J. Mater. Sci. Technol. ›› 2019, Vol. 35 ›› Issue (9): 1966-1976.DOI: 10.1016/j.jmst.2019.04.013
• Orginal Article • Previous Articles Next Articles
Linggen Kong*(), Inna Karatchevtseva, Hanliang Zhu, Meng Jun Qin, Zaynab Aly
Received:
2018-10-29
Revised:
2018-12-07
Accepted:
2019-01-26
Online:
2019-09-20
Published:
2019-07-26
Contact:
Kong Linggen
About author:
1 These authors contributed equally to this work.
Linggen Kong, Inna Karatchevtseva, Hanliang Zhu, Meng Jun Qin, Zaynab Aly. Synthesis and microstructure characterization of tetragonal Zr1-xTixO2 (x = 0-1) solid solutions[J]. J. Mater. Sci. Technol., 2019, 35(9): 1966-1976.
Fig. 1. XRD patterns of (a) ZrO2, (b) Zr0.83Ti0.17O2, (c) Zr0.75Ti0.25O2, (d) Zr0.67Ti0.33O2, (e) Zr0.5Ti0.5O2, (f) Zr0.25Ti0.75O2, (g) TiO2 powders calcined for 4 h at 600 °C.
Fig. 2. XRD patterns of (a) ZrO2, (b) Zr0.83Ti0.17O2, (c) Zr0.75Ti0.25O2, (d) Zr0.67Ti0.33O2, (e) Zr0.5Ti0.5O2, (f) Zr0.25Ti0.75O2, (g) TiO2 powders calcined for 4 h at 700 °C. R and M refer to rutile and monoclinic phase, respectively.
Fig. 3. XRD patterns of (a) ZrO2, (b) Zr0.83Ti0.17O2, (c) Zr0.75Ti0.25O2, (d) Zr0.67Ti0.33O2, (e) Zr0.5Ti0.5O2, (f) Zr0.25Ti0.75O2, (g) TiO2 powders calcined for 4 h at 800 °C. R and M refer to rutile and monoclinic phase, respectively.
Materials | Experiment data | Reference data [ | ||
---|---|---|---|---|
a | c | a | c | |
ZrO2 | 3.599 | 5.159 | 3.610 | 5.168 |
Zr0.83Ti0.17O2 | 3.576 | 5.191 | ||
Zr0.75Ti0.25O2 | 3.569 | 5.197 | ||
Zr0.67Ti0.33O2 | 3.537 | 5.228 | ||
TiO2 | 3.787 | 9.547 | 3.785 | 9.514 |
Table 1 Lattice parameters (?) of tetragonal materials calcined at 600 °C for 4 h.
Materials | Experiment data | Reference data [ | ||
---|---|---|---|---|
a | c | a | c | |
ZrO2 | 3.599 | 5.159 | 3.610 | 5.168 |
Zr0.83Ti0.17O2 | 3.576 | 5.191 | ||
Zr0.75Ti0.25O2 | 3.569 | 5.197 | ||
Zr0.67Ti0.33O2 | 3.537 | 5.228 | ||
TiO2 | 3.787 | 9.547 | 3.785 | 9.514 |
Fig. 4. Raman spectra of (a) ZrO2, (b) Zr0.83Ti0.17O2, (c) Zr0.75Ti0.25O2, (d) Zr0.67Ti0.33O2, (e) Zr0.5Ti0.5O2, (f) Zr0.25Ti0.75O2, (g) TiO2 powders calcined for 4 h at 600 °C.
Fig. 5. TEM images (a, d, g), HRTEM images (b, e, h), and SAED ring patterns (c, f, i) for samples ZrO2 (a, b, c), Zr0.75Ti0.25O2 (d, e, f), TiO2 (g, h, i) calcined for 4 h at 600 °C.
Materials | Calcination (oC) | Surface area (m2/g) | Pore volume (cm3/g) | Pore size (nm) |
---|---|---|---|---|
ZrO2 | 600 | 49.6 | 0.032 | 3.2 |
800 | 11.2 | 0.041 | 14 | |
Zr0.83Ti0.17O2 | 600 | 34.8 | 0.039 | 4.9 |
700 | 18.4 | 0.035 | 7.6 | |
800 | 3.71 | 0.024 | 21 | |
Zr0.75Ti0.25O2 | 600 | 34.4 | 0.035 | 4.8 |
800 | 2.01 | 0.015 | 29 | |
Zr0.67Ti0.33O2 | 600 | 34.0 | 0.038 | 4.9 |
700 | 12.9 | 0.032 | 9.1 | |
800 | 2.81 | 0.021 | 29 | |
Zr0.5Ti0.5O2 | 600 | 11.3 | 0.022 | 6.1 |
TiO2 | 600 | 9.85 | 0.021 | 8.7 |
Table 2 N2 sorption data of powders calcined for 4 h.
Materials | Calcination (oC) | Surface area (m2/g) | Pore volume (cm3/g) | Pore size (nm) |
---|---|---|---|---|
ZrO2 | 600 | 49.6 | 0.032 | 3.2 |
800 | 11.2 | 0.041 | 14 | |
Zr0.83Ti0.17O2 | 600 | 34.8 | 0.039 | 4.9 |
700 | 18.4 | 0.035 | 7.6 | |
800 | 3.71 | 0.024 | 21 | |
Zr0.75Ti0.25O2 | 600 | 34.4 | 0.035 | 4.8 |
800 | 2.01 | 0.015 | 29 | |
Zr0.67Ti0.33O2 | 600 | 34.0 | 0.038 | 4.9 |
700 | 12.9 | 0.032 | 9.1 | |
800 | 2.81 | 0.021 | 29 | |
Zr0.5Ti0.5O2 | 600 | 11.3 | 0.022 | 6.1 |
TiO2 | 600 | 9.85 | 0.021 | 8.7 |
Eluant volume (mL) | TiO2 (1 g) | ZrO2 (1 g) | Zr0.75Ti0.25O2 (1 g) | |
---|---|---|---|---|
Ti (mg/L) | Zr (mg/L) | Ti (mg/L) | Zr (mg/L) | |
100 | 0.15 | 0.09 | 2.14 | 0.07 |
200 | 0.08 | 0.02 | 0.72 | 0.04 |
300 | 0.05 | 0.03 | 0.38 | 0.03 |
400 | 0.02 | 0.01 | 0.53 | 0.03 |
500 | 0.01 | 0.01 | 0.26 | 0.03 |
600 | 0.03 | 0.02 | 0.23 | 0.02 |
700 | <0.01 | 0.01 | 0.27 | 0.03 |
800 | <0.01 | 0.01 | 0.20 | 0.02 |
900 | 0.02 | 0.01 | 0.42 | 0.02 |
1000 | <0.01 | 0.01 | 0.24 | 0.02 |
Table 3 Chemical stability of ceramic powders eluted by 0.5 mol/L HCl (element concentration in each 100 mL eluant).
Eluant volume (mL) | TiO2 (1 g) | ZrO2 (1 g) | Zr0.75Ti0.25O2 (1 g) | |
---|---|---|---|---|
Ti (mg/L) | Zr (mg/L) | Ti (mg/L) | Zr (mg/L) | |
100 | 0.15 | 0.09 | 2.14 | 0.07 |
200 | 0.08 | 0.02 | 0.72 | 0.04 |
300 | 0.05 | 0.03 | 0.38 | 0.03 |
400 | 0.02 | 0.01 | 0.53 | 0.03 |
500 | 0.01 | 0.01 | 0.26 | 0.03 |
600 | 0.03 | 0.02 | 0.23 | 0.02 |
700 | <0.01 | 0.01 | 0.27 | 0.03 |
800 | <0.01 | 0.01 | 0.20 | 0.02 |
900 | 0.02 | 0.01 | 0.42 | 0.02 |
1000 | <0.01 | 0.01 | 0.24 | 0.02 |
Materials | Eluted | Surface area (m2/g) | Pore volume (cm3/g) | Pore size (nm) |
---|---|---|---|---|
ZrO2 | Before | 49.6 | 0.032 | 3.2 |
By 0.1 M HCl | 45.7 | 0.034 | 4.1 | |
By 0.5 M HCl | 43.7 | 0.033 | 4.1 | |
Zr0.75Ti0.25O2 | Before | 34.4 | 0.035 | 4.8 |
By 0.1 M HCl | 32.7 | 0.034 | 4.8 | |
By 0.5 M HCl | 31.0 | 0.038 | 4.8 | |
TiO2 | Before | 9.85 | 0.021 | 8.7 |
By 0.1 M HCl | 9.88 | 0.021 | 8.7 | |
By 0.5 M HCl | 9.90 | 0.021 | 9.0 |
Table 4 N2 sorption data of powders calcined for 4 h at 600 °C.
Materials | Eluted | Surface area (m2/g) | Pore volume (cm3/g) | Pore size (nm) |
---|---|---|---|---|
ZrO2 | Before | 49.6 | 0.032 | 3.2 |
By 0.1 M HCl | 45.7 | 0.034 | 4.1 | |
By 0.5 M HCl | 43.7 | 0.033 | 4.1 | |
Zr0.75Ti0.25O2 | Before | 34.4 | 0.035 | 4.8 |
By 0.1 M HCl | 32.7 | 0.034 | 4.8 | |
By 0.5 M HCl | 31.0 | 0.038 | 4.8 | |
TiO2 | Before | 9.85 | 0.021 | 8.7 |
By 0.1 M HCl | 9.88 | 0.021 | 8.7 | |
By 0.5 M HCl | 9.90 | 0.021 | 9.0 |
Fig. 9. DFT optimized the most stable (low-energy) Zr0.75Ti0.25O2 (Zr12Ti4O32): (a) monoclinic, (b) tetragonal, (c) orthorhombic, and (d) high-energy monoclinic structures. Red, green and blue spheres refer to oxygen, zirconium and titanium atoms, respectively.
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