Fabrication of bioactive glass scaffolds by stereolithography: Influence of particle size and surfactant concentration

For decades, bioactive glass (BAG) has been utilized as a competent bone substitute owing to its intrinsic properties, such as outstanding biocompatibility and bioresorbability. Stereolithography (SL) is an additive manufacturing technology used to produce highly accurate three-dimensional BAG-based bone substitutes. However, the preparation of BAG-based SL resin is always a challenge, especially because of the inevitable sedimentation of BAG particles. In this study, BAG particles with different sizes were prepared by dry grinding (BAG_dry, greater particle size) and wet grinding (BAG_wet, finer particle size). Then, BAG_dry or BAG_wet SL resins with various amounts of surfactant were analyzed. The sedimentation rate for BAG powder increased with increasing particle size but decreased with increasing amounts of surfactant added to the resin. BAG_wet SL resins had a longer shelf life, so printing could still be finished after 14 days, whereas BAG_dry SL resins were no longer useable after 5 days. However, the BAG particle size did not affect the printing accuracy or scaffold strength. According to our results, BAG-based SL resin fabricated with BAG_wet (particle size <1.6 μm) and 5 wt% surfactant exhibited better resistance to sedimentation.     

Effects of particle size distribution and sintering temperature on properties of alumina mold material prepared by stereolithography

Alumina mold materials prepared by stereolithography usually have considerable sintering shrinkage, and their properties related to casting have been rarely studied. In this study, alumina molds materials were prepared by stereolithography, and the effects of particle size distribution and sintering temperature on the properties of the materials were investigated. Results show that the viscosity of the slurries decreases as the fraction of fine powder increases, and the particle size distribution affects the curing behaviors slightly. Sintering shrinkage increases as the fraction of fine powder or the sintering temperature increases. Although lower sintering shrinkage can be achieved by sintering at 1350 °C or 1450 °C, the mold materials sintered at lower temperatures would continue to shrink under the service temperature of 1550 °C, and thus 1550 °C is determined as the optimal sintering temperature. As the fraction of fine powder increases, the creep resistance first increases and then decreases, and specimens prepared with 0.1 fraction of fine powder exhibit the best creep resistance with the droop distance of 4.44 ± 0.45 mm. Specimens prepared with 0.1 fraction of fine powder and sintered at 1550 °C exhibit linear shrinkage of 6.36% along the X/Y direction and 11.39% along the Z direction, and have a flexural strength of 78.15 ± 3.50 MPa and porosity of 30.12 ± 0.08%. The resulting material possesses relatively low sintering shrinkage, proper mechanical strength, porosity and high-temperature properties that meet the requirements for casting purposes.     

Stereolithographical fabrication of dense Si3N4 ceramics by slurry optimization and pressure sintering

Photocurable gray-colored Si₃N₄ ceramic slurry with high solid loading, suitable viscosity and high curing depth is critical to fabricate dense ceramic parts with complex shape and high surface precision by stereolithography technology. In the present study, Si₃N₄ ceramic slurry with suitable viscosity, high solid loading (45 vol %) and curing depth of 50 μm was prepared successfully when surface modifier KH560 (1 wt%) and dispersant Darvan (1 wt%) were used. The slurry exhibits the shear thinning behavior. Based on the Beer-Lambert formula, D_p (the attenuation length) and E_c (the critical energy dose) of Si₃N₄ ceramic slurry with solid loading of 45 vol % were derived as 0.032 mm and 0.177 mJ/mm², respectively. Si₃N₄ ceramic green parts with complex shape and high surface precision were successfully fabricated by stereolithography technology. After optimizing the debinding and sintering process for green parts, dense Si₃N₄ ceramics with 3.28 g/cm³ sintering density were fabricated. The microhardness and fracture toughness of as-sintered Si₃N₄ ceramics are ~14.63 GPa and ~5.82 MPa m^1/2, respectively, which are comparable to those of the samples by traditional dry-pressed and pressureless sintering technology. These results show that ceramic stereolithography technology could be promising to fabricate high performance ceramics, especially for gray-colored monolithic Si₃N₄ ceramics.     

The effect of particle size distribution on the microstructure and properties of Al2O3 ceramics formed by stereolithography

Stereolithography (SL) shows advantages for preparing alumina-based ceramics with complex structures. The effects of the particle size distribution, which strongly influence the sintering properties in ceramic SL, have not been systematically explored until now. Herein, the influence of the particle size distribution on SL-manufactured alumina ceramics was investigated, including bending strength at room temperature, post-sintering shrinkage, porosity, and microstructural morphology. Seven particle size distributions of alumina ceramics were studied (in μm/μm: 30/5, 20/3, 10/2, 5/2, 5/0.8, 3/0.5, and 2/0.3); a coarse:fine particle ratio of 6:4 was maintained. At the same sintering temperature, the degree of sintering was greater for finer particle sizes. The particle size distribution had a larger influence on flexural strength, porosity and shrinkage than sintering temperature when the particle size distribution difference reached 10-fold but was weaker for 10 μm/2 μm, 5 μm/2 μm and 5 μm/0.8 μm. The sintering shrinkage characteristics of cuboid samples with different particle sizes were studied. The use of coarse particles influenced the accuracy of small-scale samples. When the particle size was comparable to the sample width, such as 30 μm/5 μm and 5 mm, the width shrinkage was consistent with the height shrinkage. When the particle size was much smaller than the sample width, such as 2 μm/0.3 μm and 5 mm, the width shrinkage was consistent with the length shrinkage. The results of this study provide meaningful guidance for future research on applications of SL and precise control of alumina ceramics through particle gradation.     

Effect of SiC powder on the properties of SiC slurry for stereolithography

Silicon carbide (SiC) is a kind of structural ceramics with excellent properties and it is widely used in industrial fields. Stereolithography (SL) is a potential additive manufacturing technique to fabricate fine complex SiC components, the resin-based SiC slurry with superior rheological and photo-polymerization properties is important for SL. In this paper, we investigated the influence of SiC powder on the properties of the SiC slurries for SL. The physical characteristics of SiC powder such as particle size, size distribution and appearance were tested and observed, and their influence on the dispersion, sedimentation and photo-polymerization property of the SiC slurry were investigated and discussed in detail based on their correlative theory, we finally prepared SiC slurry with superior rheological and photo-polymerization properties, and fabricated the fine complex SiC green body with low defects, high accuracy and high bending strength successfully. The SiC slurry with the solid content of 40 vol% was fabricated by the SiC powder with the median diameter D₅₀ ≈ 10.0 μm and a narrow particle size distribution, it is Bingham fluid with good fluidity and the viscosity of it is 464.40 mPa s under the shear rate of 51.08 s^?1, the cured SiC parts with Z – axis dimension change of 0.75% was finally fabricated, the three points bending strength of it is 50.18 MPa. Our research work provides some fundamental understanding of the SL technique for fabricating fine complex SiC components, explored a suitable way to fabricate high quality SiC green parts through SL, and offers some valuable references for preparing SiC slurry with superior rheological and photo-polymerization properties.     

Photosensitive Si3N4 slurry with combined benefits of low viscosity and large cured depth for digital light processing 3D printing

Digital light processing 3D printing can be applied to fabricate complex silicon nitride (Si₃N₄) components. However, because of the surface hydroxyl groups and large refractive index, it is still a foremost challenge to realize a stable photosensitive Si₃N₄ slurry with combined benefits of low viscosity and large curing depth. In this study, we propose a new formulation strategy to prepare Si₃N₄ slurry. Starting from the optimization of monomer ratio, we have systematically optimized powder particle size, dispersant and photoinitiator on the rheological properties and curing properties of Si₃N₄ slurry. Specifically, we have fabricated a stable photosensitive Si₃N₄ slurry (48 vol%) with a viscosity of 2.09 Pa s (30 s^?1), a critical curing energy of 126.09 mJ/cm² and a maximum curing depth of 80 µm. Finally, based on this optimized slurry, we have successfully obtained complex Si₃N₄ green body with no defect, which demonstrates great potential to fabricate arbitrary complex ceramic components for various applications.     

硅铁粉粒度对合成氮化硅铁的影响

采用FeSi75为原料,利用直接氮化合成法制备了氮化硅铁粉末,研究了中位径(d50)分别为13.41μm、8.023μm和5.229μm的3种硅铁粉分别在1150℃、1250℃和1350℃保温9h处理后的氮化规律。借助XRD、SEM等测试手段测定和观察了产物的物相组成和显微形貌。结果表明:较细的硅铁粉(d50=5.229μm)氮化时,反应快速、剧烈,导致烧结严重,氮化效果差,而较粗硅铁粉(d50=13.41μm)氮化效果较好;较细硅铁粉氮化后易于形成须状、纤维状和柱状氮化硅晶体,较粗硅铁粉氮化后易于形成球状氮化硅团聚体。制备的氮化硅铁中有大量充满氮化硅的孔洞,产物中的Fe3Si与FexSi被其包围,这种结构有利于体现氮化硅铁的优异性能。     

粒度组成对铝镁浇注料基质性能的影响

以电熔白刚玉细粉(≤0.088mm和≤0.047mm)、活性α-Al2O3微粉(d50=2.4μm)、电熔镁砂细粉(≤0.088mm)、CA-80水泥和SiO2微粉作为铝镁浇注料的基质部分,三聚磷酸钠为外加剂,加水共混后,振动成型为25mm×25mm×125mm的试样。自然养护24h后脱模,分别经110℃24h、1400℃3h和1600℃3h热处理。采用跳桌法研究粒度组成对基质浆体流动性的影响,按国标测量烧后试样的线变化率、显气孔率、体积密度和常温强度,并借助XRD、SEM和压汞仪研究粒度组成对基质常温物理性能和处理温度对基质中微孔孔径的影响。结果表明:(1)粒度组成对基质浆体流动性有较大影响,适当降低≤0.088mm白刚玉细粉含量能提高浆体流动性;α-Al2O3微粉的加入量为7.8%时浆体流动性最好。(2)随较细白刚玉细粉(≤0.047mm)含量的增加,1600℃处理后试样的线收缩增大;随α-Al2O3微粉加入量的增加,试样线收缩增大,试样的强度先增大后减小。(3)处理温度从1400℃升至1600℃时,试样内微孔孔径由2μm增大至3.5μm左右。     

Digital light processing of high-strength hydroxyapatite ceramics: Role of particle size and printing parameters on microstructural defects and mechanical properties

Dense hydroxyapatite (HA) bars were fabricated using digital light processing. The roles of HA median particle size (MPS), curing depth-to-layer thickness ratio (CD/LT), and debinding process on the printing/debinding flaws and flexural strength of the sintered parts were investigated. Commercial HA was milled for different times to provide powders with an MPS ranging from 0.3 to 2.7 µm. Thermal debinding led to delamination and vertical cracks, which decreased with increasing MPS; the minimum value required to fabricate specimens with appreciable flexural strength was 0.9 µm. At a given MPS (2.7 µm), the CD/LT varied between 1.4 and 3.3, indicating a progressive disappearance of the above major flaws. Finally, the positive effect of water debinding prior to thermal debinding on reducing crack formation was demonstrated. After optimisation, the bars achieved a flexural strength greater than 100 MPa, which is the highest value among dense HA fabricated using lithography-based techniques.     

Cure behaviour and mechanical properties of Si3N4 ceramics with bimodal particle size distribution prepared using digital light processing

Digital light processing is a vital additive manufacturing technology used for manufacturing ceramic parts. The particle size distribution of ceramic suspensions significantly affects the cure behaviour and mechanical properties of ceramics. In this study, the cure behaviour and mechanical properties of Si₃N₄ ceramics with a bimodal particle size distribution were studied. The results indicated that the suspension with coarse particles had a higher cure depth for a lower absorbance but poor mechanical properties. The bending strength of the samples with the optimal ratio (coarse:fine particles = 3:7) reached a maximum of 728.7 ± 10.33 MPa, which is 16.5% higher than that of the samples prepared using only fine particles.     

Effects of fine grains and sintering additives on stereolithography additive manufactured Al2O3 ceramic

Al₂O₃ ceramics are fabricated by stereolithography based additive manufacturing in present reports. To improve the densification and performance of Al₂O₃ ceramic, the introduction of fine grains or sintering additives has been studied by traditional fabrication techniques. However, no research has focused on the effects of adding fine grains and sintering additives on the stereolithography additive manufactured Al₂O₃ ceramic. In this study, both fine grains and sintering additives were added firstly, and then the effects of fine grains and sintering additives on the relative density, microstructure, mechanical properties, and physical properties of the stereolithography additive manufactured Al₂O₃ ceramics were investigated. Finally, defect-free Al₂O₃ ceramic lattice structures with high precise and high compressive strength were manufactured.     

Effects of surfactant and particle size on the microstructure and strength of Si3N4 foams with high porosity

The highly porous Si₃N₄ ceramic foams were prepared by direct foaming with mixed surfactants. The surface tension and viscosity of slurries were tailored by different carbon chain length of surfactants and different mean Si₃N₄ particle size to achieve the pore size controlling. The nearly linear relationship between the pore size and the ratio of surface tension to viscosity was observed, which indicates that the pore size could be precisely tailored by the slurry properties. Si₃N₄ ceramic foams with porosity of nearly 94%, mean pore size of 110–230 µm, and compressive strength of 1.24–3.51 MPa were obtained.     

Fabrication strategy of complicated Al2O3-Si3N4 functionally graded materials by stereolithography 3D printing

For multi-ceramic materials based on the stereolithography (SL) principle, a 3D printing strategy was developed, and then an Al₂O₃-Si₃N₄ functionally graded material (FGM) ceramic part was fabricated using this strategy. Six groups of mixtures, with a Si₃N₄ content gradient of 20 vol% and a certain bimodal particle size distribution, were prepared using UV-curable pastes. A modified formula was proposed to evaluate the relationship between the actual minimum voidage of mixtures and the viscosities of their corresponding pastes. The viscosity of each paste was controlled using the prediction formula and optimization of dispersants. To design theprinting layer thickness, a mathematical relationship was established between Si₃N₄ content and curing depth of paste. The Al₂O₃-Si₃N₄ green body without deformation was printed using optimized parameters such as a layer thickness of 40 μm and a paste viscosity of ∼13,000 mPa·s. Finally, using debinding and sintering, denseparts having a complicated shape were obtained.     

Effects of particle size on microstructure and mechanical strength of a fly ash based ceramic membrane

Recycling fly ash for ceramic membrane fabrication not only reduces solid waste discharge, but also decreases the membrane cost. Now, fly ash is becoming a promising substitute material for ceramic membrane preparation. A significant difference between fly ashes from different plants is the particle size, which makes performances of fly ash membranes unpredictable. The novelty of this work is to clarify the effects of the particle size of fly ash on ceramic membranes, thereby giving practical suggestions on fly ash selection for ceramic membrane preparation. Ceramic membranes were fabricated with different sizes of fly ashes. Effects of particle size on porosity, pore size, microstructure, mechanical strength and gas permeability of the membrane were investigated. Results indicate that a broader particle size distribution of fly ash leads to a denser structure of membrane with a lower porosity. Pore size and gas permeability of membrane increase while bending strength decreases with the particle size increasing. Bending strength of a fly ash membrane is largely determined by large particles in the fly ash because the large particles lead to cracks in the membrane. This work provides experimental bases for developing high performance ceramic membranes from fly ash.     

Improving cure performance of Si3N4 suspension with a high refractive index resin for stereolithography-based additive manufacturing

Silicon nitride (Si₃N₄) slurries with high solid loading, low viscosity and good stability is difficulty prepared, due to low intrinsic surface charge and a large refractive index (RI) difference between Si₃N₄ powder and resin. In this paper, the curing behavior of Si₃N₄ slurry with different functional group and RI of resin monomer were systematically researched, and then the kind and optimum content of dispersant were investigated. Subsequently, a high solid loading Si₃N₄ slurry (44 vol%) with good curing behavior, low viscosity and favorable stability was successfully prepared. Lastly, the dense Si₃N₄ ceramic parts were fabricated by the suitable Si₃N₄ slurry (44 vol%) via stereolithography. After debinding and sintering process, the relative density and flexural strength of Si₃N₄ ceramic were 98.28% and 800 ± 27.28 Mpa, respectively.     

Analysis of the spectral reflectance and color of mineral pigments affected by their particle size

The color of mineral pigments changes obviously with their particle size. However, how the particle size of these mineral pigments affects the color of the mineral pigment color block remains unclear. Based on optical principles and the physical properties of mineral pigment particles, our analysis found that changes in the particle size not only nonlinearly affect the behavior of light at the first surface of the mineral pigment color block, but also affect the interaction of light with the particles within the body of the mineral pigment color block, ultimately changing the spectral reflectance and color of the mineral pigment color block. Finally, we derived a nonlinear monotonically decreasing relationship between the particle size and the spectral reflectance. The experiment conducted in this article selected six kinds of mineral pigments as color block samples and observed the changes in the spectral reflectance and color value with the particle size. These studies are beneficial for color researchers conducting scientific research related to mineral pigments.     

Development and analysis of a high refractive index liquid phase Si3N4 slurry for mask stereolithography

Ceramic mask stereolithography additive manufacturing technology has the abilities of fast and accurate printing complex and personalized ceramic parts. However, since the ultraviolet light is strongly blocked by the ceramic particles in the slurry during exposure, the slurry with high refractive index ceramic particles has low cure depth, and serious light scattering. This investigation developed a curable silicon nitride slurry with a high refractive index liquid phase, which significantly reduced the refractive index difference between the liquid phase and the silicon nitride ceramic particles. The high refractive index acrylate monomer and solvent were chosen to increase the cure depth while ensuring the curing accuracy. Compared with the slurry whose liquid phase was pure HDDA, the addition of OPPEA and ACMO in the liquid phase showed a better refractive index increasing effect and the strongest cure depth and dimensional accuracy improvement. POE was verified as a suitable non-reactive high refractive solvent. The composition of 20 wt% OPPEA, 10 wt% ACMO, 40 wt% HDDA, and 30 wt% POE were optimized as the high refractive index liquid phase for 40 vol% solid phase silicon nitride slurry. A finite element analysis model of silicon nitride slurry was established, and the distribution of ultraviolet light intensity in silicon nitride slurry with high refractive index liquid phase was numerically simulated.     

Effects of N2 pressure and Si particle size on mechanical properties of porous Si3N4 ceramics prepared via SHS

Porous silicon nitride ceramics with high flexural strength and high porosity were directly fabricated by self-propagating high temperature synthesis (SHS). The effects of N₂ pressure and Si particle size on the phase composition, microstructure, and mechanical property were investigated. N₂ influences not only the thermodynamics but also the kinetics of the SHS as initial reactant. Flexural strength ranged between 67 MPa and 134 MPa with increasing N₂ pressure. On the other hand, flexural strength ranged from 213 MPa to 102 MPa with different Si particle sizes. This plays an important role on the final diameter and length of β-Si₃N₄ grains and the formation mechanism of porous Si₃N₄ ceramics.     

粒度分布对超低水泥刚玉质浇注料流变性的影响

用浇注料流变仪研究了粒度分布对超低水泥刚玉质浇注料流变性的影响。结果表明 :粒度分布对超低水泥浇注料的流变性影响较大。随着粒度分布系数 (q)的减小 (从 0 .2 9、0 .2 6到 0 .2 3) ,浇注料的剪切应力、粘度和屈服应力增加 ,需水量上升 ,说明流变性变差。以 2 %的SiO2 微粉等量替代q =0 .2 3的浇注料中的Al2 O3微粉后 ,试样的流变性得到明显改善 ,更适合用于泵送施工 :浇注料的需水量减少 ,自流值提高。