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A method is reported for assessing the compositional fluctuations in a ceramic sample, based only on the determination of the crystalline lattice parameters. Pure tetragonal phase partially stabilized zirconia powders are synthesized through the co-precipitation method by incorporating 4% Eu3+. The powder is subjected to compression cycles to promote the tetragonal-to-monoclinic transformation. The Rietveld analysis of the X-ray powder diffraction patterns, recorded after each compression cycle, gives information about the lattice parameters and monoclinic phase content. The determination of europium content in the residual tetragonal phase is accomplished considering the unit cell volume of t-ZrO2 using Vegard's law. Using this information the compositional fluctuations over the sample were determined by considering two possible distributions of lanthanide ion content in the powders: a Gaussian and a Log-normal one. It was found that the Gaussian distribution better fits the experimental data. It was eventually demonstrated that these results are physically meaningful.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520615021083/wf5122sup1.cif
Contains datablocks global, ZE0, ZE1_tetr, ZE1_mono, ZE2_tetr, ZE2_mono, ZE3_tetr, ZE3_mono, ZE4_tetr, ZE4_mono, ZE5_tetr, ZE5_mono

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE0sup2.rtv
Contains datablock ZE0

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE1_tetrsup3.rtv
Contains datablock ZE1_tetr

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE1_monosup4.rtv
Contains datablock ZE1_mono

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE2_tetrsup5.rtv
Contains datablock ZE2_tetr

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE2_monosup6.rtv
Contains datablock ZE2_mono

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE3_tetrsup7.rtv
Contains datablock ZE3_tetr

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE3_monosup8.rtv
Contains datablock ZE3_mono

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE4_tetrsup9.rtv
Contains datablock ZE4_tetr

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE4_monosup10.rtv
Contains datablock ZE4_mono

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE5_tetrsup11.rtv
Contains datablock ZE5_tetr

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520615021083/wf5122ZE5_monosup12.rtv
Contains datablock ZE5_mono

CCDC references: 1435457; 1435458; 1435459; 1435460; 1435461; 1435462; 1435463; 1435464; 1435465; 1435466; 1435467

Experimental top

Sample prepared via alkaline coprecipitation from solution, followed by calcination at 1273 K for 6 h. The powder was subjected to cyclic compression stresses (and, at the end, ball milling) in order to promote martensitic transformation. After each compression cycle the powders were analyzed by means of X-ray diffraction.

Refinement top

The as synthesized powder was indexed as pure tetragonal zirconia, while, after the application of an external compression stress the monoclinic phase appears along with the tetragonal polymorph. With increasing cycles of stress the monoclinic content in the sample increases. The aplication of the stress along the same axes several times determines the appearance of a preferential orientation which was taken into account refining the March-Dollase parameter for the 111 direction of the tetragonal phase.

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
(ZE0) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98Z = 2
Mr = 125.33Cu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
Tetragonal, P42/nmcT = 293 K
a = 3.6047 (2) ÅParticle morphology: plate-like
c = 5.1840 (4) Åwhite
V = 67.36 (1) Å3Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Specimen mounting: adhesive tape2θmin = 15°, 2θmax = 80°, 2θstep = 0.05°
Refinement top
Rp = 0.050Profile function: pseudo-Voigt
Rwp = 0.07315 parameters
Rexp = ?Background function: square polynomial
χ2 = 1.277Preferred orientation correction: none
1301 data points
Crystal data top
Zr0.96Eu0.04O1.98V = 67.36 (1) Å3
Mr = 125.33Z = 2
Tetragonal, P42/nmcCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 3.6047 (2) ÅT = 293 K
c = 5.1840 (4) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Specimen mounting: adhesive tape2θmin = 15°, 2θmax = 80°, 2θstep = 0.05°
Data collection mode: reflection
Refinement top
Rp = 0.050χ2 = 1.277
Rwp = 0.0731301 data points
Rexp = ?15 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.750.250.25?.961
Eu0.750.250.25?.039
O0.750.250.045 (1)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE1_tetr) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98Z = 2
Mr = 125.33Cu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
Tetragonal, P42/nmcT = 293 K
a = 3.6053 (1) ÅParticle morphology: plate-like
c = 5.1843 (2) Åwhite
V = 67.39 (1) Å3Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.037Profile function: pseudo-Voigt
Rwp = 0.05224 parameters
Rexp = ?Background function: square polynomial
χ2 = 1.769Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98V = 67.39 (1) Å3
Mr = 125.33Z = 2
Tetragonal, P42/nmcCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 3.6053 (1) ÅT = 293 K
c = 5.1843 (2) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.037χ2 = 1.769
Rwp = 0.0521701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.750.250.25?.958
Eu0.750.250.25?.042
O0.750.250.0442 (7)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE1_mono) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98V = 141.54 (8) Å3
Mr = 125.33Z = 4
Monoclinic, P21/cCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 5.164 (1) ÅT = 293 K
b = 5.206 (1) ÅParticle morphology: plate-like
c = 5.325 (1) Åwhite
β = 98.70 (1)°Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.037Profile function: pseudo-Voigt
Rwp = 0.05224 parameters
Rexp = ?Background function: square polynomial
χ2 = 1.769Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98β = 98.70 (1)°
Mr = 125.33V = 141.54 (8) Å3
Monoclinic, P21/cZ = 4
a = 5.164 (1) ÅCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
b = 5.206 (1) ÅT = 293 K
c = 5.325 (1) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.037χ2 = 1.769
Rwp = 0.0521701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.2729 (5)0.0352 (5)0.2121 (5)?.960
Eu0.2729 (5)0.0352 (5)0.2121 (5)?.040
O10.094 (3)0.335 (3)0.361 (3)?
O20.448 (4)0.762 (3)0.481 (4)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE2_tetr) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98Z = 2
Mr = 125.33Cu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
Tetragonal, P42/nmcT = 293 K
a = 3.6055 (1) ÅParticle morphology: plate-like
c = 5.1841 (3) Åwhite
V = 67.39 (1) Å3Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.045Profile function: pseudo-Voigt
Rwp = 0.06024 parameters
Rexp = ?Background function: square polynomial
χ2 = 2.341Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98V = 67.39 (1) Å3
Mr = 125.33Z = 2
Tetragonal, P42/nmcCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 3.6055 (1) ÅT = 293 K
c = 5.1841 (3) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.045χ2 = 2.341
Rwp = 0.0601701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.750.250.25?.958
Eu0.750.250.25?.042
O0.750.250.042 (1)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE2_mono) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98V = 141.41 (6) Å3
Mr = 125.33Z = 4
Monoclinic, P21/cCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 5.1623 (7) ÅT = 293 K
b = 5.2052 (9) ÅParticle morphology: plate-like
c = 5.3229 (8) Åwhite
β = 98.630 (8)°Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.045Profile function: pseudo-Voigt
Rwp = 0.06024 parameters
Rexp = ?Background function: square polynomial
χ2 = 2.341Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98β = 98.630 (8)°
Mr = 125.33V = 141.41 (6) Å3
Monoclinic, P21/cZ = 4
a = 5.1623 (7) ÅCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
b = 5.2052 (9) ÅT = 293 K
c = 5.3229 (8) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.045χ2 = 2.341
Rwp = 0.0601701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.2736 (5)0.0343 (4)0.2129 (5)?.960
Eu0.2736 (5)0.0343 (4)0.2129 (5)?.040
O10.088 (3)0.332 (3)0.340 (3)?
O20.442 (3)0.771 (3)0.485 (3)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE3_tetr) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98Z = 2
Mr = 125.33Cu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
Tetragonal, P42/nmcT = 293 K
a = 3.6059 (2) ÅParticle morphology: plate-like
c = 5.1838 (4) Åwhite
V = 67.40 (1) Å3Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.048Profile function: pseudo-Voigt
Rwp = 0.06624 parameters
Rexp = ?Background function: square polynomial
χ2 = 2.856Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98V = 67.40 (1) Å3
Mr = 125.33Z = 2
Tetragonal, P42/nmcCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 3.6059 (2) ÅT = 293 K
c = 5.1838 (4) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.048χ2 = 2.856
Rwp = 0.0661701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.750.250.25?.957
Eu0.750.250.25?.043
O0.750.250.044 (4)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE3_mono) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98V = 141.31 (6) Å3
Mr = 125.33Z = 4
Monoclinic, P21/cCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 5.1595 (7) ÅT = 293 K
b = 5.2069 (8) ÅParticle morphology: plate-like
c = 5.3223 (8) Åwhite
β = 98.780 (7)°Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.048Profile function: pseudo-Voigt
Rwp = 0.06624 parameters
Rexp = ?Background function: square polynomial
χ2 = 2.856Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98β = 98.780 (7)°
Mr = 125.33V = 141.31 (6) Å3
Monoclinic, P21/cZ = 4
a = 5.1595 (7) ÅCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
b = 5.2069 (8) ÅT = 293 K
c = 5.3223 (8) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.048χ2 = 2.856
Rwp = 0.0661701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.2747 (4)0.0358 (4)0.2125 (4)?.960
Eu0.2747 (4)0.0358 (4)0.2125 (4)?.040
O10.101 (2)0.330 (3)0.351 (2)?
O20.439 (2)0.768 (2)0.479 (3)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE4_tetr) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98Z = 2
Mr = 125.33Cu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
Tetragonal, P42/nmcT = 293 K
a = 3.6062 (3) ÅParticle morphology: plate-like
c = 5.1841 (6) Åwhite
V = 67.42 (2) Å3Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.056Profile function: pseudo-Voigt
Rwp = 0.07524 parameters
Rexp = ?Background function: square polynomial
χ2 = 3.610Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98V = 67.42 (2) Å3
Mr = 125.33Z = 2
Tetragonal, P42/nmcCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 3.6062 (3) ÅT = 293 K
c = 5.1841 (6) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.056χ2 = 3.610
Rwp = 0.0751701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.750.250.25?.956
Eu0.750.250.25?.044
O0.750.250.043 (2)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE4_mono) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98V = 141.29 (6) Å3
Mr = 125.33Z = 4
Monoclinic, P21/cCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 5.1604 (7) ÅT = 293 K
b = 5.2072 (8) ÅParticle morphology: plate-like
c = 5.3208 (8) Åwhite
β = 98.822 (7)°Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.056Profile function: pseudo-Voigt
Rwp = 0.07524 parameters
Rexp = ?Background function: square polynomial
χ2 = 3.610Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98β = 98.822 (7)°
Mr = 125.33V = 141.29 (6) Å3
Monoclinic, P21/cZ = 4
a = 5.1604 (7) ÅCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
b = 5.2072 (8) ÅT = 293 K
c = 5.3208 (8) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.056χ2 = 3.610
Rwp = 0.0751701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.2748 (4)0.0371 (4)0.2120 (4)?.960
Eu0.2748 (4)0.0371 (4)0.2120 (4)?.040
O10.099 (2)0.331 (3)0.346 (2)?
O20.437 (2)0.767 (2)0.478 (3)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE5_tetr) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98Z = 2
Mr = 125.33Cu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
Tetragonal, P42/nmcT = 293 K
a = 3.612 (1) ÅParticle morphology: plate-like
c = 5.172 (3) Åwhite
V = 67.48 (8) Å3Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.049Profile function: pseudo-Voigt
Rwp = 0.06424 parameters
Rexp = ?Background function: square polynomial
χ2 = 3.062Preferred orientation correction: none
1701 data points
Crystal data top
Zr0.96Eu0.04O1.98V = 67.48 (8) Å3
Mr = 125.33Z = 2
Tetragonal, P42/nmcCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 3.612 (1) ÅT = 293 K
c = 5.172 (3) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 100°, 2θstep = 0.05°
Refinement top
Rp = 0.049χ2 = 3.062
Rwp = 0.0641701 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.750.250.25?.952
Eu0.750.250.25?.048
O0.750.250.048 (5)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(ZE5_mono) zirconium dioxide top
Crystal data top
Zr0.96Eu0.04O1.98V = 141.29 (6) Å3
Mr = 125.33Z = 4
Monoclinic, P21/cCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
a = 5.1603 (6) ÅT = 293 K
b = 5.2086 (7) ÅParticle morphology: plate-like
c = 5.3211 (7) Åwhite
β = 98.912 (6)°Specimen preparation: Prepared at 1273 K
Data collection top
Philips PW 1319
diffractometer
Data collection mode: reflection
Radiation source: sealed X-ray tubeScan method: step
Graphite monochromator2θmin = 15°, 2θmax = 80°, 2θstep = 0.05°
Refinement top
Rp = 0.049Profile function: pseudo-Voigt
Rwp = 0.06424 parameters
Rexp = ?Background function: square polynomial
χ2 = 3.062Preferred orientation correction: none
1301 data points
Crystal data top
Zr0.96Eu0.04O1.98β = 98.912 (6)°
Mr = 125.33V = 141.29 (6) Å3
Monoclinic, P21/cZ = 4
a = 5.1603 (6) ÅCu Kα1, Cu Kα2 radiation, λ = 1.540562 Å
b = 5.2086 (7) ÅT = 293 K
c = 5.3211 (7) Å
Data collection top
Philips PW 1319
diffractometer
Scan method: step
Data collection mode: reflection2θmin = 15°, 2θmax = 80°, 2θstep = 0.05°
Refinement top
Rp = 0.049χ2 = 3.062
Rwp = 0.0641301 data points
Rexp = ?24 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.2746 (3)0.0373 (3)0.2130 (3)?.960
Eu0.2746 (3)0.0373 (3)0.2130 (3)?.040
O10.071 (2)0.327 (2)0.348 (2)?
O20.450 (2)0.754 (2)0.481 (2)?
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????

Experimental details

(ZE0)(ZE1_tetr)(ZE1_mono)(ZE2_tetr)
Crystal data
Chemical formulaZr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98
Mr125.33125.33125.33125.33
Crystal system, space groupTetragonal, P42/nmcTetragonal, P42/nmcMonoclinic, P21/cTetragonal, P42/nmc
Temperature (K)293293293293
a, b, c (Å)3.6047 (2), 3.6047 (2), 5.1840 (4)3.6053 (1), 3.6053 (1), 5.1843 (2)5.164 (1), 5.206 (1), 5.325 (1)3.6055 (1), 3.6055 (1), 5.1841 (3)
α, β, γ (°)90, 90, 9090, 90, 9090, 98.70 (1), 9090, 90, 90
V3)67.36 (1)67.39 (1)141.54 (8)67.39 (1)
Z2242
Radiation typeCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 Å
Specimen shape, size (mm)Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?
Data collection
DiffractometerPhilips PW 1319Philips PW 1319Philips PW 1319Philips PW 1319
Specimen mountingAdhesive tape
Data collection modeReflectionReflectionReflectionReflection
Scan methodStepStepStepStep
2θ values (°)2θmin = 15 2θmax = 80 2θstep = 0.052θmin = 15 2θmax = 100 2θstep = 0.052θmin = 15 2θmax = 100 2θstep = 0.052θmin = 15 2θmax = 100 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.050, Rwp = 0.073, Rexp = ?, χ2 = 1.277Rp = 0.037, Rwp = 0.052, Rexp = ?, χ2 = 1.769Rp = 0.037, Rwp = 0.052, Rexp = ?, χ2 = 1.769Rp = 0.045, Rwp = 0.060, Rexp = ?, χ2 = 2.341
No. of parameters15242424
No. of restraints????


(ZE2_mono)(ZE3_tetr)(ZE3_mono)(ZE4_tetr)
Crystal data
Chemical formulaZr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98
Mr125.33125.33125.33125.33
Crystal system, space groupMonoclinic, P21/cTetragonal, P42/nmcMonoclinic, P21/cTetragonal, P42/nmc
Temperature (K)293293293293
a, b, c (Å)5.1623 (7), 5.2052 (9), 5.3229 (8)3.6059 (2), 3.6059 (2), 5.1838 (4)5.1595 (7), 5.2069 (8), 5.3223 (8)3.6062 (3), 3.6062 (3), 5.1841 (6)
α, β, γ (°)90, 98.630 (8), 9090, 90, 9090, 98.780 (7), 9090, 90, 90
V3)141.41 (6)67.40 (1)141.31 (6)67.42 (2)
Z4242
Radiation typeCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 Å
Specimen shape, size (mm)Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?
Data collection
DiffractometerPhilips PW 1319Philips PW 1319Philips PW 1319Philips PW 1319
Specimen mounting
Data collection modeReflectionReflectionReflectionReflection
Scan methodStepStepStepStep
2θ values (°)2θmin = 15 2θmax = 100 2θstep = 0.052θmin = 15 2θmax = 100 2θstep = 0.052θmin = 15 2θmax = 100 2θstep = 0.052θmin = 15 2θmax = 100 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.045, Rwp = 0.060, Rexp = ?, χ2 = 2.341Rp = 0.048, Rwp = 0.066, Rexp = ?, χ2 = 2.856Rp = 0.048, Rwp = 0.066, Rexp = ?, χ2 = 2.856Rp = 0.056, Rwp = 0.075, Rexp = ?, χ2 = 3.610
No. of parameters24242424
No. of restraints????


(ZE4_mono)(ZE5_tetr)(ZE5_mono)
Crystal data
Chemical formulaZr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98Zr0.96Eu0.04O1.98
Mr125.33125.33125.33
Crystal system, space groupMonoclinic, P21/cTetragonal, P42/nmcMonoclinic, P21/c
Temperature (K)293293293
a, b, c (Å)5.1604 (7), 5.2072 (8), 5.3208 (8)3.612 (1), 3.612 (1), 5.172 (3)5.1603 (6), 5.2086 (7), 5.3211 (7)
α, β, γ (°)90, 98.822 (7), 9090, 90, 9090, 98.912 (6), 90
V3)141.29 (6)67.48 (8)141.29 (6)
Z424
Radiation typeCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 ÅCu Kα1, Cu Kα2, λ = 1.540562 Å
Specimen shape, size (mm)Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?Flat sheet, ? × ? × ?
Data collection
DiffractometerPhilips PW 1319Philips PW 1319Philips PW 1319
Specimen mounting
Data collection modeReflectionReflectionReflection
Scan methodStepStepStep
2θ values (°)2θmin = 15 2θmax = 100 2θstep = 0.052θmin = 15 2θmax = 100 2θstep = 0.052θmin = 15 2θmax = 80 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.056, Rwp = 0.075, Rexp = ?, χ2 = 3.610Rp = 0.049, Rwp = 0.064, Rexp = ?, χ2 = 3.062Rp = 0.049, Rwp = 0.064, Rexp = ?, χ2 = 3.062
No. of parameters242424
No. of restraints???

 

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