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Effect of sintering parameters using the central composite design method, electronic structure and physical properties of yttria-partially stabilized ZrO2 commercial ceramics

A.M. Mendes
A.M. Mendes
, 
M.C.B. Costa
M.C.B. Costa
, 
V.D. Araújo
V.D. Araújo
, 
F.V. Motta
F.V. Motta
, 
C.A. Paskocimas
C.A. Paskocimas
, 
W. Acchar
W. Acchar
, 
E. Longo
E. Longo
, 
M.R.D. Bomio
M.R.D. Bomio
 und 
L.S. Cavalcante
L.S. Cavalcante
   | 24. Feb. 2017
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Online veröffentlicht: 24. Feb. 2017
Seitenbereich: 225 - 238
Eingereicht: 15. Sept. 2016
Akzeptiert: 28. Jan. 2017
DOI: https://doi.org/10.1515/msp-2017-0035
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© 2017 A.M. Mendes, M.C.B. Costa, V.D. Araújo, F.V. Motta, C.A. Paskocimas, W. Acchar, E. Longo, M.R.D. Bomio, L.S. Cavalcante
This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

(a) XRD patterns of 3Y-PSZ non-sintered ceramics (I) and 3Y-PSZ ceramics sintered at different temperatures (II to XII) and times, (b) Indexed monoclinic and tetragonal phases in XRD patterns of 3Y-PSZ ceramics. The vertical lines indicate the relative positions of the diffraction peaks described in ICSD No. 66782 and No. 18190 and (c) Indexed tetragonal phase XRD patterns for 3Y-PSZ ceramics sintered at 1550 °C for 12 h, respectively.
(a) XRD patterns of 3Y-PSZ non-sintered ceramics (I) and 3Y-PSZ ceramics sintered at different temperatures (II to XII) and times, (b) Indexed monoclinic and tetragonal phases in XRD patterns of 3Y-PSZ ceramics. The vertical lines indicate the relative positions of the diffraction peaks described in ICSD No. 66782 and No. 18190 and (c) Indexed tetragonal phase XRD patterns for 3Y-PSZ ceramics sintered at 1550 °C for 12 h, respectively.

(a) Rietveld refinement plot of 3Y-PSZ non-sintered ceramics and (b) 3Y-PSZ ceramics sintered at 1550 °C for 12 h.
(a) Rietveld refinement plot of 3Y-PSZ non-sintered ceramics and (b) 3Y-PSZ ceramics sintered at 1550 °C for 12 h.

(a) Schematic representation of the monoclinic unit cells corresponding to ZrO2 crystal illustrating distorted deltahedral [ZrO7] clusters, (b) tetragonal unit cells corresponding to ZrO2 crystal illustrating distorted deltahedral [ZrO8] clusters and (c) tetragonal unit cells corresponding to ZrO2 crystals illustrating distorted deltahedral [ZrO8]/[YO8] clusters, respectively.
(a) Schematic representation of the monoclinic unit cells corresponding to ZrO2 crystal illustrating distorted deltahedral [ZrO7] clusters, (b) tetragonal unit cells corresponding to ZrO2 crystal illustrating distorted deltahedral [ZrO8] clusters and (c) tetragonal unit cells corresponding to ZrO2 crystals illustrating distorted deltahedral [ZrO8]/[YO8] clusters, respectively.

Electron density maps on: (a) (1 2 1), (b) (1 4 1), (c) (6 3 6) and (d) (1 2 0) planes of 3Y-PSZ non-sintered ceramics and ceramics sintered at 1550 °C for 12 h.
Electron density maps on: (a) (1 2 1), (b) (1 4 1), (c) (6 3 6) and (d) (1 2 0) planes of 3Y-PSZ non-sintered ceramics and ceramics sintered at 1550 °C for 12 h.

FE-SEM images for 3Y-PSZ ceramics sintered at: (a) 1350 °C for 4 h, (b) 1350 °C for 12 h, (c) 1550 °C for 4 h and (d) 1550 °C for 12 h.
FE-SEM images for 3Y-PSZ ceramics sintered at: (a) 1350 °C for 4 h, (b) 1350 °C for 12 h, (c) 1550 °C for 4 h and (d) 1550 °C for 12 h.

Average grain size distribution of 3Y-PSZ ceramics sintered at: (a) 1350 °C for 4 h, (b) 1350 °C for 12 h, (c) 1550 °C for 4 h and (d) 1550 °C for 12 h.
Average grain size distribution of 3Y-PSZ ceramics sintered at: (a) 1350 °C for 4 h, (b) 1350 °C for 12 h, (c) 1550 °C for 4 h and (d) 1550 °C for 12 h.

Response surfaces of 3Y-PSZ ceramics sintered at different temperatures and times for: (a) volumetric shrinkage, (b) average grain size and (c) hardness.
Response surfaces of 3Y-PSZ ceramics sintered at different temperatures and times for: (a) volumetric shrinkage, (b) average grain size and (c) hardness.

Volumetric shrinkage (VS), average grain size (AGS) and Vickers hardness (VH) for all combinations of sintering temperature and times.

3Y-PSZ sintered ceramicsMeasured values
VS [%]AGS [μm]VH [GPa]
VII44.1±3.40.194±0.0435.45±0.12
XII40.6±5.40.216±0.0536.05±0.22
X45.0±5.80.228±0.0577.49±0.42
VIII50.2±5.90.276±0.07411.3±0.18
VI50.7±2.30.31±0.1113.01±0.42
II50.3±2.80.384±0.09113.27±0.38
XI50.2±2.90.377±0.09613.06±0.41
III53.1±5.20.454±0.08513.71±0.12
IX54.2±5.50.55±0.1413.26±0.30
IV54.8±4.20.75±0.1912.52±0.32
V54.8±1.70.54±0.1813.24±0.16

Coded and uncoded values of levels for sintering temperature and time and its execution order.

3Y-PSZ sintered ceramicsCoded LevelsUncoded Levels
TemperaturetimeTemperature [°C]time [h]
VII–1.41013098
XII–1–113504
X–11135012
VIII0–1.4114502.37
VI0014508
II0014508
XI0014508
III01.41145013.64
IX1–115504
IV11155012
V1.41015918

Rietveld refinement results for 3Y-PSZ non-sintered ceramics and ceramics sintered at 1550 °C for 12 h.

AtomsWyckoffSitexyz
Zr4e10.269770.035420.21178
O14e10.072870.342620.35167
O24e10.438430.761340.48151
Zr2a–4m20.750.250.25
O14d2mm.0.250.250.46829
[Phase 1: ZrO2; P21/c (14) – Monoclinic (a = 5.18449(8), b = 5.21618(4) Å, c = 5.32812(7) Å; V = V=142.22(3) Å3; β = 99.23(8)° and Z = 4)] and [Phase 2: ZrO2; P42/nmc (137) – Tetragonal (a = b = 3.5792 Å, c = 5.1782 Å; c/a = 1, V = 66.34 Å3; Z = 2]; Rp = 6.785 %; Rwp = 11.835 %; Rexp = 6.218 %; χ2 = 3.6214 and GoF = 1.903. Weights of the phases in the ZrO2 Monoclinic = 49.17 % and ZrO2 Tetragonal = 50.83 %.
Zr2a– 4m20.750.250.25
O14d2mm.0.250.250.44896
[Monophasic for ZrO2; P42/nmc (137) – Tetragonal (a = b = 3.5578(6) Å, c = 5.1559(1) Å; V = 65.26(2) Å3; Z = 2); Rp = 5.231 %; Rwp = 10.124 %; Rexp = 8.173 %; χ2 = 1.52364 and GoF = 1.238.
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