Journal of Inorganic Materials ›› 2019, Vol. 34 ›› Issue (7): 755-760.DOI: 10.15541/jim20180472
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CHEN Chuan-Jie1,WEI Li-Geng1,WU Yue1,HU Cheng-Pei1,HU Yuan-Cong1,JIANG Jiu-Xin1,2,3()
Received:
2018-10-10
Revised:
2018-12-03
Published:
2019-07-20
Online:
2019-06-26
Supported by:
CLC Number:
CHEN Chuan-Jie, WEI Li-Geng, WU Yue, HU Cheng-Pei, HU Yuan-Cong, JIANG Jiu-Xin. Synthesis of Metastable Vaterite Phase of CaCO3 via Ethanol-calcium Method and Ethanol-water Binary Solvent Method[J]. Journal of Inorganic Materials, 2019, 34(7): 755-760.
Fig. 1 XRD patterns of CaCO3 prepared from ethanol-calcium method (a-e) and EWBS method (f-j) after aging for different time (a, f) 0 min; (b, g) 20 min; (c, h) 90 min; (d, i) 22 h; (e, j) 42 h
Aging time/min | Temperature/℃ | *Polymorphs/% | **Polymorphs/% | ||
---|---|---|---|---|---|
Vaterite | Calcite | Vaterite | Calcite | ||
0 | 20 | 90.4 | 9.6 | 46.5 | 53.5 |
20 | 20 | 84.4 | 15.6 | 12.3 | 87.7 |
90 | 20 | 83.5 | 15.9 | 10.5 | 89.5 |
1320 | 20 | 82.5 | 17.5 | 0 | 100 |
2520 | 20 | 81.4 | 18.6 | 0 | 100 |
60/10# | 0 | 85.8 | 14.2 | 57.1 | 42.9 |
60/10# | 20 | 84.1 | 15.9 | 44.3 | 55.7 |
60/10# | 40 | 73.3 | 26.7 | 22.6 | 77.4 |
60/10# | 60 | 70.2 | 29.8 | 0 | 100 |
60/10# | 80 | 64.8 | 35.2 | 0 | 100 |
Table 1 Phase compositions of CaCO3 prepared at different conditions
Aging time/min | Temperature/℃ | *Polymorphs/% | **Polymorphs/% | ||
---|---|---|---|---|---|
Vaterite | Calcite | Vaterite | Calcite | ||
0 | 20 | 90.4 | 9.6 | 46.5 | 53.5 |
20 | 20 | 84.4 | 15.6 | 12.3 | 87.7 |
90 | 20 | 83.5 | 15.9 | 10.5 | 89.5 |
1320 | 20 | 82.5 | 17.5 | 0 | 100 |
2520 | 20 | 81.4 | 18.6 | 0 | 100 |
60/10# | 0 | 85.8 | 14.2 | 57.1 | 42.9 |
60/10# | 20 | 84.1 | 15.9 | 44.3 | 55.7 |
60/10# | 40 | 73.3 | 26.7 | 22.6 | 77.4 |
60/10# | 60 | 70.2 | 29.8 | 0 | 100 |
60/10# | 80 | 64.8 | 35.2 | 0 | 100 |
Fig. 2 SEM images of CaCO3 prepared from ethanol-calcium method (a-d) and EWBS method (e-h) after aging for different times (a, e) 0 min; (b, f) 20 min; (c, g) 90 min; (d, h) 42 h
Fig. 3 XRD patterns of CaCO3 prepared from ethanol-calcium method (a-e) and EWBS method (f-j) at different reaction temperatures (a, f) 0 min; (b, g) 20 ℃; (c, h) 40 ℃; (d, i) 60 ℃; (e, j) 80 ℃
Fig. 4 SEM images of CaCO3 prepared from ethanol-calcium method (a-e) and EWBS method (f-j) at different reaction temperatures (a, f) 0 min; (b, g) 20 ℃; (c, h) 40 ℃; (d, i) 60 ℃; (e, j) 80 ℃
Fig. 5 The reaction process of ethanol-calcium method (a) Homogeneous anhydrous ethanol; (b) Formation of CaCl2·6C2H5OH complex and complex solution; (c) Decomplexation of CaCl2·6C2H5OH complex after the addition of Na2CO3 aqueous solution; (d) Ionization of CaCl2 in ethanol-aqueous solution and combination of Ca2+ and CO32-; (e) Formation of ACC; (f) Transformation of ACC to vaterite and calcite; (g) Growth of vaterite and calcite and phase transformation of vaterite to calcite at different aging time (g1) and different temperatures (g2)
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