J. Mater. Sci. Technol. ›› 2020, Vol. 36: 118-127.DOI: 10.1016/j.jmst.2019.05.067
• Research Article • Previous Articles Next Articles
Zhi Dong, Nan Liu, Weiqiang Hu, Zongqing Ma*(), Chong Li, Chenxi Liu, Qianying Guo, Yongchang Liu
Received:
2019-01-18
Revised:
2019-04-10
Accepted:
2019-05-06
Published:
2020-01-01
Online:
2020-02-11
Contact:
Ma Zongqing
Zhi Dong, Nan Liu, Weiqiang Hu, Zongqing Ma, Chong Li, Chenxi Liu, Qianying Guo, Yongchang Liu. Controlled synthesis of high-quality W-Y2O3 composite powder precursor by ascertaining the synthesis mechanism behind the wet chemical method[J]. J. Mater. Sci. Technol., 2020, 36: 118-127.
Sample ID | H2O (mL) | APT (g) | Y(NO3)3·6H2O (g) | HNO3 (mL) | ρ(H+) (mol L-1) |
---|---|---|---|---|---|
15Y | 120 | 20 | 2.57 | 15 | 1.58 |
20Y | 120 | 20 | 2.57 | 20 | 2.03 |
25Y | 120 | 20 | 2.57 | 25 | 2.45 |
30Y | 120 | 20 | 2.57 | 30 | 2.82 |
35Y | 120 | 20 | 2.57 | 35 | 3.21 |
40Y | 120 | 20 | 2.57 | 40 | 3.55 |
50Y | 120 | 20 | 2.57 | 50 | 4.18 |
60Y | 120 | 20 | 2.57 | 60 | 4.79 |
20 | 120 | 20 | - | 20 | 2.03 |
50 | 120 | 20 | - | 50 | 4.18 |
Table 1 List of co-deposited powder samples and corresponding experiment condition.
Sample ID | H2O (mL) | APT (g) | Y(NO3)3·6H2O (g) | HNO3 (mL) | ρ(H+) (mol L-1) |
---|---|---|---|---|---|
15Y | 120 | 20 | 2.57 | 15 | 1.58 |
20Y | 120 | 20 | 2.57 | 20 | 2.03 |
25Y | 120 | 20 | 2.57 | 25 | 2.45 |
30Y | 120 | 20 | 2.57 | 30 | 2.82 |
35Y | 120 | 20 | 2.57 | 35 | 3.21 |
40Y | 120 | 20 | 2.57 | 40 | 3.55 |
50Y | 120 | 20 | 2.57 | 50 | 4.18 |
60Y | 120 | 20 | 2.57 | 60 | 4.79 |
20 | 120 | 20 | - | 20 | 2.03 |
50 | 120 | 20 | - | 50 | 4.18 |
Fig. 1. XRD patterns of (a) co-deposited composite powders produced by wet chemical method in the H+ ion concentration range from 1.58 to 4.79 mol L-1. Inset, white composite powder prepared in the H+ ion concentration of 2.03 mol L-1 and yellow composite powder prepared in the H+ ion concentration of 4.18 mol L-1, (b) reduced W-Y2O3 composite powder precursors corresponding to the co-deposited composite powders in Fig. 1(a).
Fig. 2. (a) SEM image of the co-deposited composite powder 20Y, (b) TEM image of the co-deposited composite powder 20Y, (c) EDX spectrum of the agglomerates region in Fig. 2(b), (d) SEM image of the co-deposited composite powder 50Y, (e) TEM image of the co-deposited composite powder 50Y, (f) EDX spectrum of the agglomerates region in Fig. 2(e).
Fig. 3. (a) and (b) HRTEM image of sample 20Y, (c) SAED pattern recorded from sample 20Y, (d) and (e) HRTEM image of the sample 50Y and (f) SAED pattern recorded from sample 50Y.
Fig. 4. (a) Wide-scan XPS spectra of the sample 20Y and 50Y, (b) Y 3d core level spectrum of the sample 20Y and 50Y, (c) W 4f core level spectrum of the sample 20 and 50, (d) W 4f core level spectrum of the sample 20Y and 50Y, (e) O 1s core level spectrum of the sample 20 and 50 and (f) O 1s core level spectrum of the sample 20Y and 50Y.
Sample ID | W 4f (eV) | Y 3d (eV) | O 1s (eV) | ||||
---|---|---|---|---|---|---|---|
W 4f7/2 | W 4f5/2 | Y 3d5/2 | Y 3d3/2 | W—O | W—OH | W—OH2 | |
20 | 35.65 | 37.78 | - | - | 530.60 | 531.23 | 532.40 |
20Y | 35.82 | 37.96 | 158.45 | 160.49 | 530.88 | 531.68 | 532.66 |
50 | 35.88 | 38.01 | - | - | 530.61 | 531.45 | 532.40 |
50Y | 35.92 | 38.06 | - | - | 530.73 | 531.86 | 532.66 |
Y(NO3)3·6H2O | - | - | 159.24 | 161.29 | 533.56 |
Table 2 List of the binding energy values corresponding to Y 3d, W 4f and O 1s core level of sample 20, 20Y, 50, 50Y and Y(NO3)3·6H2O, respectively.
Sample ID | W 4f (eV) | Y 3d (eV) | O 1s (eV) | ||||
---|---|---|---|---|---|---|---|
W 4f7/2 | W 4f5/2 | Y 3d5/2 | Y 3d3/2 | W—O | W—OH | W—OH2 | |
20 | 35.65 | 37.78 | - | - | 530.60 | 531.23 | 532.40 |
20Y | 35.82 | 37.96 | 158.45 | 160.49 | 530.88 | 531.68 | 532.66 |
50 | 35.88 | 38.01 | - | - | 530.61 | 531.45 | 532.40 |
50Y | 35.92 | 38.06 | - | - | 530.73 | 531.86 | 532.66 |
Y(NO3)3·6H2O | - | - | 159.24 | 161.29 | 533.56 |
Fig. 7. The proposed chemical structure of the co-deposited powder of white tungstic acid particles and Y3+ ions. Color code: WO6 octahedra (yellow octahedra), W (gray ball), O (blue ball), yttrium (red ball) and YO bond (red line).
Fig. 8. Schematics showing the microstructural evolution of the co-deposited composite powder 20Y and 50Y during wet chemical reaction and subsequent thermal processing.
Fig. 9. (a) TEM image of the reduced W-Y2O3 composite powder precursor corresponding to sample 20Y, (b) EDX spectrum of the agglomerates region in Fig. 9(a), (c) HRTEM image corresponding to the agglomerates region in Fig. 9(a), (d) TEM image of the reduced W-Y2O3 composite powder precursor corresponding to sample 50Y, (e) EDX spectrum of the agglomerates region in Fig. 9(d), and (f) HRTEM image corresponding to the agglomerates region in Fig. 9(d).
Fig. 10. TEM image of reduced W-Y2O3 composite powder precursor under the H+ ion concentration of (a) 1.23 mol L-1, (b) 1.58 mol L-1 and (c) 2.45 mol L-1.
|
[1] | Weiqiang Hu, Zhi Dong, Liming Yu, Zongqing Ma, Yongchang Liu. Synthesis of W-Y2O3 alloys by freeze-drying and subsequent low temperature sintering: Microstructure refinement and second phase particles regulation [J]. J. Mater. Sci. Technol., 2020, 36(0): 84-90. |
[2] | Luo Kun,Xiang Yongdong,Wang Haiming,Xiang Li,Luo Zhihong. Multiple-Sized Amphiphilic Janus Gold Nanoparticles by Ligand Exchange at Toluene/Water Interface [J]. J. Mater. Sci. Technol., 2016, 32(8): 733-737. |
[3] | Ronghui Li, Weiyi Yang, Yu Su, Qi Li, Shian Gao, Jian Ku Shang. Ionic Potential: A General Material Criterion for the Selection of Highly Efficient Arsenic Adsorbents [J]. J. Mater. Sci. Technol., 2014, 30(10): 949-953. |
Viewed | ||||||
Full text |
|
|||||
Abstract |
|
|||||