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Firing-Induced Microstructural Properties of Quasi-Diamagnetic Carbonate-Based Porous Ceramics: a 1H NMR Relaxation Correlation Study

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Abstract

This study deals with the application of two-dimensional proton nuclear magnetic resonance relaxometry (2D 1H NMR-R) to the characterization of porous ceramics nearly free of magnetic compounds. Different microstructural properties were obtained by firing a diamagnetic mixture of kaolin, calcium, and magnesium carbonate over a wide range of maximum temperatures (600–1100 °C) and firing times at the maximum temperature (soaking times) (0–10 h). The 2D 1H NMR-R method relies on the correlated measurement of 1H longitudinal (T 1) and transverse (T 2) relaxation times of pore-filling water by which the properties of the interconnected pore space may be investigated. In the absence of significant magnetic susceptibility effect due to para- and ferro-magnetic compounds, the 2D 1H NMR-R maps allow studying the conjoint effects on pore size distribution and inter-pore coupling due to the variations in both time and temperature of firing. The NMR experiments were performed with a low-field 1H NMR sensor, which allows non-destructive and in situ analysis. For ceramic specimens fired at 600 and 700 °C, the fraction of smallest pores increases with firing time at the expenses of those with intermediate size. The pore shrinkage occurring at this stage, and likely associated with the transformation of kaolinite in metakaolinite, is affected in a similar way by soaking time and firing temperature, in line with the concept of equivalent firing temperature. At temperatures from 800 to 1100 °C, the structural modifications involving interconnectivity and average pore size are driven primarily by firing temperature and, secondarily, by soaking time. The 2D 1H NMR-R results are confirmed by more traditional, but destructive, mineralogical, and structural analyses like X-ray powder diffraction, helium pycnometry, mercury intrusion porosimetry, and nitrogen adsorption/desorption method.

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Acknowledgments

We are indebted to M.D. Hürlimann (Schlumberger-Doll Research) for having supplied the 2D Laplace Inversion Software.

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Authors and Affiliations

  1. Dipartimento di Fisica, Sapienza Università di Roma, P.le A. Moro 2, 00185, Rome, Italy

    Camilla Terenzi & Valentina Tudisca

  2. Dipartimento di Scienze Fisiche e Chimiche, Università de L’Aquila, Via Vetoio 10, 67010, Coppito, L’Aquila, Italy

    Cinzia Casieri

  3. CNR-IPCF UOS Roma and Dipartimento di Fisica, Sapienza Università di Roma, P.le A. Moro 2, 00185, Rome, Italy

    Francesco De Luca

  4. Dipartimento di Ingegneria Civile, Edile-Architettura, Ambientale, Università de L’Aquila, 67040, Roio, L’Aquila, Italy

    Raimondo Quaresima

  5. Istituto per i Beni Archeologici Monumentali, IBAM, CNR, 73100, Lecce, Italy

    Giovanni Quarta

Authors
  1. Camilla Terenzi
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  2. Cinzia Casieri
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  3. Francesco De Luca
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Correspondence to Cinzia Casieri.

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Terenzi, C., Casieri, C., De Luca, F. et al. Firing-Induced Microstructural Properties of Quasi-Diamagnetic Carbonate-Based Porous Ceramics: a 1H NMR Relaxation Correlation Study. Appl Magn Reson 46, 1159–1178 (2015). https://doi.org/10.1007/s00723-015-0701-4

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  • DOI: https://doi.org/10.1007/s00723-015-0701-4

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