Fabrication of Al2O3-SiO2 ceramics through combined selective laser sintering and SiO2-sol infiltration

In this study, different posttreatment methods, including silica-sol infiltration (SI), vacuum silica-sol infiltration (vSI), debinding (DB), and pressure-less sintering (PS), were combined with selective laser sintering (SLS) to fabricate Al₂O₃-SiO₂ ceramics. The macro-morphology and microstructure of sample fabricated under different laser processing parameters and posttreatment process were investigated. Results show that the geometric dimension accuracy and surface quality of the final samples can be effectively improved with appropriate SLS parameters and posttreatment. The optimal SLS processing parameters are determined to be 0.15 mm, 10 W, 0.1 mm, and 1500 mm/s for the hatch spacing, laser power, layer thickness, and scanning speed, respectively. The SLS/DB/vIN/FS samples have the smallest linear shrinkage ratio (<1%), the least warpage degree (<3%), and the best surface quality (surface altitude difference <170 μm). Mullite, quartz, corundum, and cristobalite composed the phases of the sample, of which cristobalite came largely from the infiltrated silica-sol. Since a higher amount of silica-sol infiltrated into the sample under SLS/DB/vIN/FS process, more cristobalite phase formed in the pore of the sample during sintering, which avoided excessive microstructure shrinkage during sintering and ensured the high geometric accuracy and surface quality of the final sample.     

Indirect selective laser sintering of epoxy resin-Al2O3 ceramic powders combined with cold isostatic pressing

To fabricate Al₂O₃ ceramic components with complex shape, selective laser sintering (SLS) combined with cold isostatic pressing (CIP) process was used to consolidate Al₂O₃ powder with additive of epoxy resin E06 (ER06) and polyvinyl alcohol (PVA). The starting material preparation combined spray drying with mechanical mixing to formulate compound powder consisting of PVA (1.5 wt%), ER06 (8 wt%) and Al₂O₃ and provide a good fluidity for SLS. Experimental investigations were carried the shrinkage, relative density, bending strength of Al₂O₃-ER06 SLS specimens in order to optimize the laser sintering parameters. It was found that Al₂O₃-ER06 SLS specimens represented acceptable shrinkage, high density and bending strength when laser power, scanning speed, scanning space and layer thickness were, respectively, 21 W, 1600 mm/s, 100 μm and 150 μm. Following that, the SLS specimens were processed through CIP to eliminate the pores in green ceramics. Finally, the optimized SLS/CIP Al₂O₃ specimens were debinded, sintered to produce crack-free Al₂O₃ bodies. The final Al₂O₃ components achieved a relative high density of more than 92% after furnace sintering. The study shows a novel and promising approach to fabricate complex ceramic matrix and ceramic components via indirect SLS and CIP process.     

Additive manufacturing of zirconia parts by indirect selective laser sintering

Thermally induced phase separation (TIPS) was used to produce spherical polypropylene–zirconia composite powder for selective laser sintering (SLS). The influence of the composition of the composite starting powder and the SLS parameters on the density and strength of the composite SLS parts was investigated, allowing realizing SLS parts with a relative density of 36%. Pressure infiltration (PI) and warm isostatic pressing (WIPing) were applied to increase the green density of the ZrO₂–PP SLSed parts. Infiltrating the SLS parts with an aqueous 30 vol.% ZrO₂ suspension allowed to increase the sintered density from 32 to 54%. WIPing (135 °C and 64 MPa) of the SLS and SLS/infiltrated complex shape green polymer–ceramic composite parts prior to debinding and sintering allowed raising the sintered density of the 3 mol Y₂O₃ stabilized ZrO₂ parts to 92 and 85%, respectively.     

Ceramic Powder Bed Laser Sintering (CPBLS) on copper-doped hydroxyapatite: Creation of thin (5–50 μm thick) consolidated ceramic patterns

Implants made of ceramics, and more particularly of calcium phosphates (hydroxyapatite: HA, mainly), promoting intimate contact with natural bone are nowadays merging. Addition of copper ions in bio-ceramics is expected to increase the biological compatibilities of bone graft substitutes. Previous works have shown that copper-doped hydroxyapatite (Cu-doped HA) ceramics can be prepared by solid-state sintering between HA and CuO powder mixtures at about 1100 °C; but, copper-substituted HA was found to be metastable leading to apatitic grains and Cu-rich grain boundaries during the sintering process. Ultra-rapid sintering is so needed. Selective laser sintering (SLS) is an additive manufacturing process that possesses the advantage to be based on ultra-fast sintering process under laser irradiation. SLS being used in literature for the application of laser on polymer-ceramic or poymer-metal composites the proper term all along the paper is Ceramic Powder Bed Laser Sintering (CPBLS). To achieve densification of Cu-doped HA ceramics from CPBLS process, one should control the composition/morphology/structure of the powder bed as well as three other important CPBLS parameters: (i) the applied energy from the laser beam, (ii) the laser power and the laser scanning speed, (iii) the distance between two successive lased lines. In this paper, the impact of all the main CPBLS parameters controlling the sintering of dip-coated Cu-doped HA layers on glass substrates is carefully investigated. Possibility of the creation of thin consolidated Cu-doped HA ceramic patterns, using the ultra-fast CPBLS process, is finally shown.     

Research on selective laser sintering of Kaolin–epoxy resin ceramic powders combined with cold isostatic pressing and sintering

In order to fabricate traditional products with complex shapes consisting of Kaolin ceramic, selective laser sintering (SLS) combined with cold isostatic pressing (CIP) process was used to consolidate Kaolin powder with additive of epoxy resin E06. To begin preparing the material, epoxy resin (10 wt%) and Kaolin were combined through mechanical mixing, which provided a good fluidity for SLS. Investigations on the shrinkage and micro topography of Kaolin–epoxy resin SLS samples were conducted to optimize the laser sintering parameters. It was found that SLS samples represented acceptable shrinkage and high density when laser energy density was 0.3300–0.3763 J/mm². Then the SLS samples were processed by CIP to eliminate the pores in green ceramics. Finally, the optimized SLS/CIP Kaolin samples were debinded and sintered to produce crack-free Kaolin ceramics. The “Yellow Duck” Kaolin ceramic product was fabricated by combining SLS/CIP with colored glazing. The study shows a novel and promising approach to fabricate complex traditional ceramic products via SLS combined with CIP and sintering.     

Enhancement of piezoelectric properties of BF–BT ceramics by using ZrO2 powder bed during the sintering process

ZrO₂ powders of various particle sizes (0.15, 0.7, 500 µm) were used to simulate loose powder bed sintering to prepare BF–BT piezoelectric ceramics. The phase structure, dielectric properties, ferroelectric properties, and piezoelectric properties were compared with the samples sintered by the conventional powder bed method (i.e., powder of the same composition as the sample). Results showed that the use of loose ZrO₂ powder bed could improve the heat conduction rate and the sintering quality of bulk BF–BT piezoelectric ceramics. The XPS results showed that the samples sintered with 500 µm ZrO₂ powder beds had the lowest concentration of Fe²⁺, exhibited the largest piezoelectric coefficients (d₃₃ = 201 pC/N). In contrast, the sample sintered with a conventional powder bed under the same sintering conditions had a piezoelectric coefficient d₃₃ of 156 pC/N.     

Formability of Fe-doped bioglass scaffold via selective laser sintering

Because of its outstanding characteristics, bioglass is considered a potential bone substitute; however, it is difficult to be fabricated into a scaffold because of insufficient strength. Although there are several methods for producing a three-dimensional ceramic scaffold, most of these methods cannot completely mimic the bone structure. In this study, a bioglass scaffold was fabricated through selective laser sintering (SLS) with the addition of the iron element that could ascend the laser absorption rate with the improvement of the formability and mechanical strength of scaffolds. As a result, the laser absorption proficiency improved with an increase in the amount of iron added; a competent bioglass scaffold could be successfully manufactured with a 5% iron element addition at the energy density of 2.5 cal/cm² (3-W power and 120 mm/s scan speed). In a comparison of scaffolds sintered with various parameters of the heat treatment, scaffolds that had favourable mechanical strength and cell survival rate could be acquired after sintering at 1100 °C. According to the result of the present study, a competent biocompatible bioglass scaffold could be obtained using the SLS process with the addition of the iron element and suitable post-processing parameters.     

工艺参数对PS/改性滑石粉SLS烧结件力学性能的影响

利用硅烷偶联剂KH560对滑石粉进行表面改性,之后将其与聚苯乙烯(PS)粉机械共混,制备PS/改性滑石粉复合粉末。在预热温度85℃和8层网格支撑等条件下,采用选择性激光烧结(SLS)工艺将粉末制备成烧结件。采用扫描电子显微镜观察了滑石粉与PS的界面,发现通过对滑石粉进行表面改性,不仅可以使其均匀地分散于PS粉中,而且两者的相容性也得到了改善。通过正交实验法研究了SLS工艺参数对PS/改性滑石粉烧结件力学性能的影响。利用极差分析法与综合平衡法得到了多指标下的最优工艺参数组合,即单层厚度0.18 mm,扫描间距0.28 mm,激光功率27 W,扫描速度1 200 mm/s,此时PS/改性滑石粉烧结件的拉伸强度为4.29 MPa,弯曲强度为14.4 MPa,冲击强度为4.4 k J/m~2,相比纯PS粉烧结件分别提高了4.9%,10%和56%。     

Ultra-fast,selective, non-melting,laser sintering of alumina with anisotropic and size-suppressed grains

In this paper, we report an ultra-fast sintering phenomenon of alumina achieved by the scanning laser irradiation method. Using CO₂ laser irradiation, we found that micrometer-sized alumina powder (d₅₀ = 1.2 µm) can be sintered close to full density within a few tens of seconds. The microstructure of laser-sintered alumina was different from that of the furnace-sintered alumina. The relative density and grain size of the laser-sintered alumina gradually decreased from the center of the laser beam to the edge. Anisotropy of the grain size was measured along and perpendicular to the scanning direction. This anisotropy decreased as the scanning speed decreased from 0.1 mm/s to 0.01 mm/s. The sintering master curve of grain size versus relative density, which reflects the sintering mechanism, was found to be affected by the laser scanning speed. When the laser scanning speed was 0.1 mm/s, grain size suppression was found for the almost fully dense alumina. However, at lower scanning speed (e.g., 0.01 mm/s), there was significant grain growth in the regions where the relative density was greater than 90%. These results clearly indicate that alumina can be sintered, in the solid-state, to a high density in a short time using scanning laser and the microstructure is different from the furnace-sintered alumina.     

Sintering mechanisms of Yttria with different additives

The sintering behaviour of conventional yttria powder was investigated, with emphasis on the effect of sintering additives such as B₂O₃, YF₃, Al₂O₃, ZrO₂, and TiO₂, etc. at sintering temperatures from 1000 °C to 1600 °C. Powder shrinkage behaviour was analysed using a dilatometer. The powder sintering mechanisms were identified at different temperatures using powder isothermal shrinkage curves. This analysis showed that the sintering additives B₂O₃ and YF₃ could improve yttria sintering by changing the diffusion/sintering mechanisms at certain temperatures, while sintering additives TiO₂, Al₂O₃ and ZrO₂ appeared to retard the powder densification at temperatures around 1000 °C and are more suitable when used at temperatures in excess of 1300 °C. The powder with La₂O₃ added had the slowest densification rate throughout the test temperatures in this experiment and was also found to be more suitable when used at temperatures higher than 1550 °C.     

High-strength and wave-transmitting Si3N4–Si2N2O-BN composites prepared using selective laser sintering

In this study, high-strength and wave-transmission silicon nitride (Si₃N₄) composites were successfully developed via selective laser sintering (SLS) with cold isostatic pressing (CIP) after debinding and before final sintering, and the optimal moulding process parameters for the SLS Si₃N₄ ceramics were determined. The effects of the sintering aids and secondary CIP on the bulk density, porosity, flexural strength, fracture toughness, and wave-transmitting properties of the Si₃N₄ composites were studied. The results showed that the increased CIP pressure was beneficial to the densification of SLS Si₃N₄ ceramics and improved their mechanical properties. However, the wave-transmitting performance decreased as the CIP pressure increased. The Si₃N₄ ceramics prepared by the moulding of sample S₁₁ were more in line with the performance requirements of the radomes. To obtain good comprehensive performance, an additional 3% of interparticle Y₂O₃ was added to the pre-printed mixed powder of granulated Si₃N₄ particles and resin and the secondary CIP pressure was adjusted to 280 MPa. After sintering, the bending strength, fracture toughness, and dielectric constant of the Si₃N₄ ceramics were 651 MPa, 6.0 MPa m^1/2, and 3.48 respectively. This study provides an important method for preparing of Si₃N₄ composite radomes using SLS process.     

Direct selective laser sintering of hexagonal barium titanate ceramics

A direct selective laser sintering (SLS) process was combined with a laser preheating procedure to decrease the temperature gradient and thermal stress, which was demonstrated as a promising approach for additive manufacturing of BaTiO₃ ceramics. The phase compositions in BaTiO₃ ceramics fabricated by SLS were investigated by X-ray and neutron diffractions. The surface morphologies and cross-section microstructures were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). A dense hexagonal h-BaTiO₃ layer was formed on the surface and extended to a depth of 500 μm, with a relative density higher than 97% and absence of pores or microcracks. SLS resulted in the formation of the high-temperature phase, h-BaTiO₃, which was retained at room temperature possibly due to the high cooling rate. The grain boundaries of SLSed h-BaTiO₃ ceramics consist of a Ti-rich secondary phase. Compared with that of the pressureless sintered t-BaTiO₃ ceramics, the Vickers hardness of SLSed h-BaTiO₃ is 70% higher.     

Preparation of alumina/polystyrene core-shell composite powder via phase inversion process for indirect selective laser sintering applications

Indirect selective laser sintering (SLS) is one of the promising additive manufacturing (AM) methods that can process conventionally difficult or even impossible materials such as ceramics. In this work, an innovative phase inversion technique is used to fabricate spherical alumina particles coated with a thin layer of polystyrene (PS). Then, indirect SLS is used to fabricate green parts from the 6 wt% PS coated alumina particles via a Nd:YAG laser. The assessed SLS process parameters were the scan speed, laser power, scan spacing, pulse frequency, and pulse width. The characterization of the AL₂O₃/PS core-shell composite particles was described using techniques including SEM (for morphology), FT-IR (for chemical bonding at the interfaces), TGA (for mass loss), and DSC (for glass transition temperature, T_g). 3D green parts were then fabricated using proper process parameters as a proof of the feasibility of using SLS technique for AL₂O₃/PS core-shell composite powder. The results showed that using a Nd:YAG laser with less absorption by alumina and PS provides greater penetration through a powder bed. In addition, the possibility of sound connections among particles in every direction was observed due to the uniformity of the coating process in spite of a minimal amount of binder. In addition, green part density measurements show high values compared to previously reported results.     

尼龙6的选择性激光烧结成型工艺实验研究

使用尼龙6(PA6)粉末材料进行选择性激光烧结(SLS)成型实验,以成型件的成型精度和表面粗糙度作为衡量指标,通过控制变量法、正交试验以及极差分析研究了预热温度、激光功率和扫描速度对其成型质量的影响。结果表明,PA6粉末材料SLS成型件的X向和Y向尺寸精度以及侧面表面粗糙度并不会明显受到相关工艺参数的影响,其均存在于-1.26%^-0.99%和-1.96%^-1.29%以及16.91~19.87μm范围内;以成型件的成型精度和上表面粗糙度作为衡量指标,PA6粉末材料SLS成型的最优工艺参数组合为:预热温度115℃,激光功率35 W和扫描速度1800 mm/s;在最优条件下进行烧结验证实验,得出成型件的X向、Y向和Z向的成型尺寸精度分别为-1.13%、-1.48%和0.75%;上表面及侧面的粗糙度分别为14.6和18.55μm。     

A comparative study of the properties of terbium aluminum garnet powder sintered in air,vacuum and by laser irradiation

The structural and optical properties of terbium aluminum garnet (TAG) powder sintered (～1100 °C) in air, vacuum (～10^?6 mbar) and with 70 W of unfocussed CW CO₂ laser radiation, have been studied using X-ray powder diffraction (XRD), scanning electron microscopy (SEM/TEM), FTIR, optical absorption and photoluminescence techniques. Structural properties of TAG are found to be independent of the sintering procedure except that the pure TAG crystalline phase (Tb₃Al₅O₁₂) is evolved in about 2 h in the case of laser sintering compared to 8 h needed in air sintering (by furnace) and 4 h needed in the case of vacuum furnace sintering. On the other hand, the absorption/emission intensity (300–600 nm region) of TAG samples sintered in vacuum is higher compared to that of laser/furnace sintering in air.     

Mechanisms responsible for the onset of selective laser flash sintering of 8-YSZ

Selective laser flash sintering (SLFS) is a variation of flash sintering where the only external heat source is a scanning laser. The scanning laser locally heats a region of the sample between two electrodes, initiating measured current flow at a threshold electric field and laser energy density. This study focuses on understanding how charge transport occurs during stage I SLFS in 8 mol% yttria stabilized zirconia. Two potential charge transport mechanisms are considered: (1) a continuous current moving along a hot line between electrodes and (2) charge transported in a discrete bundle within a hot spot, localized to the area under the laser beam. Two laser scan patterns are employed to experimentally determine how charge is transported during stage I SLFS. Numerical modeling is used to estimate the temperatures at which SLFS initiates, which allows the calculation of charge carrier densities and mobilities relevant for the onset of SLFS. Results demonstrate that both a discrete bundle of charges and continuous flow of charge carriers contribute to the current at the onset of SLFS.     

Microstructure and electrical properties of ZnO–Bi2O3-based varistor ceramics by different sintering processes

The effect of sintering processes, such as open sintering, sintering inside a closed crucible, and sintering within a powder bed, on the microstructure and V–I characteristics of ZnO–Bi₂O₃-based varistor ceramics was investigated at sintering temperatures in the range 1000–1200 °C. The results from the experiments showed that the microstructure and electrical properties of the samples varied according to the sintering method and temperature. Optimal values for the electrical characteristics of the varistor ceramics by different sintering processes were obtained when the sintering was conducted at 1100 °C. At the same sintering temperature, the different processes affected the properties differently. At 1000 °C, the samples sintered within a powdered bed showed better electrical properties than those subjected to the other two processes, while at 1100 or 1200 °C, the samples sintered in an open crucible exhibited the best electrical properties.     

Selective laser sintering of clay‐reinforced polyamide

An experimental investigation has been carried out to study the feasibility of processing blended powder of polyamide (PA) and organically modified nanoclay using selective laser sintering. The effect of nanoclay on the sintering parameters and mechanical properties of the sintered specimen have been studied. This article presents the details of preprocessing studies required and conducted to find suitability of the blended powder material to be processed on SLS machine. A suitable part bed temperature has also been found to avoid curling as well as to ensure the powder reusability. In this work, laser power, beam speed, scan spacing have been considered as influential operating process parameters and are explored using Taguchi's L₉ orthogonal array. Tensile specimens of PA and PA/clay composite have been fabricated as per ASTM D638 standard and tested for ultimate tensile strength, elongation at break, and Young's modulus using universal testing machine. Ultimate tensile strength and elongation at break are found to be decreased in case of PA/clay composite when compared with virgin polyamide. To understand the sintering insight and to explain the behavior of obtained mechanical properties, further investigations have been carried out using material characterization techniques like X‐ray diffraction and scanning electron microscopy. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

Effect of mechanically alloyed sintering aid on sinterability of TiB2

High-melting-point borides are attractive for structural and functional materials used in extreme environments. However, their poor sinterability due to their high melting point and strong covalent bonding have prevented their further applications. In this study, a new sintering process, called transient liquid-phase diffusion sintering (TLPDS), has been developed for high-melting-point borides. TiB₂ compacts were fabricated by spark plasma sintering at 50 MPa for 15 min at temperatures of 1300 and 1600 °C via TLPDS of TiB₂ powder with a eutectic TiB–Ti powder as the sintering aid, prepared via mechanical alloying (MA). Differential scanning calorimetry results indicated that the melting temperature of the obtained sintering aid was lower than its equilibrium melting point. MA of the sintering aid suppressed the open pore fraction to one-third of that in the compact sintered with the aid prepared without MA when sintering at 1300 °C. We also propose a possible mechanism for TLPDS of TiB₂.     

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.