Calculation of Pore Size Distribution in the Ellipsometric Porosimetry: Method and Reliability

1999 ◽  
Vol 565 ◽  
Author(s):  
K. P Mogilnikov ◽  
V. G Polovinkin ◽  
F. N Dultsev ◽  
M. R Baklanov

AbstractEllipsometric porosimetry allows measurement of the pore size distribution in a thin porous film deposited on top of any solid substrate. The most important concept of this technique is the use of in-situ ellipsometry to determine the amount of adsorbate adsorbed/condensed in the film. Changes in refractive index and film thickness are used for calculation of the amount of adsorbate. A room temperature porosimetry based on adsorption of vapours of some organic solvents has been developed. In this paper, a method of calculation of the pore size distribution and reliability of the ELP results is discussed and the validity of the Gurvitsch rule for organic adsorbates (toluene, heptane, CCl4) is examined. Porous silica films on top of Si wafers were used for this analysis.

Materials ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3371
Author(s):  
Bangyun Xiong ◽  
Jingjing Li ◽  
Chunqing He ◽  
Jiale Lai ◽  
Xiangjia Liu ◽  
...  

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.


2000 ◽  
Vol 612 ◽  
Author(s):  
M.R. Baklanov ◽  
K.P. Mogilnikov

AbstractEllipsometric porosimetry (EP) is a simple and effective method for the characterization of the porosity (volume of both open and close pores), average pore size, specific surface area and pore size distribution (PSD) in thin porous films deposited on top of any smooth solid substrat e. Because a laser probe is used, small surface area can be analyzed. Therefore, EP can be used on patterned wafers and it is compatible with microelectronic technology. This method is a new version of adsorption (BET) porosimetry. In situ ellipsometry is used to determine the amount of adsorptive which adsorbed/condensed in the film. Change in refractive index is used to calculate of the quantity of adsorptive present in the film. EP also allows the study of thermal stability, adsorption and swelling properties of low-K dielectric films. Room temperature EP based on the adsorption of vapor of some suitable organic solvents and method of calculation of porosity and PSD is discussed. Examination of the validity of Gurvitsch rule for various organic adsorptives (toluene, heptane, carbon tetrachloride and isopropyl alcohol) has been carried out to assess the reliability of measurements of pore size distribution by the ellipsometric porosimetry.


2016 ◽  
Vol 69 (2) ◽  
pp. 183 ◽  
Author(s):  
Juanrong Chen ◽  
Fengxian Qiu ◽  
Ying Zhang ◽  
Shunsheng Cao

A new trend in supercapacitor research has focussed on the construction of inexpensive electrode materials with high capacitor performances. In this study, we demonstrate the successful preparation of carbon-doped hollow titania spheres. The as-prepared titania spheres not only exhibit an advantage over existing methods because they are created in situ by directly carbonizing cationic polystyrene templates without the addition of carbon precursors, but also feature a narrow pore size distribution and a tuneable shell architecture. When the materials were applied as supercapacitor anodes, the electrochemical results reveal the superior performances of the supercapacitors over that of commercial P25. The higher performances were attributed to carbon doping. Thus, the reported C-doped hollow titania shows more potential as electrode materials for high-performance supercapacitors.


1992 ◽  
Vol 290 ◽  
Author(s):  
J.-P. Korb ◽  
A. Delville ◽  
Shu Xu ◽  
J. Jonas

AbstractThis work shows how the geometrical confinements enhances the nuclear relaxation of a non wetting liquid in a model porous systems. Application of the proposed theory is made to interpret the size and frequency dependences of the 1H relaxation of methylcyclohexane liquid in sol-gel porous silica glasses with narrow pore-size distribution.


2014 ◽  
Vol 118 (16) ◽  
pp. 8474-8480 ◽  
Author(s):  
Hai-Jing Wang ◽  
Alfred Kleinhammes ◽  
Thomas P. McNicholas ◽  
Jie Liu ◽  
Yue Wu

2019 ◽  
Vol 95 ◽  
pp. 363-370 ◽  
Author(s):  
Lenka Novotna ◽  
Lukas Kucera ◽  
Ales Hampl ◽  
Daniel Drdlik ◽  
Jaroslav Cihlar ◽  
...  

2003 ◽  
Vol 766 ◽  
Author(s):  
N. Hata ◽  
C. Negoro ◽  
S. Takada ◽  
K. Yamada ◽  
Y. Oku ◽  
...  

AbstractWe have shown previously the results from out-of-plane and in-plane X-ray scattering /diffraction measurements together with transmission electron microscope and X-ray reflectance measurements and shown that they are effective in characterization of a periodic porous silica low-k film [1]. In the present work, we report the results on pore-size distribution, pore-diameter anisotropy, and size and macroscopic isotropy of domain structure.


1990 ◽  
Vol 180 ◽  
Author(s):  
Douglas M. Smith ◽  
Pamela J. Davis ◽  
C. Jeffrey Brinker

ABSTRACTThe use of NMR relaxation measurements for the in-situ study of pore structure evolution during gel aging and drying is illustrated. The change in the pore size distribution and surface area of both wet and dried gels is examined as a function of aging conditions including temporal aging, thermal aging, changing pH, and changing pore fluid. The effect of pore fluid pH on dissolution/reprecipitation in ordered packings of monodisperse silica spheres is also examined as a model system for particulate gels. As expected, the pore size distribution narrows with increasing time of treatment in high pH pore fluids. Interpretation of high pH results for the wet state is complicated by a microporous layer which forms on colloidal silica resulting in significantly larger wet surface area as compared to the final dried material. Narrowing of the pore size distribution, which is of interest for maximizing drying rates, is maximized in the least time by using either high pH or repeated ethanol washes for the base-catalyzed gel (B2) used.


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