Hot pressing 0f Y2O3-stabilized ZrO2 with Cr2O3 additions

The sinterbility of Y₂O₃-stabilized zirconia with Cr₂O₃ additive was studied by a hot pressing technique using graphite and alumina dies; the dependence of the density on temperature, pressure and time was measured. Using graphite dies, it was found that the addition of Cr₂O₃ to Y₂O₃-stabilized zirconia was effective as an at for densification due to formation of chromium at higher temperatures. Addition of Cr₂O₃ inhibited the grain growth of Y₂O₃-stability zirconia. The solubility of Cr₂O₃ in ZrO₂ was found to be 0.7 mol% at 1450° C. The results could be explained in relation to the phase relations of the system ZrO₂-Y₂O₃-Cr₂O₃.     

Fatigue and R-curve behavior of an Al2O3-10vol%Cr3C2 composite

The static and dynamic fatigue properties of an Al₂O₃-10 composite were studied. The R-Curve behavior was determined using the indentation strength in bending (ISB) technique. Results indicated that both alumina and the Al₂O₃-Cr₃C₂ composite exhibit time-dependent slow crack growth under static fatigue test conditions. In addition, the resistance for slow crack growth in the Al₂O₃-Cr₃C₂ composite is higher than that in monolithic alumina. The toughness of alumina was substantially increased and R-curve behavior became evident after the incorporation of Cr₃C₂ particles.     

Microstructure and Mechanical Properties of ZrO2(2Y)-Toughened Al2O3 Ceramics Fabricated by Spark Plasma Sintering

Spark plasma sintering (SPS) has been performed for 5 min at 1500°C and 30 MPa using submicrometer-sized Al₂O₃/ZrO₂(2Y) composite powders in the Al₂O₃-rich region. Dense ZrO₂-toughened Al₂O₃ (ZTA) ceramics show excellent mechanical strength; the strength of 1620 MPa is achieved in the ZTA with 50 mol% ZrO₂. The grain size of Al₂O₃ in ZTA decreases from 1.5 to 0.6 m with increased ZrO₂ content. Almost all the ZrO₂ grains (0.3 m) are located in the boundaries of the Al₂O₃ grains. Mechanical properties are discussed, with an emphasis on the relation between t-/m-ZrO₂ ratios and microstructures of ZTA.     

Preparation and study of YSTZ-Al2O3 nanocomposites

Yttria stabilized zirconia-alumina (YSTZ-Al₂O₃) nanocomposite system with various Al₂O₃ concentrations has been synthesized by sol-gel route. The experimental techniques XRD, DTA, TGA, FT-Raman, FT-IR, SEM, Vickers hardness measurements, density measurements and Impedance spectroscopy were used to characterize the synthesized specimens. DTA result shows two exothermic reactions: one around 760°C and another around 960°C. XRD results confirm that the specimen starts to crystallize on heating above 750°C. Well resolved XRD reflections corresponding to tetragonal (t) ZrO₂ were obtained after the specimens were heated at 1000°C. FT-Raman results confirmed that the crystallites developed above 750°C was t-ZrO₂. It was observed from the XRD and DTA results that the bulk and grain boundary region crystallize independently in two different temperatures with a difference in temperature of about 200°C. The crystallization temperatures increase with Al₂O₃ contents. At 1300°C, the pure YSTZ and 5 and 10 wt % Al₂O₃ added YSTZ specimens underwent structural transformation from tetragonal to monoclinic ZrO₂. But, the tetragonal symmetry remains stable at 1300°C with an addition of 15 wt % Al₂O₃. The system which retain its tetragonal symmetry at its processing temperature (1300°C) gives high hardness and maximum density values. Almost 100% theoretical density value was obtained at 1300°C with an addition of 15 wt % of Al₂O₃.     

The structure of Al2O3-Cr2O3 powders condensed from a plasma

The structure of Al₂O₃-Cr₂O₃ powders prepared by plasma oxidation of the mixed halides has been examined by X-ray diffraction, electron microscopy and electron spin resonance. The powders consisted predominantly of faceted spherical particles of a well crystallized solid solution of Cr₂O₃ in θ-Al₂O₃, with diameters of the order of 0.1 μm. Some larger particles of α-Cr₂O₃ were present in powders containing 17.8 and 24 wt% Cr₂O₃. The maximum solid solubility of Cr₂O₃ in θ-Al₂O₃ observed was 18 wt%. It is suggested that nucleation of crystallization of liquid Al₂O₃-Cr₂O₃ droplets occurs as a structure based on cubic close packing of oxygen ions and that the presence of chromium results in ordering to the θ-Al₂O₃ form rather than the δ-Al₂O₃ form usually observed in alumina powders prepared by plasma methods.     

The friction and wear characteristics of plasma-sprayed ZrO2-Cr2O3-CaF2 from room temperature to 800°C

The friction and wear characteristics of low-pressure plasma-sprayed (LPPS) ZrO₂-Cr₂O₃-CaF₂ from room temperature to 800°C were studied by using a high-temperature reciprocating wear tester. At room temperature, friction of ZrO₂-Cr₂O₃-CaF₂ composite coating against Al₂O₃ sphere was quite high, and exhibited a decrease trend with the increase of load from 30 N to 80 N. At 700°C, the composite exhibited the lowest friction and wear among all selected temperature conditions. Brittle fracture and delamination with large wear sheets were considered as the dominant wear mechanism at room temperature. At 400°C, microfracture dropping become more dominated. However, plastic deformation, formation of CaF₂ lubrication films and particle removal of Cr₂O₃ appeared as the main wear mechanisms at elevated temperatures. CaF₂ acting as an effective lubricant at 600°C and 700°C reduced the friction and wear of the composite. Cr₂O₃ particles played a very important role on controlling the size and type of microcracks and preventing or deflecting the microcrack propagation during 700°C test. Cr₂O₃ particles also acted as hard barriers to resist the scratching and high-temperature deformation of ZrO₂-CaF₂ matrix without increasing the friction. To a great extent, wear mainly depended on the degree of debonding and removal of Cr₂O₃ particles at 700°C.     

Effect of calcination on characteristics and sintering behaviour of Al2O3-ZrO2 composite powders

The effect of calcination on the characteristics and sintering behaviour of zirconia-toughened alumina (ZTA) composite powders has been investigated. TiO₂ was selected as an additive to promote the sinterability of ZTA powders. The starting materials were Al₂O₃ powder, Zr(OC₃H₇)₄ and Ti(OC₃H₇)₄, and homogeneous ZTA powder containing Zr-O-Ti bonding was prepared. Calcination affected the tetragonalmonoclinic phase transformation temperature of ZrO₂ crystallizing from the gels. Calcination improved the densification rate of ZTA powder compact during sintering, which was attributed to the optimal ZrO₂ particle size and distribution on the surface of alumina. A ZTA specimen with high bulk density and high tetragonal ZrO₂ content was obtained under the conditions of 850°C/1 h calcination and 1500°C/1 h sintering.     

Effect of cerium zirconate (Ce2Zr2O7) on microstructure and mechanical properties of Ce-ZTA

Powders for ZrO₂ toughened Al₂O₃ (ZTA) composites containing 8, 11, 13.8 and 16.5 vol% ZrO₂ (stabilized with 11.5 mol% CeO₂) are prepared by a hybrid sol-gel method using Al₂O₃ powders and a sol formed from Zr-alkoxide and cerium nitrate. Besides ZrO₂, a small amount of a Ce-zirconate phase (Ce₂Zr₂O₇) forms when the powders are calcined in air. The zirconate phase persists in the sintered specimens and its amount increases from surface to centre of the specimen. Presence of higher amount of Ce₂Zr₂O₇ promotes exaggerated grain growth of Al₂O₃. Particles of Zr rich phases are found to be trapped inside the Al₂O₃ grains. Composites exhibit higher fracture toughness despite lower transformability of t-ZrO₂ during fracture when they contain high amount of zirconate. Crack bridging is shown to be an important mechanism contributing to enhancement in fracture toughness in these composites.     

Slip casting of Al2O3 and Al2O3/ZrO2 composites

Al₂O₃ and Al₂O₃/ZrO₂ composites have been fabricated by slip casting from aqueous suspensions. The physical and structural characteristics of the starting powders, composition of the suspensions, casting behaviour, microstructure of the green and fired bodies and the mechanical properties of the products were investigated. The addition of ZrO₂ to Al₂O₃ leads to a significant increase in fracture toughness when ZrO₂ particles are retained in the tetragonal form (transformation-toughening mechanism) but when microcracking (due to the spontaneous transformation of ZrO₂ from the tetragonal phase to the monoclinic one) is dominant, an excellent toughness value is accompanied by a drastic drop in strength and hardness.     

Pressureless-sintering behavior of nanocrystalline ZrO2–Y2O3–Al2O3 system

ZrO₂–Y₂O₃–Al₂O₃ nanocrystalline powders have been synthesized using chemical coprecipitation method. Nano-powders were compacted uniaxially and densified in a muffle furnace. Densification studies showed that a fully dense pellet of ZrO₂(3Y) and a 99% relative density for 5 mol% Al₂O₃ doped ZrO₂(3Y) were obtained after sintering at 1200 °C. The presence of Al₂O₃ inhibits grain growth and suppresses the densification process. Full densification and the maximum microhardness of 17.8 GPa were achieved for the ZrO₂(3Y)/5 mol% Al₂O₃ composites sintered at 1250 °C.     

Mechanical properties of sinter-forged Al2O3-ZrO2 ceramics

Two kinds of composites, Al₂O₃-25 wt% ZrO₂(2 mol% Y₂O₃) (Y-ZTA), Al₂O₃-25 wt% ZrO₂(8 mol% CeO₂) (Ce-ZTA) were produced by the sinter-forging process. The effect of presintering temperature on the mechanical properties of the composites was examined. The sinter-forging process increased the room-temperature bending strength in comparison with pressureless sintering, owing to the smaller grain size in sinter-forged bodies than in pressureless sintered ones. It was found necessary to keep the presintering temperature considerably lower than sinter-forging temperature in order to improve the room-temperature strength. The strength of sinter-forged Ce-ZTA was higher than that of sinter-forged Y-ZTA. The residual surface compressive stress induced by the phase transition during grinding in Ce-ZTA was found to be effective to further improve the strength and fracture toughness.     

Einfluß der Korngröße auf mechanische Eigenschaften und den ungeschmierten reversierenden Gleitverschleiß von Al2O3-Keramik

Influence of grain size on mechanical properties and dry oscillating sliding wear of Al₂O₃-ceramics Specimens with average grain sizes varying between about 0.8 μm and 12 μm were produced by cold isostatic pressing of high purity Al₂O₃-powder followed by sintering between 1300°C and 1700°C. Hardness, Young's modulus, bending strength and fracture toughness were measured as a function of average grain sizes. Tribological tests were carried out on the different microstructures at normal laboratory air and room temperature by using a ring-on-block tribometer. Experimental results showed the dependence of mechanical properties on grain size, hardness and bending strength obeying a Hall-Petch type relation, approximately. Coefficient of friction was relatively independent of grain size under the test conditions used. However, wear intensity increased substantially if a critical grain size was surpassed. This was due to a change in mechanisms of material removal which was confirmed by scanning electron microscopical studies of the worn surfaces.     

Microstructure of sol–gel synthesized Al2O3–ZrO2(Y2O3) nano-composites studied by transmission electron microscopy

The Al₂O₃–ZrO₂(Y₂O₃) composite powder was synthesized through a sol–gel process using aluminum sec-butoxide and zirconium butoxide as precursors. The as-received powders in an amorphous phase were crystallized with c-ZrO₂ at around 980 °C. As the calcination temperature increased, the c-ZrO₂ crystalline phase was transformed to t-ZrO₂ at about 1200 °C. However, the Al₂O₃ phase in the Al₂O₃–ZrO₂(Y₂O₃) composite powders still existed in an amorphous phase up to 1050 °C. In the sintered body using the calcined powders at 400 °C, the Al₂O₃ phase was crystallized in an α-phase at 1200 °C during the sintering for 2 h. Using the sol–gel Al₂O₃–ZrO₂(Y₂O₃) powder, a typical nano-composite having a nano-crystalline phase (less than 20 nm) can be successfully obtained by a pressureless-sintering process even at 1200 °C for 2 h.Using the sol–gel Al₂O₃–ZrO₂(Y₂O₃) powder, a typical nano-composite having a nano-crystalline phase (less than 20 nm) can be successfully obtained by a pressureless-sintering process even at 1200 °C for 2 h. The values of relative density and Vickers hardness were comparatively high value with about 96.2% and 1100 Hv, respectively, even though it was made at low temperature. In the composite sintered at 1400 °C, the hardness value was saturated with 1570 Hv and the values of fracture toughness were almost same with about 6 MPa m^1/2.     

Friction and wear of ZrO2-TiO2 surface-alloyed Al2O3 ceramics in unlubricated sliding contact

Slightly and highly porous Al₂O₃ ceramics were surface remelted and alloyed by adding ZrO₂ and TiO₂ using infrared CO₂ laser radiation. The resulting composite layers of thickness of about 200 m?m contained about 31 vol.% of ZrO₂- and TiO₂-rich phases which were homogeneously distributed at the grain boundaries of the alumina matrix. Microstructures and worn surfaces were analysed by electron microscopy and EDX analysis. Tribological tests were carried out unlubricated using conditions of abrasive wear and oscillating slinging wear, respectively. The results showed that the average grain size and hardness of the ceramics were reduced due to alloying. Despite decreasing hardness the wear resistance was substantially increased. Friction and wear of the untreated ceramics depended strongly on the amount of porosity which was removed or substantially reduced by laser treatment. Surface alloying of Al₂O₃ ceramics can offer an effective process for producing components showing very different surface and bulk properties and particularly improved tribological behaviour. For the alloying elements and experimental conditions used, the improvement was more pronounced in wear resistance than in friction coefficient.     

Fabrication and interaction mechanism of Ni-encapsulated ZrO2-toughened Al2O3 powders reinforced high manganese steel composites

In order to solve the cast-infiltration difficulty and low interface bonding strength of ZrO₂-toughened Al₂O₃ (ZTA) powders reinforced high manganese steel (HMS) matrix composite, uniform and continuous Ni-encapsulated ZTA powders (ZTA_p@Ni) as reinforced phase are fabricated by electroless deposition assisted with ionic liquid additive. The effects of Ethaline concentration, temperature, ZTA concentration and deposition times on the morphology of ZTA_p@Ni have been investigated. Experimental results show that the thickness of Ni coating is about 7–10 μm, and there is no casting crack or shrink on the composite, so compact bonding between ceramic and matrix is obtained. In addition, the impact abrasive wear resistance testing demonstrates that the performance of ZTA_p@Ni reinforced HMS composite is superior to that of matrix. On the basis of experimental analysis, a schematic illustration of the cast-infiltration process is put forward. It implies that Ni-encapsulated ZTA can be wetted with molten HMS matrix to form a ZTA/Al₂NiO₄-Al₂MnO₄/Fe interface layer through Ni diffusion and reactive wetting. The interdiffusion of Ni and other elements at ZTA interface layer can reinforce the interfacial bonding strength to form an interface layer between metal and hard phases.     

Electrical conductivity of Cr2O3-doped Y2O3-stabilized ZrO2

The electrical conductivity of Cr₂O₃-doped Y₂O₃-stabilized ZrO₂ (YSZ) has been studied as functions of composition, temperature and oxygen pressure. The specimens have been prepared by hot preoning of co precipitated oxides to yield >99.7% density. The Cr₂O₃ added above the solubility limit ( 0.7 mol %) precipitated as a secondary phase at the grain boundaries. The conductivity of Cr₂O₃-doped YSZ was almost independent of the oxygen pressure in the range 10¹⁸ to 10⁵ Pa, indicating a dominant ionic condition. The electronic conductivity of dopant CR₂O₃ would be hindered by the higher ionic conductivity in thep _O2 ranges studied. The conductivity and the activation energy for conduction decreased slightly with the addition of Cr₂O₃. These phenomena seemed to be caused by vacancy trapping or polarization at the grain boundaries with the Cr₂O₃ precipitates. The samples with 1 mol % Cr₂O₃ addred to zirconia containing various Y₂O₃ contents showed similar conduction behaviour to those without Cr₂O₃ addition; that is, the conductivity maxima are observed at around 8 mol % Y₂O₃ addition to zirconia, and the activation energies increased with tha Y₂O₃ addition.     

Interface structure and mechanical properties of Al2O3-20 vol% ZrO2-20 vol% SiCW ceramic composite

The microstructure, mechanical properties, fracture behaviour and toughening mechanisms of Al₂O₃-20 vol% ZrO₂ (2 mol% Y₂O₃)-20 vol% SiC_W ceramic matrix composite were investigated by X-ray diffraction, scanning and transmission electron microscopies, energy dispersive analysis of X-rays, high-resolution electron microscopy techniques and three-point bending tests. The results show that the Al₂O₃ matrix is simultaneously strengthened and toughened by both ZrO₂ particles and SiC whiskers. The interfacial amorphous layers between SiC whiskers and ZrO₂, and Al₂O₃ grains were observed by both TEM dark-field and high-resolution electron microscopy techniques.     

Superplasticity of ZrO2 and ZrO2/Al2O3 composite consisting of nano-sized grains

 Y₂O₃-stabilized ZrO₂ and Y₂O₃-stabilized ZrO₂/10 mol%Al₂O₃ composite both consisting of homogeneous nano-sized grains were successfully fabricated by a pulse electric current sintering through solution chemistry technique. The relative density was above 97% for both the obtained materials, and the grain size was less than 90 nm and 40 nm for the ZrO₂ monolith and the ZrO₂/Al₂O₃ composite, respectively. The materials showed superplastic behavior in compression at temperature of 1200°C. Received: 2 March 1998 / Accepted: 10 March 1998     

Preparation and properties evaluation of zirconia-based/Al2O3 composites as electrolytes for solid oxide fuel cell systems

Yttria-doped zirconia powders containing 3 to 8 mol% Y₂O₃ and 0 to 20 wt% Al₂O₃ were prepared by both mixing commercial oxides and a coprecipitation method, and the mechanical and electrical properties have been examined as a function of the Al₂O₃ content. The bending strength of the composite at room temperature increased with increasing Al₂O₃ content. In the temperature range 500–1000 °C the bending strength increased with Al₂O₃ content up to 10 wt% and then decreased, the measured value at 1000 °C (200 MPa) being higher than those at lower temperatures for cubic zirconia materials. Fracture toughness (K_IC) decreased with increasing Y₂O₃ content in the Al₂O₃-free zirconia materials. Al₂O₃ additions enhanced the fracture toughness and this was maximum (7 MPa m^1/2) for the composite ZrO₂-3 mol% Y₂O₃/10 wt% Al₂O₃. The electrical conductivity of cubic ZrO₂/Al₂O₃ composites decreased monotonically with Al₂O₃ content, but in tetragonal ZrO₂/Al₂O₃ composites hardly varied or apparently increased up to 10 wt% Al₂O₃. At 1000 °C the highest electrical conductivity was 0.30 S cm^–1 for ZrO₂-8 mol% Y₂O₃, and this decreased up to 0.10 S cm^–1 for the composite ZrO₂-8mol% Y₂O₃/20 wt% Al₂O₃.     

Subsolidus,high temperature phase relations in the systems Al2O3-Cr2O3-ZrO2, MgO-Cr2O3-ZrO2 and MgO-Al2O3-ZrO2

In the temperature range 1600 to 1900° C, the system A₂O₃-Cr₂O₃-ZrO₂ is characterized by the coexistence of ZrO₂ (unstablilized) and an (Al, Cr)₂O₃ solid solution series. In the systems MgO-Cr₂O₃-ZrO₂ and MgO-Al₂O₃-ZrO₂ a nearly stoichiometric spinel coexists with both stabilized and unstabilized ZrO₂. At temperatures above 1600°C a new ternary Mg-Al-Zr oxide becomes stable in the MgO-rich part of the MgO-Al₂O₃-ZrO₂ system.