X-ray powder diffraction structural characterization of Pb1 − xBaxZr0.65Ti0.35O3 ceramic

Mir, M.; Mastelaro, V.R.; Neves, P.P.; Doriguetto, A.C.; Garcia, D.; Lente, M.H.; Eiras, J.A.; Mascarenhas, Y.P.

doi:10.1107/S0108768107022197

X-ray powder diffraction structural characterization of Pb_1 − xBa_xZr_0.65Ti_0.35O₃ ceramic

M. Mir, V. R. Mastelaro, P. P. Neves, A. C. Doriguetto, D. Garcia, M. H. Lente, J. A. Eiras and Y. P. Mascarenhas

The structure of Pb_1 − xBa_xZr_0.65Ti_0.35O₃ (PBZT) ceramic materials with 0.00 ≤ x ≤ 0.40 was studied using synchrotron X-ray powder diffraction data. According to the Rietveld refinements, the structure of PBZT ceramics with x = 0.00, 0.10 and 0.20 at room temperature was rhombohedral R3c. A phase transition from rhombohedral to cubic was observed at 543 and 463 K for x = 0.10 and 0.20, respectively. The refinement for the compositions x = 0.30 and x = 0.40 showed a cubic structure from 10 to 450 K, in good agreement with the dielectric properties of these samples.

Keywords: X-ray powder diffraction; PBZT ceramics; phase transition.

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Supporting information

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768107022197/kd5005sup1.cif
Contains datablocks global, PBZT00_300K_R3c, PBZT00_650K_cubic, PBZT10_300K_R3c, PBZT10_750K_cubic, PBZT20_300K_R3c, PBZT20_630K_cubic, PBZT_30_300K_cubic, PBZT_40_300K_cubic

Computing details top

For all compounds, program(s) used to refine structure: FULLPROF.

(PBZT00_300K_R3c) Lead Zirconium Titanium Oxide top

Crystal data top

PbZi_0.65Ti_0.35O₃	γ = 120°
Rhombohedral, R3c	V = 412.55 (1) Å³
Hall symbol: R 3 -2"c	Z = 6
a = 5.777917 (1) Å	X-ray radiation
c = 14.269205 (1) Å	T = 300 K
α = 90°

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

46 reflections	0 restraints
13 parameters

Special details top

Refinement. Micro-structural analysis (strain):Broadening Model (Quartic form) Micro-structural analysis (size):The parameter Y was used in the Rietveld refinement. The standard deviations appearing in the global average apparent size and strain is calculated using the different reciprocal lattice directions. It is a measure of the degree of anisotropy, not of the estimated error. Average apparent size and standard deviation (anisotropy):2277.79 (1.05) Average maximum strain and standard deviation (anisotropy):7.8170 (2.1559)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.00000*
Ti1	0.00000	0.00000	−0.252 (3)	0.00000*	0.65000
Zr1	0.00000	0.00000	−0.252 (3)	0.00000*	0.35000
O1	0.16324	0.34281	−0.1990 (13)	0.00000*

(PBZT00_650K_cubic) Lead Zirconium Titanium Oxide top

Crystal data top

PbZi_0.65Ti_0.35O₃	V = 68.84 (1) Å³
Cubic, Pm3m	X-ray radiation
Hall symbol: -P 4 2 3	T = 650 K
a = 4.09836 (3) Å

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

23 reflections	0 restraints
11 parameters

Special details top

Refinement. Micro-structural analysis (strain):Broadening Model (Quartic form) Micro-structural analysis (size): The parameter Y was used in the Rietveld refinement. The standard deviations appearing in the global average apparent size and strain is calculated using the different reciprocal lattice directions. It is a measure of the degree of anisotropy, not of the estimated error. Average apparent size and standard deviation (anisotropy):2408.04 (0.82) Average maximum strain and standard deviation (anisotropy):4.0543 (1.5160)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.0217 (5)*
Zr1	0.50000	0.50000	0.50000	0.00000*	0.65000
Ti1	0.50000	0.50000	0.50000	0.00000*	0.35000
O1	0.50000	0.50000	0.00000	0.026 (3)*

(PBZT10_300K_R3c) Lead Barium Zirconium Titanium Oxide top

Crystal data top

Pb_0.9Ba_0.1Zi_0.65Ti_0.35O₃	α = 90°
Rhombohedral, R3c	γ = 120°
Hall symbol: R 3 -2"c	V = 414.11 (1) Å³
a = 5.78826 (5) Å	X-ray radiation
c = 14.27227 (16) Å	T = 300 K

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

76 reflections	0 restraints
16 parameters

Special details top

Refinement. Micro-structural analysis (strain):Broadening Model (Quartic form) Micro-structural analysis (size):The parameter Y was used in the Rietveld refinement. The standard deviations appearing in the global average apparent size and strain is calculated using the different reciprocal lattice directions. It is a measure of the degree of anisotropy, not of the estimated error. Average apparent size and standard deviation (anisotropy):1798.09 (1.46) Average maximum strain and standard deviation (anisotropy):8.3534 (2.0029)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.0121 (4)*	0.90000
Ba1	0.00000	0.00000	0.00000	0.0121 (4)*	0.10000
Ti1	0.00000	0.00000	−0.2640 (3)	0.00000*	0.35000
Zr1	0.00000	0.00000	−0.2640 (3)	0.00000*	0.65000
O1	0.152 (4)	0.346 (3)	−0.1990 (8)	0.00000*

(PBZT10_750K_cubic) Lead Barium Zirconium Titanium Oxide top

Crystal data top

Pb_0.9Ba_0.1Zi_0.65Ti_0.35O₃	V = 69.30 (1) Å³
Cubic, Pm3m	X-ray radiation
Hall symbol: -P 4 2 3	T = 750 K
a = 4.10755 (3) Å

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

23 reflections	0 restraints
11 parameters

Special details top

Refinement. Micro-structural analysis:The parameters X and Y were used in the Rietveld refinement. The standard deviations appearing in the global average apparent size and strain is calculated using the different reciprocal lattice directions. It is a measure of the degree of anisotropy, not of the estimated error. Average apparent size and standard deviation (anisotropy):9953.78 (8.82) Average maximum strain and standard deviation (anisotropy):5.6763 (0.0040)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.0242 (5)*	0.90000
Ba1	0.00000	0.00000	0.00000	0.0242 (5)*	0.10000
Zr1	0.50000	0.50000	0.50000	0.00000*	0.65000
Ti1	0.50000	0.50000	0.50000	0.00000*	0.35000
O1	0.50000	0.50000	0.00000	0.030 (3)*

(PBZT20_300K_R3c) Lead Barium Zirconium Titanium Oxide top

Crystal data top

Pb_0.8Ba_0.2Zi_0.65Ti_0.35O₃	α = 90°
Rhombohedral, R3c	γ = 120°
Hall symbol: R 3 -2"c	V = 415.34 (1) Å³
a = 5.79776 (5) Å	X-ray radiation
c = 14.26758 (15) Å	T = 300 K

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

75 reflections	0 restraints
16 parameters

Special details top

Refinement. Micro-structural analysis (strain): Broadening Model (Quartic form) Micro-structural analysis (size): The parameter Y was used in the Rietveld refinement. The standard deviations appearing in the global average apparent size and strain is calculated using the different reciprocal lattice directions. It is a measure of the degree of anisotropy, not of the estimated error. Average apparent size and standard deviation (anisotropy):2277.79 (1.05) Average maximum strain and standard deviation (anisotropy):7.8170 (2.1559)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.0106 (4)*	0.80000
Ba1	0.00000	0.00000	0.00000	0.0106 (4)*	0.20000
Ti1	0.00000	0.00000	−0.2613 (3)	0.00000*	0.35000
Zr1	0.00000	0.00000	−0.2613 (3)	0.00000*	0.65000
O1	0.158 (5)	0.359 (4)	−0.1941 (10)	0.00000*

(PBZT20_630K_cubic) Lead Barium Zirconium Titanium Oxide top

Crystal data top

Pb_0.8Ba_0.2Zi_0.65Ti_0.35O₃	V = 69.51 (1) Å³
Cubic, Pm3m	X-ray radiation
Hall symbol: -P 4 2 3	T = 630 K
a = 4.111610 (17) Å

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

23 reflections	0 restraints
10 parameters

Special details top

Refinement. Micro-structural analysis (strain): The parameter X was used in the Rietveld refinement. The standard deviations appearing in the global average apparent size and strain is calculated using the different reciprocal lattice directions. It is a measure of the degree of anisotropy, not of the estimated error. Average maximum strain and standard deviation (anisotropy):2.4176(0.0005)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.02193 (4)*	0.80000
Ba1	0.00000	0.00000	0.00000	0.02193 (4)*	0.20000
Zr1	0.50000	0.50000	0.50000	0.00000*	0.65000
Ti1	0.50000	0.50000	0.50000	0.00000*	0.35000
O1	0.50000	0.50000	0.00000	0.0196 (2)*

(PBZT_30_300K_cubic) Lead Barium Zirconium Titanium Oxide top

Crystal data top

Pb_0.7Ba_0.3Zi_0.65Ti_0.35O₃	V = 69.55 (1) Å³
Cubic, Pm3m	X-ray radiation
Hall symbol: -P 4 2 3	T = 300 K
a = 4.11241 (6) Å

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

28 reflections	0 restraints
13 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.0239 (4)*	0.70000
Ba1	0.00000	0.00000	0.00000	0.0239 (4)*	0.30000
Zr1	0.50000	0.50000	0.50000	0.0002 (5)*	0.65000
Ti1	0.50000	0.50000	0.50000	0.0002 (5)*	0.35000
O1	0.50000	0.50000	0.00000	0.0206 (19)*

(PBZT_40_300K_cubic) Lead Barium Zirconium Titanium Oxide top

Crystal data top

Pb_0.6Ba_0.4Zi_0.65Ti_0.35O₃	V = 69.73 (1) Å³
Cubic, Pm3m	X-ray radiation
Hall symbol: -P 4 2 3	T = 300 K
a = 4.11604 (2) Å

Data collection top

Si monochromator	k = →
θ/2θ step scans	l = →
h = →

Refinement top

30 reflections	0 restraints
8 parameters

Special details top

Refinement. Micro-structural analysis (strain): Broadening Model (Quartic form) Micro-structural analysis (size): The parameter Y was used in the Rietveld refinement. The standard deviations appearing in the global average apparent size and strain is calculated using the different reciprocal lattice directions. It is a measure of the degree of anisotropy, not of the estimated error. Average apparent size and standard deviation (anisotropy):1180.46 (0.89) Average maximum strain and standard deviation (anisotropy):6.9758 (0.2622)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pb1	0.00000	0.00000	0.00000	0.0217 (3)*	0.60000
Ba1	0.00000	0.00000	0.00000	0.0217 (3)*	0.40000
Zr1	0.50000	0.50000	0.50000	0.00000*	0.65000
Ti1	0.50000	0.50000	0.50000	0.00000*	0.35000
O1	0.50000	0.50000	0.00000	0.0035 (10)*

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X-ray powder diffraction structural characterization of Pb_1 − xBa_xZr_0.65Ti_0.35O₃ ceramic

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