Abstract
Absorption-based X-ray micro-tomography (X-μCT) provides fundamental in-situ information on the 3D microstructure of complex multiphase materials such as cements. However, since the phases present in a hydrating cement paste may be characterized by similar values of the attenuation coefficient, leading to low absorption contrast between different crystalline or amorphous phases, micro-structural interpretation can be equivocal. 3D phase mapping by X-ray diffraction micro-tomography proved to be a successful technique for investigating the spatial distribution of the products in the paste during the hydration process, in a totally non-invasive mode and with enhanced phase selectivity compared to absorption tomography. Phase-selective maps, in the case of crystalline phases, can be extracted from single Bragg peaks or from the Rietveld-refined scale factor. However, even poorly crystalline and/or amorphous phases present in the cement paste, such as calcium silicate hydrates, can be successfully mapped by the use of selected portions of the measured powder data containing the relevant scattering of the phase. The reconstructed maps can be directly modeled by multifractal analysis and compared with computer-generated distributions.
References
[1] H.F.W.Taylor: Cement chemistry, 2nd Edition, Thomas Telford, London (1997). 10.1680/cc.2592910.1680/cc.25929Search in Google Scholar
[2] P.C.Hewlett (Ed.): Lea's chemistry of cement and concrete, 4th Edition, Butterworth-Heimann, Oxford (1998).Search in Google Scholar
[3] J.Bensted, P.Barnes (Eds.): Structure and performance of cements, 2nd Edition, Spon Press, London–New York (2002).Search in Google Scholar
[4] E.M.Gartner, J.F.Young, D.A.Damidot, I.Jawed: Hydration of Portland cement. In: J.Bensted, P.Barnes (Eds.) Structure and performance of cements, 2nd Edition, Spon Press, London–New York, (2002) 57–113.Search in Google Scholar
[5] J.W.Bullard, H.M.Jennings, R.A.Livingston, A.Nonat, G.W.Scherer, J.S.Schweitzer, K.L.Scrivener, J.J.Thomas: Cem. Concr. Res. (in press). 10.1016/j.cemconres.2010.09.011Search in Google Scholar
[6] K.L.Scrivener, A.Nonat: Cem. Concr. Res.41 (2011) 651–665. 10.1016/j.cemconres.2011.03.02610.1016/j.cemconres.2011.03.026Search in Google Scholar
[7] J.J.Thomas, J.J.Biernacki, J.W.Bullard, S.Bishnoi, J.S.Dolado, G.W.Scherer, A.Luttge: Cem. Concr. Res.41 (2011) 1257–1278. 10.1016/j.cemconres.2010.10.00410.1016/j.cemconres.2010.10.004Search in Google Scholar
[8] J.W.Bullard, E.J.Garboczi, W.L.George, N.S.Martys, S.G.Satterfield, J.E.Terrill: Concr. Intern. January2011 (2011) 24–29. Concerning the CEMHYD3D software see: http://ciks.cbt.nist.gov/∼garbocz/monograph/appendix2.html.Search in Google Scholar
[9] D.H.Campbell: Microscopical examination and interpretation of Portland cement and clinker, 2nd Edition, Portland Cement Association, Skokie, IL (1999).Search in Google Scholar
[10] J.P.Ingham: Proc. Royal Micr. Soc.22 (2011) 4–22.Search in Google Scholar
[11] S.Diamond: Cem. Concr. Comp.26 (2004) 919–933. 10.1016/j.cemconcomp.2004.02.02810.1016/j.cemconcomp.2004.02.028Search in Google Scholar
[12] K.L.Scrivener: Cem. Concr. Comp.26 (2004) 935–945. 10.1016/j.cemconcomp.2004.02.02910.1016/j.cemconcomp.2004.02.029Search in Google Scholar
[13] J.Makar: Proc. 29th Intern. Cem. Microsc. Ass. Conf., Quebec City, Canada (2007) 472–489.Search in Google Scholar
[14] A.Zingg, L.Holzer, A.Kaech, F.Winnefeld, J.Pakusch, S.Becker, L.Gauckler: Cem. Concr. Res.38 (2008) 522–529. 10.1016/j.cemconres.2007.11.00710.1016/j.cemconres.2007.11.007Search in Google Scholar
[15] E.J.Garboczi: Cem. Concr. Res.32 (2002) 1621–1638. 10.1016/S0008-8846(02)00836-010.1016/S0008-8846(02)00836-0Search in Google Scholar
[16] T.J.Chotard, M.P.Boncoeur-Martel, A.Smith, J.P.Dupuy, C.Gault: Cem. Concr. Res.25 (2003) 145–152. 10.1016/S0958-9465(01)00063-410.1016/S0958-9465(01)00063-4Search in Google Scholar
[17] M.C.Garci Juenger: Concr. Int.26 (2004) 38–41.Search in Google Scholar
[18] L.Helfen, F.Dehn, P.Mikulik, T.Baumbach: Adv. Cem. Res.17 (2005) 103–111. 10.1680/adcr.2005.17.3.10310.1680/adcr.2005.17.3.103Search in Google Scholar
[19] E.Gallucci, K.L.Scrivener, A.Groso, M.Stampanoni, G.Margaritondo: Cem. Concr. Res.37 (2007) 360–368. 10.1016/j.cemconres.2006.10.01210.1016/j.cemconres.2006.10.012Search in Google Scholar
[20] S.Diamond, E.Landis: Mater. Struct.40 (2007) 989–993. 10.1617/s11527-006-9194-910.1617/s11527-006-9194-9Search in Google Scholar
[21] L.Holzer, Ph.Gasser, A.Kaech, M.Wegmann, A.Zingg, R.Wepf, B.Muench: J. Microsc.227 (2007) 216–228. 10.1111/j.1365-2818.2007.01804.x10.1111/j.1365-2818.2007.01804.xSearch in Google Scholar PubMed
[22] T.Scherer, M.Schwotzer, C.Kübel, A.Gerdes: Microsc. Microanal.16 (2010) 224–225. 10.1017/S143192761005900310.1017/S1431927610059003Search in Google Scholar
[23] G.Ferrari, G.Artioli, M.Parisatto, in: Lake C.B., Hills C.D. (Eds.) Proceedings of the 2010 International Solidification/Stabilization Technology Forum, Dalhousie University, Canada, (2010) 193–203.Search in Google Scholar
[24] J.Baruchel, J.Y.Buffière, E.Maire, P.Merle, G.Peix: X-ray Tomography in Material Science, Hermès Sciences Pub, Paris (2000).Search in Google Scholar
[25] J.Baruchel, J.-Y.Buffiere, P.Cloetens, M.Di Michiel, E.Ferrie, W.Ludwig, E.Maire, L.Salvo: Scripta Materialia55 (2006) 41–46. 10.1016/j.scriptamat.2006.02.01210.1016/j.scriptamat.2006.02.012Search in Google Scholar
[26] J.Banhart, A.Borbély, K.Dzieciol, F.Garcia-Moreno, I.Manke, N.Kardjilov, A.R.Kaysser-Pyzalla, M.Strobl, W.Treimer: Int. J. Mat. Res. (2010) 1069–1079. 10.3139/146.11038210.3139/146.110382Search in Google Scholar
[27] S.R.Stock: Intern. Mater. Rev.53 (2008) 129–181. 10.1179/174328008X27780310.1179/174328008X277803Search in Google Scholar
[28] G.Artioli, T.Cerulli, G.Cruciani, M.C.Dalconi, G.Ferrari, M.Parisatto, A.Rack, R.Tucoulou: Anal. Bioanal. Chem.397 (2010) 2131–2136. 2035818310.1007/s00216-010-3649-010.1007/s00216-010-3649-0Search in Google Scholar PubMed
[29] J.Baruchel, P.Cloetens, J.Hartwig, W.Ludwig, L.Mancini, P.Pernot, M.Schlenker: J. Synchrotron Rad.7 (2000) 196–201. 16609195 10.1107/S090904950000299510.1107/S0909049500002995Search in Google Scholar PubMed
[30] S.Zabler, P.Cloetens, J.-P.Guigay, J.Baruchel, M.Schlenker: Rev. Sci. Instrum.76 (2005) 073705,. 10.1063/1.196079710.1063/1.1960797Search in Google Scholar
[31] T.Weitkamp, D.Haas, D.Wegrzynek, A.Rack: J. Synch. Rad.18 (2011) 617–629. 2168568010.1107/S090904951100289510.1107/S0909049511002895Search in Google Scholar PubMed
[32] M.Parisatto: Applications of X-Ray Tomographic Techniques to the Study of Cement-Based Materials, PhD Dissertation, Università di Padova (2011).Search in Google Scholar
[33] P.Bleuet, E.Welcomme, E.Dooryhée, J.Susini, J.-L.Hodeau, P.Walter: Nature Mat.7 (2008) 468–472. 18425135 10.1038/nmat216810.1038/nmat2168Search in Google Scholar PubMed
[34] W.De Nolf, K.Janssens: Surf. Interface Anal.42 (2009) 411–418. 10.1002/sia.312510.1002/sia.3125Search in Google Scholar
[35] XRDUA Software Package by Wout De Nolf. http://xrdua.ua.ac.be.Search in Google Scholar
[36] L.Valentini, M.C.Dalconi, M.Parisatto, G.Cruciani, G.Artioli: J. Appl. Cryst.44 (2011) 272–280. 10.1107/S002188981005470110.1107/S0021889810054701Search in Google Scholar
[37] S.Igarashi, W.Chen, H.J.H.Brouwers: Cem. Concr. Comp.31 (2009) 637–646. 10.1016/j.cemconcomp.2009.06.00810.1016/j.cemconcomp.2009.06.008Search in Google Scholar
[38] C.C.T.Hansson, K.H.Khor, R.J.Cernik: Cryst. Rep.55 (2010) 1162–1173. 10.1134/S106377451007010210.1134/S1063774510070102Search in Google Scholar
[39] I.G.Richardson: Cem. Concr. Res.34 (2004) 1733–1777. 10.1016/j.cemconres.2004.05.034.10.1016/j.cemconres.2004.05.034Search in Google Scholar
[40] M.Merlini, G.Artioli, C.Meneghini, T.Cerulli, A.Bravo, F.Cella: Powd. Diffr.22 (2007) 201–208. 10.1154/1.275471310.1154/1.2754713Search in Google Scholar
[41] T.Mazumdar, S.Mazumder, D.Sen: Phys. Rev. B83 (2010) 104302. 10.1103/PhysRevB.83.10430210.1103/PhysRevB.83.104302Search in Google Scholar
[42] L.Valentini, M.C.Dalconi, M.Parisatto, G.Cruciani, G.Artioli: Proc. 13th ICCC, Madrid (2011).Search in Google Scholar
© 2012, Carl Hanser Verlag, München