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Open Porosity and Pore Size Distribution of Mesoporous Silica Films Investigated by Positron Annihilation Lifetime Spectroscopy and Ellipsometric Porosimetry.

ABSTRACT: Tunable mesoporous silica films were prepared though a sol-gel process directed by the self-assembly of various triblock copolymers. Positron annihilation γ-ray energy spectroscopy and positron annihilation lifetime spectroscopy (PALS) based on intense pulsed slow positron beams as well as ellipsometric porosimetry (EP) combined with heptane adsorption were utilized to characterize the open porosity/interconnectivity and pore size distribution for the prepared films. The consistency between the open porosities was examined by the variations of orthopositronium (o-Ps) 3γ annihilation fractions and the total adsorbed volumes of heptane. The average pore sizes deduced by PALS from the longest-lived o-Ps lifetimes are in good agreement with those by EP on the basis of the Barrett-Joyner-Halenda model, as indicated by a well fitted line of slope k = 1. The results indicate that the EP combined with heptane adsorption is a useful method with high sensitivity for calibrating the mesopore size in highly interconnected mesoporous films, whereas PALS is a novel, complementary tool for characterizing both closed and open pores in them.

SUBMITTER: Xiong B

PROVIDER: S-EPMC8235386 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:Plastic deformation of low/high density polyethylene (LDPE/HDPE) was analyzed in this work using positron annihilation lifetime spectroscopy (PALS). It was shown that in undeformed LDPE, both the mean ortho-positronium lifetime (τ3) and its dispersion (σ3), corresponding to the average size and size distribution of the free-volume pores of the amorphous component, respectively, were clearly higher than in HDPE. This effect was induced by a lower and less uniform molecular packing of the amorphous regions in LDPE. During the deformation of LDPE, an increase in the τ3 value was observed within the local strains of 0-0.25. This effect was mainly stimulated by a positive relative increase in interlamellar distances due to the deformation of lamellar crystals oriented perpendicular (increased by 31.8%) and parallel (decreased by 10.1%) to the deformation directions. At the same time, the dimension of free-volume pores became more uniform, which was manifested by a decrease in the σ3 value. No significant effect of temperature or strain rate on the τ3 and σ3 values was observed during LDPE deformation. In turn, in the case of HDPE, with an increase in the strain rate/or a decrease in temperature, an intensification of the cavitation phenomenon could be observed with a simultaneous decrease in the τ3 value. This effect was caused by the lack of annihilation of ortho-positonium (o-Ps) along the longer axis of the highly anisotropic/ellipsoidal cavities. Therefore, this dimension was not detectable by the PALS technique. At the same time, the increase in the dimension of the shorter axis of the cavities was effectively limited by the thickness of amorphous layers. As the strain rate increased or the temperature decreased, the σ3 value during HDPE deformation increased. This change was correlated with the initiation and intensification of the cavitation phenomenon. Based on the mechanical response of samples with a similar yield stress, it was also proven that the susceptibility of the amorphous regions of LDPE to the formation of cavities is lower than in the case of amorphous component of HDPE.

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Open Porosity and Pore Size Distribution of Mesoporous Silica Films Investigated by Positron Annihilation Lifetime Spectroscopy and Ellipsometric Porosimetry.

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