<i>In Situ</i> Monitoring of Atomic Layer Deposition in Nanoporous Thin Films Using Ellipsometric Porosimetry

Dendooven, Jolien; Devloo-Casier, Kilian; Levrau, Elisabeth; Hove, Robbert Van; Sree, Sreeprasanth Pulinthanathu; Baklanov, Mikhaı̈l R.; Martens, Johan A.; Detavernier, Christophe

doi:10.1021/la300045z

Cited by 55 publications

(61 citation statements)

References 50 publications

(97 reference statements)

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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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“…The porous silica film has mesopores of the order of several nanometers. As has already been shown in literature, 21,34,60 these structures can be either conformally coated with ALD or the pores can be sealed. To ensure a large enough penetration depth for the x-rays, and incident angle of 1 was chosen for these experiments, instead of the previously used incident angle of 0.…”

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confidence: 85%

“…Examples are surface photoabsorption, 15,16 FTIR absorption, [17][18][19] spectroscopic ellipsometry, 20 and ellipsometric porosimetry. 21 These optical techniques are the easiest to use in practice, since no measuring equipment needs to be incorporated within the ALD chamber. They can remotely probe the sample surface and only require an entry and exit window to pass light into and out of the reactor chamber.…”

Section: Introductionmentioning

confidence: 99%

In situ synchrotron based x-ray techniques as monitoring tools for atomic layer deposition

Devloo-Casier

Ludwig

Detavernier

et al. 2013

Journal of Vacuum Science &Amp; Technology A: Vacuum, Surfaces, and Films

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Atomic layer deposition (ALD) is a thin film deposition technique that has been studied with a variety of in situ techniques. By exploiting the high photon flux and energy tunability of synchrotron based x-rays, a variety of new in situ techniques become available. X-ray reflectivity, grazing incidence small angle x-ray scattering, x-ray diffraction, x-ray fluorescence, x-ray absorption spectroscopy, and x-ray photoelectron spectroscopy are reviewed as possible in situ techniques during ALD. All these techniques are especially sensitive to changes on the (sub-)nanometer scale, allowing a unique insight into different aspects of the ALD growth mechanisms.

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“…18 The inner chamber configurations of the CCP-RIE and ICP-remote plasma chambers used are as shown in …”

Section: Methodsmentioning

confidence: 99%

Modification of Ultra Low-k Dielectric Films by O₂and CO₂Plasmas

Olawumi

Levrau

Krishtab

et al. 2014

ECS J. Solid State Sci. Technol.

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Low-k materials developed for ULSI interconnects should have sufficient resistance to processing plasma. CO 2 plasma is being considered as a promising candidate for low damage photoresist ash and as a surface activation chemistry for self-assembled monolayers and atomic layer deposition on low-k materials. This article explores the interaction of two organosilicate (OSG) based low-k materials with different k-values (OSG2.4 and OSG2.2) with CO 2 plasma in both CCP and ICP-remote plasma chambers. Time dependent exposure of the materials to CO 2 plasma revealed quick and effective sealing of OSG2.4 surface whereas it takes longer time for OSG2.2. The sealing reduces further plasma damage and leads to accumulation of CO 2 in the pores of both materials. The same behavior occurs in ICP-remote plasma but without a complete sealing of the surface. This suggests the important role of ion bombardment. Damage to low-k by conventional O 2 plasma was studied alongside and it was found that for t < 60 s, O 2 plasma exerts more damage on OSG2.2 than CO 2 . This trend is reversed at t > 60 s. Furthermore, lesser time exposure to CO 2 plasma was investigated with respect to source power at constant pressure and it was discovered that damage although small, increases with varying source power. The performance enhancement of electronic circuits was majorly centered on reducing the transistor sizes, increasing transistor speed and density. However, in advanced technology nodes the performance of the resulting integrated circuits (IC) is greatly hindered by the resistance -capacitance (RC) delay experienced during the signal propagation within the interconnects.1 In order to solve this problem, the traditional Al was replaced by Cu, which has lower resistivity and SiO 2 with k = 4.0 was replaced by low dielectric constants (low-k) materials. Organosilicate glasses (OSG) deposited by Plasma Enhanced Chemical Vapor Deposition (PECVD) and/or by Spin-on Glass technology (SOG) are presently the most popular low-k materials.Photoresist strip using O 2 based plasma is a conventionally used processing technique but this has been found to be severely damaging to porous low-k materials. The modifications to the porous low-k materials lead to increased k-values from densification and hydrophilization.2-5 The CO 2 -based plasma has been reported to be less damaging with respect to the O 2 counterpart. Fuller et al. proposed the use of CO 2 based RIE plasma for photoresist stripping. Ming-Shu Kuo et al. and Hualiang Shi extensively studied the surface modification of ultralow-k materials by CO 2 plasma and the results are published in their PhD dissertations 7,8 and in several papers. 9-13 They reported that i) CO 2 and O 2 plasma damage to ultralow-k films are comparable ii) there is lower atomic oxygen density in CO 2 discharge than O 2 discharge because of higher activation energy (11.5 eV) required to liberate atomic oxygen from CO 2 than from O 2 molecules (6 eV) -this is why there is supposedly a reduction in damage by CO 2 discharge wi...

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In Situ Monitoring of Atomic Layer Deposition in Nanoporous Thin Films Using Ellipsometric Porosimetry

Cited by 55 publications

References 50 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

In situ synchrotron based x-ray techniques as monitoring tools for atomic layer deposition

Modification of Ultra Low-k Dielectric Films by O₂and CO₂Plasmas

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In Situ Monitoring of Atomic Layer Deposition in Nanoporous Thin Films Using Ellipsometric Porosimetry

Cited by 55 publications

References 50 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

In situ synchrotron based x-ray techniques as monitoring tools for atomic layer deposition

Modification of Ultra Low-k Dielectric Films by O2and CO2Plasmas

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Modification of Ultra Low-k Dielectric Films by O₂and CO₂Plasmas