Insights into the nano- and microstructures of cementitious materials using synchrotron X-rays
Source abstract
Abstract
Synchrotron X-ray techniques have been extensively applied to characterise the mineralogy of anhydrous cementitious materials, the hydration processes and products in cementitious systems, and the alterations induced by different environmental exposure conditions. However, with changes in cement compositions and performance requirements, and an increased focus on materials design for sustainability, there is now strong emphasis on the use of advanced analytical tools to bring fundamentally based, multi-scale, multi-modal, spatially-resolved and/or time-resolved understanding of the physico-chemical factors influencing cementitious materials in the fluid, hardening and cured states. Beamline-based analysis complements conventional laboratory techniques, bringing unique capabilities to develop high-level insights. Here we provide a critical overview of the application of synchrotron radiation-based techniques to cementitious materials, and the opportunities and research needs to unlock their full potential for their use in future cement materials research, including issues related to handling and processing the very large datasets that can be generated.
Source: openalex_inverted_index · Quality: baseline
Research context
OpenAlex topics: Concrete and Cement Materials Research · Concrete Properties and Behavior · Advanced X-ray Imaging Techniques
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (100+)
Show source-provided references
1. Willmott · 2019
2. Mobilio · 2015
3. Schlachter · 2021
4. Development and trends in synchrotron studies of ancient and historical materials10.1016/j.physrep.2012.03.003 ↗
5. Recent studies of cements and concretes by synchrotron radiation crystallographic and cognate methods10.1080/0889311X.2015.1070260 ↗
6. Materials characterization by synchrotron x-ray microprobes and nanoprobes10.1103/RevModPhys.90.025007 ↗
7. Advances in characterizing and understanding the microstructure of cementitious materials10.1016/j.cemconres.2019.105806 ↗
8. Advances in imaging, scattering, spectroscopy, and machine learning-aided approaches for multiscale characterization of cementitious systems10.1016/j.cemconres.2023.107335 ↗
9. A review of micro-resolved crystochemical and mechanical probes for sustainable cement-based material studies10.1038/s44296-024-00044-6 ↗
10. 4D synchrotron X-ray nanoimaging for early age cement curing: where are we and where should we go?10.1021/accountsmr.5c00018 ↗
11. The PONKCS method applied for time resolved XRD quantification of supplementary cementitious material reactivity in hydrating mixtures with ordinary Portland cement10.1016/j.conbuildmat.2019.04.157 ↗
12. Quantification of phases with partial or no known crystal structures10.1154/1.2362855 ↗
13. Mix and measure - combining in situ X-ray powder diffraction and microtomography for accurate hydrating cement studies10.1016/j.cemconres.2023.107370 ↗
14. Mix and measure II: joint high-energy laboratory powder diffraction and microtomography for cement hydration studies10.1107/S1600576724004527 ↗
15. Micro X-ray diffraction and elemental study on Al-tobermorite formation in aged modern concrete10.1111/jace.18624 ↗
16. The crystal structure of a new calcium aluminate phase containing formate10.1016/j.cemconres.2021.106490 ↗
17. Two-step nucleation process of calcium silicate hydrate, the nanobrick of cement10.1021/acs.chemmater.7b04245 ↗
18. Multi-scale synchrotron X-ray scattering studies on thermo-induced changes in structural and mechanical properties of CSH/PCE composites10.1016/j.conbuildmat.2024.139742 ↗
19. Composition and density of nanoscale calcium–silicate–hydrate in cement10.1038/nmat1871 ↗
20. The rise of the X-ray atomic pair distribution function method: a series of fortunate events10.1098/rsta.2018.0413 ↗
21. Local structure and Ca/Si ratio in C-S-H gels from hydration of blends of tricalcium silicate and silica fume10.1016/j.cemconres.2021.106405 ↗
22. Time-dependent phase quantification and local structure analysis of hydroxide-activated slag via X-ray total scattering and molecular modeling10.1016/j.cemconres.2021.106642 ↗
23. Effect of magnesium silicate hydrate (M-S-H) formation on the local atomic arrangements and mechanical properties of calcium silicate hydrate (C-S-H): in situ X-ray scattering study10.1016/j.cemconres.2022.106869 ↗
24. Watching nanomaterials with X-ray eyes: probing different length scales by combining scattering with spectroscopy10.1016/j.pmatsci.2020.100667 ↗
25. X-ray ptychography10.1038/s41566-017-0072-5 ↗
26. Ptychography: a solution to the phase problem10.1063/PT.3.4835 ↗
27. X-ray computed tomography
28. X-ray phase contrast imaging from synchrotron to conventional sources: a review of the existing techniques for biological applications10.3390/app12199539 ↗
29. Overview of the use of micro-computed tomography (micro-CT) to investigate the relation between the material characteristics and properties of cement-based materials10.1016/j.conbuildmat.2019.116843 ↗
30. A review of X-ray computed tomography of concrete and asphalt construction materials10.1016/j.conbuildmat.2018.12.049 ↗
31. Multiscale X-ray tomography of cementitious materials: a review10.1016/j.cemconres.2019.105824 ↗
32. Advancing concrete durability research through X-ray computed tomography10.3151/jact.19.730 ↗
33. Simultaneous phase and amplitude extraction from a single defocused image of a homogeneous object10.1046/j.1365-2818.2002.01010.x ↗
34. Multi-contrast 3D X-ray imaging of porous and composite materials10.1063/1.4918617 ↗
35. Time resolved X-ray dark-field tomography revealing water transport in a fresh cement sample10.1038/srep29108 ↗
36. Multi-resolution X-ray phase-contrast and dark-field tomography of human cerebellum with near-field speckles10.1364/BOE.502664 ↗
37. On mesoscale modeling of concrete: role of heterogeneities on local stresses, strains, and representative volume element10.1016/j.cemconres.2022.107031 ↗
38. Examining the micromechanics of cementitious composites using in-situ X-ray measurements10.1016/j.ijsolstr.2023.112162 ↗
39. Grain-scale stress heterogeneity in concrete from in-situ X-ray measurements10.1016/j.cemconres.2025.107789 ↗
40. Coherent diffraction study of calcite crystallization during the hydration of tricalcium silicate10.1016/j.matdes.2018.07.031 ↗
41. In situ Bragg coherent diffraction imaging study of a cement phase microcrystal during hydration10.1021/cg5013389 ↗
42. WayForLight
43. Cement hydration mechanisms through time – a review10.1007/s10853-023-08651-9 ↗
44. Advances in understanding cement hydration mechanisms10.1016/j.cemconres.2019.105823 ↗
45. Advances in multiscale/multimodal X-ray tomography10.1080/08940886.2024.2414705 ↗
46. Effects of cement particle size distribution on performance properties of Portland cement-based materials10.1016/S0008-8846(99)00163-5 ↗
47. Fauth · 2013
48. The crystallography stations at the Alba synchrotron10.1140/epjp/i2015-15160-y ↗
49. Dissolution and initial hydration behavior of tricalcium aluminate in low activity sulfate solutions10.1016/j.cemconres.2020.105989 ↗
50. A kinetic and mechanistic study into the transformation of calcium sulfate hemihydrate to dihydrate10.1107/S1600577519001929 ↗
51. First seconds in a building’s life—in situ synchrotron X-ray diffraction study of cement hydration on the millisecond timescale10.1002/anie.201200993 ↗
52. Tricalcium aluminate hydration in additivated systems. A crystallographic study by SR-XRPD10.1016/j.cemconres.2007.11.011 ↗
53. Hydration mechanisms of two polymorphs of synthetic ye’elimite10.1016/j.cemconres.2014.05.010 ↗
54. Multiscale understanding of tricalcium silicate hydration reactions10.1038/s41598-018-26943-y ↗
55. Time-resolved 3D characterisation of early-age microstructural development of Portland cement10.1007/s10853-022-06952-z ↗
56. High-throughput powder diffraction measurement system consisting of multiple MYTHEN detectors at beamline BL02B2 of SPring-810.1063/1.4999454 ↗
57. MYTHEN III: advancements in single photon counting detectors for synchrotron powder diffraction experiments10.1107/S1600577525000438 ↗
58. Single-photon counting detectors for diffraction-limited light sources10.3389/fphy.2024.1304896 ↗
59. Two-dimensional detector software: from real detector to idealised image or two-theta scan10.1080/08957959608201408 ↗
60. Boyce · 2013
61. Data Analysis WorkbeNch (DAWN)10.1107/S1600577515002283 ↗
62. Phase-selective degree of hydration at setting: an in situ synchrotron diffraction study10.1016/j.conbuildmat.2022.127117 ↗
63. Mechanisms of cement hydration10.1016/j.cemconres.2010.09.011 ↗
64. HEMC modifications to tricalcium silicate hydration: changes in kinetics and nanostructure examined by time-resolved high energy X-ray scattering10.1016/j.cemconres.2025.107915 ↗
65. Unveiling the key factors for clinker reactivity and cement performance: a physic-chemical and performance investigation of 40 industrial clinkers10.1016/j.cemconres.2024.107717 ↗
66. The role of clinker mineralogy in cement properties: an analysis using statistical mixture design10.1016/j.cemconres.2025.108102 ↗
67. Vigor · 2019
68. In-situ early-age hydration study of sulfobelite cements by synchrotron powder diffraction10.1016/j.cemconres.2013.10.009 ↗
69. Early hydration of belite-ye’elimite-ferrite cements: role of admixtures10.1016/j.conbuildmat.2023.130765 ↗
70. Hydration activation of alite-belite-ye’elimite cements by doping with boron10.1021/acssuschemeng.9b05975 ↗
71. Rietveld quantitative amorphous content analysis10.1107/S0021889801002485 ↗
72. C-S-H seeding activation of Portland and Belite cements: an enlightening in situ synchrotron powder diffraction study10.1016/j.cemconres.2022.106946 ↗
73. Portland and belite cement hydration acceleration by C-S-H seeds with variable w/c ratios10.3390/ma15103553 ↗
74. In situ synchrotron powder diffraction study of LC3 cement activation at very early ages by C-S-H nucleation seeding10.1016/j.cemconres.2024.107463 ↗
75. High-pressure and -temperature spinning capillary cell for in situ synchrotron X-ray powder diffraction10.1107/S1600577519005150 ↗
76. In situ investigation of phosphonate retarder interaction in oil well cements at elevated temperature and pressure conditions10.1111/jace.17373 ↗
77. Rietveld quantitative phase analysis of oil well cement: in situ hydration study at 150 bars and 150 °C10.3390/ma12121897 ↗
78. Belite hydration at high temperature and pressure by in situ synchrotron powder diffraction10.1016/j.conbuildmat.2020.120825 ↗
79. In-situ X-ray computed tomography characterisation of 3D fracture evolution and image-based numerical homogenisation of concrete10.1016/j.cemconcomp.2016.10.001 ↗
80. Characterisation of fracture evolution of a single cemented brittle grain using in-situ X-ray computed tomography10.1016/j.ijrmms.2021.104835 ↗
81. 4D characterisation of damage and fracture mechanisms of ultra high performance fibre reinforced concrete by in-situ micro X-ray computed tomography tests10.1016/j.cemconcomp.2019.103473 ↗
82. In situ observation for the influence of hydraulic pressure on internal damage of cement-based materials10.1016/j.matdes.2022.110556 ↗
83. X-ray computed tomography images based phase-field modeling of mesoscopic failure in concrete10.1016/j.engfracmech.2019.01.005 ↗
84. Automated correction for the movement of suspended particulate in microtomographic data10.1016/j.ces.2020.115736 ↗
85. Examining microstructural evolution of Portland cements by in-situ synchrotron micro-tomography10.1007/s10853-014-8743-9 ↗
86. Direct in-situ observation of early age void evolution in sustainable cement paste containing fly ash or limestone10.1016/j.compositesb.2019.107099 ↗
87. Direct observation of void evolution during cement hydration10.1016/j.matdes.2017.09.056 ↗
88. Visualization and quantification of pore structure of oil-well cement slurry in liquid-solid transition stage using high-resolution computed tomography10.1016/j.cemconcomp.2020.103633 ↗
89. Synchrotron X-ray micro-tomography investigation of the early hydration of blended cements: a case study on CaCl2-accelerated slag-based blended cements10.1016/j.conbuildmat.2022.126412 ↗
90. Hierarchical synchrotron diffraction and imaging study of the calcium sulfate hemihydrate–gypsum transformation10.1107/S1600576723002881 ↗
91. Mechanical response of cement and shale admixtures under cyclic triaxial loading monitored by in-situ synchrotron micro-computed tomography10.1016/j.cemconres.2024.107682 ↗
92. In-situ microtomography image segmentation for characterizing strain-hardening cementitious composites under tension using machine learning10.1016/j.cemconres.2023.107164 ↗
93. Chemistry and mass density of aluminum hydroxide gel in eco-cements by ptychographic X-ray computed tomography10.1021/acs.jpcc.6b10048 ↗
94. Quantitative disentanglement of nanocrystalline phases in cement pastes by synchrotron ptychographic X-ray tomography10.1107/S2052252519003774 ↗
95. Calcium aluminate cement conversion analysed by ptychographic nanotomography10.1016/j.cemconres.2020.106201 ↗
96. 4D nanoimaging of early age cement hydration10.1038/s41467-023-38380-1 ↗
97. Atomic-scale identification of defects in alite10.1016/j.cemconres.2023.107391 ↗
98. Influence of tertiary alkanolamines on Portland cement hydration10.1111/j.1151-2916.1993.tb03934.x ↗
99. Synchrotron x-ray techniques for fluid dynamics10.1007/s00348-014-1686-8 ↗
100. Time-resolved 2D concentration maps in flowing suspensions using X-ray10.1122/1.4994063 ↗