Determination of pore size distribution in thin films by ellipsometric porosimetry

Baklanov, Mikhaı̈l R.; Mogilnikov, K. P.; Polovinkin, V. G.; Dultsev, F. N.

doi:10.1116/1.591390

Cited by 511 publications

(486 citation statements)

References 8 publications

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“…In the EP experiment, the ellipsometric angles Ψ and Δ were recorded over the spectral range of 245-1000 nm during adsorption and desorption of toluene in and out of the porous film. The sorption isotherm was derived from the ellipsometric data according to a published method 15,30 and revealed an accessible porosity of ca. 15% (Fig.…”

Section: Resultsmentioning

confidence: 99%

Atomic layer deposition-based tuning of the pore size in mesoporous thin films studied by in situ grazing incidence small angle X-ray scattering

et al. 2014

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Atomic layer deposition (ALD) enables the conformal coating of porous materials, making the technique suitable for pore size tuning at the atomic level, e.g., for applications in catalysis, gas separation and sensing. It is, however, not straightforward to obtain information about the conformality of ALD coatings deposited in pores with diameters in the low mesoporous regime (<10 nm). In this work, it is demonstrated that in situ synchrotron based grazing incidence small angle X-ray scattering (GISAXS) can provide valuable information on the change in density and internal surface area during ALD of TiO 2 in a porous titania film with small mesopores (3-8 nm). The results are shown to be in good agreement with in situ X-ray fluorescence data representing the evolution of the amount of Ti atoms deposited in the porous film. Analysis of both datasets indicates that the minimum pore diameter that can be achieved by ALD is determined by the size of the Ti-precursor molecule.

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Section: Resultsmentioning

confidence: 99%

Atomic layer deposition-based tuning of the pore size in mesoporous thin films studied by in situ grazing incidence small angle X-ray scattering

et al. 2014

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“…A similar technique based on the ellipsometric analysis of the thin films as a function of the relative humidity has been reported for other types of transparent thin films. [26][27][28][29][30] The procedure utilized here is more general and could also be used for thin films prepared by sol-gel ͑e.g., mesoporous films 31 ͒ where the existence of a general procedure for determination of porosity is a clear need.…”

Section: Introductionmentioning

confidence: 99%

Relationship between scaling behavior and porosity of plasma-depositedTiO2thin films

et al. 2007

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The growth of TiO 2 thin films prepared by plasma enhanced chemical vapor deposition has been studied by analyzing their roughness with the concepts of the dynamic scaling theory. Differences in the growth and roughness exponents have been found depending on the composition of the plasma by using either O 2 or mixtures Ar+ O 2 as plasma gas and titanium isopropoxide as the precursor. The slope of the representations of the film roughness against the deposition time yielded values of the exponent ␤ of 0.45 and 0.32 for, respectively, thin films prepared with plasmas of O 2 or mixtures Ar+ O 2 . Meanwhile, values of the exponent ␣ of 1.15 and 1.89/0.35 were deduced from the power spectral density representations for the films prepared under these two experimental conditions. These values are congruent with growth processes dominated, respectively, by shadowing or diffusion processes. A columnar microstructure was observed by scanning electron microscopy for the thin films prepared with pure oxygen. Meanwhile, homogeneous films were obtained with mixtures of Ar+ O 2 . The open porosity of the films was determined by measuring water adsorption-desorption isotherms with a quartz crystal monitor. This analysis showed that in the samples prepared with mixtures of Ar+ O 2 the porosity consisted exclusively of micropores ͑d Ͻ 2 nm͒, while in the films prepared with an oxygen plasma there were micro-and meso-pores ͑d Ͼ 2 nm͒. It is concluded that the different growth mechanisms found by just changing the chemistry of the plasma are responsible for the quite distinct microstructures, porosities, and optical properties obtained for the films.

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“…11 If the film is not swollen by toluene, then the electron density determined from the critical edges of the dry and the toluene-infiltrated films can be used to calculate the mass uptake of toluene. By further assuming the density of the toluene is the same as the bulk, as is the practice of other thin-film measurements, 8 the total open pore-volume fraction and the average mass density of the wall and closed pores can be calculated. If the density of toluene in confined, small pores is higher than bulk toluene, this will slightly underestimate the pore volume.…”

Section: Resultsmentioning

confidence: 99%

“…8 EP is similar to N 2 adsorption in that the sample is exposed to a gaseous adsorbate or probe molecule. As the partial pressure increases, the gas condenses into increasingly larger pores via capillary condensation.…”

Section: Introductionmentioning

confidence: 99%

Pore size distributions in low‐k dielectric thin films from X‐ray porosimetry

Lee

Soles

Liu

et al. 2002

J Polym Sci B Polym Phys

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X-ray reflectivity has been used to determine the mass uptake of probe molecules in porous thin films supported on thick silicon wafers. The adsorption occurs by capillary condensation when the films are exposed to probe vapor at controlled partial vapor pressures. The probe solvent partial pressure was varied by mixing saturated air and dry air at constant temperature or by changing sample temperature at a constant vapor concentration. Pore size distribution in the films can be calculated from the probe uptake with typical porosimetric approaches such as the application of the Kelvin equation to convert partial pressure into pore size. For illustration, the pore size distribution of three different nanoporous thin films, the primary candidate of ultra-low-k interlevel dielectrics in the next generation of integrated circuit chips, was determined with this technique. These samples represent different generations of low-k dielectrics developed by industry.

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Determination of pore size distribution in thin films by ellipsometric porosimetry

Cited by 511 publications

References 8 publications

Atomic layer deposition-based tuning of the pore size in mesoporous thin films studied by in situ grazing incidence small angle X-ray scattering

Atomic layer deposition-based tuning of the pore size in mesoporous thin films studied by in situ grazing incidence small angle X-ray scattering

Relationship between scaling behavior and porosity of plasma-depositedTiO2thin films

Pore size distributions in low‐k dielectric thin films from X‐ray porosimetry

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