Abstract
Nuclear magnetic resonance (NMR) cryoporometry is an experimental technique for the structural characterization of mesoporous materials. In this updated review, different aspects of its application to study details of the pore structure in mesoporous silicon are presented. In particular, the information obtained with the help of NMR cryoporometry is compared to that assessed using more conventional gas sorption techniques. The potentials of NMR cryoporometry to reveal fine details of the pore structure in intentionally nanostructured mesoporous silicon are demonstrated. The technique’s ability to monitor structural evolution in liquids is also starting to find uses in biomedical applications such as drug delivery.
References
Brun M, Lallemand A, Quinson JF, Eyraud C (1977) New method for simultaneous determination of size and shape of pores: the thermoporometry. Thermochim Acta 21(1):59–88
Dash JG, Rempel AW, Wettlaufer JS (2006) The physics of premelted ice and its geophysical consequences. Rev Mod Phys 78(3):695–741
Dvoyashkin M, Khokhlov A, Valiullin R, Kärger J (2008) Freezing of fluids in disordered mesopores. J Chem Phys 129(15):154702–154706
Elia P, Nativ-Roth E, Zeiri Y, Porat Z (2016) Determination of the average pore size and total porosity in porous silicon layers by image processing of SEM micrographs. Micropor Mesopor Mat 225:465–471
Gopinathan N, Yang B, Lowe JP, Edler KJ, Rigby SP (2014) NMR cryoporometery characterization of the relation between drug release profile and pore structural evolution of polymeric nanoparticles. Int J Pharm 469(1):146–158
Jackson CL, McKenna GB (1990) The melting behavior of organic materials confined in porous solids. J Chem Phys 93(12):9002–9011
Khokhlov A (2009) Nanoporous silicon: structural characterization using nmr and applications. University of Leipzig, Leipzig
Khokhlov A, Valiullin R, Kärger J, Steinbach F, Feldhoff A (2007) Freezing and melting transitions of liquids in mesopores with ink-bottle geometry. New J Phys 9(8):272
Khokhlov AG, Valiullin RR, Kärger J, Zubareva NB, Stepovich MA (2008a) Estimation of pore sizes in porous silicon by scanning electron microscopy and nmr cryoporometry. J Synch Investig 2(6):919–922
Khokhlov AG, Valiullin RR, Stepovich MA, Kärger J (2008b) Characterization of pore size distribution in porous silicon by nmr cryoporosimetry and adsorption methods. Colloid J 70(4):507–514
Kondrashova D, Valiullin R (2013) Improving structural analysis of disordered mesoporous materials using NMR cryoporometry. Micropor Mesopor Mat 178:15–19
Kondrashova D, Valiullin R (2015) Freezing and melting transitions under mesoscalic confinement: application of the Kossel–Stranski crystal growth model. J Phys Chem C 119(8):4312–4323
Kondrashova D, Dvoyashkin M, Valiullin R (2011) Structural characterization of porous solids by simultaneously monitoring the low-temperature phase equilibria and diffusion of intrapore fluids using nuclear magnetic resonance. New J Phys 13(1):015008
Mitchell J, Webber JBW, Strange JH (2008) Nuclear magnetic resonance cryoporometry. Phys Rep 461(1):1–36
Morishige K, Yasunaga H, Denoyel R, Wernert V (2007) Pore-blocking-controlled freezing of water in cagelike pores of KIT-5. J Phys Chem C 111(26):9488–9495
Nephryahin A, Fletcher RS, Holt EM, Rigby SP (2016) Techniques for direct experimental evaluation of structure-transport relationships in disordered porous materials. Adsorption 22(7):993–1000
Perkins EL, Lowe JP, Edler KJ, Tanko N, Rigby SP (2008) Determination of the percolation properties and pore connectivity for mesoporous solids using NMR cryodiffusometry. Chem Eng Sci 63(7):1929–1940
Petrov OV, Furó I (2009) NMR cryoporometry: principles, applications and potential. Prog Nucl Magn Reson Spectrosc 54(2):97–122
Schulz PS (2010) Ionic liquids as solvent probes for NMR cryoporometry. ChemPhysChem 11(1):87–89
Strange JH, Rahman M, Smith EG (1993) Characterization of porous solids by NMR. Phys Rev Lett 71(21):3589–3591
Thommes M, Kaneko K, Neimark AV, Olivier JP, Rodriguez-Reinoso F, Rouquerol J, Sing KSW (2015) Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report). Pure Appl Chem 87(9–10):1051–1069
Valiullin R, Furo I (2002) The morphology of coexisting liquid and frozen phases in porous materials as revealed by exchange of nuclear spin magnetization followed by h-1 nuclear magnetic resonance. J Chem Phys 117(5):2307–2316
Vargas-Florencia D, Petrov OV, Furo I (2007) NMR cryoporometry with octamethylcyclotetrasiloxane as a probe liquid: accessing large pores. J Colloid Interface Sci 305(2):280–285
Vonszombathely M, Brauer P, Jaroniec M (1992) The solution of adsorption integral-equations by means of the regularization method. J Comput Chem 13(1):17–32
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2017 Springer International Publishing AG
About this entry
Cite this entry
Valiullin, R. (2017). NMR Cryoporometry Characterization of Mesoporous Silicon. In: Canham, L. (eds) Handbook of Porous Silicon. Springer, Cham. https://doi.org/10.1007/978-3-319-04508-5_44-2
Download citation
DOI: https://doi.org/10.1007/978-3-319-04508-5_44-2
Received:
Accepted:
Published:
Publisher Name: Springer, Cham
Print ISBN: 978-3-319-04508-5
Online ISBN: 978-3-319-04508-5
eBook Packages: Springer Reference Chemistry and Mat. ScienceReference Module Physical and Materials ScienceReference Module Chemistry, Materials and Physics
Publish with us
Chapter history
-
Latest
NMR Cryoporometry Characterization of Mesoporous Silicon- Published:
- 11 February 2017
DOI: https://doi.org/10.1007/978-3-319-04508-5_44-2
-
Original
NMR Cryoporometry and Estimation of Pore Sizes in Mesoporous Silicon- Published:
- 24 May 2014
DOI: https://doi.org/10.1007/978-3-319-04508-5_44-1