骨料密度对高纯氧化锆制品性能的影响

为了提高氧化锆制品的综合性能,设计了配料组成中骨料分别为65％(w)的电熔氧化锆致密颗粒、45％(w)的电熔氧化锆致密颗粒加20％(w)的电熔氧化锆空心球、65％(w)电熔氧化锆空心球三种骨料密度不同的试样,经混料、液压成型、烘干后,分别在1650、1720和1800℃保温6 h制成w(ZrO2+HfO2+Y2 O3)...     

氧化锆活性对烧结性能的影响

分别以化学法和电熔法制备的氧化锆及二者混合共磨粉为原料,通过造粒、成型、干燥、烧成制得样品,对烧成样品物理性能和微观结构进行分析,研究原料活性对烧结性能的影响.研究结果表明:在加入同样稳定剂的条件下,电熔氧化锆活性较差,烧结后气孔率较高,化学氧化锆烧结后收缩大,开裂严重,两者都无法满足作为制备氧化锆质定径水口基质原料要求,当二者的混合比例为1:1时,试样的烧结温度合适,气孔率、烧成收缩、耐压强度等各项理化指标较好,满足用作制备氧化锆质定径水口基质要求.     

微、少量添加剂对高纯Y－TZP粉料烧结性能的影响

采用高纯的Ｙ－ＴＺＰ超细粉料，研究了不同种类添加剂对该高纯超细粉料等速升温烧结性能和显微结构发展的影响。实验发现：氧化钙或氧化铁加入量不大于１％（以质量计，下同），对材料的致密化过程影响不大；氧化钠的加入可明显阻碍粉料的致密化过程；氧化铜则可显著地加速粉料的致密化过程，并且这种影响在加入量为１％时十分明显。氧化钠对致密化的影响主要是由于粉料中团聚体的形成；氧化铜则因可与ＺｒＯ２形成低共熔液相而加速其致密化。氧化铜在加速材料致密化的同时，促进其晶粒的生长。此外，氧化钠和氧化铜均可破坏Ｙ－ＴＺＰ的稳定性，促使其向单斜相转变。     

团聚体含量对氧化锆粉料烧结性能的影响

用共沉淀－喷雾干燥的方法制得了具有不同团聚性质的氧化锆粉料。粉料成型后团聚体可能破碎，也可能继续存在。通过团聚体对烧结影响的研究发现，烧结过程中团聚体含量是影响烧结密度和显微结构形成的主要因素，而成型后素坯中团聚体含量又取决于团聚体的强度。讨论了团聚体之间及团聚体与基体之间的相互作用对烧结的影响。     

添加剂对锆质定径水口烧结性能和抗热震性的影响

采用粉末成型工艺,以粒度为0.045mm的斜锆石粉和粒度均为0.154mm和0.074mm的MgO部分稳定电熔氧化锆和CaO部分稳定电熔氧化锆为原料,分别加入不同添加剂Y2O3、CeO2和Y2O3 CeO2,在300MPa的压力下成型,并于1720℃烧后制成锆质定径水口试样。结果表明通过合理控制颗粒级配和优化工艺参数,当添加剂中Y2O3和CeO2的含量(w)分别为0.6%和0.4%时,氧化锆的稳定率约为70%,同时可得到显气孔率低,体积密度高,抗热震次数≥5次的锆质定径水口。     

烧结温度对氧化锆陶瓷磨球性能的影响

利用滚制成型法制备了氧化锆陶瓷磨球,研究了烧结温度对陶瓷球体积密度和耐磨性的影响.结果表明,滚制法成型的陶瓷球坯体在1550℃、保温2 h的烧结条件下得到最佳效果,其体积密度达到5.91 g/cm3,自磨损率为2.6 ×10-6/h.     

稳定剂种类对高纯氧化锆空心球制品性能的影响

为制备隔热性能更好的高纯氧化锆空心球制品,分别以CaO稳定氧化锆空心球颗粒及细粉、Y₂O₃稳定氧化锆空心球颗粒及细粉、CaO+Y₂O₃复合稳定氧化锆空心球颗粒及细粉为主要原料,以工业级Y₂O₃微粉为烧结助剂,以水溶性树脂为结合剂,采用振动加压成型,于1 800℃保温6 h烧成制备了含不同稳定剂的高纯氧化锆空心球制品。研究了稳定剂种类对这些制品性能的影响。结果表明：1)烧后各试样的物相主要为立方氧化锆;骨料与基质细粉都很好结合在一起,含CaO稳定剂试样的内部气孔相对狭长,呈相互贯通网络状,力学性能适中,抗热震性最优;含Y₂O₃稳定剂试样的内部气孔大小不均、分散孤立,力学性能最差;含CaO+Y₂O₃复合稳定剂试样的内部孔径更小、分布更均匀,致密化趋势明显,力学性能最优,但抗热震性最差。2)烧后试样的线膨胀率和热导率随温度升高均逐渐增大;在高温阶段,含CaO稳定剂试样的线膨胀...     

氧化锆质滑板性能的研究

本文以电熔MgO稳定氧化锆（1.5μm）、电熔单斜锆（3～7μm）、共沉淀法制备的单斜锆聚晶（10μm聚晶）为主要原料.通过用电熔镁稳定氧化锆细粉制备出粒径在120目以下的聚晶作为骨料,以电熔单斜锆（3～7μm）作为细粉,可以制备出高强度、高致密度、热震性能较好的氧化锆试样.     

ZnO对8YSZ电解质材料的烧结性与电化学性能的影响

用机械混合方法,在8%(摩尔分数,下同)Y2O3稳定的ZrO2(8%in mole yttria stabilized zirconia,8YSZ)中添加ZnO量分别为0,1%,2%,3%,4%,在不同温度下常压烧结制备了ZnO:8YSZ电解质。研究了烧结温度和ZnO含量对ZnO:8YSZ样品的烧结性、致密度、弯曲强度和电导率的影响。由ZnO:8YSZ电解质作为支撑组装了单电池,对电池的性能进行测试和评价。结果表明:在8YSZ中添加ZnO能改善8YSZ材料的烧结性,1400℃烧结2h的4%ZnO:8YSZ样品的致密度达99.9%,3%ZnO:8YSZ样品的弯曲强度超过200MPa,获得明显提高。4%ZnO:8YSZ样品在800℃下的电导率达1.68×10-2S/cm。在相同工作条件下,ZnO:8YSZ单电池比8YSZ单电池具有更好的工作性能和更高的效率,以3%ZnO:8YSZ单电池性能最好。     

烧结温度对钇部分稳定氧化锆陶瓷性能研究

本文采用了一种改进的制备工艺生产钇部分稳定氧化锆细粉,通过X-射线衍射（XRD）分析了粉料的相组成,研究发现,制备的粉体结构由t—ZrO2和m—ZrO2相共同组成。制备的粉料采用半干压成型、烧结。在不同的烧结温度下,对其部分力学性能及其形貌进行了研究分析。     

Morphology and sintering behaviour of yttria stabilised zirconia (8-YSZ) powders synthesised by spray pyrolysis

This work is focused on the synthesis of nano-crystallised yttria stabilised zirconia (YSZ) powders by the spray pyrolysis method, the aim of the study being a better understanding of the influence of the spray pyrolysis parameters on the morphology of the produced powders. Spray pyrolysed powder consists of polycrystalline particles, which are spherical. Each particle consists of nanometric primary grains. The morphology of these polycrystalline particles was characterised by scanning electron microscopy (SEM), helium pycnometry, thermogravimetric analysis (TGA) and mass spectroscopy (MS), and the results are compared. Thus, particle size, particle size distribution and particle porosity were determined and correlated to the process parameters. Finally, by dilatometric measurements, sintering curves of pellets prepared from different sets of powders were analysed in regard of their morphologies. Two main conclusions could be deduced from these studies. Firstly, the process parameters influence both internal porosity and particle size distribution of the synthesised powders. Secondly, the morphologies of the spray pyrolysed nano-powders lead to particularly high sintering activities.     

Influence of sintering parameters on tribological properties of ceria stabilized zirconia bio-ceramics

Nano-structured ceria stabilized zirconia powder was synthesized from their respective nitrate salts using a wet chemical co-precipitation method. Dried powder was calcined at different temperatures. Particle size of calcined powders was measured by X-ray diffraction (Scherrer equation) and high resolution transmission electron microscopy. Relative quantities of phases (e.g. monoclinic, tetragonal and cubic) were estimated using rigorous Rietveld analysis. The powder was compacted and sintered conventionally following different time and temperature schedules in order to optimize the sintering schedule for fabrication of dense material. The microstructures of the sintered samples were observed by field emission scanning electron microscopy. Vickers hardness (∼945 VHN) showed appreciable increase (>35%) in the hardness value compared to earlier reported ones. Fretting wear of some of the selected samples was carried out in un-lubricated condition. Wear volume and specific wear rate were estimated and correlated with the microstructure. Fatigue microcrack formation, plastic deformation, grain pull-out and abrasion were found to be the main wear mechanisms.     

Flash microwave sintering of zirconia by multiple susceptors cascade strategy

In the field of flash sintering, microwave energy represents an interesting way to densify ceramics complex shapes, thanks to a contactless volumetric heating. Attaining a fast and homogeneous heating is a critical parameter and hybrid heating, using silicon carbide susceptors, is generally used. In this study, an original multiple susceptors cascade strategy is developed, using both SiC and 3D-printed ZrO₂ susceptors. This novel configuration follows perfectly the flash heating scheme, even for high heating rates up to 1000 K.min^-1 and leads to a high stability of the “flash” hybrid heating. Flash microwave sintering produced dense (97 % relative density) microstructures within 45 s. Based on comprehensive multiphysics simulations of the overall process, in-situ dilatometry measurements, kinetics method analysis and microstructural characterizations, this work highlights the sintering behavior of zirconia and the temperature distribution during flash microwave sintering.     

Influence of additives on the purity of tetragonal phase and grain size of ceria-stabilized tetragonal zirconia polycrystals (Ce-TZP)

A comprehensive study on the influence of typical additives on zirconia (ZrO₂) crystallization was presented. Zirconium nitrate pentahydrate (Zr(NO₃)₄·5H₂O) and cerium(III) nitrate hexahydrate (Ce(NO₃)₃·6H₂O) were employed as reagents, ethylenediaminetetraacetic acid disodium salt (EDTA-2Na) or glycerol were adopted as additives, and ammonia water was adopted as pH regulator. The ZrO₂ powders were prepared by hydrothermal method. The crystal phase purity, grain size and micro morphology of the ZrO₂ powders were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) equipped with energy dispersive spectrometer (EDS) to investigate the influence of EDTA-2Na, glycerol and Ce⁴⁺ content on the purity of tetragonal phase and the grain size of ceria-stabilized tetragonal zirconia polycrystals (Ce-TZP). It was found that EDTA-2Na could decrease the purity of tetragonal phase and alter the grain size of Ce-TZP nonlinearly, while glycerol could not decrease the purity of tetragonal phase and the grain size of Ce-TZP, and the grain size was not linear with the amount of glycerol; Doping Ce⁴⁺ could increase the purity of tetragonal phase of zirconia but could not decrease the grain size, and the grain size was not linear with the Ce⁴⁺ content; In addition, it was indicated that EDTA-2Na and glycerol could not improve the distribution uniformity of Ce⁴⁺. This study is expected to have provided a novel path to achieve tailored ZrO₂ crystals with reduced low-temperature degradation.     

Transparent high-strength nanosized yttria stabilized zirconia obtained by pressure-less sintering

This work describes the development of transparent high-strength Yttria-Stabilized Zirconia (YSZ) ceramics with ultra-fine grain size utilizing conventional pressure-less densification. Starting with nanoparticles with diameter < 10 nm, it was possible to achieve full densification (>99.5% of theoretical density) at a sintering temperature of 1100–1200 °C. The average grain size of the resulting dense ceramics was 75 nm in 3 mol. % YSZ and 85 nm in 8 mol. % YSZ, showing in-line light transmission of 38% and 51% at a wavelength of 800 nm and average biaxial strength (piston on three balls test on samples of diameter 12 mm and thickness 1 mm) of 1980 MPa and 680 MPa, respectively. The nano-grained structure, absence of color centers, and miniaturization of residual pores enable the excellent light transmission. The high biaxial strength is attributed to the refined microstructure, but also to the martensitic tetragonal-to-monoclinic phase transformation that remains active even in nano-sized zirconia grains.     

High-pressure sintered yttria stabilized zirconia ceramics

Fast densification of 8YSZ ceramics under a high pressure of 4.5 GPa was carried out at different temperatures (800, 1000, 1450 °C), by which a high relative density above 92% could be obtained. FT-Raman spectra indicate that the 8YSZ underwent a phase transition from partially tetragonal to partially cubic phase as temperatures increase from 1000 to 1450 °C when sintering under high pressure. The electrical properties of the samples under different high-pressure sintering conditions were measured by complex impedance method. The total conductivity of 0.92 × 10⁻² S cm⁻¹ at 800 °C has been obtained for 8YSZ under high pressure at 1450 °C, which is about 200 °C lower than that of the samples prepared by conventional pressureless sintering.     

Effect of manganese addition on sintering behavior and mechanical properties of alumina toughened zirconia

The effect of MnO₂ additives on the sintering behavior and mechanical properties of alumina-toughened zirconia (ATZ, with 10 vol% alumina) composites was investigated by incorporating different amounts of MnO₂ (0, 0.5, 1.0, and 1.5 wt%) and sintering at various temperatures ranging from 1300 to 1450 °C. The addition of MnO₂ up to 1.0 wt% improved the sintered density, hardness, flexural strength, and fracture toughness of the composite. However, the addition of 1.5 wt% MnO₂ degraded the relative density, hardness, and flexural strength of the composite due to the transformation of the ZrO₂ phase from tetragonal to monoclinic and grain coarsening. Optimal results were obtained with 1.0 wt% MnO₂ and sintering at 1450 °C, which improved the mechanical properties (hardness: 13.5 GPa, flexural strength: 1.2 GPa, fracture toughness: 8.5 MPa m^1/2) and lowered the sintering temperature compared to the conventional sintering temperature of ATZ composites (1550 °C). Thus, the ATZ composite doped with MnO₂ is a promising material for structural engineering ceramics owing to its improved mechanical properties and lower sintering temperature.     

Effect of zirconia particle size on the properties of alumina-spinel castables

The industrial application of alumina-spinel refractory castables has crucial requirements on the service performance. Thus, the effects of different sized desilicated zirconia particles on the castables microstructure, thermal-mechanical properties and high temperature elastic modulus have been investigated. The zirconia particle sizes were varied from 1000 µm to 2.5 µm (d₅₀). It was observed that the finer (below 88 µm) zirconia particles were beneficial to improve the cold modulus of rupture (CMOR) and the hot modulus of rupture (HMOR), but could not effectively enhance the thermal shock resistance. Fine zirconia particles can homogeneously disperse in the matrix and significantly promote the sintering process. Accompanied with the phase transformation of zirconia, both the high density of matrix cracks and the strong ceramic bonding (between the coarse grains and the matrix) were found in the refractory castables, which was responsible for an increase of CMOR. However, the binding characteristic could also give rise to the high stored elastic energy that was adverse to the thermal shock resistance, and the excessive amount of preexisting matrix cracks could induce more microdamage during the thermal shock. Additionally, it was proposed that the second-phase dispersion reinforcement and the highly ceramics bonding resulted in the superior HMOR when introducing fine ZrO₂ particles.     

Microstructure and high-temperature sintering properties of APS coatings prepared from spherical thin-walled hollow-shell powders

High-performance thermal barrier coatings (TBCs) made of 4 mol.% Y₂O₃–stabilized ZrO₂ (4YSZ) powder with a spherical thin-walled hollow-shell (STHS) structure exhibited a special microstructure different from the conventional lamellar structure of air plasma-sprayed (APS) coatings. The as-sprayed STHS APS coatings had a completely tetragonal prime (t′) structure and non-lamellated closed-cell structure with high porosity, which resulted in relatively low thermal conductivity (～1.0 W m^?1 K^?1) and high Vicker's hardness (～6 GPa). The influences of high-temperature aging on the microstructure stability, phase stability, and sintering capability were investigated after long-time heat treatment at different temperatures. The characterization results indicated that the pore content was basically constant, and it was less than 0.5% for sintered linear shrinkage of the STHS coatings after heat treatment at 1500 °C for 100 h. Furthermore, no spalling appeared in the STHS APS coating with the t′ phase structure after 101 thermal cycles of the water-quenching method at 1050 °C, and no monoclinic ZrO₂ (m-ZrO₂) phase was present in all of the STHS coatings after aging at 1200 °C for 1–1100 h. The excellent anti-sintering properties and phase stability of the STHS coatings are attributed to the closed-pore microstructure and the highly pure t′ phase composition with uniform distribution of ions, respectively. The results suggested that the non-lamellated closed-cell microstructure is beneficial for improving the coating properties, and the results also provide guidelines for microstructure design of TBCs using a feedstock powder.