Structural Modifications of Single-Crystal Aragonite CaCO3 Beginning at ~15 GPa: In Situ Vibrational Spectroscopy and X-Ray Diffraction Evidence
Abstract
:1. Introduction
2. Materials and Methods
2.1. Sample Description
2.2. Single-Crystal X-Ray Diffraction (XRD)
2.3. Fourier Transform Infrared Spectroscopy (FTIR)
2.4. Raman Spectroscopy
3. Results and Discussions
3.1. X-ray Diffraction of Aragonite up to 27.1 GPa
3.2. Vibrational Spectra of Aragonite at Ambient Conditions
3.3. Vibrational Spectra of Aragonite upon Pressures below 15 GPa
3.4. Vibrational Spectra of Aragonite above 15 GPa
3.5. Vibrational Spectra of Aragonite upon Decompression
3.6. Mode Grüneisen Parameters
4. Concluding Remarking
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Pressure (GPa) | a (Å) | b (Å) | c (Å) | V (Å3) |
---|---|---|---|---|
0.9 | 4.960(7) | 7.921(4) | 5.719(2) | 224.9(3) |
2.6 | 4.932(7) | 7.899(4) | 5.667(2) | 220.8(3) |
4.8 | 4.902(7) | 7.834(4) | 5.589(2) | 215.9(3) |
7.6 | 4.859(7) | 7.794(4) | 5.515(2) | 210.6(3) |
10.1 | 4.812(6) | 7.734(4) | 5.464(2) | 204.4(2) |
11.9 | 4.798(6) | 7.707(4) | 5.424(2) | 201.3(2) |
12.9 | 4.779(6) | 7.683(4) | 5.378(2) | 200.0(2) |
13.7 | 4.770(6) | 7.672(4) | 5.357(2) | 198.1(2) |
16.4 | 4.749(6) | 7.661(4) | 5.306(2) | 195.4(2) |
19.2 | 4.729(6) | 7.648(4) | 5.246(2) | 191.6(2) |
21.6 | 4.709(6) | 7.629(4) | 5.195(1) | 188.8(2) |
23.5 | 4.691(6) | 7.611(4) | 5.148(1) | 186.4(2) |
25.3 | 4.678(6) | 7.607(4) | 5.112(1) | 184.0(2) |
27.1 | 4.666(6) | 7.603(4) | 5.078(1) | 182.2(2) |
Pressure (GPa) | ν4-1 | ν4-2 | ν2 | νOH | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Wavenumber (cm−1) | FWHM (cm−1) | Intensity (Counts) | Wavenumber (cm−1) | FWHM (cm−1) | Intensity (Counts) | Wavenumber (cm−1) | Wavenumber (cm−1) | |||||
0.0001● | 700.21(2) | 3.23(5) | 53,045(625) | 712.88(5) | 7.87(2) | 118,883(928) | 842.36(2) | 856.47(3) | 868.87(2) | |||
0.0001 (P↓) | 700.54(6) | 3.62(3) | 65,135(742) | 713.11(3) | 7.97(5) | 119,105(833) | 843.61(3) | 857.26(4) | 869.28(4) | |||
1.3 | 702.23(5) | 9.05(3) | 52,855(533) | 715.81(2) | 10.80(6) | 102,445(863) | 844.25(4) | 856.30(2) | 867.39(2) | 3399.19(2) | 3541.16(6) | 3606.41(1) |
2.3 | 703.66(3) | 8.74(2) | 40,114(528) | 718.34(5) | 11.40(3) | 115,321(631) | 843.35(2) | 855.24(3) | 868.19(6) | 3394.22(1) | 3530.50(1) | 3600.23(2) |
3.5 | 705.59(5) | 9.77(6) | 46,036(631) | 720.37(6) | 11.65(6) | 95,356(742) | 842.58(5) | 853.64(3) | 867.23(2) | 3388.58(6) | 3524.58(6) | 3589.31(4) |
4.4 | 706.28(6) | 10.50(5) | 32,201(561) | 722.86(1) | 12.68(3) | 86,498(849) | 842.98(4) | 854.87(4) | 868.23(3) | 3380.79(2) | 3515.44(6) | 3587.23(6) |
5.5 | 708.33(2) | 10.59(6) | 36,262(763) | 724.29(2) | 12.67(6) | 85,205(561) | 842.27(5) | 852.27(2) | 868.06(5) | 3374.15(1) | 3508.65(1) | 3579.61(7) |
6.4 | 709.68(3) | 12.14(2) | 34,324(831) | 726.72(1) | 13.50(1) | 72,669(763) | 841.50(3) | 852.38(5) | 867.56(4) | 3368.15(5) | 3503.28(5) | 3577.74(7) |
7.5 | 711.19(1) | 12.31(5) | 29,625(731) | 728.21(1) | 14.73(2) | 64,652(628) | 841.65(3) | 851.15(6) | 868.69(6) | 3359.49(6) | 3496.99(7) | 3571.05(5) |
8.5 | 712.20(2) | 13.52(3) | 32,568(649) | 730.92(5) | 16.22(6) | 51,912(729) | 840.44(2) | 851.01(2) | 867.51(3) | 3355.12(2) | 3491.81(6) | 3565.48(1) |
9.5 | 713.53(5) | 15.47(6) | 27,842(463) | 732.31(6) | 17.43(1) | 58,946(561) | 842.62(5) | 852.52(5) | 868.59(5) | 3350.50(6) | 3490.91(2) | 3561.20(4) |
10.5 | 715.06(2) | 15.20(1) | 24,104(561) | 735.02(3) | 18.22(3) | 58,643(549) | 841.53(4) | 850.60(2) | 866.62(4) | 3344.05(1) | 3488.59(1) | 3557.30(2) |
11.5 | 717.09(3) | 16.99(6) | 22,518(442) | 736.61(3) | 19.24(2) | 47,827(633) | 842.21(4) | 851.83(4) | 867.24(6) | |||
13.4 | 719.38(6) | 19.30(2) | 24,095(633) | 739.35(5) | 22.15(5) | 62,242(525) | 840.24(2) | 851.45(4) | 868.42(2) | |||
14.5 | 721.09(5) | 20.10(3) | 24,095(725) | 741.76(3) | 23.13(3) | 53,516(631) | 841.06(3) | 851.53(3) | 867.10(4) | |||
17.5 | 722.99(2) | 21.07(6) | 47,782(731) | 745.24(6) | 24.26(6) | 70,728(528) | 839.54(4) | 850.81(2) | 867.25(4) | |||
21.5 | 725.18(6) | 19.48(5) | 46,558(763) | 748.17(5) | 25.28(1) | 56,595(649) | 840.62(2) | 851.33(5) | 866.64(3) |
Pressure (GPa) | νE2 | νE3 | ν1 | ||||||
---|---|---|---|---|---|---|---|---|---|
Wavenumber (cm−1) | FWHM (cm−1) | Intensity (Counts) | Wavenumber (cm−1) | FWHM (cm−1) | Intensity (Counts) | Wavenumber (cm−1) | FWHM (cm−1) | Intensity (Counts) | |
0.0001● | 152.8(1) | 8.0(1) | 3012(66) | 205.5(1) | 10.2(2) | 2965(68) | 1082.19(1) | 3.63(2) | 4268(48) |
0.8 | 154.2(2) | 9.2(7) | 2952(78) | 208.8(3) | 13.2(9) | 3064(131) | 1084.97(1) | 4.33(4) | 4826(52) |
2.0 | 159.6(2) | 7.0(7) | 1837(80) | 217.9(1) | 8.23(3) | 2660(93) | 1090.56(2) | 4.53(7) | 3300(38) |
5.2 | 167.2(2) | 7.4(7) | 1356(95) | 232.0(1) | 6.3(3) | 2246(93) | 1098.99(1) | 5.00(4) | 4187(40) |
7.5 | 173.4(2) | 10.0(8) | 1247(98) | 245.0(1) | 5.7(3) | 1842(81) | 1107.37(1) | 4.92(4) | 5413(59) |
10.5 | 177.8(1) | 9.6(6) | 1168(97) | 257.6(2) | 8.3(6) | 1621(97) | 1115.40(4) | 5.44(12) | 5519(138) |
12.5 | 181.5(1) | 9.0(5) | 1435(65) | 265.5(1) | 7.3(3) | 1510(56) | 1121.44(4) | 5.88(11) | 3263(73) |
14.2 | 185.7(1) | 9.1(4) | 1937(77) | 270.2(1) | 7.2(3) | 1642(66) | 1124.46(2) | 6.26(8) | 4085(62) |
16.0 | 189.3(1) | 10.1(4) | 2327(74) | 275.8(2) | 9.5(7) | 1802(70) | 1128.03(2) | 6.38(7) | 5384(64) |
17.5 | 193.6(1) | 12.6(5) | 2600(96) | 280.5(5) | 15.0(9) | 1981(97) | 1130.27(2) | 7.03(8) | 3800(40) |
19.0 | 195.9(1) | 15.2(6) | 3080(100) | 281.6(8) | 22.3(10) | 2191(122) | 1132.53(2) | 8.30(10) | 4206(34) |
20.5 | 198.6(2) | 18.8(7) | 3509(99) | 288.1(9) | 28.0(10) | 2558(143) | 1135.16(2) | 9.74(9) | 8270(86) |
23.5 | 203.2(2) | 23.6(9) | 3845(94) | 290.4(6) | 41.0(11) | 3270(108) | 1140.52(6) | 13.27(23) | 6909(149) |
20.0 | 200.7(2) | 21.6(9) | 3703(94) | 287.2(5) | 32.4(12) | 3038(160) | 1138.20(5) | 11.77(20) | 8849(159) |
17.5 | 196.8(2) | 20.7(9) | 3807(104) | 279.2(7) | 28.2(13) | 3205(163) | 1132.84(6) | 9.82(25) | 8354(301) |
4.5 | 168.9(1) | 17.8(8) | 4897(131) | 229.8(3) | 21.7(10) | 3825(125) | 1096.16(2) | 6.58(8) | 5389(84) |
0.0001 (P↓) | 153.0(2) | 17.4(9) | 6343(142) | 205.0(4) | 16.9(10) | 4068(193) | 1082.63(1) | 5.09(4) | 4722(35) |
Modes | ν0 (cm−1) | β (cm−1·GPa−1) | γi (B0 = 71 GPa) | Assignments | ||
---|---|---|---|---|---|---|
<15 GPa | >15 GPa | <15 GPa | >15 GPa | |||
ν4-1 | 700.2(1) | 1.42(1) | 0.54 | 0.14 | 0.05 | C-O in-plane bending |
ν4-2 | 712.8(1) | 1.95(4) | 0.72 | 0.19 | 0.07 | |
ν2-1 | 842.3(1) | −0.18(4) | 0.26 | 0.01 | 0.02 | C-O out-of-plane bending |
ν2-2 | 856.4(1) | −0.45(6) | 0.12 | 0.03 | 0.009 | |
ν2-3 | 868.8(1) | −0.01(3) | 0.15 | 0.0008 | 0.01 | |
ν1 | 1082.19(1) | 3.72(9) | 3.6(1) | 0.24 | 0.23 | C-O symmetrical stretching |
νE2 | 152.8(1) | 2.5(1) | 2.5(2) | 1.16 | 1.16 | External vibration |
νE3 | 205.5(1) | 5.9(1) | 5.7(2) | 2.03 | 1.96 |
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Gao, J.; Liu, Y.; Wu, X.; Yuan, X.; Liu, Y.; Su, W. Structural Modifications of Single-Crystal Aragonite CaCO3 Beginning at ~15 GPa: In Situ Vibrational Spectroscopy and X-Ray Diffraction Evidence. Minerals 2020, 10, 924. https://doi.org/10.3390/min10100924
Gao J, Liu Y, Wu X, Yuan X, Liu Y, Su W. Structural Modifications of Single-Crystal Aragonite CaCO3 Beginning at ~15 GPa: In Situ Vibrational Spectroscopy and X-Ray Diffraction Evidence. Minerals. 2020; 10(10):924. https://doi.org/10.3390/min10100924
Chicago/Turabian StyleGao, Jing, Yungui Liu, Xiang Wu, Xueyin Yuan, Yingxin Liu, and Wen Su. 2020. "Structural Modifications of Single-Crystal Aragonite CaCO3 Beginning at ~15 GPa: In Situ Vibrational Spectroscopy and X-Ray Diffraction Evidence" Minerals 10, no. 10: 924. https://doi.org/10.3390/min10100924