In Situ X-ray Diffraction at High Temperatures: Formation of Ca2SiO4 and Ternesite in Recycled Autoclaved Aerated Concrete
Abstract
:1. Introduction
2. Materials and Methods
2.1. Raw Material Analysis
2.2. High-Temperature XRD
3. Results
3.1. Raw Material Composition
3.2. Qualitative Phase Contents In Situ at 1000 °C and 25 °C after Heating Experiments
3.3. In Situ Measurements during Heating
3.4. In Situ Measurements during Cooling
3.5. Influence of Heating Rate/Residence Time
3.6. Increase in C/S-Ratio
3.7. Lattice Parameters
4. Discussion
4.1. Formation Mechanisms of C2S and Ternesite
4.2. Quantitative Results: Influence of Heating Rate, C/S-Ratio, and Sulfate Content
4.3. Foreign Ion Incorporation in C2S
4.4. Influence of Cooling Rate and Reaction Progress on Quench Product
4.5. Thermal Expansion of Ternesite
5. Conclusions
- Increased residence time during heating increases the ternesite content but promotes also the formation of high crystalline α’H-C2S;
- The sulfate content has a positive effect on the formation of α’H-C2S (phase content and crystallinity);
- The C/S-ratio has to be adapted carefully to the sulfate content, otherwise the formation of ternesite takes place at the expense of C2S;
- The ternesite stability during quench depends on the C/S-ratio and cooling rate: Ternesite stays stable or even increases in amount in experiments with residual quartz and lime. In the case of a low C/S-ratio where only residual quartz is present, a decrease in ternesite amount during very slow cooling was observed;
- The temperature and range of the α’H-C2S→β-C2S transformation depend strongly on the cooling rate. The first formation of β-C2S was observed at 540 °C (slow quench) and 450 °C (fast quench);
- Thermal expansion coefficients of ternesite are similar to literature data of larnite. However, the incorporation of CaSO4 modules in the structure switches the direction of maximum compression.
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Sample | LoI (wt.%) | SiO2 (wt.%) | CaO (wt.%) | SO3 (wt.%) | Al2O3 (wt.%) | Fe2O3 (wt.%) | MgO (wt.%) | K2O (wt.%) | Na2O (wt.%) |
---|---|---|---|---|---|---|---|---|---|
SM(P) | 6.68 | 49.2 | 31.4 | 4.20 | 3.14 | 1.29 | 0.96 | 0.75 | 0.75 |
SM(D1) | 11.6 | 56.1 | 24.7 | 1.44 | 2.00 | 0.63 | 0.40 | 0.60 | 0.60 |
SM(D2) | 9.90 | 47.0 | 26.3 | 10.7 | 2.28 | 0.84 | 0.48 | 0.58 | 0.58 |
SM(D3) | 14.3 | 43.3 | 25.7 | 9.42 | 2.84 | 1.12 | 0.57 | 0.60 | 0.60 |
Sample | Amorphous (wt.%) | Quartz (wt.%) | Calcite (wt.%) | Vaterite (wt.%) | Aragonite (wt.%) | Toberm. (wt.%) | Feldspars (wt.%) | Anhydrite (wt.%) | Bassanite (wt.%) |
---|---|---|---|---|---|---|---|---|---|
SM(P) | 64.7(1.0) | 13.2(2) | 3.20(16) | 1.16(11) | 0.21(6) | 13.3(3) | 0.5(3) | 2.38(14) | 1.36(13) |
SM(D1) | 52.0(6) | 25.9(2) | 3.95(11) | 2.82(11) | 4.97(17) | 5.33(17) | 2.7(4) | 0.48(10) | 1.87(12) |
SM(D2) | 60.5(6) | 22.2(2) | 4.25(13) | 2.30(13) | 1.80(14) | 2.4(2) | 5.00(13) | 1.59(16) | |
SM(D3) | 60.4(6) | 19.64(2) | 4.01(12) | 2.64(12) | 2.69(14) | 3.5(2) | 3.37(12) | 3.75(15) |
Sample | Weight Loss 30–950 °C (wt.%) | H2O 30–450 °C (wt.%) | CO2 450–830 °C (wt.%) | SO3 830–1400 °C (wt.%) | Amorphous CaCO3 (wt.%) | Amorphous CaSO4 (wt.%) | Amorphous C-S-H (wt.%) |
---|---|---|---|---|---|---|---|
SM(P) | 6.3 | 2.9 | 2.4 | 4.9 | 1.4 | 5.6 | 59.1 |
SM(D1) | 13.9 | 3.7 | 9.7 | 1.6 | 9.0 | 1.4 | 41.2 |
SM(D2) | 10.2 | 2.0 | 7.6 | 10.9 | 8.6 | 12.5 | 39.6 |
SM(D3) | 15.9 | 2.5 | 9.9 | 11.3 | 11.8 | 13.3 | 34.9 |
Sample and Temperature (°C) | Amorph | α’H-C2S | β-C2S | Ternesite | Quartz | Calcite | Lime | Anh. | Wollast. |
---|---|---|---|---|---|---|---|---|---|
P 600 | 18.0(8) | 75.7(1.2) | 2.7(4) | ||||||
P 700 | 37.0(1.0) | 13.4(6) | 44.4(1.1) | 2.8(3) | |||||
P 800 | 55.2(1.0) | 7.1(4) | 0.6(2) | 24.4(5) | 1.84(15) | 9.2(4) | |||
P 1000 | 89.9(8) | 2.2(4) | 1.6(2) | 0.03(2) | 1.5(3) | ||||
P 600 | 95.6(7) | 1.5(3) | 0.25(9) | ||||||
P 500 | 93.6(1.0) | 2.3(8) | 1.4(3) | 0.26(10) | |||||
P 400 | 75.2(1.0) | 21.6(8) | 0.8(2) | 0.32(15) | 0.5(3) | ||||
P 25 | 1.7(9) | 87.4(1.3) | 0.5(3) | 1.3(2) | 1.1(3) | 1.0(3) | |||
(P)Std | - | 90.0(6) | 0.44(13) | 2.52(7) | 0.63(11) | 0.14(5) | |||
D1 600 | 18.8(6) | 79.1(7) | 0.52(16) | ||||||
D1 700 | 16.1(7) | 17.5(2) | 63.4(9) | 0.9(2) | 0.42(14) | ||||
D1 800 | 38.2(6) | 14.6(4) | 1.0(2) | 38.0(5) | 0.25(8) | 4.6(4) | |||
D1 1000 | 64.4(5) | 1.9(2) | 7.9(2) | 16.26(17) | 0.21(6) | 4.6(2) | |||
D1 600 | 67.6(7) | 2.7(2) | 8.3(3) | 4.02(13) | 11.44(17) | 2.09(19) | |||
D1 500 | 63.6(7) | 3.1(4) | 1.9(2) | 9.8(5) | 3.9(2) | 10.28(17) | 2.3(3) | ||
D1 400 | 58.4(7) | 7.4(6) | 1.40(17) | 10.0(4) | 4.3(2) | 10.59(18) | 2.5(2) | ||
D1 25 | 14.6(8) | 46.7(1.6) | 1.95(18) | 9.4(4) | 6.7(3) | 12.0(4) | 0.52(14) | 2.46(19) | |
(D1)Std | 10.2(1.7) | 4.2(3) | 47.2(9) | 1.17(11) | 8.76(16) | 7.02(15) | 12.07(17) | 4.32(12) | |
D2 600 | 20.3(6) | 65.9(1.0) | 10.6(9) | ||||||
D2 700 | 20.0(1.0) | 18.2(6) | 47.0(1.1) | 0.6(2) | 11.6(9) | ||||
D2 800 | 51.8(1.0) | 11.7(4) | 26.7(6) | 5.9(4) | 2.9(4) | ||||
D2 1000 | 72.5(7) | 8.1(2) | 5.1(3) | 1.93(6) | 6.90(17) | 1.13(14) | |||
D2 600 | 72.5(6) | 9.8(3) | 4.87(18) | 0.37(10) | 5.1(2) | 0.44(17) | |||
D2 500 | 73.0(7) | 0.8(3) | 9.9(2) | 4.4(4) | 0.65(6) | 4.7(2) | 0.57(17) | ||
D2 400 | 50.3(6) | 22.8(5) | 10.4(3) | 4.9(4) | 0.3(2) | 0.66(6) | 5.0(2) | 0.6(2) | |
D2 25 | 5.9(5) | 65.2(9) | 11.0(3) | 3.7(2) | 0.84(16) | 1.10(7) | 4.47(17) | 0.86(18) | |
(D2)Std | 4.8(1.3) | 1.08(1.7) | 62.6(6) | 11.36(17) | 5.62(12) | 1.49(11) | 2.52(5) | 4.50(9) | 0.64(10) |
D3 600 | 20.2(6) | 65.0(1.0) | 11.2(9) | ||||||
D3 700 | 30.8(9) | 15.3(5) | 37.4(1.0) | 0.7(2) | 13.3(8) | ||||
D3 800 | 55(2) | 11.8(6) | 22.3(9) | 7.3(5) | 1.9(5) | ||||
D3 1000 | 74.2(6) | 9.2(3) | 4.9(2) | 0.90(10) | 5.1(2) | 1.2(2) | |||
D3 600 | 73.2(7) | 10.6(3) | 4.7(3) | 0.25(5) | 3.8(2) | 0.7(3) | |||
D3 500 | 74.8(8) | 0.9(3) | 10.2(3) | 3.0(4) | 0.25(6) | 3.6(29 | 0.74(19) | ||
D3 400 | 53.9(7) | 20.3(5) | 10.6(3) | 3.2(4) | 1.0(3) | 0.23(6) | 3.6(2) | 0.9(3) | |
D3 25 | 5.6(5) | 64.7(1.0) | 11.1(3) | 4.1(2) | 0.77(16) | 0.50(7) | 4.00(17) | 1.06(18) | |
(D3)Std | - | 1.35(18) | 65.4(6) | 8.31(16) | 5.57(13) | 1.23(12) | 1.84(5) | 7.46(11) | 0.99(11) |
D3_step10 950 | 65.9(5) | 19.0(2) | 1.71(9) | 0.04(2) | 0.18(7) | 4.7(3) | |||
D3_step10 25 | 1.1(2) | 67.3(5) | 14.10(15) | 0.45(10) | 0.41(9) | 0.16(7) | 4.43(10) | ||
D3_2.5 950 | 62.9(5) | 4.5(3) | 6.0(2) | 15.6(2) | 6.2(2) | 0.9(2) | |||
D3_2.5 1000 | 66.7(5) | 11.8(2) | 3.14(18) | 6.77(9) | 5.61(15) | 1.17(18) | |||
D3_2.5 25 | 10.2(5) | 49.9(1.1) | 18.6(5) | 1.6(29 | 1.83(15) | 4.68(12) | 4.23(15) | 0.90(17) |
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Ullrich, A.; Garbev, K.; Bergfeldt, B. In Situ X-ray Diffraction at High Temperatures: Formation of Ca2SiO4 and Ternesite in Recycled Autoclaved Aerated Concrete. Minerals 2021, 11, 789. https://doi.org/10.3390/min11080789
Ullrich A, Garbev K, Bergfeldt B. In Situ X-ray Diffraction at High Temperatures: Formation of Ca2SiO4 and Ternesite in Recycled Autoclaved Aerated Concrete. Minerals. 2021; 11(8):789. https://doi.org/10.3390/min11080789
Chicago/Turabian StyleUllrich, Angela, Krassimir Garbev, and Britta Bergfeldt. 2021. "In Situ X-ray Diffraction at High Temperatures: Formation of Ca2SiO4 and Ternesite in Recycled Autoclaved Aerated Concrete" Minerals 11, no. 8: 789. https://doi.org/10.3390/min11080789