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ww.sciencedirect.com j o u r n a l o f m a t e r i a l s r e s e a r c h and t e c hno l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0 Available online at w journal homepage: www.elsevier .com/locate/ jmrt Original Article Development and characterization of alumina- toughened zirconia (ATZ) ceramic composites doped with a beneficiated rare-earth oxide extracted from natural ore Eduardo de Sousa Lima a,*, Camila Catalano Gall a, Manuel Fellipe R.P. Alves b, Jos�e Brant de Campos c, Tiago Moreira Bastos Campos d, Claudinei dos Santos a,e a Materials Science Department, Military Institute of Engineering, Praça Gen. Tibúrcio, 80, Praia Vermelha, 22290- 270, Rio de Janeiro, RJ, Brazil b Mechanical and Energy Department, Rio de Janeiro State University, UERJ-FAT, Rodovia Presidente Dutra, Km 298, 27537-000, Resende, RJ, Brazil c Mechanical Engineering Department, Rio de Janeiro State University, Rua Fonseca Teles, 121, S~ao Cristov~ao, 20940- 200, Rio de Janeiro, RJ, Brazil d Physics Department, Aeronautics Institute of Technology, Praça Marechal Eduardo Gomes, 50 Vila Das Ac�acias, 12228-900, S. J. Campos, SP, Brazil e Federal Fluminense University - UFF/EEIMVR, Av. Dos Trabalhadores,420, V. S.Cecı́lia, 27255-125, Volta Redonda, RJ, Brazil a r t i c l e i n f o Article history: Received 27 October 2021 Accepted 25 November 2021 Available online 4 December 2021 Keywords: Ce-TZP/Al2O3 composites Rare-earth oxides YAG - Y3Al5O12 Characterization Mechanical properties Brazilian xenotima * Corresponding author. E-mail address: sousalima@ime.eb.br (E.S https://doi.org/10.1016/j.jmrt.2021.11.141 2238-7854/© 2021 Published by Elsevier B.V. T licenses/by-nc-nd/4.0/). a b s t r a c t This work analysed the effect of the addition of rare-earth mixed oxide (RE2O3), a solid solution of Y2O3 and other rare earths benefited from a Brazilian natural ore called Xen- otime, on the sintering and properties of a commercial nanopowder composed of Ce- tetragonal polycrystal zirconia (TZP) þ 15 wt.% Al2O3. Powder mixtures were prepared, adding 10 wt.% of Y2O3 or 10 wt.% RE2O3 in Ce-TZP/Al2O3 powder, which were compacted and sintered at 1500 �C for 2 h. Sintered samples were characterized by X-ray diffraction, scanning electron microscopy, and relative density. Structural analyses and phase quan- tification were performed using the Rietveld refinement method. Mechanical character- ization - Vickers hardness and fracture toughness - of the samples was carried out by Vickers indentation. The results indicated that the RE2O3 is composed of a solid Y2O3 so- lution with lattice parameters slightly lower than those of pure Y2O3 due to the presence of other oxides such as Yb2O3 (19.7%), Er2O3 (13.9%), or Dy2O3 (10.2%). During sintering, the oxides added to the composite were completely consumed by the Ce-TZP/Al2O3 matrix to form two different crystalline phases: ZrO2-Cubic and Y3Al5O12. As a consequence, multi- phase composites with relative density of 93.8 ± 1.2 (Y2O3 reinforced) and 94.5 ± 1.7 (RE2O3 reinforced), average hardness in the order of 10.5 GPa, and fracture toughness of 7.1 e8.5 MPa m1/2 were obtained. The high fracture toughness observed was a consequence of . Lima). his is an open access article under the CC BY-NC-ND license (http://creativecommons.org/ mailto:sousalima@ime.eb.br http://crossmark.crossref.org/dialog/?doi=10.1016/j.jmrt.2021.11.141&domain=pdf www.sciencedirect.com/science/journal/22387854 http://www.elsevier.com/locate/jmrt https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 http://creativecommons.org/licenses/by-nc-nd/4.0/ http://creativecommons.org/licenses/by-nc-nd/4.0/ j o u r n a l o f ma t e r i a l s r e s e a r c h a nd t e c h no l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0452 Table 1 e Specification of the materials Material Manufacturer (commercial specification) ZrO2 CeO2 Al2O3 SiO2 þ Na2O TiO2 Y2O3 Other rare-earth elements Density (g/cm3) Average particle size (mm) Specific surface area (m2/g) a Not determined. the presence of different coupled toughening mechanisms resulting from the multiphase characteristic of these composites. © 2021 Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/). 1. Introduction With the advancement of synthesis techniques in nano- crystalline ceramic powders, many crystallographic and microstructural phenomena and mechanical, thermal and/or chemical properties have been explored in recent years aim- ing to increase the potential use of these materials within the engineering supply chain. Among these materials, those intended for use as structural ceramics [1e5] that present high fracture toughness, hardness, thermal shock and corrosion/ degradation resistance are of particular importance in appli- cations such as ballistic shielding or protective layers for ar- tefacts in marine environments. ZrO2eAl2O3 composites [6e9], also known as alumina- toughened zirconia (ATZ) ceramics, have great potential for structural applications. These ceramic materials are usually composed of a tetragonal zirconia polycrystalline (TZP) matrix stabilized with yttria (Y-TZP). They are aimed at generating solid bodies mainly composed of tetragonal grains (t-ZrO2) that present a peculiar toughening mechanism through tetragonal-to-monoclinic (t/m) phase transformation [10e13]. When combined with alumina (Al2O3), this ATZ composite presents higher hardness and fracture toughness than those of other conventional ceramics such as monolithic alumina (Al2O3), silicon carbide (SiC), silicon nitride (Si3N4), among others [14e16]. On the other hand, these tetragonal zirconia grains present in the ATZ composite have low resis- tance to hydrothermal degradation, and thus are not indicated for use in aqueous media for long periods. Therefore, Ce-TZP/ Al2O3 composites, which present ceria oxide (CeO2)-stabilized grains in the TZP matrix and superior fracture toughness and used in this work (man Ce-TZP/Al2O3 Saint-Gobain, UprYZr-Shock (France) Balance 6 ± 0.7 wt.% 15 ± 1 wt.% <0.04 wt.% <0.005 wt.% e e 5.65 0.2 8.5 hydrothermal degradation resistance, are a technological advance in these ATZ ceramics [17e19]. The yttrium aluminium garnet (YAG - Y3Al5O12) compound is formed by the combination of yttrium oxide (Y2O3) and alumina (Al2O3). This formation of Y3Al5O12 occurs under thermal treatments at >1300 �C, and the YAG widely used in optical applications [1,20,21], as Al2O3 toughener [22], as well as the component used in the formation of the liquid phase required for sintering/densification of covalent ceramics based on silicon carbide (SiC) and/or silicon nitride (Si3N4) [23,24], promote significant improvement in the mechanical properties of these materials. Recently, a process was developed in Brazil to obtain an yttrium and rare-earth mixed oxide (RE2O3) with structural characteristics close to those of pure Y2O3, but at a much lower cost. RE2O3 production is based on the use of a very abundant mineral called xenotime [25e27]. Xenotime, which is basically an yttrium and rare-earth phosphate (Y,RE)PO4, is mixed with NaOH and heated up to 700 �C, allowing the reaction 1 to occur: (Y,RE)PO4 þ 6NaOH / Na3(Y,RE)O3 þ Na3PO4 þ 3H2O (1) This material is milled, lixiviated, precipitated with oxalic acid, and calcined again to obtain a solid solution of Y2O3, Yb2O3, Er2O3, Dy2O3 and smaller amounts of other rare earths [28,29]. This study aimed to obtain the in situ formation of the Y3Al5O12 phase during sintering of the Ce-TZP/Al2O3 com- posite using a comparative form: addition of Y2O3 or RE2O3 to the reaction with Al2O3 present in the chemical composition of the mixture. Microstructural and crystallographic aspects, ufacturing data). Y2O3 RE2O3 H.C.Starck (Germany) University of S~ao Paulo (USP) (Brazil) e e e e e e e e 99.9 wt.% 44.6mol% Yb2O3 (19.7%), Er2O3 (13.9%), Dy2O3 (10.2%), Ho2O3 (3.2%), Tm2O3 (2.8), Lu2O3 (2.6%); (Gd2O3 þ Tb2O3 þ Sm2O3 - balance) (mol %) 5.01 5.12 0.5 0.8 a a http://creativecommons.org/licenses/by-nc-nd/4.0/ https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 Fig. 1 e XRD patterns of the starting powders: a) (Ce,Y)-TZP/ Al2O3. b) Y2O3; c) RE2O3. j o u r n a l o f m a t e r i a l s r e s e a r c h and t e c hno l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0 453 aswell as the presence of three simultaneous phases and their effects on densification, microstructure, and mechanical properties were discussed. 2. Methods 2.1. Materials Table 1 presents the specifications of the starting powders used in this work. 2.2. Processing Two compositions of the (Ce,Y)-TZP/Al2O3 composite were studied in this work: one containing 10 wt.% Y2O3 and another containing 10 wt.% RE2O3. Preparation of the ceramic bodies started with mixing the powders with isopropyl alcohol for 2 h, aiming homogenization. After mixing, the powder batches were dried in oven at 100 �C for 24 h. The powder mixtureswere sieved through a 60-mesh screen. Themixtures were compacted into a cylindrical matrix of 15 mm in diam- eter by cold uniaxial pressing at 70 MPa for 30 s. Then the green compacts were sintered in a MoSi2 furnace (Fortelab F1600, Brazil). The heating rates varied as follows: 2 �C/min up to 700 �C and 5 �C/min up to 1500 �C, with no sintering plateau. The cooling rate was 10 �C/min. Comparatively, the as- Table 2 e Crystallographic characteristics of the Y2O3, RE2O3 ox Parameters Y2O3 RE2O3 Present phase Y2O3 Y2O3 (solid solution) Percentage (%) 100 100 System Cubic Cubic Space group Ia e3 (n� 206) Ia e3 (n� 206) a (�A) 10.6079 (3) 10.588 (1) Rp (%)/Rwp (%)/Rexp (%) 9.2/15.4/11.3 11.3/14.0/10.9 c2 1.88 1.66 received composite powder, was compacted, sintered under similar processing conditions, and characterized. 2.3. Characterization The apparent density and consequent relative density of the composites were measured by the immersion in distilled watermethod using the Archimedes principle. The theoretical density of the samples was calculated according to the rule of mixtures. The crystalline phases were determined by X-ray diffrac- tion (XRD) on a PANalytical EMPYREAN diffractometer equippedwith a graphitemonochromator and Cu Ka radiation (l ¼ 1.5406 �A), operating at a voltage of 40 kV and a current emission of 40 mA, with a q-2q scanning system configured in BraggeBrentano geometry. The data were obtained over a 2q range of 10e90� at a scan rate of 0.2�/min and step size of 0.6 s/ step. Quantitative and present phase calculations and basic parameters were obtained by applying the Rietveld refine- ment method. For microstructural analysis of the sintered samples, pol- ished surfaces were thermally etched at 1400 �C for 15 min using a furnace (FE1750-MAITEC, Brazil). The etched surfaces were metalized using an Emitech K550X Sputter Coater (Quorum Technologies - Kent, UK) with 30 mA for 2 min. Microstructural analyses were performed in a scanning elec- tron microscopy (JEOL® FEG JSM 7100FT) with an 80 mm2 EDS detector (Oxford X-Max, UK). Microstructural analysis of the sintered sampleswas performed using the ImageJ software on a population of approximately 500 grains. Hardness and fracture toughness (KIc) were determined by the Vickers indentationmethod [30,31] using hardness testing equipment (Emcotest DuraScan). In each group of samples, 20 indentations were measured under a load of 98 N for 30 s. Fracture toughness was calculated according to Equation (2), valid for Palmqvist-type cracks [32,33]. KIC ¼0:035 � l a ��1 2 � Hv EF ��2 5 Hva 1 2 F ! (2) where: KIC ¼ fracture toughness (MPa.m1/2); “l” ¼ length of the crackmeasured from the tip of the indentation to the tip of the crack (mm); “a” ¼ half length of the indentation diagonal (mm); “HV” ¼ Vickers hardness (GPa); “E” ¼ Young's modulus (GPa); "F" ¼ dimensionless constant developed by Niihara (F ¼ 2.7). The crack lengths generated by the Vickers indentations were observed by scanning electron microscopy (SEM) using a TESCAN VEGA 3 XMU microscope in the secondary-electron imaging mode. ides and (Ce,Y)-TZP/Al2O3 composite from XRD analysis. (Ce,Y)-TZP/Al2O3 ZrO2-m ZrO2-t CeO2 Al2O3 77.1 4.3 4.4 14.2 Monoclinic Tetragonal Cubic Hexagonal Not evaluated 1.78 https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 Fig. 2 e a) XRD patterns of Ce-TZP/Al2O3 doped with 10% Y2O3 and 10% RE2O3 after sintering at 1500 �C for 2 h; b) expanded 2 q (38� ~ 42�); c) expanded 2 q (65� ~ 75�). Fig. 3 e Quantification of the phases in the sintered ceramic composites doped with 10% Y2O3 or 10% RE2O3. j o u r n a l o f ma t e r i a l s r e s e a r c h a nd t e c h no l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0454 3. Results and discussion 3.1. Characterization of the starting powders Figs. 1 (a-c) and Table 2 present the results of X-ray diffraction and Rietveld refinement of the RE2O3 and Y2O3 oxides and the Ce-TZP/Al2O3 powder. The X-ray diffraction (XRD) patterns of the yttrium and rare-earth mixed oxide powders show that all peaks are related to the Y2O3-type structure. It can be noted that the peaks are less intense and wider, Fig. 1 (a), than those of pure Y2O3 (Fig. 1 (b)). The full width at halfmaximum (FWHM) of the most intense peak (222) was determined to be 0.50�. Comparing the diffraction patterns of RE2O3 (Fig. 1 (a)) and of Y2O3 (Fig. 1 (b)), the intensity of the main peak (222) for the mixed oxide is about 9 times smaller than that of pure yttria. It can also be observed that the peaks of the mixed oxide were well adjusted for a pseudo-Voigt profile function. The well- defined peaks evidence the formation of a true solid solu- tion, as noted in previous work [34]. The refined structural parameters for yttria and the mixed oxide are shown in Table 2. It can be observed that the lattice parameter of RE2O3 is slightly lower than that of pure Y2O3, which can be explained by the smallermean lattice parameter of the rare-earth oxides that constitute the studied mixture. The (Ce,Y)-TZP/Al2O3 composite powder presents different phases: m-ZrO2 (77.1%), t-ZrO2 (4.3%), CeO2 (4.4%), and Al2O3 (14.2%). These proportions are in accordance with data pro- vided by the manufacturer. 3.2. Characterization of the sintered specimens Figs. 2 (a-c) shows the XRD results of the sintered samples containing 10 wt.% RE2O3 or 10 wt.% de Y2O3 as a dopant, and https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 Table 3 e Rietveld refinement of sintered ceramic composites doped with 10% Y2O3 or 10% RE2O3. Ce-TZP/Al2O3/Y2O3 Al2O3 (Corundum) Y3Al5O12 (YAG) t- ZrO2 c- ZrO2 Crystalline composition (%) 46.4 t-ZrO2 37.3 c-ZrO2 12.7% - Al2O3 3.6% - YAG Crystalline structure Rhombohedral Cubic Tetragonal Cubic Space group R-3cH Ia-3d P42/nmcZ e Lattice parameters (Â) a ¼ 4.755 c ¼ 12.956 a ¼ 12.011 a ¼ 3.608 c ¼ 5.191 e Phase density (g/cm3) 4.002 4.555 6.053 e Crystallite size (nm) 326.641 93.834 72.226 e Ce-TZP/Al2O3/RE2O3 Al2O3 (Corundum) Y3Al5O12 ZrO2 c- ZrO2 Crystalline composition 47.4% t - ZrO2 34% c - ZrO2 5.9% - Al2O3 12.7% - YAG Crystalline structure Rhombohedral Cubic Tetragonal Cubic Space group R-3cH Ia-3d P42/nmcZ e Lattice parameters (Â) a ¼ 4.751 c ¼ 12.961 a ¼ 11.990 a ¼ 3.610 c ¼ 5.184 e Phase density (g/cm3) 4.008 4.574 6.056 e Crystallite size (nm) 355.640 138.767 54.836 e j o u r n a l o f m a t e r i a l s r e s e a r c h and t e c hno l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0 455 Fig. 3 presents the results of phase quantification in the sin- tered samples. The Rietveld refinement results are presented in Table 3. Figure 2 (a) shows the presence of tetragonal (t-ZrO2) and cubic (c-ZrO2) zirconia regardless of the use of Y2O3 or RE2O3. In addition, difference in intensity betweenthe crystalline peaks can be noticed: the ceramic composite doped with 10 wt.% Y2O3 presents more intense cubic phase (c-ZrO2) peaks, whereas the ceramic composite doped with 10 wt.% RE2O3 shows more intense Y3Al5O12 peaks, as shown in magnifica- tions of the diffractograms in Fig. 2 (b-c). An associated anal- ysis of Fig. 2 and Fig. 3 shows that both materials have a considerable amount of t-ZrO2 after sintering, in the order of 47%, from the reaction between monoclinic zirconia and cerium oxide present in the starting powder, reaction 3. Considerable differences are observed in the quantification of the c-ZrO2 phase, where the composite doped with 10% Y2O3 (37.3%) presented larger amount of cubic phase than the Fig. 4 e SEM micrographs of the sintered (Ce,Y)-TZP-Al2O3 comp 10,000£). composite doped with 10% RE2O3 (34%). On the other hand, there is a great difference between Al2O3 and Y3Al5O12, which results from the greater propensity of RE2O3 to form REAG (Y(ss)2Al5O12) compared with Y2O3, according to reaction 4. ZrO2 (m) þ CeO2 / ZrO2 (t) (3) 3/2 Y(ss)2O3 þ 5/2 Al2O3 / Y(ss)3Al5O12 (4) Assuming that, the use of Y2O3 as a dopant facilitates for- mation of the c-ZrO2 phase (Eq. (5)); the original alumina quantifications are maintained with a little YAG formation in the structure, with excess Y2O3. ZrO2 (m) þ Y2O3 / ZrO2 (c) (5) Thus, when RE2O3 is used to dope the ceramic composite, there isgreaterpresenceofYAGintheoverall compositionof the osite highlighting hexaluminate platelets (magnification - https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 j o u r n a l o f ma t e r i a l s r e s e a r c h a nd t e c h no l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0456 sintered composite and, consequently, smaller fractions of cubicphaseZrO2-(c)andAl2O3areobserved.Thisoccursbecause RE2O3 is a mixture of oxides that presents greater atomic dis- order, increasing the reactivity of the powder. In this case, the associated energy is greater and, therefore, the reactions in the solid state begin at temperatures lower than those of the high purity oxides. In Table 1, the mean grain size of RE2O3 is on the order of 0.8 mm, but the FWHMof the XRD peak in Fig. 1 is large, although it is a true solid solution. As the RE2O3 particles are formed fromfine crystallite aggregates, theywill have excellent reactivity, which justifies the clear XRD peaks of Y3Al5O12 observed in the sample with the addition of RE2O3. Figure 4 Present micrographs obtained by SEM of the composite without additions of Y2O3 or RE2O3, indicating the presence of submicrometric equiaxed grains of zirconia (light phase) and alumina (dark phase). Some platelets larger than 2 mm are also seen. These platelets are formed during sinter- ing, by the solid state reaction of alumina contained in the initial powder mixture and cerium oxide, forming hex- aluminates, and are indicated as reinforcements for these Ce- TZP-Al2O3 composites [39]. Fig. 5 and Fig. 6 present the SEM micrographs of composites containing 10 wt.% Y2O3 and 10 wt.% RE2O3 respectively. Furthermore, Fig. 7 (a-c) shows the average grain size of the samples containing 10 wt.% Y2O3 and 10 wt.% RE2O3. It is possible to observe a zirconia matrix with submicrometric characteristics, as well as equiaxial alumina grains (Al2O3) distributed throughout the zirconia matrix, which are preferentially found in triple junctions. Fig. 5 e SEMmicrographs of the sintered (Ce,Y)-TZP-Al2O3 comp indicate equiaxed grains of Al2O3 (dark phase, Fig. 5(b), and gro The addition of Y2O3 (Fig. 5) or RE2O3 (Fig. 6) inhibits the formation of hexaluminate platelets, therefore platelets are not observed in these composites. Furthermore, the insertion of Y2O3 as an additive promotes an increase in the number of c-ZrO2 grains in a behaviour predicted by Li et al. [40] in ZrO2eCeO2eY2O3 system, whose microstructure presents grains remarkably larger than the tetragonal (t-ZrO2) grains. Furthermore, a microstructural heterogeneity due to prefer- ential growth of cubic c-ZrO2 phase grains is observed. The use of RE2O3 as a dopant favoured the formation of large YAG (Y3Al5O12) grains, Fig. 6(c), characterized by the absence of alumina grains in the vicinity due to having been consumed according to the reaction (4), and in agreement with the re- sults X-ray diffraction, Fig. 3, It is also noted that the residual alumina present in this composite is composed of equiaxed grains of submicrometric size, as indicated in Fig. 6(a,b). Figure 7 (a) shows that the sintered composite doped with Y2O3 has a large population of zirconia grains with average size <1 mm. Moreover, a population of zirconia grains with exaggerated growth is identified and, finally, the larger grains (3.1e4.9 mm) are characteristic of Y3Al5O12. The use of RE2O3 as a dopant also allows the grains of the zirconia matrix to remain with submicrometric characteristics, with sizes be- tween 0.1 and 0.7 mm, with a small population of larger cubic grains in addition to YAG grains >2 mm (Fig. 7 (b)). The analysis also showed that the Al2O3 grains, regardless of their average size, do not present significant variations as a function of the type of dopant used in the mixture (Fig. 7 (c)). osite containing 10 wt.% Y2O3: a) 5000 x; b) 10,000 x. Arrows wn grains of ZrO2-Cubic, Fig. 5(c). https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 Fig. 6 e SEM micrographs of the sintered (Ce,Y)-TZP-Al2O3 composite containing 10 wt.% RE2O3: a) 10,000 x; b) 40,000 x; c) 10,000 x (highlighting gray YAG grains with no black Al2O3 grains on their boundaries). j o u r n a l o f m a t e r i a l s r e s e a r c h and t e c hno l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0 457 3.3. Mechanical properties The hardness and fracture toughness values of the samples sintered at 1500 �C determined at room-temperature are summarized in Table 4. Results of the mechanical properties are probably corre- lated with material densification. The composite doped with Y2O3 had a relative density of 93.8 ± 1.2%, while the composite doped with RE2O3 presented a slightly higher density value (94.5 ± 1.7%) and were thus considered statistically similar. The microstructural and crystallographic configuration pre- sented by the materials, as well as the residual porosity in the order of 5.5e5.2%, after sintering, led to mean Vickers hard- ness values of 9.8 ± 1.2 GPa (Y2O3) and 10.1 ± 1.7 GPa (RE2O3), as shown in Table 4. The composites developed in this work showed that the use of 10 wt.% Y2O3 induces the formation of the cubic phase ZrO2-(c) as well as of the ZrO2-(t) phase stabilized with ceria (Ce-TZP), an amount of Al2O3 close to the original proportion, and a small fraction of transformed YAG. This complex microstructural configuration, allowed high fracture tough- ness values (8.5 ± 0.9 MPa m1/2). In contrast, the composite doped with 10 wt.% RE2O3 induces formation of four distinct phases: Ce-TZP (majority), cubic-ZrO2, Al2O3, and Y3Al5O12, which associated with densification, enabled fracture tough- ness values in the order of 7.1 ± 0.4 MPa m1/2. As the densification and mechanical properties of the original commercial composite without the addition of Y2O3 or RE2O3 oxides are slightly superior to doped composites, even without the presence of hexaluminate platelets, new sintering conditions involving higher final temperatures or prolonged isothermal holding times may be suggested for future investigations, aiming to improve densification and mechanical properties, adjusting their properties to the intended final application of this composite. Figure 8 (a) shows the Vickers indentation and 8(b), the radial cracks developed. Results of the microstructural analysis suggest that the use of rare-earth oxides enables greater refinement of the Ce-TZP grain, responsible for the toughening of the material due to toughening mechanisms by phase transformation.It is known that tetragonal zirconia with average grain size <0.8 mm has higher toughening capacity than zirconia with larger grain size [35]. This toughening mechanism by phase transformation is more relevant when using CeO2 as a dopant in substitution for the traditional Y2O3 (Y-TZP) [35,36]. Therefore, the shielding zone at the tip of the crack in Ce-TZP is higher than in Y-TZP, thus inducing greater https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 Fig. 7 e Grain size distribution analysis of: a) Ce-TZP/Al2O3 doped with 10 wt.% Y2O3; b) Ce-TZP/Al2O3 doped with 10 wt.% RE2O3; c) Al2O3 grains. j o u r n a l o f ma t e r i a l s r e s e a r c h a nd t e c h no l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0458 crack locking and more effective reduction of crack propagation. The Al2O3 grains present in the matrix are considered a secondary toughening mechanism that generates residual stress around the ZrO2matrix. Thus, during crack propagation in biphasic regions of the composite, higher fracture energies are necessary for the crack to continue propagating. In addi- tion, the presence of a third phase in greater quantity, when using RE2O3, favours the appearance of residual thermal ten- sions in the material. As Al2O3 is preferentially found in triple junctions, spontaneous crack locking is obtained considering that, as the cracks are intergranular, they are located along the grain boundaries. Theoretically, residual thermal stresses in Table 4 e Properties of the ceramic composites doped with Y2O3 or RE2O3. Sample Relative density (%) Vickers Hardness HV98N (GPa) Fracture toughness KIC 98 N (MPa.m1/2) (Ce,Y) - TZP/Al2O3 95.2 ± 0,7 11.3 ± 1.4 8.6 ± 0.7 Ce-TZP/Al2O3/10%Y2O3 93.8 ± 1.2 9.8 ± 1.2 8.5 ± 0.9 Ce-TZP/Al2O3/10%RE2O3 94.5 ± 1.7 10.1 ± 1.7 7.1 ± 0.4 multiphase materials can be calculated using the mathemat- ical approximation given in the Equations (6)e(8) [37,38]: sb ¼ Eb , ða�abÞ,DT (6) sm ¼ Em , ða�amÞ,DT (7) a¼ abCbEb þ acCcEc þ amCmEm CbEb þ CcEc þ CmEm (8) Considering the Young's modulus of the ZrO2, Al2O3 and Y3Al5O12 phases as 190 GPa, 390 GPa and 300 GPa, respectively, and their respective thermal expansion coefficients (a) as 10.5 � 10�6 K�1, 8.5 � 10�6 K�1, 6.2 � 10�6 K�1, the residual stresses in each phase for the ATZ-Y2O3 composite are esti- mated to be sZrO2 ¼ �182.1 MPa, sAl2O3 ¼ 776.6 MPa, and sY3Al5O12 ¼ 1615 MPa, whereas the ATZ-Re2O3 composite pre- sents calculated residual stresses of sZrO2 ¼ �257,8 MPa, sAl2O3 ¼ 621.3 MPa, and sY3Al5O12 ¼ 1495 MPa. Reflections of these thermal stresses distributed among the phases present in the composites contribute to generate stress fields that act to hinder crack propagation in a stable way. This reduced crack propagation, in combination with the shielding zones around the major phase of ZrO2-(t) grains (Ce- TZP), hinder crack growth and provide the material with high fracture toughness. https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 Fig. 8 e a) Example of Vickers indentation (magnification 1000£); b) emphasis on the propagation of cracks and their behaviour (magnification near to 17,000£). j o u r n a l o f m a t e r i a l s r e s e a r c h and t e c hno l o g y 2 0 2 2 ; 1 6 : 4 5 1e4 6 0 459 4. Conclusions Themixed yttrium and rare-earth oxide (RE2O3) obtained from mineral xenotime is a solid solution of yttria and other rare- earth oxides with partial similarity to high purity Y2O3. Within the experimental limits investigated in this manu- script, it was observed that the use of this oxide (RE2O3) as a dopant in ZrO2eAl2O3eCeO2 systems induced the preferential formation of Y3Al5O12 during sintering, partially consuming Al2O3 from the initial chemical composition, while the use of Y2O3 it tends to form cubic-ZrO2 while maintaining the orig- inal Al2O3 contents. The results indicated that the addition of this oxide (10 wt.%) to a Ce-TZP/15%Al2O3 powder mixture resulted in ceramic composite with high hardness and frac- ture toughness values, in the order of 10.1 ± 1,7 GPa and 7.1 ± 1.7 MPa m1/2, respectively, containing a complex micro- structure formed by ZrO2(t), ZrO2(c), Al2O3, and Y3Al5O12. This microstructural configuration allows the material to resist well to crack propagation, because different toughening mechanisms act simultaneously during crack growth. These results are similar to those of composites obtained with addition of Y2O3 to this ceramic composite and demonstrate the feasibility of using RE2O3 to replace high purity commer- cial Y2O3. Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. Acknowledgments Dr. Eduardo de Sousa Lima would like to thank National Council for Scientific and Technological Development e CNPq (project nº 312161/2020e4) for the financial support received. Dr. Claudinei dos Santos would like to thank FAPERJ (grant nº E-26/202.997/2017) and National Council for Scientific and Technological Development e CNPq (project nº 311119/ 2017e4) for the financial support received. 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http://refhub.elsevier.com/S2238-7854(21)01420-4/sref40 https://doi.org/10.1016/j.jmrt.2021.11.141 https://doi.org/10.1016/j.jmrt.2021.11.141 Development and characterization of alumina-toughened zirconia (ATZ) ceramic composites doped with a beneficiated rare-eart ... 1. Introduction 2. Methods 2.1. Materials 2.2. Processing 2.3. Characterization 3. Results and discussion 3.1. Characterization of the starting powders 3.2. Characterization of the sintered specimens 3.3. Mechanical properties 4. Conclusions Declaration of Competing Interest Acknowledgments References
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