Thermal kinetics of free volume in porous spin-on dielectrics: Exploring the network- and pore-properties

Attallah, Ahmed G.; Koehler, N.; Liedke, Maciej Oskar; Butterling, Maik; Hirschmann, Eric; Ecke, Ramona; Schulz, Stefan E.; Wagner, A.

doi:10.1016/j.micromeso.2020.110457

Cited by 6 publications

(18 citation statements)

References 42 publications

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“…In the case of systems with open porosity, the vacuum-annihilation (3γ) probability is relatively high. The value of 3γ to 2γ is also a parameter reflecting the material porosity and the pore size distribution . Analysis of the DB-PAS spectrum allows estimation of the 3γ/2γ o-Ps ratio, pore accessibility, and interconnectivity threshold. , DB-PAS measurements were conducted at the slow positron beamline (SPONSOR) .…”

Section: Ftir Spectroscopymentioning

confidence: 99%

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Modification of Porous Ultralow-k Film by Vacuum Ultraviolet Emission

Zotovich

Zyryanov

Lopaev

et al. 2022

ACS Appl. Electron. Mater.

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Modification of spin-on-deposited porous PMO (periodic mesoporous organosilica) ultralow-k (ULK) SiCOH films (k = 2.33) containing both methyl terminal and methylene bridging groups by vacuum ultraviolet (VUV) emission from Xe plasma is studied. The temporal evolution of chemical composition, internal defects, and morphological properties (pore structure transformation) is studied by using Fourier transform infrared spectroscopy, in situ laser ellipsometry, spectroscopic ellipsometry, ellipsometric porosimetry (EP), positron-annihilation lifetime spectroscopy (PALS), and Doppler broadening positron-annihilation spectroscopy. Application of the different advanced diagnostics allows making conclusions on the dynamics of the chemical composition and pore structure. The time frame of the VUV exposure in the current investigation can be divided into two phases. During the first short phase, film loses almost all of its surface methyl and matrix bridging groups. An increase of material porosity due to removal of methyl groups with simultaneous matrix shrinkage is found by in situ ellipsometry. The removal of bridging bonds leads to an increase of matrix intrinsic porosity. Nevertheless, when the treated material is exposed to the ambient air, the sizes of micro- and mesopores and pores interconnectivity decrease with the VUV exposure time according to PAS and EP data. The last is the result of the additional film shrinkage caused by atmosphere exposure. During the second phase the increase of mesopore size is detected by both EP and PAS. The increase of mesopore size goes all the time as it is expected from in situ ellipsometry, but it is masked by the air exposure.

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Section: Ftir Spectroscopymentioning

confidence: 99%

“…The value of 3γ to 2γ is also a parameter reflecting the material porosity and the pore size distribution. 68 Analysis of the DB-PAS spectrum allows estimation of the 3γ/2γ o-Ps ratio, pore accessibility, and interconnectivity threshold. 69,70 DB-PAS measurements were conducted at the slow positron beamline (SPONSOR).…”

Section: A4 Db-pasmentioning

confidence: 99%

Modification of Porous Ultralow-k Film by Vacuum Ultraviolet Emission

Zotovich

Zyryanov

Lopaev

et al. 2022

ACS Appl. Electron. Mater.

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“…are used to eventually cause the porogen to evaporate 19 . These porogen removal methods are notorious for producing interconnected pores, which may extend towards the film surface 20 . For example, the relatively low ramping rates of ~ 10 K/min 20 , 21 during thermal curing at 400–450 °C allows for agglomerating the porogen, whereby interconnected and open-to-surface pores are developed 20 .…”

Section: Introductionmentioning

confidence: 99%

“…These porogen removal methods are notorious for producing interconnected pores, which may extend towards the film surface 20 . For example, the relatively low ramping rates of ~ 10 K/min 20 , 21 during thermal curing at 400–450 °C allows for agglomerating the porogen, whereby interconnected and open-to-surface pores are developed 20 . Similarly, plasma- and UV–thermal assisted methods, despite their short curing time (~ few minutes) 22 and reduced thermal budget 23 , leave interconnected pores 24 , which often limits the versatility of these approaches.…”

Section: Introductionmentioning

confidence: 99%

Millisecond flash lamp curing for porosity generation in thin films

Attallah,

Prucnal,

Buttering

et al. 2023

Sci Rep

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Flash lamp annealing (FLA) with millisecond pulse durations is reported as a novel curing method for pore precursor's degradation in thin films. A case study on the curing of dielectric thin films is presented. FLA-cured films are being investigated by means of positron annihilation spectroscopy (PAS) and Fourier-transform infrared (FTIR) spectroscopy in order to quantify the nm-scale porosity and post-treatment chemistry, respectively. Results from positron annihilation reveal the onset of the formation of porous voids inside the samples at 6 ms flash treatment time. Moreover, parameter's adjustment (flash duration and energy density) allows for identifying the optimum conditions of effective curing. Within such a systematic investigation, positron results indicate that FLA is able to decompose the porogen (pore precursors) and to generate interconnected (open porosity) or isolated pore networks with self-sealed pores in a controllable way. Furthermore, FTIR results demonstrate the structural evolution after FLA, that help for setting the optimal annealing conditions whereby only a residual amount of porogen remains and at the same time a well-densified matrix, and a hydrophobic porous structures are created. Raman spectroscopy suggests that the curing-induced self-sealing layer developed at the film surface is a graphene oxide-like layer, which could serve as the outside sealing of the pore network from intrusions.

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“…Positron annihilation spectroscopy (PAS) is an advanced characterization technique widely used in metals and metallic alloys [9], semiconductors [10], polymers [11], or dielectrics [12], and in many applications such as solar cells [13], photonics [14], or electronic materials [15] among others, PAS allows to obtain information about the lattice defects (from single vacancies to vacancy clusters) as they act as traps for thermalized positrons. Positron lifetime spectroscopy (PLS) provides information about the size and abundance of these types of defects providing longer lifetime components as the size of the defect grows.…”

Section: Introductionmentioning

confidence: 99%

Positron lifetime spectroscopy applied to pure Tellurium

Domínguez‐Reyes

2021

Indian J Phys

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High-purity crystalline Tellurium has been investigated using positron lifetime spectroscopy technique in order to determine basic information missing in the current experimental knowledge of the positron annihilation spectroscopy field. Three different pairs of samples have been studied in the as-received state and, in order to eliminate the vacancy-type defects, after consecutive isothermal treatments at 300 °C. Lifetime corresponding to the annihilation in the Tellurium bulk has been determined as 282(1) ps. Previous theoretical calculations present in the bibliography that used different methods and parameterization provided a wide range of values for the annihilation lifetime of the positron in the bulk of Tellurium. The obtained result has been used to identify the most accurate results among them.

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Thermal kinetics of free volume in porous spin-on dielectrics: Exploring the network- and pore-properties

Cited by 6 publications

References 42 publications

Modification of Porous Ultralow-k Film by Vacuum Ultraviolet Emission

Modification of Porous Ultralow-k Film by Vacuum Ultraviolet Emission

Millisecond flash lamp curing for porosity generation in thin films

Positron lifetime spectroscopy applied to pure Tellurium

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