Studies of water and ice in hydrophilic and hydrophobic mesoporous silicas : Pore characterisation and phase transformations

Abstract A study has been made as a function of temperature of the phase transformation of water and ice in two samples of mesoporous silica gel with pore diameters of ∼50Å. One sample was modified by coating with a layer of trimethylchlorosilane, giving a predominantly hydrophobic internal surface, whereas the unmodified sample has a hydrophilic interface. The pore structure was characterised by nitrogen gas adsorption and NMR cryoporometry and the melting/freezing behaviour of water and ice in the pores was studied by DSC and neutron diffraction for cooling and heating cycles, covering a range of 200 to 300K. Measurements were made for several filling-factors in the range 0.2 to 0.9. The results show a systematic difference in the form of ice created in each of the samples. The non-modified sample gives similar results to previous studies with hydrophilic silicas, exhibiting a defective form of cubic ice superimposed on a more disordered pattern that changes with temperature and has been characterised as 'plastic' ic