We report a study of the oxidation of TiN. In previous work, the oxidation kinetics for 350–450 °C were reported and an initiation time prior to fast oxidation was identified. In this study, x‐ray photoelectron spectroscopy was used to investigate the oxidation mechanisms at 350 °C during this initiation time period. The oxide thickness increases slowly with oxidation time and the film appears to change from an amorphous TiO2 layer to a crystalline TiO2 layer. Spectral features which are intermediate between TiO2 and TiN are reported and a model involving grain boundary oxidation is proposed. One of the thicker oxides studied was annealed in vacuum to 700 °C. Following oxidation, some of the capping oxide and much of the intermediate material is no longer in the analysis volume and we suggest that the oxygen and nitrogen is being dissolved into the bulk in much the same way that nonevaporable getters are activated before use.

Titanium nitride oxidation chemistry: An x‐ray photoelectron spectroscopy study

Thermal stability of nitride thin films

The surface oxidized layer of a TiN barrier metal thin film grown on a Pt electrode was used as a resistive switching material. The fabricated memory cell shows bipolar resistive switching on a nanosecond order. A TiO2 anatase layer of about 2.5nm thick on TiN thin film was characterized by high-resolution scanning transmission electron microscopy. The results suggested that the high-speed resistive change was derived from the Mott transition in the TiO2 anatase nanolayer, and the obtained results could relate to the formation of filament paths previously reported in binary transition metal oxide thin films exhibiting resistive switching.

TiO2 anatase nanolayer on TiN thin film exhibiting high-speed bipolar resistive switching

Low-temperature deposition of TiN by reactive evaporation or sputter deposition onto amorphous substrates leads to highly underdense layers which develop mixed 111/002 orientations through competitive growth. In contrast, we demonstrate here the growth of low-temperature (450 °C) fully dense polycrystalline TiN layers with complete 111 texture. This was achieved by reactive magnetron sputter deposition using a combination of: (1) highly oriented 25-nm-thick 0002 Ti underlayers to provide 111 TiN orientation through texture inheritance (local epitaxy) and (2) high flux (JN2+/JTi=14), low-energy (EN2+≃20 eV), N2+ ion irradiation in a magnetically unbalanced mode to provide enhanced adatom diffusion leading to densification during TiN deposition. The Ti underlayers were also grown in a magnetically unbalanced mode, in this case with an incident Ar+/Ti flux ratio of 2 and EAr+≃11 eV. All TiN films were slightly overstoichiometric with a N/Ti ratio of 1.02±0.03. In order to assess the diffusion-barrier propert...

Dense fully 111-textured TiN diffusion barriers: Enhanced lifetime through microstructure control during layer growth

The oxidation of TiN in room air and in dry O2 at various partial pressures at temperatures of 350, 400, and 450 °C has been studied using ellipsometry, Auger electron spectroscopy, Rutherford backscattering spectrometry, and x‐ray photoelectron spectroscopy. The film that forms is TiO2 and the oxidation kinetics are quadratic for both room air and dry O2. An initiation time prior to the quadratic growth is observed that is a function of the oxidation temperature, with longer times required for lower temperature. The partial pressure affects the growth as the cube root of the concentration of O2.

Oxidation of titanium nitride in room air and in dry O2

The usefulness of reactively sputtered TiN as a diffusion barrier in the AlTiN/Ti/Si metallization scheme in very large scale integration was reported in a previous publication. Two types of TiN thin films were studied in these experiments. Depending on the applied substrate bias voltage, the resulting TiN films can have different properties. Under no‐bias conditions, dark brown colored films (called B films) with low density (3.22 g/cm3), high electrical resistivity (∼400 μΩ cm), and 5%–8% O2 are obtained. A+ ‐75 V dc substrate bias, bright golden colored films (called G films) with high density (∼5.0 g/cm3), low resistivity (∼20 μΩ cm), and negligible O2 are obtained. Even though the B films contain more O2, the G films were found to be better diffusion barriers for silicon. To investigate the effect of film microstructure on the diffusion barriers, cross‐sectional and planar transmission electron microscopy samples were used. Both, brown and golden, types of films have columnar grain structure with app...

Transmission electron microscopy studies of brown and golden titanium nitride thin films as diffusion barriers in very large scale integrated circuits

Growth and properties of TiN and TiOxNy diffusion barriers in silicon on sapphire integrated circuits

Polycrystalline thin films of titanium nitride with a resistivity in the range 20–25 μΩ cm have been consistently produced on water‐cooled silicon wafers by using reactive sputtering of a titanium target in Ar/N2 mixture. The variations of resistivity and the deposition rate as the functions of N2 partial pressure and applied substrate bias voltage are investigated. The N2 partial pressure as a function of nitrogen flow rate is plotted for various radio frequency (rf) power levels. The TiN films have been characterized by a wide variety of analytical techniques, such as Rutherford backscattering (RBS), Auger electron spectroscopy (AES), x‐ray diffraction (XRD), scanning electron microscopy (SEM), and four‐point probe. These films are golden yellow in color. RBS shows these films to be stoichiometric and AES shows them to be free of any measurable oxygen. Two multilayer metallization systems (Si/TiN/Al and Si/Ti/TiN/Al) were built to test the effectiveness of these films as a diffusion barrier. Preliminary...

Growth and properties of radio frequency reactively sputtered titanium nitride thin films

Failure mechanisms of TiN thin film diffusion barriers

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Transmission electron microscopy studies of brown and golden titanium nitride thin films as diffusion barriers in very large scale integrated circuits

Growth and properties of TiN and TiOxNy diffusion barriers in silicon on sapphire integrated circuits

Growth and properties of radio frequency reactively sputtered titanium nitride thin films

Failure mechanisms of TiN thin film diffusion barriers