dispersing process

The objective of this work is the development of a laser-supported process that allows to modify the electric and thermal properties of ceramics on a local scale. The principle of the process is based on local melting of the ceramic by a CO₂ laser beam and application of an additive to the molten area on the surface. During solidification, a metal–ceramic composite is formed with modified material properties compared to the bulk material. Different alumina samples were treated with metal powders of tungsten, copper, and oxides of these metals. Scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDX) analysis reveal that the physical and chemical properties of a peripheral zone are changed in the heated region down to a depth of approximately 500 μm. The resulting resistance of the laser tracks can be adjusted from semi-conducting to metallic behavior with a resistivity down to 2×10⁻⁶ Ω/m. The modified ceramic can be used for heating elements working at operation temperatures of up to 1000 °C, high current resistance which can be loaded with current of up to 100 A.     

Preparation and indirect selective laser sintering of alumina/PA microspheres

Indirect selective laser sintering (SLS) is a promising additive manufacturing technique to produce ceramic parts with complex shapes in a two-step process. In the first step, the polymer phase in a deposited polymer/alumina composite microsphere layer is locally molten by a scanning laser beam, resulting in local ceramic particle bonding. In the second step, the binder is removed from the green parts by slowly heating and subsequently furnace sintered to increase the density. In this work, polyamide 12 and submicrometer sized alumina were used. Homogeneous spherical composite powders in the form of microspheres were prepared by a novel phase inversion technique. The composite powder showed good flowability and formability. Differential scanning calorimetry (DSC) was used to determine the thermal properties and laser processing window of the composite powder. The effect of the laser beam scanning parameters such as laser power, scan speed and scan spacing on the fabrication of green parts was assessed. Green parts were subsequently debinded and furnace sintered to produce crack-free alumina components. The sintered density of the parts however was limited to only 50% of the theoretical density since the intersphere space formed during microsphere deposition and SLS remained after sintering.     

Al2O3 loss prediction model of selective laser melting Al2O3–Al composite

The element/phase loss is undesirable but existing during selective laser melting (SLM) of materials with volatile element/phase, which not only changes the material composition but also affects the molten pool flow. In the previous researches, the effect of remelting on the element/phase loss was neglected during the SLM process, instead, laser energy density was thought to be uppermost. In fact, the SLM process fabricates the parts in a manner of line by line and layer by layer, i.e., additive character, and the remelting in the overlap zone occurs during the SLM process. In this paper, three different Al₂O₃ loss prediction models of SLM Al₂O₃–Al composite by considering the additive character of SLM and the distribution of the Al₂O₃ associated with the different molten pool driving forces were developed. By comparing with the experimental results and predicted results, it is found that the Al₂O₃ is distributed on both sides of the molten pool under the combined action of the Marangoni flow and the evaporation recoil pressure. This kind of Al₂O₃ distribution enhances the effect of the remelting on the Al₂O₃ loss, i.e., the remelting brings a logarithmic increase in the Al₂O₃ loss rate. This determines the final Al₂O₃ loss rate of the SLMed 3D samples. During this study, although the Al₂O₃ loss rate of the single-track is only 33%, the loss rate of SLMed 3D samples increases significantly to 97% when the hatching space of 60 μm and scanning speed of 200 mm/s are utilized, i.e., almost no Al₂O₃ in the 3D sample. Thus, it is more important to reduce the remelting, i.e., overlap rate for reducing the element/phase loss. This study is a benefit for understanding and reducing the element/phase loss in SLM.     

Additively manufactured mesostructured MoSi2-Si3N4 ceramic lattice

Lattice structures, their shape, orientation, and density make the critical building blocks for macro-scale geometries during the AM process and, therefore, manipulation of the lattice structure extends to the overall quality of the final product. This work reports on manufacturing of MoSi₂-Si₃N₄ ceramic lattices through a selective laser melting (SLM) approach. The strategy first employs the production of core-shell structured MoSi₂/(10-13?wt%)Si composite powders of 3–10?μm particle size by combustion synthesis followed by SLM assembly of MoSi₂/Si lattices and their further nitridation to generate MoSi₂-Si₃N₄ mesostructures of designed geometry. Experimental results revealed that the volumetric energy density of SLM laser has remarkable influence on the cell parameters, strength, porosity and density of lattices. Under compressive test, samples sintered at a higher laser current demonstrated a higher strength value. Selective laser melting has shown its potential for production of cellular lattice mesostructures of ceramic-based composites with a low content of a binder metal, which can be subsequently converted into a ceramic phase to produce ceramic-ceramic structure.     

Densification behaviour and three-dimensional printing of Y2O3 ceramic powder by selective laser sintering

The selective laser sintering (SLS) of an yttria (Y₂O₃) ceramic powder was studied to understand both the effects of i) the initial yttria particle characteristics on the powder bed behaviour and ii) the process conditions (laser power, scanning speed, hatching space) on the sintering/melting of three-dimensionally printed objects. The roughness of the powder bed, a sensitive indicator of the layer bed quality, was determined through three-dimensional optical profilometry and the powder bed packing density was modelled using the discrete-element method. Complex shaped objects including spheres and open rings were successfully fabricated by the SLS three-dimensional printing. In addition, SLS cube-shaped samples were characterized by X-ray diffraction and scanning electron microscopy. The open pore volume fraction significantly decreased from 41% without a post-SLS heat treatment to 31% with a post-SLS heat treatment at 1750 °C for 20 h under secondary vacuum. Finally, an anisotropy in elastic properties has been highlighted, Young's modulus reaches 11 GPa in the stiffest direction.     

Ni–YSZ cermet micro-tubes with textured surface

Tubular Ni–YSZ porous cermets, with the external surface textured in the form of submicron size alternating YSZ and porous Ni lamellae aligned perpendicular to the tube surface have been fabricated. The surface of the ceramic tubes of eutectic composition was directionally solidified in the radial direction using the laser zone melting procedure where the power of the laser was adjusted to melt a thin surface layer. The melt solidified in the very high thermal growth radial gradient produced by radiation losses and convention cooling. A crack free layer with typical eutectic lamellar microstructure, with domains aligned perpendicular to the tube surface, was produced along the external surface of the tubes. The porous cermet tubes were prepared by thermo-chemical reduction of the NiO phase in the previously textured binary NiO–YSZ eutectic precursors. After reduction, porous Ni leaves of about 100 nm lateral dimension were confined between the YSZ lamellae in the textured layer. The influence of growth parameters over microstructure size and morphology is discussed.     

Laser transmission welding of PMMA to alumina ceramic

In this paper, a method of laser transmission welding on ceramic surface after pulse laser microtexture pretreatment was proposed to address the problem that welding ceramics with high transparency polymers is demanded but difficult to be performed. In this method, the polymer flows into the micro-texture of the blind hole on the surface to form mechanical riveting to enhance the welding strength. The formation characteristics and welding mechanism of PMMA welded joint with micro-texture alumina ceramics were studied experimentally and simulatively. The effects of blind hole microtexture size, continuous laser power and continuous laser scanning rate on solution flow and welding strength were studied. The results showed that the air bubbles formed in the welded seam by entering the micro-texture blind hole and trapped air in the blind hole were the key factors affecting the strength of the joint. A 3D finite element model of the transient temperature field and flow field of polymer during laser welding was established. The simulation results showed that the polymer on the left side of the blind hole melted first when heated and inflowed along the wall due to the effects of self-gravity and buoyancy caused by temperature differences. The gas expanded and extruded upward to the left, forming bubbles in the polymer melt pool and pushing the polymer melt into the blind pore microtexture. Finally, a complete molten pool was formed. The flow of polymer melt, the formation of bubbles and the formation of joint were revealed.     

聚碳酸酯粉末的选择性激光烧结成型

以聚碳酸酯(PC)粉末为烧结材料,研究了激光功率等工艺参数对PC烧结件的微观形态、密度和力学性能的影响规律。结果表明,PC烧结件的密度、拉伸强度及拉伸弹性模量、冲击强度均随激光功率增加而增大;但过高的激光功率会导致激光扫描区域的粉末过热,使PC烧结件产生颜色变黄、轮廓不清晰等缺陷。