Tailoring of functionally graded zirconia–mullite/alumina ceramics

A new tailored zirconia–mullite/(0–100 vol%) alumina as functionally graded ceramics (FGCs) was designed and synthesized by reaction sintering of zircon and alumina. Zircon and alumina powder mixtures were mixed, stacked, compacted in a cylindrical die and sintered. The sintered samples made of 11 layers and varied gradually in composition by 10 vol% from one layer to the other layer (i.e. from zirconia–mullite layer to alumina layer) resulted in continuous functionally graded ceramics without sharp interfaces. Phase composition and densification behaviors of the samples were investigated. Microstructure, mechanical and thermal properties of FGC and its non-layered composites were studied. Results showed that the tailored FGZM/A gave continuous homogenous structure with highly improved physical, mechanical and thermal properties. The different properties of tailored FGZM/A recorded average values or rather better of its non-layered composites which gave a new way for material design.     

髋关节整体替代陶瓷材料

许多材料在医学领域应用广泛,例如,整体替换硬组织或软组织的元件(如骨盆、骨头、关节、植牙等)、修补、诊断或矫正仪器(如起搏器、心脏阀等)。这些材料不仅要有好的力学性能,还要保持长期稳定,不能与人体相排斥。由于陶瓷材料在生理环境中具有强度高、生物相容性强和稳定性好的优点,人们研究用陶瓷材料替换骨骼。从20 世纪70 年代起,欧洲人用陶瓷组件置换整个髋关节。这些组件主要由氧化铝和氧化锆单体制成。然而,在有水环境中,氧化锆会发生低温降解。目前人们的研究重点在于提高陶瓷组件的强度和耐磨性,同时缩小其尺寸并延长其使用寿命。研究中使用的材料是氧化锆增韧的氧化铝复合陶瓷和其它氧化铝复合陶瓷,不再是单体陶瓷。另外,还可以使用氧化铝和氧化锆功能梯度复合材料。该梯度材料可以利用电泳沉积法(EPD)制得,其表面为纯氧化铝,中心部分为均匀的氧化铝、氧化锆复合材料,中间过渡部分是呈连续梯度渐变的氧化铝、氧化锆复合材料,烧成后会产生剩余热应力。设计这样的梯度结构是为了使复合材料具有最大表面压应力和最小内部张应力,与纯氧化铝组件相比,提高了强度和耐磨性。     

Additive manufacturing of zirconia parts with organic sacrificial supports

Ceramic On-Demand Extrusion (CODE) process has been recently proposed for additive manufacturing of strong ceramic components via extrusion. This paper focuses on fabricating 3 mol% yttria-stabilized zirconia (3YSZ) components using CODE process, and enabling CODE to produce parts with support structures. A colloidal suspension of 3YSZ was developed and deposited through the main nozzle, and an organic feedstock was developed and deposited by means of another nozzle to fabricate supports. After printing and drying of raw parts, supports were removed by increasing the temperature and parts were then sintered to near theoretical (~99%) density. The maximum overhang angle that could be built with no support was also found out to be approximately 60 degrees. Three organic support materials, that is, polycaprolactone (PCL), silicone, and petrolatum were prepared and tested. PCL and petrolatum were identified as feasible support materials. Specimens were fabricated to validate the efficiency of the support materials and to evaluate CODE's capability for building parts with complex geometry. The microstructures of these parts were also analyzed via scanning electron microscopy.     

Sintering behavior and mechanical properties of alumina/zirconia multilayers composite via nano-powder processing

The present research has been focused on the development of functionally graded alumina–zirconia composites, which particularly have high mechanical and thermal properties. In this study, different components of alumina–zirconia layers were enhanced between two layers of pure alumina and alumina with 20 mol% zirconia. The effect of this enhancement on consolidation, sintering condition, hardness and toughness values of the multilayer samples was evaluated. The results showed that the cracks were distributed in the co-sintering multi-layered structure. The cracks were formed due to the residual stress caused by differences in thermal expansion and sintering between successive layers. The final shape and mechanical properties of the gradual samples were found to be improved.     

Charge trapping characteristics of alumina based ceramics

The space charge dynamics is very important for electrical breakdown of alumina based ceramics. In this paper, the charge trapping/detrapping characteristics of alumina based ceramics were studied by means of isothermal surface potential decay (ISPD) method. For alumina and zirconia toughened alumina (ZTA) ceramic samples, the ISPD curves charged by corona discharge as well as microstructure characterization were carried out. For the first time, crossover phenomenon and hollow shaped potential profile were observed and reported in alumina based ceramics, indicating a surface potential decay process dominated by charge injection and volume conduction affected by the trap states in materials. In addition, the comparative trapping characteristics were evaluated based on a charge detrapping controlled decay model. The correlation between trap distribution and microstructure of alumina based ceramics was investigated. It was proposed that different charge trapping characteristics of alumina based ceramic samples was caused by varied shallow trap density of grain boundary.     

FEM simulations of microstructure effects on thermoelastic properties of sintered ceramics

A model was developed to simulate macroscopic material properties of polycrystalline ceramics from the material properties of the constituting phases and the microstructure. Cubic and random structures were included. The model allows a variation of volume fractions of the phases, grain size and grain boundary areas. Representative for a large number of material properties, elastic tensor, thermal conductivity, coefficient of thermal expansion and thermal stress are calculated for individual microstructures using finite element methods (FEM). Simulations focus on two types of bi-continuous ceramic composites: zirconia toughened alumina (ZTA) and a porous zirconia ceramic which was infiltrated by a spinel-glass. Microstructure of experimental samples is represented by two different model structures: a Voronoi type structure for the ZTA ceramic and a cubic structure of cubes interconnected by cylinders for the infiltrated zirconia system. A substantial impact of microstructure on macroscopic material properties and internal stress distribution is obtained. A good agreement between measured and simulated material properties was found.     

Measurement of ceramics cracking during water quenching by digital image correlation

Measuring the thermal shock crack growth process is crucial for revealing ceramic materials and structures’ thermal shock failure mechanisms and evaluating their reliability. We used a self-made water quenching system to conduct thermal shock tests on alumina and zirconia ceramics. The thermal shock process was recorded by high-speed digital image correlation (DIC) during the test. The process of thermal shock crack initiation and propagation in two kinds of ceramics was determined by analyzing the speckle image change on the sample’s surface. It is found that the crack growth rate of alumina is faster than that of zirconia, which is caused by different material parameters. This paper presents an in-situ measurement method for the initiation and propagation of thermal shock cracking in ceramic materials. It can provide a measurement method to identify and predict the thermal shock damage of ceramic components.     

Characterization of zirconia specimens fabricated by ceramic on-demand extrusion

The Ceramic On-Demand Extrusion (CODE) process is a novel additive manufacturing method for fabricating dense (~99% of theoretical density) ceramic components from aqueous, high solids loading pastes (>50?vol%). In this study, 3?mol% Y₂O₃ stabilized zirconia (3YSZ) specimens were fabricated using the CODE process. The specimens were then dried in a humidity-controlled environmental chamber and afterwards sintered under atmospheric conditions. Mechanical properties of the sintered specimens were examined using ASTM standard test techniques, including density, Young’s modulus, flexural strength, Weibull modulus, fracture toughness, and Vickers hardness. The microstructure was analyzed and grain size measured using scanning electron microscopy. The results were compared with those from Direct Inkjet Printing, Selective Laser Sintering, Lithography-based Ceramic Manufacturing (LCM), and other extrusion-based processes, and indicated that zirconia specimens produced by CODE exhibit superior mechanical properties among the additive manufacturing processes. Several sample components were produced to demonstrate CODE’s capability for fabricating geometrically complex ceramic components. The surface roughness of these components was also examined.     

Computer-Aided, Single-Specimen Controlled Bending Test for Fracture-Kinetics Measurement in Ceramics

Fracture testing of ceramics by using controlled crack growth is proposed to allow study of crack-kinetics behavior under a given loading history. A computer-aided, real-time data acquisition system improves the quality of crack-growth parameters obtained in a simple, single-specimen bend test. Several ceramic materials were tested in the present study: aluminum nitride as a linear-elastic material; and alumina and yttria-stabilized zirconia, both representative of ceramics with microstructure-dependent nonlinear fracture properties. Ambiguities in the crack-growth diagrams are discussed to show the importance of accounting for crack-growth history in correctly describing nonequilibrium fracture behavior.     

Load-bearing increase in alumina evoked by introduction of a functional glass gradient

Alumina is the most commonly used ceramic in orthopedics due mainly to its wear resistance and chemical inertness. However, alumina has relatively low load-bearing capacity compared to other advanced ceramics, such as zirconia. We hypothesized that grading the elastic modulus at the surfaces may substantially increase the load-bearing capacity of alumina. In this study, graded structures were fabricated by infiltrating glass into dense alumina plates, resulting in a diminished modulus at the surface layers. The plates were then bonded to polycarbonate substrates and subjected to flexural loading with various loading rates spanning five orders of magnitude (dynamic fatigue) in water. Infiltrated specimens showed an increase in flexural load over homogenous controls for all loading rates, despite the graded alumina exhibiting greater load rate dependence than their homogenous counterparts. Our results indicate that controlled elastic gradients at the surface could be highly beneficial in improving the load-bearing capacity of alumina ceramics.     

泡沫陶瓷的研制

泡沫陶瓷是一种新型的功能陶瓷材料。它具有独特的结构和性能，在工业中有着广泛的应用前景。泡沫陶瓷具有密度小、透气性高、耐高温、抗化学腐蚀等特性。本研究对用颗粒强化的氧化铝骨架合成泡沫陶瓷进行了分析。这种材料比其它多孔陶瓷材料具有更好的热化学性质。这种材料可以用有机海绵浸浆获得，然后烧去海绵，留下多孔陶瓷网。这种方法的优点是它包含了过程参数和陶瓷结构，同时合成物的烧结情况及其它条件的影响在文中也有阐述。     

Low-Temperature Processing and Mechanical Properties of Zirconia and Zirconia–Alumina Nanoceramics

The 1.5- to 3-mol%-Y₂O₃-stabilized tetragonal ZrO₂ (Y-TZP) and Al₂O₃/Y-TZP nanocomposite ceramics with 1 to 5 wt% of alumina were produced by a colloidal technique and low-temperature sintering. The influence of the ceramic processing conditions, resulting density, microstructure, and the alumina content on the hardness and toughness were determined. The densification of the zirconia (Y-TZP) ceramic at low temperatures was possible only when a highly uniform packing of the nanoaggregates was achieved in the green compacts. The bulk nanostructured 3-mol%-yttria-stabilized zirconia ceramic with an average grain size of 112 nm was shown to reach a hardness of 12.2 GPa and a fracture toughness of 9.3 MPa·m^1/2. The addition of alumina allowed the sintering process to be intensified. A nanograined bulk alumina/zirconia composite ceramic with an average grain size of 94 nm was obtained, and the hardness increased to 16.2 GPa. Nanograined tetragonal zirconia ceramics with a reduced yttria-stabilizer content were shown to reach fracture toughnesses between 12.6–14.8 MPa·m^1/2 (2Y-TZP) and 11.9–13.9 MPa·m^1/2 (1.5Y-TZP).     

Highly translucent and strong ZrO2-SiO2 nanocrystalline glass ceramic prepared by sol-gel method and spark plasma sintering with fine 3D microstructure for dental restoration

Balance of better mechanical strength and good translucency for dental restorative materials is always a challenge. A translucent glass ceramic/ceramic with improved mechanical properties or a strong glass ceramic/ceramic with good translucency would therefore be interesting for dental application. Nanocrystalline glass ceramics (NCGC) attract a lot attention because of their superior optical and mechanical properties. This study aims to obtain ZrO₂-SiO₂ nanocrystalline glass-ceramic that possesses high mechanical strength as well as excellent translucency by controlling the content, size, and connection of nanocrystalline ZrO₂ in a ZrO₂-SiO₂ glass-ceramic material. Toward this end, well-homogenized nano-powders with three different compositions, 45%ZrO₂-55%SiO₂ (molar ratio, 45Zr), 55%ZrO₂-45%SiO₂ (55Zr), and 65%ZrO₂-35%SiO₂ (65Zr)_, were synthesized, followed by a fast sintering process. Highly-translucent nanocrystalline glass ceramics composed of tetragonal ZrO₂ were obtained. Samples with high zirconia content showed that the structure of the skeleton was predominately built by nano-sized ellipsoidal ZrO₂ particles bonded by grain boundaries, with amorphous SiO₂ filling the voids between the ZrO₂ particles. The achieved flexural strength measured by piston-on-three-ball test was as high as 1014 MPa. To our knowledge, this is one of the highest flexural strength values of glass ceramics ever reported, which is higher than transparent zirconia and alumina ceramics. The 3D structure of nanocrystalline zirconia in silica matrix did enhance the flexural strength of the NCGC. The results of this study suggest that the new ZrO₂-SiO₂ NCGC has great potential of using as dental restoration.     

氧化锆陶瓷凝胶注模成形研究

试验采用高纯超细氧化锆粉伴为原料,通过凝胶注模成形工艺,获得氧化锆陶瓷刀具的坯体。参照已有经验,通过研究氧化锆陶瓷凝胶注模成形工艺流程及工艺参数与所得样品的关系,进行探索性试验。通过对比试验结果,获得最佳工艺参数,确定了氧化锆凝胶注模成形的最佳配方。按照试验提供的原料配方,严格控制干燥过程和烧成制度,可以得到结构致密、性能稳定、强度较高的陶瓷刀具,为凝胶注模成形方法的工业化推广提供了可靠的参考依据。     

Multiscale modelling of the thermoelastic properties of alumina-zirconia ceramics for 3D printing

Additive manufacturing appears to facilitate the accurate manufacturing of alumina-zirconia technical ceramics. Nevertheless, the fine tuning of the manufacturing of these components by 3D printing requires an analysis of the parameters that influence their final thermoelastic properties. In this context, this work presents the application of (finite element-based) numerical procedures that aim at the prediction of the effective thermoelastic properties of 3D-printed alumina-zirconia ceramics. The numerical modelling considers three different scales: micro-, meso- and macroscale. The microscale corresponds to the microstructural level of, sintered at 1500 °$\mathrm{C}$, slip-casted samples with different compositions of alumina-zirconia. On the other hand, the macroscale corresponds to the macrostructural level of porous lattice of 3D-printed ceramics, being defined at the mesoscale level by a periodic unit cell. Thus, an initial microstructural analysis (at microscale level) provides the influence of the alumina/zirconia ratio on the (macroscopically homogeneous and isotropic) material thermoelastic properties, which together with the definition of the geometry of a periodic unit cell (at mesoscale level), provides, by a second analysis (at both the meso- and macroscale levels), the coupled influence of material and geometry of the macrostructural lattice on the structural (macroscopically heterogeneous and anisotropic) thermoelastic properties. Moreover, experimental thermoelastic properties of the sintered slip-casted specimens were obtained for several alumina/zirconia ratios and analysed together with microstructure patterns. Prediction of the microstructural effective thermoelastic properties was also made using micromechanics and composite theory (analytical) models. All the numerical, experimental and analytical results for the microstructural level are presented and compared. Numerical results for the meso- and macrostructural levels are also presented.     

Combinatorial Ink-Jet Printer for Ceramics: Calibration

This article describes an ink-jet printer for the construction of combinatorial libraries and functionally graded ceramics. It can mix and print all possible compositions for high-throughput screening. The number of components is set by the number of mixing valves that deliver ceramic ink from pressurized reservoirs into a circulation chamber. Compositional control is by either complete or incremental change. Organic liquids and ceramic inks are used in a systematic three-stage calibration. The calibration protocol accounts for the effects of ink viscosity, reservoir pressure, valve-opening time, and temperature, but reveals unexpected segregation effects that occur in the ink after deposition.     

Evidence for the Microwave Effect During Hybrid Sintering

A microwave/conventional hybrid furnace has been used to sinter three ceramics with different microwave absorption characteristics under pure conventional and a range of microwave/conventional hybrid heating regimes. The precursor powder particle size was also varied for each material. In each case it was ensured that every sample within a series had an identical thermal history in terms of its temperature/time profile. An increase in both the onset of densification and the final density achieved was observed with an increasing fraction of microwave energy used during sintering, the effect being greatest for the materials that absorbed microwaves most readily. Twenty-three percent greater densification was observed for submicron zinc oxide powder, the material with the largest microwave absorption capability, when sintered using hybrid heating involving 1 kW of microwave power compared with pure conventional power under otherwise identical conditions. For the ceramic with the lowest microwave absorption characteristic, alumina, the increase in densification was extremely small; partially stabilized zirconia, a moderate microwave absorber, was intermediate between the two. Temperature gradients within the samples, a potential cause of the effect, were assessed using two different approaches and found to be too small to explain the results. Hence, it is believed that clear evidence has been found to support the existence of a genuine "microwave effect."     

Fabrication of a material with composition gradient for metal/ceramic assembly

This study presents a method and an apparatus for fabricating graded materials with powders. The application is about making some transition interlayer components when assembling metal to ceramic by brazing for example. The chosen applicative couple is inco600 with zirconia. The densification technique is hot isostatic pressing. After calibration of the equipment designed to make some bi-constituent powder gradients, a cylindrical component with a symmetrical axial gradient has been manufactured. Phase volume fraction composition determined through image analysis and micro-hardness study has demonstrated that the obtained composition and properties vary continuously along the gradient direction. The fabricated material also exhibits some cracks probably due to low sinterability of zirconia used (50 μm balls). Other tests should be done with a finer zirconia powder. This technique should then be employed to fabricate ceramic metal assemblies through the manufacture of intermediated graded parts between the metal and ceramic components.     

Experimental investigations on enhanced alternating-magnetic field-assisted finishing of stereolithographic 3D printing zirconia ceramics

Zirconia ceramic components have great applications in the fields of medical, aerospace, and energy. Stereolithographic (SLA) 3D printing technology is widely employed for zirconia ceramic fabrication. However, the surface quality of manufactured components by direct SLA 3D printing is hard to meet stringent requirements of industrial application. In this work, an enhanced alternating-magnetic field-assisted finishing (A-MFAF) method was proposed for SLA printed zirconia ceramics. The A-MFAF was achieved using a flexible alternating-magnetic-field generator, integrating a rectangular magnetic pole and radial magnetic column. The novel finishing tool was fabricated to regulate finishing media behaviors for ensuring desirable finishing force. The unique construction of the magnetic field generator provided a controllable alternating magnetic field in the finishing zone. The magnetic control characteristics were investigated with finite element analysis (FEA). A serial of finishing experiments were carried out to verify the feasibility of the proposed A-MFAF method for SLA printed zirconia ceramics. The finishing efficiency with the developed magnetorheological shear thickening finishing (MSTF) media was improved by over 24% compared to that with the conventional magnetorheological finishing (MRF) fluids. The variation of surface roughness was qualitatively evaluated under different finishing conditions. The surface roughness of 89 nm was obtained from the initial 1.79 μm at 0.6 mm working gap and 700 r/min spindle rotational speed. Digital microscope, optical profiler and surface hydrophobicity measuring instrument were employed to investigate the surface characteristics of the finished SLA printed zirconia ceramics. Ultra-smooth surface with slight defects and deformations was obtained. The feasibility of A-MFAF method for the ultra-precision finishing of SLA printed zirconia ceramics was verified.     

Defect and microstructural evolution during drying of soapnut-based alumina foams

The present study demonstrates the use of soapnut, a naturally occurring surfactant for producing alumina ceramic foams. A range of slurry compositions with soapnut amounts ranging from 2 to 20 wt% in water, alumina loading of 35–55 vol% were studied. Though all slurry compositions foamed when subjected to mechanical agitation the formation of green ceramic foams free of macroscopic defects was found to be strongly dependent on conditions during drying of foamed slurries. Addition of guar gum to the slurries was shown to enhance foam stability and thus produce defect-free foams from compositions that otherwise either collapsed or resulted in other macroscopic defects during drying. Drying conditions also had a strong effect on microstructural parameters such as cell size and cell connectivity. Soapnut-based foams appear to have a greater connectivity between cells than foams produced by other comparable processes.