The classical external-standard method derived from the work of O'Connor & Raven [Powder Diffr. (1988), 3, 2-6] was used to examine the hydration of the major phase, alite, of ordinary Portland cements at different temperatures and different water/alite ratios. In order to estimate the accuracy of the method, heat-flow curves were calculated from the alite dissolution curves obtained from X-ray diffraction in situ experiments. The heat-flow curves calculated in this way were compared with heat-flow curves recorded using a calorimeter. It is shown that the calculated curves agree well with the curves obtained from heat-flow experiments.
Supporting information
For both compounds, data collection: XRD Commander ((Bruker); cell refinement: TOPAS V.4.2 (Bruker); data reduction: -; program(s) used to solve structure: -; program(s) used to refine structure: -; molecular graphics: -; software used to prepare material for publication: -.
'Tricalcium Silicate Oxide'
top
Crystal data top
Ca3O5Si | Z = 36 |
Monoclinic, Cm | Cu Kα1 radiation, λ = 1.5406 Å |
a = 33.085 Å | T = 298 K |
b = 7.037 Å | white |
c = 18.521 Å | flat_sheet, 22 × 22 mm |
β = 94.159° | Specimen preparation: Prepared at 298 K and 101.325 kPa |
V = 4300.7 Å3 | |
Data collection top
D8 Bruker diffractometer | Data collection mode: reflection |
Radiation source: sealed X-ray tube, KFL CU 2K Siemens | Scan method: step |
None monochromator | 2θmin = 7.0°, 2θmax = 70.018°, 2θstep = 0.022° |
Specimen mounting: sample holder (PMMA) | |
Refinement top
Least-squares matrix: full | Excluded region(s): none |
Rp = 0.043 | Profile function: fundamental parameter type peaks in a non linear least-squares refinement |
Rwp = 0.083 | |
Rexp = 0.037 | Background function: Chebychev polynomial 6th order |
2822 data points | Preferred orientation correction: none |
Special details top
Experimental. powder sample |
Refinement. Hatrurite structure from "De La Torre, A. G., Bruque, S., Campo, S.
& Aranda, M. (2002). The superstructure of C3S from synchroton and
neutron powder diffraction and its role in quantitative phase analysis.
Cement and Concrete Research, 32, 1347-1356." was used for refinement. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ca1 | −0.0024 (1) | 0 | 0.0104 (19) | 0.012 (1) | |
Ca2 | 0.6595 (10) | 0 | 0.1605 (19) | 0.012 (1) | |
Ca3 | 0.3113 (9) | 0 | 0.3342 (19) | 0.012 (1) | |
Ca4 | −0.0119 (12) | 0 | 0.4939 (19) | 0.012 (1) | |
Ca5 | 0.6531 (11) | 0 | 0.6651 (18) | 0.012 (1) | |
Ca6 | 0.3188 (11) | 0 | 0.8407 (19) | 0.012 (1) | |
Ca7 | 0.5881 (11) | 0 | −0.075 (2) | 0.012 (1) | |
Ca8 | 0.2592 (11) | 0 | 0.1012 (19) | 0.012 (1) | |
Ca9 | −0.0815 (11) | 0 | 0.2619 (19) | 0.012 (1) | |
Ca10 | 0.5848 (9) | 0 | 0.4262 (18) | 0.012 (1) | |
Ca11 | 0.2494 (11) | 0 | 0.6061 (19) | 0.012 (1) | |
Ca12 | −0.0817 (11) | 0 | 0.765 (2) | 0.012 (1) | |
Ca13 | 0.7322 (11) | 0 | −0.0925 (19) | 0.012 (1) | |
Ca14 | 0.4019 (11) | 0 | 0.078 (2) | 0.012 (1) | |
Ca15 | 0.0646 (10) | 0 | 0.2418 (19) | 0.012 (1) | |
Ca16 | 0.7236 (10) | 0 | 0.402 (2) | 0.012 (1) | |
Ca17 | 0.3895 (11) | 0 | 0.573 (2) | 0.012 (1) | |
Ca18 | 0.0617 (11) | 0 | 0.7363 (19) | 0.012 (1) | |
Ca19 | −0.0835 (10) | 0.275 (3) | −0.085 (2) | 0.0104 (8) | 0.5 |
Ca20 | −0.0833 (10) | 0.275 (3) | −0.085 (2) | 0.0104 (8) | 0.5 |
Ca21 | 0.5804 (12) | 0.277 (3) | 0.084 (2) | 0.0104 (8) | 0.5 |
Ca22 | 0.5849 (11) | 0.281 (2) | 0.0917 (18) | 0.0104 (8) | 0.5 |
Ca23 | 0.2398 (11) | 0.250 (3) | 0.2580 (18) | 0.0104 (8) | 0.5 |
Ca24 | 0.2413 (11) | 0.257 (3) | 0.2577 (18) | 0.0104 (8) | 0.5 |
Ca25 | −0.0969 (11) | 0.265 (4) | 0.4132 (18) | 0.0104 (8) | 0.5 |
Ca26 | −0.0938 (11) | 0.293 (3) | 0.4099 (18) | 0.0104 (8) | 0.5 |
Ca27 | 0.5759 (13) | 0.250 (4) | 0.597 (2) | 0.0104 (8) | 0.5 |
Ca28 | 0.5651 (11) | 0.223 (4) | 0.572 (2) | 0.0104 (8) | 0.5 |
Ca29 | 0.2436 (11) | 0.250 (4) | 0.752 (3) | 0.0104 (8) | 0.5 |
Ca30 | 0.2444 (10) | 0.241 (3) | 0.762 (2) | 0.0104 (8) | 0.5 |
Ca31 | −0.0023 (14) | 0.218 (5) | 0.847 (3) | 0.0104 (8) | 0.5 |
Ca32 | −0.0004 (14) | 0.232 (5) | 0.842 (3) | 0.0104 (8) | 0.5 |
Ca33 | 0.6675 (10) | 0.232 (3) | 0.015 (3) | 0.0104 (8) | 0.5 |
Ca34 | 0.6662 (10) | 0.241 (3) | 0.020 (3) | 0.0104 (8) | 0.5 |
Ca35 | 0.3345 (12) | 0.235 (4) | 0.172 (2) | 0.0104 (8) | 0.5 |
Ca36 | 0.3388 (10) | 0.222 (3) | 0.1825 (18) | 0.0104 (8) | 0.5 |
Ca37 | −0.0049 (10) | 0.235 (3) | 0.346 (2) | 0.0104 (8) | 0.5 |
Ca38 | −0.0051 (11) | 0.238 (3) | 0.3444 (19) | 0.0104 (8) | 0.5 |
Ca39 | 0.6608 (10) | 0.229 (3) | 0.5199 (18) | 0.0104 (8) | 0.5 |
Ca40 | 0.6570 (10) | 0.218 (2) | 0.5225 (17) | 0.0104 (8) | 0.5 |
Ca41 | 0.3312 (10) | 0.240 (4) | 0.681 (2) | 0.0104 (8) | 0.5 |
Ca42 | 0.3310 (10) | 0.236 (4) | 0.677 (3) | 0.0104 (8) | 0.5 |
Ca43 | 0.8260 (13) | 0.270 (4) | −0.012 (2) | 0.0104 (8) | 0.5 |
Ca44 | 0.8268 (10) | 0.264 (3) | −0.0093 (19) | 0.0104 (8) | 0.5 |
Ca45 | 0.4904 (10) | 0.260 (4) | 0.1593 (19) | 0.0104 (8) | 0.5 |
Ca46 | 0.4906 (10) | 0.257 (4) | 0.160 (2) | 0.0104 (8) | 0.5 |
Ca47 | 0.1502 (10) | 0.254 (4) | 0.3293 (19) | 0.0104 (8) | 0.5 |
Ca48 | 0.1509 (9) | 0.254 (3) | 0.3288 (19) | 0.0104 (8) | 0.5 |
Ca49 | 0.8127 (11) | 0.260 (3) | 0.493 (2) | 0.0104 (8) | 0.5 |
Ca50 | 0.8139 (10) | 0.261 (3) | 0.500 (2) | 0.0104 (8) | 0.5 |
Ca51 | 0.4826 (13) | 0.277 (5) | 0.6571 (19) | 0.0104 (8) | 0.5 |
Ca52 | 0.4821 (12) | 0.266 (4) | 0.6563 (19) | 0.0104 (8) | 0.5 |
Ca53 | 0.1558 (11) | 0.272 (3) | 0.8212 (19) | 0.0104 (8) | 0.5 |
Ca54 | 0.1554 (10) | 0.271 (3) | 0.8206 (18) | 0.0104 (8) | 0.5 |
Si1 | 0.0816 (11) | 0 | 0.4254 (19) | 0.004 (1) | |
Si2 | 0.2329 (11) | 0 | −0.0728 (19) | 0.004 (1) | |
Si3 | 0.4211 (11) | 0 | 0.747 (2) | 0.004 (1) | |
Si4 | 0.5603 (11) | 0 | 0.758 (2) | 0.004 (1) | |
Si5 | −0.0976 (10) | 0 | 0.0775 (17) | 0.004 (1) | |
Si6 | 0.8946 (10) | 0 | 0.5743 (18) | 0.004 (1) | |
Si7 | 0.0917 (10) | 0 | −0.0895 (19) | 0.004 (1) | |
Si8 | 0.1615 (10) | 0 | 0.1677 (18) | 0.004 (1) | |
Si9 | 0.1588 (11) | 0 | 0.6621 (18) | 0.004 (1) | |
Si10 | 0.2243 (9) | 0 | 0.4237 (17) | 0.004 (1) | |
Si11 | 0.4176 (4) | 0 | 0.2554 (8) | 0.004 (1) | |
Si12 | 0.5020 (10) | 0 | 0.0003 (19) | 0.004 (1) | |
Si13 | 0.4845 (10) | 0 | 0.4913 (18) | 0.004 (1) | |
Si14 | 0.5669 (9) | 0 | 0.2431 (17) | 0.004 (1) | |
Si15 | 0.7532 (10) | 0 | 0.0911 (19) | 0.004 (1) | |
Si16 | 0.7506 (10) | 0 | 0.5842 (19) | 0.004 (1) | |
Si17 | 0.8250 (11) | 0 | 0.3337 (19) | 0.004 (1) | |
Si18 | 0.8243 (11) | 0 | 0.8424 (19) | 0.004 (1) | |
O1 | 0.9921 (13) | 0 | 0.252 (2) | 0.031 (2) | |
O2 | 0.0342 (11) | 0 | 0.122 (2) | 0.031 (2) | |
O3 | 0.0309 (15) | 0 | 0.602 (4) | 0.031 (2) | |
O4 | −0.0101 (14) | 0 | 0.749 (2) | 0.031 (2) | |
O5 | 0.3664 (11) | 0 | −0.067 (3) | 0.031 (2) | |
O6 | 0.3313 (13) | 0 | 0.0836 (19) | 0.031 (2) | |
O7 | 0.2830 (12) | 0 | 0.2215 (19) | 0.031 (2) | |
O8 | 0.3525 (13) | 0 | 0.444 (2) | 0.031 (2) | |
O9 | 0.325 (2) | 0 | 0.593 (3) | 0.031 (2) | |
O10 | 0.2857 (13) | 0 | 0.723 (2) | 0.031 (2) | |
O11 | 0.6617 (13) | 0 | −0.084 (2) | 0.031 (2) | |
O12 | 0.6170 (9) | 0 | 0.0406 (19) | 0.031 (2) | |
O13 | 0.6976 (10) | 0 | 0.298 (2) | 0.031 (2) | |
O14 | 0.6537 (10) | 0 | 0.4255 (19) | 0.031 (2) | |
O15 | 0.6147 (11) | 0 | 0.550 (2) | 0.031 (2) | |
O16 | 0.7014 (13) | 0 | 0.770 (2) | 0.031 (2) | |
O17 | 0.9399 (13) | 0 | 0.387 (2) | 0.031 (2) | |
O18 | 0.9564 (13) | 0 | 0.903 (3) | 0.031 (2) | |
O19 | 0.1052 (13) | 0 | 0.3522 (19) | 0.016 (1) | |
O20 | 0.0327 (11) | 0 | 0.410 (2) | 0.016 (1) | |
O21 | 0.0937 (11) | 0.187 (2) | 0.4744 (19) | 0.016 (1) | |
O22 | 0.2096 (12) | 0 | 0.001 (2) | 0.016 (1) | |
O23 | 0.2806 (11) | 0 | −0.053 (2) | 0.016 (1) | |
O24 | 0.2187 (11) | 0.1794 (17) | 0.8763 (19) | 0.016 (1) | |
O25 | 0.4415 (13) | 0 | 0.671 (2) | 0.016 (1) | |
O26 | 0.3718 (10) | 0 | 0.7387 (15) | 0.016 (1) | |
O27 | 0.4338 (10) | 0.190 (2) | 0.793 (2) | 0.016 (1) | |
O28 | 0.5376 (13) | 0 | 0.832 (2) | 0.016 (1) | |
O29 | 0.6091 (11) | 0 | 0.770 (3) | 0.016 (1) | |
O30 | 0.5460 (10) | 0.1822 (17) | 0.709 (2) | 0.016 (1) | |
O31 | 0.8757 (12) | 0 | 0.1492 (19) | 0.016 (1) | |
O32 | −0.0504 (11) | 0 | 0.107 (3) | 0.016 (1) | |
O33 | 0.8933 (11) | 0.190 (2) | 0.0297 (17) | 0.016 (1) | |
O34 | 0.8717 (14) | 0 | 0.650 (2) | 0.016 (1) | |
O35 | −0.0569 (10) | 0 | 0.592 (2) | 0.016 (1) | |
O36 | 0.8832 (10) | 0.1887 (17) | 0.5270 (17) | 0.016 (1) | |
O37 | 0.1130 (12) | 0 | 0.8333 (19) | 0.016 (1) | |
O38 | 0.0435 (10) | 0 | 0.898 (3) | 0.016 (1) | |
O39 | 0.1071 (11) | 0.1873 (16) | −0.0459 (19) | 0.016 (1) | |
O40 | 0.1382 (12) | 0.030 (5) | 0.088 (2) | 0.016 (1) | 0.5 |
O41 | 0.1298 (11) | 0.875 (4) | 0.213 (2) | 0.016 (1) | 0.5 |
O42 | 0.2003 (10) | 0.864 (4) | 0.154 (2) | 0.016 (1) | 0.5 |
O43 | 0.1732 (12) | 0.191 (2) | 0.2111 (18) | 0.016 (1) | 0.5 |
O44 | 0.1803 (13) | 0 | 0.5844 (19) | 0.016 (1) | 0.41 (3) |
O45 | 0.1104 (11) | 0 | 0.648 (3) | 0.016 (1) | 0.41 (3) |
O46 | 0.1762 (12) | 0.185 (2) | 0.7047 (19) | 0.016 (1) | 0.41 (3) |
O47 | 0.1953 (13) | 0 | 0.726 (3) | 0.016 (1) | 0.59 (3) |
O48 | 0.1776 (12) | 0 | 0.583 (2) | 0.016 (1) | 0.59 (3) |
O49 | 0.1303 (12) | 0.188 (2) | 0.669 (3) | 0.016 (1) | 0.59 (3) |
O50 | 0.2397 (11) | 0 | 0.3421 (18) | 0.016 (1) | 0.41 (3) |
O51 | 0.2642 (13) | 0 | 0.481 (2) | 0.016 (1) | 0.41 (3) |
O52 | 0.1998 (11) | 0.1918 (16) | 0.430 (2) | 0.016 (1) | 0.41 (3) |
O53 | 0.1873 (14) | 0 | 0.480 (3) | 0.016 (1) | 0.59 (3) |
O54 | 0.2644 (12) | 0 | 0.478 (3) | 0.016 (1) | 0.59 (3) |
O55 | 0.2186 (10) | 0.1926 (19) | 0.3763 (18) | 0.016 (1) | 0.59 (3) |
O56 | 0.4467 (10) | 0 | 0.3284 (15) | 0.016 (1) | |
O57 | 0.3699 (7) | 0 | 0.268 (2) | 0.016 (1) | |
O58 | 0.4281 (9) | 0.179 (2) | 0.2041 (15) | 0.016 (1) | |
O59 | 0.4706 (11) | 0 | −0.070 (2) | 0.016 (1) | |
O60 | 0.4794 (15) | 0 | 0.076 (2) | 0.016 (1) | |
O61 | 0.5329 (9) | 0.1844 (17) | 0.003 (2) | 0.016 (1) | |
O62 | 0.5126 (10) | 0 | 0.4235 (18) | 0.016 (1) | |
O63 | 0.4357 (10) | 0 | 0.471 (2) | 0.016 (1) | |
O64 | 0.4939 (11) | 0.1927 (19) | 0.5364 (17) | 0.016 (1) | |
O65 | 0.5623 (14) | 0 | 0.1528 (18) | 0.016 (5) | 0.41 (5) |
O66 | 0.6162 (10) | 0 | 0.260 (2) | 0.016 (5) | 0.41 (5) |
O67 | 0.5482 (12) | 0.193 (2) | 0.272 (2) | 0.016 (5) | 0.41 (5) |
O68 | 0.6030 (10) | 0 | 0.3053 (19) | 0.016 (5) | 0.59 (5) |
O69 | 0.5860 (12) | 0 | 0.1658 (18) | 0.016 (5) | 0.59 (5) |
O70 | 0.5393 (9) | 0.1866 (17) | 0.2549 (19) | 0.016 (5) | 0.59 (5) |
O71 | 0.7352 (11) | 0 | 0.1707 (19) | 0.016 (5) | |
O72 | 0.7138 (10) | 0 | 0.032 (2) | 0.016 (5) | |
O73 | 0.7815 (10) | 0.187 (2) | 0.0832 (19) | 0.016 (5) | |
O74 | 0.7689 (11) | 0 | 0.507 (2) | 0.016 (5) | |
O75 | 0.7020 (10) | 0 | 0.579 (2) | 0.016 (5) | |
O76 | 0.7646 (10) | 0.1836 (17) | 0.6330 (19) | 0.016 (5) | |
O77 | 0.8031 (11) | 0.092 (5) | 0.262 (2) | 0.016 (5) | 0.5 |
O78 | 0.7934 (13) | 0.844 (5) | 0.363 (3) | 0.016 (5) | 0.5 |
O79 | 0.8635 (12) | 0.867 (4) | 0.315 (2) | 0.016 (5) | 0.5 |
O80 | 0.8444 (12) | 0.123 (4) | 0.400 (2) | 0.016 (5) | 0.5 |
O81 | 0.8038 (11) | 0 | −0.0796 (19) | 0.016 (5) | |
O82 | 0.8726 (11) | 0 | 0.859 (2) | 0.016 (5) | |
O83 | 0.8095 (12) | 0.191 (2) | 0.7989 (19) | 0.016 (5) | |
(Alite_Hydration_11h) 'Tricalcium Silicate Oxide'
top
Crystal data top
Ca3O5Si | Z = 36 |
Monoclinic, Cm | Cu Kα1 radiation, λ = 1.5406 Å |
a = 33.085 Å | T = 310 K |
b = 7.037 Å | white |
c = 18.521 Å | flat_sheet, 22 × 22 mm |
β = 94.160° | Specimen preparation: Prepared at 310 K and 101.325 kPa |
V = 4300.6 Å3 | |
Data collection top
D8 Bruker diffractometer | Data collection mode: reflection |
Radiation source: sealed X-ray tube, KFL CU 2K Siemens | Scan method: step |
None monochromator | 2θmin = 7.0°, 2θmax = 39.996°, 2θstep = 0.024° |
Specimen mounting: temperated sample holder (PMMA) with Kapton film cover | |
Refinement top
Least-squares matrix: full | Excluded region(s): none |
Rp = 0.043 | Profile function: fundamental parameter type peaks in a non linear least-squares refinement |
Rwp = 0.061 | |
Rexp = 0.033 | Background function: combination of Chebychev polynomial 0th order and fundamental parameter
type peaks phase |
1396 data points | Preferred orientation correction: spherical harmonics function |
Special details top
Experimental. In-situ experiment with special cooling/heating device for temperature
constancy. |
Refinement. Hatrurite structure from "De La Torre, A. G., Bruque, S., Campo, S. &
Aranda, M. (2002). The superstructure of C3S from synchroton and
neutron powder diffraction and its role in quantitative phase analysis.
Cement and Concrete Research, 32, 1347-1356." was used for refinement. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ca1 | −0.0024 (1) | 0 | 0.0104 (19) | 0.012 (1) | |
Ca2 | 0.6595 (10) | 0 | 0.1605 (19) | 0.012 (1) | |
Ca3 | 0.3113 (9) | 0 | 0.3342 (19) | 0.012 (1) | |
Ca4 | −0.0119 (12) | 0 | 0.4939 (19) | 0.012 (1) | |
Ca5 | 0.6531 (11) | 0 | 0.6651 (18) | 0.012 (1) | |
Ca6 | 0.3188 (11) | 0 | 0.8407 (19) | 0.012 (1) | |
Ca7 | 0.5881 (11) | 0 | −0.075 (2) | 0.012 (1) | |
Ca8 | 0.2592 (11) | 0 | 0.1012 (19) | 0.012 (1) | |
Ca9 | −0.0815 (11) | 0 | 0.2619 (19) | 0.012 (1) | |
Ca10 | 0.5848 (9) | 0 | 0.4262 (18) | 0.012 (1) | |
Ca11 | 0.2494 (11) | 0 | 0.6061 (19) | 0.012 (1) | |
Ca12 | −0.0817 (11) | 0 | 0.765 (2) | 0.012 (1) | |
Ca13 | 0.7322 (11) | 0 | −0.0925 (19) | 0.012 (1) | |
Ca14 | 0.4019 (11) | 0 | 0.078 (2) | 0.012 (1) | |
Ca15 | 0.0646 (10) | 0 | 0.2418 (19) | 0.012 (1) | |
Ca16 | 0.7236 (10) | 0 | 0.402 (2) | 0.012 (1) | |
Ca17 | 0.3895 (11) | 0 | 0.573 (2) | 0.012 (1) | |
Ca18 | 0.0617 (11) | 0 | 0.7363 (19) | 0.012 (1) | |
Ca19 | −0.0835 (10) | 0.275 (3) | −0.085 (2) | 0.0104 (8) | 0.5 |
Ca20 | −0.0833 (10) | 0.275 (3) | −0.085 (2) | 0.0104 (8) | 0.5 |
Ca21 | 0.5804 (12) | 0.277 (3) | 0.084 (2) | 0.0104 (8) | 0.5 |
Ca22 | 0.5849 (11) | 0.281 (2) | 0.0917 (18) | 0.0104 (8) | 0.5 |
Ca23 | 0.2398 (11) | 0.250 (3) | 0.2580 (18) | 0.0104 (8) | 0.5 |
Ca24 | 0.2413 (11) | 0.257 (3) | 0.2577 (18) | 0.0104 (8) | 0.5 |
Ca25 | −0.0969 (11) | 0.265 (4) | 0.4132 (18) | 0.0104 (8) | 0.5 |
Ca26 | −0.0938 (11) | 0.293 (3) | 0.4099 (18) | 0.0104 (8) | 0.5 |
Ca27 | 0.5759 (13) | 0.250 (4) | 0.597 (2) | 0.0104 (8) | 0.5 |
Ca28 | 0.5651 (11) | 0.223 (4) | 0.572 (2) | 0.0104 (8) | 0.5 |
Ca29 | 0.2436 (11) | 0.250 (4) | 0.752 (3) | 0.0104 (8) | 0.5 |
Ca30 | 0.2444 (10) | 0.241 (3) | 0.762 (2) | 0.0104 (8) | 0.5 |
Ca31 | −0.0023 (14) | 0.218 (5) | 0.847 (3) | 0.0104 (8) | 0.5 |
Ca32 | −0.0004 (14) | 0.232 (5) | 0.842 (3) | 0.0104 (8) | 0.5 |
Ca33 | 0.6675 (10) | 0.232 (3) | 0.015 (3) | 0.0104 (8) | 0.5 |
Ca34 | 0.6662 (10) | 0.241 (3) | 0.020 (3) | 0.0104 (8) | 0.5 |
Ca35 | 0.3345 (12) | 0.235 (4) | 0.172 (2) | 0.0104 (8) | 0.5 |
Ca36 | 0.3388 (10) | 0.222 (3) | 0.1825 (18) | 0.0104 (8) | 0.5 |
Ca37 | −0.0049 (10) | 0.235 (3) | 0.346 (2) | 0.0104 (8) | 0.5 |
Ca38 | −0.0051 (11) | 0.238 (3) | 0.3444 (19) | 0.0104 (8) | 0.5 |
Ca39 | 0.6608 (10) | 0.229 (3) | 0.5199 (18) | 0.0104 (8) | 0.5 |
Ca40 | 0.6570 (10) | 0.218 (2) | 0.5225 (17) | 0.0104 (8) | 0.5 |
Ca41 | 0.3312 (10) | 0.240 (4) | 0.681 (2) | 0.0104 (8) | 0.5 |
Ca42 | 0.3310 (10) | 0.236 (4) | 0.677 (3) | 0.0104 (8) | 0.5 |
Ca43 | 0.8260 (13) | 0.270 (4) | −0.012 (2) | 0.0104 (8) | 0.5 |
Ca44 | 0.8268 (10) | 0.264 (3) | −0.0093 (19) | 0.0104 (8) | 0.5 |
Ca45 | 0.4904 (10) | 0.260 (4) | 0.1593 (19) | 0.0104 (8) | 0.5 |
Ca46 | 0.4906 (10) | 0.257 (4) | 0.160 (2) | 0.0104 (8) | 0.5 |
Ca47 | 0.1502 (10) | 0.254 (4) | 0.3293 (19) | 0.0104 (8) | 0.5 |
Ca48 | 0.1509 (9) | 0.254 (3) | 0.3288 (19) | 0.0104 (8) | 0.5 |
Ca49 | 0.8127 (11) | 0.260 (3) | 0.493 (2) | 0.0104 (8) | 0.5 |
Ca50 | 0.8139 (10) | 0.261 (3) | 0.500 (2) | 0.0104 (8) | 0.5 |
Ca51 | 0.4826 (13) | 0.277 (5) | 0.6571 (19) | 0.0104 (8) | 0.5 |
Ca52 | 0.4821 (12) | 0.266 (4) | 0.6563 (19) | 0.0104 (8) | 0.5 |
Ca53 | 0.1558 (11) | 0.272 (3) | 0.8212 (19) | 0.0104 (8) | 0.5 |
Ca54 | 0.1554 (10) | 0.271 (3) | 0.8206 (18) | 0.0104 (8) | 0.5 |
Si1 | 0.0816 (11) | 0 | 0.4254 (19) | 0.004 (1) | |
Si2 | 0.2329 (11) | 0 | −0.0728 (19) | 0.004 (1) | |
Si3 | 0.4211 (11) | 0 | 0.747 (2) | 0.004 (1) | |
Si4 | 0.5603 (11) | 0 | 0.758 (2) | 0.004 (1) | |
Si5 | −0.0976 (10) | 0 | 0.0775 (17) | 0.004 (1) | |
Si6 | 0.8946 (10) | 0 | 0.5743 (18) | 0.004 (1) | |
Si7 | 0.0917 (10) | 0 | −0.0895 (19) | 0.004 (1) | |
Si8 | 0.1615 (10) | 0 | 0.1677 (18) | 0.004 (1) | |
Si9 | 0.1588 (11) | 0 | 0.6621 (18) | 0.004 (1) | |
Si10 | 0.2243 (9) | 0 | 0.4237 (17) | 0.004 (1) | |
Si11 | 0.4176 (4) | 0 | 0.2554 (8) | 0.004 (1) | |
Si12 | 0.5020 (10) | 0 | 0.0003 (19) | 0.004 (1) | |
Si13 | 0.4845 (10) | 0 | 0.4913 (18) | 0.004 (1) | |
Si14 | 0.5669 (9) | 0 | 0.2431 (17) | 0.004 (1) | |
Si15 | 0.7532 (10) | 0 | 0.0911 (19) | 0.004 (1) | |
Si16 | 0.7506 (10) | 0 | 0.5842 (19) | 0.004 (1) | |
Si17 | 0.8250 (11) | 0 | 0.3337 (19) | 0.004 (1) | |
Si18 | 0.8243 (11) | 0 | 0.8424 (19) | 0.004 (1) | |
O1 | 0.9921 (13) | 0 | 0.252 (2) | 0.031 (2) | |
O2 | 0.0342 (11) | 0 | 0.122 (2) | 0.031 (2) | |
O3 | 0.0309 (15) | 0 | 0.602 (4) | 0.031 (2) | |
O4 | −0.0101 (14) | 0 | 0.749 (2) | 0.031 (2) | |
O5 | 0.3664 (11) | 0 | −0.067 (3) | 0.031 (2) | |
O6 | 0.3313 (13) | 0 | 0.0836 (19) | 0.031 (2) | |
O7 | 0.2830 (12) | 0 | 0.2215 (19) | 0.031 (2) | |
O8 | 0.3525 (13) | 0 | 0.444 (2) | 0.031 (2) | |
O9 | 0.325 (2) | 0 | 0.593 (3) | 0.031 (2) | |
O10 | 0.2857 (13) | 0 | 0.723 (2) | 0.031 (2) | |
O11 | 0.6617 (13) | 0 | −0.084 (2) | 0.031 (2) | |
O12 | 0.6170 (9) | 0 | 0.0406 (19) | 0.031 (2) | |
O13 | 0.6976 (10) | 0 | 0.298 (2) | 0.031 (2) | |
O14 | 0.6537 (10) | 0 | 0.4255 (19) | 0.031 (2) | |
O15 | 0.6147 (11) | 0 | 0.550 (2) | 0.031 (2) | |
O16 | 0.7014 (13) | 0 | 0.770 (2) | 0.031 (2) | |
O17 | 0.9399 (13) | 0 | 0.387 (2) | 0.031 (2) | |
O18 | 0.9564 (13) | 0 | 0.903 (3) | 0.031 (2) | |
O19 | 0.1052 (13) | 0 | 0.3522 (19) | 0.016 (1) | |
O20 | 0.0327 (11) | 0 | 0.410 (2) | 0.016 (1) | |
O21 | 0.0937 (11) | 0.187 (2) | 0.4744 (19) | 0.016 (1) | |
O22 | 0.2096 (12) | 0 | 0.001 (2) | 0.016 (1) | |
O23 | 0.2806 (11) | 0 | −0.053 (2) | 0.016 (1) | |
O24 | 0.2187 (11) | 0.1794 (17) | 0.8763 (19) | 0.016 (1) | |
O25 | 0.4415 (13) | 0 | 0.671 (2) | 0.016 (1) | |
O26 | 0.3718 (10) | 0 | 0.7387 (15) | 0.016 (1) | |
O27 | 0.4338 (10) | 0.190 (2) | 0.793 (2) | 0.016 (1) | |
O28 | 0.5376 (13) | 0 | 0.832 (2) | 0.016 (1) | |
O29 | 0.6091 (11) | 0 | 0.770 (3) | 0.016 (1) | |
O30 | 0.5460 (10) | 0.1822 (17) | 0.709 (2) | 0.016 (1) | |
O31 | 0.8757 (12) | 0 | 0.1492 (19) | 0.016 (1) | |
O32 | −0.0504 (11) | 0 | 0.107 (3) | 0.016 (1) | |
O33 | 0.8933 (11) | 0.190 (2) | 0.0297 (17) | 0.016 (1) | |
O34 | 0.8717 (14) | 0 | 0.650 (2) | 0.016 (1) | |
O35 | −0.0569 (10) | 0 | 0.592 (2) | 0.016 (1) | |
O36 | 0.8832 (10) | 0.1887 (17) | 0.5270 (17) | 0.016 (1) | |
O37 | 0.1130 (12) | 0 | 0.8333 (19) | 0.016 (1) | |
O38 | 0.0435 (10) | 0 | 0.898 (3) | 0.016 (1) | |
O39 | 0.1071 (11) | 0.1873 (16) | −0.0459 (19) | 0.016 (1) | |
O40 | 0.1382 (12) | 0.030 (5) | 0.088 (2) | 0.016 (1) | 0.5 |
O41 | 0.1298 (11) | 0.875 (4) | 0.213 (2) | 0.016 (1) | 0.5 |
O42 | 0.2003 (10) | 0.864 (4) | 0.154 (2) | 0.016 (1) | 0.5 |
O43 | 0.1732 (12) | 0.191 (2) | 0.2111 (18) | 0.016 (1) | 0.5 |
O44 | 0.1803 (13) | 0 | 0.5844 (19) | 0.016 (1) | 0.41 (3) |
O45 | 0.1104 (11) | 0 | 0.648 (3) | 0.016 (1) | 0.41 (3) |
O46 | 0.1762 (12) | 0.185 (2) | 0.7047 (19) | 0.016 (1) | 0.41 (3) |
O47 | 0.1953 (13) | 0 | 0.726 (3) | 0.016 (1) | 0.59 (3) |
O48 | 0.1776 (12) | 0 | 0.583 (2) | 0.016 (1) | 0.59 (3) |
O49 | 0.1303 (12) | 0.188 (2) | 0.669 (3) | 0.016 (1) | 0.59 (3) |
O50 | 0.2397 (11) | 0 | 0.3421 (18) | 0.016 (1) | 0.41 (3) |
O51 | 0.2642 (13) | 0 | 0.481 (2) | 0.016 (1) | 0.41 (3) |
O52 | 0.1998 (11) | 0.1918 (16) | 0.430 (2) | 0.016 (1) | 0.41 (3) |
O53 | 0.1873 (14) | 0 | 0.480 (3) | 0.016 (1) | 0.59 (3) |
O54 | 0.2644 (12) | 0 | 0.478 (3) | 0.016 (1) | 0.59 (3) |
O55 | 0.2186 (10) | 0.1926 (19) | 0.3763 (18) | 0.016 (1) | 0.59 (3) |
O56 | 0.4467 (10) | 0 | 0.3284 (15) | 0.016 (1) | |
O57 | 0.3699 (7) | 0 | 0.268 (2) | 0.016 (1) | |
O58 | 0.4281 (9) | 0.179 (2) | 0.2041 (15) | 0.016 (1) | |
O59 | 0.4706 (11) | 0 | −0.070 (2) | 0.016 (1) | |
O60 | 0.4794 (15) | 0 | 0.076 (2) | 0.016 (1) | |
O61 | 0.5329 (9) | 0.1844 (17) | 0.003 (2) | 0.016 (1) | |
O62 | 0.5126 (10) | 0 | 0.4235 (18) | 0.016 (1) | |
O63 | 0.4357 (10) | 0 | 0.471 (2) | 0.016 (1) | |
O64 | 0.4939 (11) | 0.1927 (19) | 0.5364 (17) | 0.016 (1) | |
O65 | 0.5623 (14) | 0 | 0.1528 (18) | 0.016 (5) | 0.41 (5) |
O66 | 0.6162 (10) | 0 | 0.260 (2) | 0.016 (5) | 0.41 (5) |
O67 | 0.5482 (12) | 0.193 (2) | 0.272 (2) | 0.016 (5) | 0.41 (5) |
O68 | 0.6030 (10) | 0 | 0.3053 (19) | 0.016 (5) | 0.59 (5) |
O69 | 0.5860 (12) | 0 | 0.1658 (18) | 0.016 (5) | 0.59 (5) |
O70 | 0.5393 (9) | 0.1866 (17) | 0.2549 (19) | 0.016 (5) | 0.59 (5) |
O71 | 0.7352 (11) | 0 | 0.1707 (19) | 0.016 (5) | |
O72 | 0.7138 (10) | 0 | 0.032 (2) | 0.016 (5) | |
O73 | 0.7815 (10) | 0.187 (2) | 0.0832 (19) | 0.016 (5) | |
O74 | 0.7689 (11) | 0 | 0.507 (2) | 0.016 (5) | |
O75 | 0.7020 (10) | 0 | 0.579 (2) | 0.016 (5) | |
O76 | 0.7646 (10) | 0.1836 (17) | 0.6330 (19) | 0.016 (5) | |
O77 | 0.8031 (11) | 0.092 (5) | 0.262 (2) | 0.016 (5) | 0.5 |
O78 | 0.7934 (13) | 0.844 (5) | 0.363 (3) | 0.016 (5) | 0.5 |
O79 | 0.8635 (12) | 0.867 (4) | 0.315 (2) | 0.016 (5) | 0.5 |
O80 | 0.8444 (12) | 0.123 (4) | 0.400 (2) | 0.016 (5) | 0.5 |
O81 | 0.8038 (11) | 0 | −0.0796 (19) | 0.016 (5) | |
O82 | 0.8726 (11) | 0 | 0.859 (2) | 0.016 (5) | |
O83 | 0.8095 (12) | 0.191 (2) | 0.7989 (19) | 0.016 (5) | |
Crystal data top
CaH2O2 | Cu Kα1 radiation, λ = 1.5406 Å |
Trigonal, P3m1 | T = 310 K |
a = 3.597 Å | white |
c = 4.910 Å | flat_sheet, 22 × 22 mm |
V = 55.02 Å3 | Specimen preparation: Prepared at 310 K and 101.325 kPa |
Z = 1 | |
Data collection top
D8 Bruker diffractometer | Data collection mode: reflection |
Radiation source: sealed X-ray tube, KFL CU 2K Siemens | Scan method: step |
None monochromator | 2θmin = 7.0°, 2θmax = 39.996°, 2θstep = 0.024° |
Specimen mounting: temperated sample holder (PMMA) with Kapton film cover | |
Refinement top
Least-squares matrix: full | Profile function: fundamental parameter type peaks in a non linear least-squares refinement |
Rp = 4.29 | H-atom parameters not defined? |
Rwp = 6.06 | |
Rexp = 3.30 | Background function: combination of Chebychev polynomial 0th order and fundamental parameter
type peaks phase |
1396 data points | Preferred orientation correction: spherical harmonics function |
Excluded region(s): none | |
Special details top
Experimental. In-situ experiment with special cooling/heating device for temperature
constancy. |
Refinement. Portlandite structure from "Busing, W. R., & Levy, H. A. (1986).
Neutron diffraction study of calcium hydroxide.
Acta Crystallographica B, 42 , 51-55." was used for refinement. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Biso*/Beq | |
Ca1 | 0 | 0 | 0 | 0.88 | |
O1 | 0.3333 | 0.6667 | 0.2341 (3) | 0.797 | |
H1 | 0.3333 | 0.6667 | 0.4248 (6) | 3.26 | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
? | ? | ? | ? | ? | ? | ? |