Fracture and mechanical properties of lightweight alumina ceramics prepared by fused filament fabrication

Fused filament fabrication (FFF), as one of the additive manufacturing technology, provides cost-effective and relatively fast preparation of 3D objects of desired dimensions and design. In this work, a composite filament containing 50 vol. % of sub-micron alumina powder was successfully used for the manufacturing of samples with prismatic design. The influence of the layer thickness (0.1–0.3 mm) on the final bulk density and mechanical properties were investigated. Sintering at 1600 °C for 1 h results in relative densities ranging from 80 to 89 % and the flexural strength reached 200–300 MPa depending on the layer thickness used for the printing.     

Transparent alumina ceramics fabricated by 3D printing and vacuum sintering

Transparent alumina ceramics were fabricated using an extrusion-based 3D printer and post-processing steps including debinding, vacuum sintering, and polishing. Printable slurry recipes and 3D printing parameters were optimized to fabricate quality green bodies of varying shapes and sizes. Two-step vacuum sintering profiles were found to increase density while reducing grain size and thus improving the transparency of the sintered alumina ceramics over single-step sintering profiles. The 3D printed and two-step vacuum sintered alumina ceramics achieved greater than 99 % relative density and total transmittance values of about 70 % at 800 nm and above, which was comparable to that of conventional CIP processed alumina ceramics. This demonstrates the capability of 3D printing to compete with conventional transparent ceramic forming methods along with the additional benefit of freedom of design and production of complex shapes.     

Fabrication of alumina ceramics with functional gradient structures by digital light processing 3D printing technology

Alumina ceramics with different unit numbers and gradient modes were prepared by digital light processing (DLP) 3D printing technology. The side length of each functional gradient structure was 10 mm, the porosity ratio was controlled to 70%, and the number of units were (1 × 1 × 1 unit) and (2 × 2 × 2 unit) respectively. The different gradient modes were named FCC, GFCC-1, GFCC-2 and GFCC-3. SEM, XRD, and other characterization methods proved that these gradient structures of alumina ceramics had only α-Al2O3 phase and good surface morphology. The mechanical properties and energy absorption properties of alumina ceramics with different functional gradient structures were studied by compression test. The results show that the gradient structure with 1 × 1 × 1 unit has better mechanical properties and energy absorption properties when the number of units is different. When the number of units is the same, GFCC-2 and GFCC-3 gradient structures have better compressive performance and energy absorption potential than FCC structures. The GFCC-2 gradient structure with 1 × 1 × 1 unit has a maximum compressive strength of 19.62 MPa and a maximum energy absorption value of 2.72 × 105 J/m3. The good performance of such functional gradient structures can provide new ideas for the design of lightweight and compressive energy absorption structures in the future.     

Sol-gel infiltration of complex cellular indirect 3D printed alumina

Gelled aqueous solutions containing the soluble precursor aluminum chlorohydrate were developed for the infiltration of porous indirect 3D printed alumina. Viscosity and amplitude sweep tests confirmed the gel formation and sheer thinning behavior beneficial for the subsequent coating and infiltration process. High temperature XRD confirmed the formation of corundum at a temperature of 1000?°C. Complex alumina structures with high surface area and isotropic pore channels were achieved by indirect 3D printing. Coating and infiltration of the pre sintered alumina with a subsequent sintering step transformed the precursor to corundum and partially filled the residual porosity and decreased surface defects after 3D printing. With the gel coating a pronounced improvement up to a maximum value of Δσ_compr?=?61.9?MPa was observed and with the gel infiltration a maximum improvement of ΔE?=?136.2?GPa. The results show the possibility to infiltrate even complex alumina structures with aqueous alumina precursors without the need to disperse ceramic particles.     

3D printing of complex shaped alumina parts

Alpha-alumina powder was mixed with methyl cellulose as a binder with concentration as low as 0.25% by weight in an aquoes medium and kneaded in a high shear mixer to obtain a printable paste. The paste was subjected to rheological measurements and exhibited a shear rate exponent of 0.54 signifying the shear thinning behavior. The paste was used for printing parts with various shapes according to CAD model by employing a ram type 3D printer. Printed parts were dried and the green density was determined. Further, the parts were also subjected to X-ray radiography in order to evaluate the possible occurrence of printing defects. The samples were sintered under pressureless condition at 1650?°C in a muffle furnace and Hot Isostsically Pressed (HIP) at 1350?°C and a pressure of 1650?bar using a vacuum encapsulated SS CAN. Hot Isostatic pressing resulted in a higher density of 3.94?g/cc in comparison to 3.88?g/cc obtained under pressureless conditions and also shown superior mechanical properties. HIPing of 3D printed samples not only resulted in possible healing of printing defects as reavealed by X-ray radiography but also enhanced the diffusion at low temperature of 1350?°C leading to finer grain sizes as complemented by the microstructure.     

Silica strengthened alumina ceramic cores prepared by 3D printing

Ceramic cores based on alumina and silica are important in the manufacturing of hollow blades. However, obtaining good properties and precision is still challenging. In this research, alumina-based ceramics cores were obtained by 3D printing technology, and the effects of silica contents on the mechanical properties of the as-obtained alumina ceramic cores were evaluated. The results showed significant improvements in flexural strengths of the ceramics from 13.3 MPa to 46.3 MPa at silica contents from 0 wt% to 30 wt% due to formation of mullite phase (Al₆Si₂O₁₃). By contrast, the flexural strengths declined as silica content further increased due to the generation of massive liquid phase. Also, porous structures and cracks were observed by scanning electron microscopy due to the removal of cured photosensitive resin and the mullitization reaction between alumina and silica, respectively. The manufacturing process of hollow blades required ceramic cores with flexural strengths greater than 20 MPa to resist the strike of metal liquid, as well as open porosity above 20 % to provide space for alkali liquor to dissolve the ceramic cores. As a result, 10 wt% silica was determined as the optimal value to yield ceramics with improved properties in terms of flexural strength (35.6 MPa) and open porosity (47.5 %), thereby satisfy the application requirement for the fabrication of ceramic cores.     

Effect of particle size on mechanical properties of alumina ceramic processed by photosensitive binder jetting with powder spattering technique

As an Additive Manufacturing technique, Binder Jetting enables the fabrication of customized and complex ceramic parts. However, the insufficiency of powder packing in green parts restricts the final products’ densifications and strengths. To form a layer of ceramic green parts, Photosensitive Binder Jetting with powder spattering technique provides entrapment of ceramic powder by printing of photo-curable resin and recoating by releasing the powder through a vibrating mesh. This recoating technique enables the processing of fine alumina powders, the average particle sizes of which are 3 μm, 1.65 μm, and their mixtures. Apparent densities, porosities, mechanical properties, and microstructures of the sintered parts were investigated. The alumina sample with the apparent density of 3.70 g/cm³, the compressive strength of 94.87 MPa, the biaxial strength of 50.06 MPa, and the porosity of 41.01 % was attained by the mixture with 70:30 wt.% of the 3 μm and 1.65 μm powders respectively.     

Fabrication of complex shaped alumina parts by gelcasting on 3D printed moulds

Alumina ceramic components were produced using gelcasting and 3D printing techniques to generate the end product. The 3D printed mould made from (acrylonitrile butadiene styrene) ABS filament provides a convenient demoulding method by dissolution of the mould using acetone as a solvent. This process enables low cost production of complex shaped ceramic components. The effect of the suspension solid loading on the properties and microstructure of complex shaped alumina parts was investigated. The produced ceramic components had densities up to 99.0%, hardness of 18 GPa, flexural strength of 374 MPa and a fracture toughness of 3.8 MPa√m after sintering in air for 3 h, in good agreement with published values.     

Study on surface quality,precision and mechanical properties of 3D printed ZrO2 ceramic components by laser scanning stereolithography

Zirconia (ZrO₂) ceramic bars with three different printing sizes were fabricated by a stereolithographic (SLA) 3D-printing process and subsequent sintering. An anisotropic character of the ceramics surface quality was observed. The surface roughness of the horizontal surface was below 0.41 µm, whereas it reached 1.07 µm along the fabrication direction on the vertical surface. The warpage and flatness were utilized to measure the dimensional accuracy of the 3D printed ZrO₂. Furthermore, it was evaluated that the warpage and flatness were below 40 µm and 27 µm, respectively, even if the printed size of ceramic bar reached 3 mm × 4 mm × 80 mm. In addition, the flexural strength, the fracture toughness, the hardness and the density of ZrO₂ ceramics can reach to 1154 ± 182 MPa, 6.37 ± 0.25 MPa m^1/2, 13.90 ± 0.62 GPa and up to 99.3%, respectively. Moreover, the effects of scanning paths and printing size on properties of the sintered ZrO₂ samples were analyzed. The anisotropic character of surface quality was related to the various scanning paths. The warpage and flatness of 3D printed ZrO₂ bars were apparently affected by the various printed sizes. Also, the effects of special microstructure on the mechanical properties of sintered ZrO₂ samples were investigated.     

Digital light processing stereolithography of zirconia ceramics: Slurry elaboration and orientation-reliant mechanical properties

Digital Light Processing (DLP) is a promising technique for the preparation of ceramic parts with complex shapes and high accuracy. In this study, 3 mol% yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) UV-curable slurries were prepared and printed via DLP. Two different solid loadings (40.5 and 43.6 vol%, respectively) and printing directions were investigated to assess the influence of these parameters on physical and mechanical properties of the sintered parts. Zirconia samples were sintered at 1550 °C for 1 h, achieving a very high relative density (99.2%TD), regardless of solid loading and printing direction. FE-SEM micrographs shown a homogeneous and defect-free cross section with an average grains size of 0.56 ± 0.19 µm. Finally, mechanical properties were influenced by printing direction and zirconia vol%. Indeed, the composition with the higher solid loading (i.e. 43.6 vol%) had the highest three-point flexural strength (751 ± 83 MPa) when tested perpendicular to the printing plane.     

3D gel printing of alumina ceramics followed by efficient multi-step liquid desiccant drying

Dense alumina ceramics were additively manufactured efficiently through a 3D gel printing process. Hydroxyethyl cellulose (HEC) was applied to ensure the printability and rigid of the gel made from boehmite. A multi-step liquid desiccant drying method was implemented to improve the drying efficiency. The results showed that the solid loading and HEC addition were two useful parameters for adjusting the rheology properties of the gel to make it suitable for 3D printing. With polyethylene glycol(PEG) added as liquid desiccants, the printed bodies with section size of 10 mm could be dried within 26 h during which the deformation and crack formation was avoided despite a high linear shrinkage of 45 % was encountered. The successful preparation of dense monolithic alumna ceramics parts with an average grain size of 1 μm, 99 % of the theoretical density and a flexural strength of 380 ± 45 MPa indicated the potential of this process.     

3D printing of porous scaffolds BaTiO3 piezoelectric ceramics and regulation of their mechanical and electrical properties

A series of porous scaffolds of piezoelectric ceramic barium titanate (BaTiO₃) were successfully fabricated by Digital Light Processing (DLP) 3D printing technology in this work. To obtain a high-precision and high-purity sample, the debinding sintering profile was explored and the optimal parameters were determined as 1425 °C for 2h. With the increase of scaffolds porosity from 10% to 90%, the compressive strength and piezoelectric coefficient (d₃₃) decreased gradually. The empirical formulas about the mechanical and piezoelectric properties were obtained by adjusting BaTiO₃ ceramics with different porosity. In addition, the distribution of potential and stress under 100 MPa pressure were studied by the finite element method (FEM).     

Enhanced properties of pure alumina ceramics by oscillatory pressure sintering

A novel oscillatory pressure sintering (OPS) process to consolidate high-quality pure alumina ceramics is reported. The microstructure of the ceramics prepared by OPS develops into a higher final density, a smaller and a narrower distribution of grain sizes compared with those prepared by conventional pressureless sintering (PS) and hot-pressing (HP) processes. Enhanced mechanical properties of alumina ceramics were investigated by OPS process. The bending strength, hardness and elastic modulus of the OPS specimen reached about 546 MPa, 19.1 GPa and 374 GPa, respectively, i.e values significantly higher than that of the specimens by PS and HP. XRD analysis indicates the strengthening of atomic bonds aided by oscillatory pressure. The results suggest OPS to be an effective technique for preparing high-quality pure alumina ceramics.     

Microstructure and mechanical properties of 3D-printed nano-silica reinforced alumina cores

Ceramic cores are an important component in the preparation of hollow turbine blades for aero-engines. Compared with traditional hot injection technology, 3D printing technology overcomes the disadvantages of a long production cycle and the difficulty in producing highly complex ceramic cores. The ceramic cores of hollow turbine blades require a high bending strength at high temperatures, and nano-mineralizers greatly improve their strength. In this study, nano-silica-reinforced alumina-based ceramic cores were prepared, and the effects of nanopowder content on the microstructure and properties of the ceramic cores were investigated. Alumina-based ceramic cores contained with nano-silica were prepared using the vat photopolymerization 3D printing technique and sintered at 1500 °C. The results showed that the linear shrinkage of ceramic cores first increased and then decreased as the nano-silica powder content increased, and the bending strength showed the same trend. The fracture mode changed from intergranular to transgranular. The open porosity and bulk density fluctuated slightly. The weight loss rate was approximately 20%. When the nano-silica content was 3%, the bending strength reached a maximum of 46.2 MPa and 26.1 MPa at 25 °C and 1500 °C, respectively. The precipitation of the glass phase, change in the fracture mode of the material, pinning crack of nanoparticles, and reduction of fracture energy due to the interlocking of cracks, were the main reasons for material strengthening. The successful preparation of 3D printed nano-silica reinforced alumina-based ceramic cores is expected to promote the preparation of high-performance ceramic cores with complex structures of hollow turbine blades.     

Effect of diopside addition on sintering and mechanical properties of alumina

In this paper, diopside was introduced in alumina as a sintering aid and fine structural alumina matrix ceramic materials were fabricated by pressureless sintering. The relative density, hardness, fracture toughness and bending strength of the new fabricated composites were measured. Tribological tests were carried out at a given rotation speed of 160 rpm and in a normal load ranged from 50 to 200 N. The experiment results show that the introduction of diopside can enhance densification rate, which may contribute to the improvement in mechanical properties and result in enhanced wear resistances. The effects of diopside on mechanical properties and microstructures of fine structural alumina matrix ceramic materials were analyzed and discussed.     

DLP 3D printing of scandia-stabilized zirconia ceramics

The present article aims to explore the printability of scandia-stabilized zirconia ceramic parts using desktop and low-cost DLP 3D printer. The acrylate-based homogeneous slurries with zirconia powder stabilized by 6 mol.% of Sc₂O₃ (6ScSZ) and 10 mol.% of Sc₂O₃ and 1 mol.% of Y₂O₃ (10Sc1YSZ) were prepared with appropriate rheological and UV-curing properties. In comparison with yttria-stabilized zirconia, slurries filled with 6ScSZ and 10Sc1YSZ powders reviled lower viscosity at the same solid content. The cure depth of the suspensions was suitable to print the objects with 50 μm of layer thickness, good interlayers connection, and surface finishing. No critical defects in ceramics such as cracks or delamination were observed. Both ceramics have the Vickers microhardness value of 11 GPa and the high ionic conductivity up to 0.2 S/сm at 900 °C demonstrating that the DLP is a promising method of fabricating scandia-stabilized zirconia parts as electrolyte material for SOFC application.     

Influence of debinding holding time on mechanical properties of 3D-printed alumina ceramic cores

Herein, alumina green bodies are fabricated by three dimensional (3D) printing technology, then, the influence of debinding holding time under vacuum and argon on mechanical properties is systematically investigated by comparing the changes in microstructure, bulk density, open porosity, grain connection situation and flexural strength of ceramics. The flexural strength of alumina ceramics acquired the maximum values of 26.4 ± 0.7 MPa and 25.1 ± 0.5 MPa after debinding under vacuum and argon for 120 min and 180 min, respectively. However, the alumina ceramics rendered the flexural strength of 19.4 ± 0.6 MPa and 9.5 ± 0.4 MPa under vacuum and argon without extended holding time, respectively. The relatively low mechanical properties can be mainly attributed to the weak interlayer binding force, which is caused by layer-by-layer forming mode during 3D printing process and anisotropic shrinkage during the sintering process. Moreover, the alumina ceramics exhibited moderate bulk density and open porosity of 2.4 g/cm³ and 42% after the sintering process, respectively, which are mainly influenced by the microstructural evolution of alumina ceramics during thermal treatment. Also, the diffusion of gases is achieved by curing of photosensitive resin and influenced by different holding times during debinding, affecting the mechanical properties of sintered ceramics. The mechanical properties of as-sintered ceramics are suitable for the utilization of ceramic cores in the manufacturing of hollow blades.     

On reducing anisotropy in 3D printed polymers via ionizing radiation

The mechanical properties of materials printed using fused filament fabrication (FFF) 3D printers typically rely only on adhesion among melt processed thermoplastic polymer strands. This dramatically limits the utility of FFF systems today for a host of manufacturing and consumer products and severely limits the toughness in 3D printed shape memory polymers. To improve the interlayer adhesion in 3D printed parts, we introduce crosslinks among the polymer chains by exposing 3D printed copolymer blends to ionizing radiation to strengthen the parts and reduce anisotropy. A series polymers blended with specific radiation sensitizers, such as trimethylolpropane triacrylate (TMPTA) and triallyisocyanurate (TAIC), were prepared and irradiated by gamma rays. Differential scanning calorimetry (DSC), tensile testing, dynamic mechanical analysis (DMA) and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) were employed to characterize the thermomechanical properties and the chemical structure of the various polymers. TAIC was shown to be a very effective radiation sensitizer for 3D printed sensitized polylactic acid (PLA). The results further revealed that crosslinks induced by radiation temperatures near T_g of shape memory systems have prominently enhanced the thermomechanical properties of the 3D printed polymers, as well as the solvent resistance. This enables us to deliver a new generation of inexpensive 3D printable, crosslinked parts with robust thermomechanical properties.     

Effects of pore size on the mechanical and biological properties of stereolithographic 3D printed HAp bioceramic scaffold

In this study, hydroxyapatite (HAp) scaffolds with the pore size of 400, 500, and 600 μm were prepared by stereolithographic 3D printing (SL-3DP). The effects of pore size on mechanical and biological properties of the HAp scaffolds were investigated. Firstly, the macro- and microstructure of the HAp scaffolds were observed. Then, the compressive strength of the HAp scaffolds were tested. Finally, the biological properties of the HAp scaffolds were further characterized in vitro by the synthetic body fluid (SBF) solution immersion testing, as well as by using the cell proliferation and 3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) assay. From this study, it was found that the HAp scaffold with a pore size of 600 μm had the most promising application prospect.     

3D printing orientation controlled PMN-PT piezoelectric ceramics

Piezoelectric textured ceramics have drawn increasing research and industry interests by balancing the production cost and material performances. A new approach to realize the texture in piezoelectric ceramics is developed based on 3D printing stereolithography (SL) technique and successfully applied in the preparation of < 001 > -textured 0.71(Sm_0.01Pb_0.985)(Mg_1/3Nb_2/3)O₃-0.29(Sm_0.01Pb_0.985)TiO₃ (1 %Sm-PMN-29PT) ceramics in this work. As a critical process in texture ceramic fabrication, the alignment of BaTiO₃ templates along the horizontal direction is achieved by the shear force produced from the relative motion between the resin container and the blade during SL. The textured ceramics with obvious grain orientation features are successfully obtained. The enhanced piezoelectric properties of d₃₃ ≈ 652 pC N^?1 and d₃₃* ≈ 800 pm V^?1 are achieved in the 3D printed textured ceramic, which are about 60 % and 40 %, respectively, higher than their non-textured counterparts. Moreover, the textured sample shows a significant improvement on thermal stability of d₃₃*_T, which varies by less than ± 6 % from RT to 110 °C. Furthermore, the introduction of 3D printing into the synthesis of textured piezoelectric ceramics shows great advantages over the traditional tape-casting method. This work is expected to provide a promising way for the future design of textured piezoelectric functional materials.