Research lines

Founding member and current spokesperson of the Cement Science Research Group at University of Málaga.

"Looking deeper into the mesostructure of building materials without missing the big picture"

1. Eco-cements; industrially-relevant materials (pigments, ceramics, etc.).       The final main goal is to decrease the environmental footprint: 

2. Use of large facilities (synchrotrons and neutrons) for the quantitative characterization of materials

3. Synchrotron and laboratory powder diffraction. Rietveld method. Pair Distribution Function.

4. High pressure synchrotron diffraction.

5. Coherent diffraction imaging; ptychographic X-ray computed nanotomography; X-ray tomographic imaging.

6. Multiscale characterization (nano-, meso- and micro- structures) to help to develop a coherent picture.

7. Multimodal analysis to ensure accurate, reproducible scientific information and not just high-quality data.

8. Fast high-resolution relevant 4D nanoimaging of cement hydration. Mainly by near field ptychotomography.

9. Combined laboratory X-ray #powder diffraction and #micro computed tomography to quantify the time evolution of phases within complex chemical reactions involving crystalline and amorphous components.


Combining all the above: research and development in PC-SCMs blends (supplementary cementitious materials)
from all types: kaolinitic clays, smectitic clays, natural pozzolans (volcanic ashes, zeolites, trass, etc.), fly ashes, ...
"LOCAL SOLUTIONS FOR A GLOBAL PROBLEM"

Selected publications as leading author 2016-2024:

Reviews 

1. Cuesta, A.; Morales-Cantero, A.; De la Torre, A.G.; Aranda, M.A.G. Recent advances in C-S-H nucleation seeding for improving cement performancesMaterials, 2023, 16, 1462. https://doi.org/10.3390/ma16041462
Highlight: Review about C-S-H gel nucleation seeding mainly from commercial sources to improve the performances of low-carbon cements (those using SCMs).

2. Cuesta, A.; Ayuela, A.; Aranda, M.A.G.Belite cements and their activationCement and Concrete Research, 2021, 140, 106319. https://doi.org/10.1016/j.cemconres.2020.106319
Highlight: Review about the activation of belite-rich (C-S-H forming) cements. The activation can be at the clinkering stage, physically (i.e. milling and fast cooling) and chemically (admixtures at the hydration stage).

3. Aranda, M.A.G. “Recent studies of cements and concretes by synchrotron radiation crystallographic and cognate methods Crystallography Reviews, 2016, 22, 150196. https://doi.org/10.1080/0889311X.2015.1070260
Highlight: Review about the use of synchrotron radiation techniques (imaging, diffraction, scattering, etc.) in the building materials field.

Synchrotron ptychotomography (for very detailed microstructural studies):

1. Shirani, S.; Cuesta, A.; Morales-Cantero, A.; Santacruz, I.; Diaz, A.; Trtik, P.; Holler, M.; Rack, A.; Lukic, B.; Brun, E.; Salcedo, I.R.; Aranda, M.A.G.4D nanoimaging of early age cement hydrationNature Communications, 2023, 14, 2652. https://doi.org/10.1038/s41467-023-38380-1
Highlight: We have tailored near-field ptycho-tomography for the in situ 4D study of dissolution and precipitation processes, with ~250 nm of spatial resolution and very good contrast between the components. The spatial dissolution rate of small alite grains, ~100 nm/h, is four times faster than that of large alite grains, ~25 nm/h. C-S-H gel shell, surrounding alite particles, was quantified and etch-pit growth rate was estimated. 

2. Shirani, S.; Cuesta, A.; De la Torre, A.G.; Diaz, A.; Trtik, P.; Holler, M.; Aranda, M.A.G.Calcium aluminate cement conversion analysed by ptychographic nanotomographyCement and Concrete Research, 2020, 137, 106201. https://doi.org/10.1016/j.cemconres.2020.106201
Highlight: Mass density determination of nano-gibbsite gels as function of temperature and chiefly the determination of secondary porosity development after calcium aluminate conversion, sizes ~140 nm. 

3. Cuesta, A.; De la Torre, A.G.; Santacruz, I.; Diaz, A.; Trtik, P.; Holler, M.; Lothenbach, B.; Aranda, M.A.G. Quantitative disentanglement of nanocrystalline phases in cement pastes by synchrotron ptychographic X-ray tomographyIUCrJ, 2019, 6, 473–491. https://doi.org/10.1107/S2052252519003774
Highlight: Spatially-resolved mass density determination of amorphous phases including C-S-H (inner and outer products) and iron-siliceous hydrogarnet. 3D spatial resolution better than 70 nm. 

4. Cuesta, A.; De la Torre, A.G.; Santacruz, I.; Trtik, P.; da Silva, J.C.; Diaz, A.; Holler, M.; Aranda, M.A.G.Chemistry and Mass Density of Aluminum Hydroxide Gel in Eco-Cements by Ptychographic X-ray Computed TomographyJournal Physical Chemistry C, 2017, 121, 3044–3054. https://doi.org/10.1021/acs.jpcc.6b10048
Highlight: Spatially-resolved mass density determination of aluminium hydroxide gels. 3D phase component reconstruction and segmentation with spatial resolution better than 200 nm.


Synchrotron phase contrast tomography  (for fast microstructural studies):

1. Shirani, S.; Cuesta, A.; Morales-Cantero, A.; De la Torre, A.G.; Olbinado, M.; Aranda, M.A.G. “Influence of curing temperature on belite cement hydration: a comparative study with Portland cement Cement and Concrete Research, 2021, 147, 106499. https://doi.org/10.1016/j.cemconres.2021.106499
Highlight: We have been able to explain (using several techniques and chiefly synchrotron m-CT) the improved mechanical performances at mild curing temperatures, 40-60ºC, of BCs respect to PCs because larger belite degree of reaction at 40ºC with lower porosity coarsening of BCs with T also playing a role.

2. Bernal, I.M.R.; Shirani, S.; Cuesta, A.; Santacruz, I.; Aranda, M.A.G. “Phase and microstructure evolutions in limestone calcined clay cements by multi-technique approach including synchrotron microtomographyConstruction and Building Materials, 2021, 300, 124054. https://doi.org/10.1016/j.conbuildmat.2021.124054
Highlight: It is the first paper reporting the use of synchrotron microtomography in LC3 binders. Porosity connectivities, within the attained spatial resolution, decreased from 92% at 7 hydration days to 9% at 60 days helping to explain the good durability properties of these binders. Limestone could be segmented because the additional information from phase-contrast Paganin phase retrieval.


Laboratory tomography  (for accurate studies when combined to in situ laboratory diffraction):

1. Shirani, S.; Cuesta, A.; De la Torre, A.G.; Santacruz, I.; Morales-Cantero, A.; Koufany, I.; Redondo-Soto, C.; Salcedo, I.R.; Leon-Reina, L. Aranda, M.A.G. “Mix and Measure - combining in situ X-ray powder diffraction and microtomography for accurate hydrating cement studiesCement and Concrete Research, 2024, 175, 107370. https://doi.org/10.1016/j.cemconres.2023.107370
Highlight: Combined use of powder diffraction and micro computed tomography in the same volume of the same capillary for an in situ study of PC 42.5 R hydrating cement. Ex situ studies have also been carried out to determine the accuracy of the procedures for the two in situ studies: (i) Rietveld analysis of powder diffraction data (without an internal standard) for phase development; and (ii) Machine Learning segmentation of tomographic data for analysis of components and microstructures from microtomographic data.

2.  Salcedo, I.R.; Cuesta, A.; Shirani, S.; León-Reina, L.; Aranda, M.A.G. “Accuracy in cement hydration investigations: combined X-ray microtomography and powder diffraction analysesMaterials, 2021, 14, 6953. https://doi.org/10.3390/ma14226953
Highlight: Combined use of powder diffraction and micro computed tomography in the same volume of the same capillary of a hydrating cement. The final goal is to quantify complex phase developments like the  hydration degree of the amorphous fraction of supplementary cementitious materials in cement blends as function of time/temperature/etc.


Synchrotron X-ray powder diffraction for in situ evolution of crystalline phases :

1.  Morales-Cantero, A.; De la Torre, A.G.; Cuesta, A.; Santacruz, I.; Bernal, I.M.R.; Mazanec, O.; Dalla-Libera, A.; Dhers, S.; Borralleras, P.; Aranda, M.A.G. “In situ synchrotron powder diffraction study of LC3 cement activation at very early ages by C-S-H nucleation seeding” Cement and Concrete Research, 2024,  178, 107463. 

Highlight: The hydration reactions of LC3 during the first day of hydration have been studied processed with two different superplasticizers and three strength-enhancing admixtures. Moreover, C-S-H nucleation seeding was proved to enhance mainly the C3A and C4AF phases. Chiefly, the pozzolanic reaction was observed to take place after 7 hours of hydration as C3S keeps hydrating but portlandite content stagnated.

2. Morales-Cantero, A.; Cuesta, A.; De la Torre, A.G.; Santacruz, I.; Mazanec, O.; Borralleras, P.; Weldert, K.S.; Gastaldi, D.; Canonico, F.; Aranda, M.A.G.C-S-H seeding activation of Portland and Belite Cements: an enlightening in situ synchrotron powder diffraction studyCement and Concrete Research, 2022, 161, 106946.

Highlight: It showed that C-S-H nucleation seeding did not importantly accelerate alite hydration, which disagrees with the accepted mechanism, but it accelerates sulfate and aluminate dissolutions. Indirectly, it remarks the importance of detailed microstructural studies as this seeding seems to profoundly modify the inner/outer C-S-H ratio. 

3. Cuesta, A.; Zea-Garcia, J.D.; Londono-Zuluaga, D.; De la Torre, A.G.; Santacruz, I.; Vallcorba, O.; Dapiaggi, M.; Sanfélix, S.G.; Aranda, M.A.G. “Multiscale understanding of tricalcium silicate hydration reactionsScientific Reports, 2018, 8, 8544.

Highlight: New model for C-S-H gel explaining two apparently contradictory observations: i) the gel has a Ca/Si ratio of ~1.8 at the micrometre scale; but ii) it shows tobermorite local structure (~1.2 Ca/Si ratio) at the nanoscale. We showed signatures of intersperse calcium hydroxide monolayers in the gel pores. Very important implications for reactivity of C-S-H. It also justifies its variable local Ca/Si ratio.