A single chamber system for plasma-enhanced chemical vapor deposition was employed to deposit different films of SiOx:N,H with 0.85⩽x⩽1.91, which are studied here by Fourier transform infrared transmission spectroscopy. The sample composition was determined by Rutherford backscattering spectrometry, nuclear reaction, and elastic recoil detection analysis. Moreover, physical properties such as thickness uniformity, deposition rate, density, wet and dry etch rates, and stress are determined. A quantitative study of Si–OH, N–H, and Si–H bonds was performed and interpreted on the basis of the random bonding model; in addition, the presence of NH2, Si–O–Si, H2SiO2, and Si–N groups was detected. The effect of sample annealing at 600 and 900 °C was studied and two species of Si–H bonds were identified, one more stable and the other one easily releasable. A reordering effect of annealing was also detected as a reduction of the amorphous network stress and as the increase of the bond angle in the Si–O–Si groups up to the value typical of thermal SiO2.

This work is devoted to the characterization of the Si:H system obtained by high-fluence, low-energy, hydrogen implantation into single-crystal silicon. The implanted hydrogen profile and the ones resulting after thermal annealing in the range 100–800 °C are detected by secondary-ion mass spectrometry and elastic-recoil detection analysis. The displacement field in the crystal, measured by channeling Rutherford-backscattering spectrometry, is found to depend on the direct radiation damage, the extended defects formed after ion implantation (revealed by transmission electron microscopy), and the implanted species. The contribution to the displacement field due to hydrogen-related defects has a characteristic ‘‘reverse annealing’’ in the range 100–400 °C, essentially due to their formation kinetics.

The depth profile of open volume defects has been measured in Si implanted with He at an energy of 20 keV, by means of a slow-positron beam and the Doppler broadening technique. The evolution of defect distributions has been studied as a function of isochronal annealing in two series of samples implanted at the fluence of $5\times {10}^{15}$ and $2\times {10}^{16}{\mathrm{He}\mathrm{}\mathrm{cm}}^{-2}.$ A fitting procedure has been applied to the experimental data to extract a positron parameter characterizing each open volume defect. The defects have been identified by comparing this parameter with recent theoretical calculations. In as-implanted samples the major part of vacancies and divacancies produced by implantation is passivated by the presence of He. The mean depth of defects as seen by the positron annihilation technique is about five times less than the helium projected range. During the successive isochronal annealing the number of positron traps decreases, then increases and finally, at the highest annealing temperatures, disappears only in the samples implanted at the lowest fluence. A minimum of open volume defects is reached at the annealing temperature of $250°\mathrm{C}$ in both series. The increase of open volume defects at temperatures higher than $250°\mathrm{C}$ is due to the appearance of vacancy clusters of increasing size, with a mean depth distribution that moves towards the He projected range. The appearance of vacancy clusters is strictly related to the out diffusion of He. In the samples implanted at $5\times {10}^{15}{\mathrm{cm}}^{-2}$ the vacancy clusters are mainly four vacancy agglomerates stabilized by He related defects. They disappear starting from an annealing temperature of $700°\mathrm{C}.$ In the samples implanted at $2\times {10}^{16}{\mathrm{cm}}^{-2}$ and annealed at $850–900°\mathrm{C}$ the vacancy clusters disappear and only a distribution of cavities centered around the He projected range remains. The role of vacancies in the formation of He clusters, which evolve in bubble and then in cavities, is discussed.

The interaction of helium atoms with the radiation damage imparted to (100) silicon single crystal by ${\mathrm{He}}^{+}$ implantation at ${\text{5×10}}^{15}\hspace{0.17em}{\mathrm{cm}}^{\text{−2}},$ 20 keV, and liquid–nitrogen temperature is investigated by means of various complementary techniques during and after thermal treatments. Thermal programmed desorption was used to study the dissociation kinetics of helium from the defects and to plan suitable heat treatments for the other techniques. The helium profiles were determined by 8 MeV ${}^{15}{\mathrm{N}}^{\text{2+}}$ elastic recoil detection, quantitative data on damage were obtained by channeling Rutherford backscattering spectrometry, double crystal x-ray diffraction, and positron annihilation spectroscopy. Isothermal treatments at $\text{250\hspace{0.17em}°}\mathrm{C}$ produce first helium redistribution and trapping in vacancy-like defects, rather than helium desorption from traps. The process is thermally activated with an effective activation energy, dispersed in a band from 1.1 to about 1.7 eV. For higher temperature treatments (2 h at $\text{500\hspace{0.17em}°}\mathrm{C})$ the traps are almost emptied and at 700 °C all vacancy-like defects are annealed out. No bubbles or voids are observed by transmission electron microscopy, either in the as-implanted or in annealed samples.

The 3γ annihilation of orthopositronium and the Doppler broadening of the positron annihilation line have been measured by implanting low energy positrons in low dielectric constant (low-k) SiOCH films. The evolution and stability of film porosity with thermal treatments in the 400–900 °C temperature range has been studied. The films have been produced by plasma enhanced chemical vapor deposition and after annealing in N2 atmospheres at 480 °C have been treated in N2+He plasma. The minimum free volume of the pores in the as-produced samples has been estimated to correspond to that of a sphere with radius r=0.6 nm. The treatment in the N2 plasma was found to seal the pores up to 45 nm depth. Both the composition of the films (as obtained by Rutherford backscattering spectroscopy and elastic recoil detection analysis) and the chemical environment of the pores probed by positrons were found to be very stable up to 600 °C thermal treatment. Above such a temperature a reduction of the hydrogen content accompanied by a change in the structure and in the chemical environment of the pores has been observed. In the samples thermal treated at 800–900 °C, the positronium formation is reduced by one-third respect with the as produced sample. In the annealed and as-produced films, a natural aging of 30 days in air was enough to contaminate the porosity, as pointed out by a strong reduction of the 3γ annihilations. The effect of contamination and the distribution of the pores were completely recovered after a thermal treatment at 400 °C. Artificial aging of SiOCH films in controlled atmospheres of H2, O2, H2O has shown that H2O is the more efficient contaminant in reducing the effective volume of the pores.

Thermal desorption measurements are performed on (100)-oriented $p$-type Si wafers implanted with He ions at 20 keV. The doses have been selected in order to produce crystal damage avoiding the formation of detectable bubbles. The He effusion kinetics, studied both in isothermal and in constant heating rate conditions, exhibit effective activation energy heterogeneity indicating the presence of various kinds of traps, precursor of the bubbles. The energy distribution results peaked at about 1.1 eV with an exponential decay towards higher energies and a width of about 0.2 eV. A semiquantitative model, based on the present knowledge about the Si:He system, is proposed, that accounts for He filled nanoblisters formation through interstitial He clustering and precipitation. The observed energy heterogeneity is ascribed to variations of the He solution energy from these cavities due to He-He and He-wall interactions.