Thermal stability and crystallization kinetics of sputtered amorphous Si3N4 films

Schmidt, Harald; Gruber, Wolfgang; Borchardt, Günter; Bruns, Michael; Rudolphi, M.; Baumann, H.

doi:10.1016/j.tsf.2003.11.274

Cited by 43 publications

(27 citation statements)

References 23 publications

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“…No crystallization of silicon nitride is expected at this annealing temperature ͑600°C͒ 22,23 and even in Al/ SiN x :H/ Si structures, interface state density decreases when a RTA is applied to the samples. 24 Anyway, these values are lower than those we obtained in an earlier work 8 where we used a SiO 2 barrier layer instead of SiN x : H. In that case we obtained D it values of about 3 ϫ 10 11 cm −2 eV −1 slightly higher than that obtained here for silicon nitride layers thick enough.…”

Section: -3mentioning

confidence: 85%

Influence of interlayer trapping and detrapping mechanisms on the electrical characterization of hafnium oxide/silicon nitride stacks on silicon

García

Dueñas

Castán

et al. 2008

Journal of Applied Physics

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Al/ HfO 2 / SiN x :H/ n-Si metal-insulator-semiconductor capacitors have been studied by electrical characterization. Films of silicon nitride were directly grown on n-type silicon substrates by electron cyclotron resonance assisted chemical vapor deposition. Silicon nitride thickness was varied from 3 to 6.6 nm. Afterwards, 12 nm thick hafnium oxide films were deposited by the highpressure sputtering approach. Interface quality was determined by using current-voltage, capacitance-voltage, deep-level transient spectroscopy ͑DLTS͒, conductance transients, and flatband voltage transient techniques. Leakage currents followed the Poole-Frenkel emission model in all cases. According to the simultaneous measurement of the high and low frequency capacitance voltage curves, the interface trap density obtained for all the samples is in the 10 11 cm −2 eV −1 range. However, a significant increase in this density of about two orders of magnitude was obtained by DLTS for the thinnest silicon nitride interfacial layers. In this work we probe that this increase is an artifact that must be attributed to traps existing at the HfO 2 / SiN x : H intralayer interface. These traps are more easily charged or discharged as this interface comes near to the substrate, that is, as thinner the SiN x : H interface layer is. The trapping/detrapping mechanism increases the capacitance transient and, in consequence, the DLTS measurements have contributions not only from the insulator/substrate interface but also from the HfO 2 / SiN x : H intralayer interface.

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Section: -3mentioning

confidence: 85%

Influence of interlayer trapping and detrapping mechanisms on the electrical characterization of hafnium oxide/silicon nitride stacks on silicon

García

Dueñas

Castán

et al. 2008

Journal of Applied Physics

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“…The crystallization becomes more pronounced when the annealing is performed at 1000°C, although other diffraction peaks from the ␣-Si 3 N 4 phase were not observed, possibly due to preferential orientation. Si 3 N 4 crystallization induced by annealing has been reported, 11 where the authors showed that the ␤-Si 3 N 4 phase is observed only at higher annealing temperatures and times, namely 1600°C and 8 h, respectively. We attribute the increase in hardness and the decrease of the reduced elastic modulus after annealing at 1000°C observed in Fig.…”

Section: Mechanical and Structural Properties Of Si 3 N 4 Films Amentioning

confidence: 97%

“…[1][2][3]8,9 Silicon nitride is a promising coating candidate for high temperature tools, die coatings, and other engineering components owing to its reasonably high hardness, combined with thermodynamical stability, corrosion resistance, and oxidation resistance at the high temperatures addressed. [10][11][12][13] Since most of the hard coatings investigated so far loose substantially their hardness when submitted to high temperatures, either at work or in laboratory furnace heating, it is very useful to know whether the hardness and elastic modulus of silicon nitride coatings would be retained up to temperatures of practical interest, such as 1000°C. Another aspect of major interest for practical purposes would be the thickness, composition, and adherence of any eventual oxide or oxynitride layer formed due to high temperature processing that can act as a protective and lubricant layer near the silicon nitride film surface.…”

Section: Introductionmentioning

confidence: 99%

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Physicochemical, structural, and mechanical properties of Si3N4 films annealed in O2

Aguzzoli

Marin

Figueroa

et al. 2010

Journal of Applied Physics

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The physicochemical, structural, and mechanical properties of silicon nitride films deposited by radio frequency reactive magnetron sputtering were investigated before and after thermal annealing in 18 O 2 . As-deposited films were essentially amorphous, stoichiometric, and free from contaminants for a wide range of deposition parameters, with hardness figures ranging from 16.5-22 GPa, depending mainly on the deposition temperature. After 18 O 2 annealing at 1000°C, films hardness converged to 21 GPa, independently of the deposition temperature, which is explained based on the crystallization of the films at this annealing temperature. Moreover, oxygen is incorporated only in 7.5 nm of the Si 3 N 4 , forming silicon oxynitride at the top surface of the film, indicating a good oxidation resistance at high temperature. Finally, the elastic strain to failure ͑H 3 / E 2 ͒, which mimics the wear resistance of the film, doubles after the 1000°C annealing. These observations show the great potential of silicon nitride as a hard coating for high temperature applications.

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“…At the same time this compound is metastable with a liability to crystallize during annealing at high temperatures. [16] We used NR on [Si 14 N x /Si 15 N x ] isotope multilayers to determine the first reliable self-diffusivities in a covalently bound amorphous system. [11] The determined nitrogen diffusivities correspond to diffusion lengths between 0.6 and 6 nm.…”

Section: Self-diffusion In Amorphous Sin Xmentioning

confidence: 99%

Neutron Reflectometry: A Tool to Investigate Diffusion Processes in Solids on the Nanometer Scale

et al. 2009

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The investigation of self‐diffusion for the characterization of kinetic process in solids is one of the most fundamental tasks in materials science. We present the method of neutron reflectometry (NR), which allows the detection of extremely short diffusion lengths in the order of 1 nm and below at corresponding low self‐diffusivities between 10−25 and 10−20 m2 s−1. Such a combination of values cannot be achieved by conventional methods of diffusivity determination, like the radiotracer method, secondary ion mass spectrometry, quasielastic neutron scattering, or nuclear magnetic resonance. Using our method, the extensive characterization of materials which are in a non‐equilibrium state, like amorphous or nanocrystalline solids becomes possible. Due to the small experimentally accessible diffusion length microstructural changes (grain growth and crystallization) taking place simultaneously during the actual diffusion experiment can be avoided. For diffusion experiments with NR isotope multilayers are necessary, which are chemical homogeneous but isotope modulated films. We illustrate the basic aspects and potential of this technique using model systems of different classes of materials: single crystalline germanium, amorphous silicon nitride, and nanocrystalline iron.

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Thermal stability and crystallization kinetics of sputtered amorphous Si3N4 films

Cited by 43 publications

References 23 publications

Influence of interlayer trapping and detrapping mechanisms on the electrical characterization of hafnium oxide/silicon nitride stacks on silicon

Influence of interlayer trapping and detrapping mechanisms on the electrical characterization of hafnium oxide/silicon nitride stacks on silicon

Physicochemical, structural, and mechanical properties of Si3N4 films annealed in O2

Neutron Reflectometry: A Tool to Investigate Diffusion Processes in Solids on the Nanometer Scale

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