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Institute
In this thesis the detailed investigations concerning processing and stability of thin films including carbon species and their possible application as materials of a low dielectric constant (low k) are presented. In order to gather a complex information regarding the chemical, morphological and dielectric properties of the produced layer a combination of the spectroscopy: X-ray photoelectron spectroscopy (XPS), near edge X-ray absorption fine structure spectroscopy (NEXAFS) and Fourier transform infrared spectroscopy (FTIR), microscopy: atomic force microscopy (AFM) and electrical characterization: capacitance-voltage technique (CV) have been applied.
The films deposited by means of variety of techniques have been described, ranging from evaporation, through spraying and dropping to spin-coating. Regarding the possible low-k application, a considerable attention has been paid to the hybrid organic-inorganic 3-aminopropyl-trimethoxysilane (APTMS) based composite materials enriched with carbon species coming from the following dopants: C60 fullerenes, [6,6]-phenyl-C61-butyric acid (PCBM), copper phthalocyanine (CuPc), and tris(dimethylvinylsilyloxy)-POSS (POSS).
In the following thesis progressive steps leading to gradual decreasing of the resulting permittivity of the hybrid material is presented. As revealed by the performed investigations, the replacement of C60 within the APTMS based matrix by its better soluble derivative PCBM allows the increase of the concentration of the carbon species within the composite films. The introduction of POSS as an additional dopant gave the opportunity of increasing the resistance of the produced material against the ambient influence. With the excess of the POSS concentration an original fractal-shaped cluster formation has been observed. Finally, the dispersion of the properly chosen low concentration of CuPc and POSS molecules within the APTMS based matrix led to the fabrication of homogenous layer with an ultra-low dielectric constant of 1.8.
Spectroscopic investigations of interaction between C60 fullerene and nitrogen atom from amine group
(2010)
We investigated interactions between fullerene molecule and amine group from 3-aminopropyl-trimethoxysilane (3AT). Theoretical calculations show that the material obtained as a result of interactions between 3AT and C60 fullerene may have extremely low dielectric constant around 1.6, so it could be considered as a candidate for ultra low-k (ULK) material applications. We prepared films composed of 3AT and fullerene by using two preparation techniques: spin-coating and evaporation. Interactions between these two components were investigated by using X- ray photoelectron spectroscopy (XPS) and Near Edge X-ray Absorption Fine Structure Spectroscopy (NEXAFS). We found that there are strong chemical reactions between the nucleophilic nitrogen atom from 3AT and electrophilic fullerene molecule. Results of NEXAFS measurements suggest that due to direct interactions between 3AT and C60 the shape of fullerene molecule is changed.
In this study we produced 3-aminopropyltrimethoxysilane based hybrid nanocomposites using fullerene derivative [6,6]–phenyl–C61–butyric acid methyl ester (PCBM) as nanodopants. Additionally,
we modified obtained material with incompletely condensed cage polyhedral oligomeric silsesqiuox-anes (POSS) in order to improve its properties. Thin films were deposited by means of the spin-coating method. The films were characterized by atomic force microscopy (AFM), X-ray photoelectron
spectroscopy (XPS) and capacitance–voltage (CV) measurements. We observed that a properly chosen
PCBM concentration may be a crucial factor to obtain high quality APTMS based films by the spin-coating technique. XPS revealed the presence of the C-NH-C species within POSS containing films
indicating chemical interaction between the amino group of APTMS and the POSS molecules. AFM results suggest that at high POSS monomer concentration in the range of 1% the creation of fractal-shaped aggregates takes place. The CV characterization of the samples exhibits a decrease of the APTMS based films dielectric constant due to the POSS and PCBM contribution. The combination of the applied methods delivers complementary information concerning the properties of the analyzed films.
The C60 fullerenes and some of its -OH, -CF3 and -Cl derivates are candidates for application as ultra-low-k insulators in the semiconductor industry. Future preparation of thin films based on these materials requires the stability of the substituted fullerenes against chemical handling and processing steps. The latter issue was addressed by our NEXAFS studies that were done by synchrotron radiation at the beam line U49/2-PGM2 at BESSY II. Performed were the C K-edge NEXAFS studies in total fluorescence and total electron yield modes. The C60 based films were deposited on silicon by spraying from solutions. The influence of the different substitutional groups with C60 molecules was studied. The data were compared to the reference spectra of a pure C60 film. For C60(OH)24, C60-Cl2 and C60(CF3)12 a variance of the intensity of the π*-resonance as well as shift to higher energies of 0.5 eV (-OH), 0.6 eV (-F), 0.7 eV (-Cl) were observed. The results confirm the necessary stability of the used C60 derivatives and shall be used for optimization of the film deposition chemistry and conditions.