Fracture Properties of LPCVD Silicon Nitride and Thermally Grown Silicon Oxide Thin Films From the Load-Deflection of Long Si3N4 and SiO2/Si3N4 Diaphragms

The bulge test is successfully extended to the determination of the fracture properties of silicon nitride and oxide thin films. This is achieved by using long diaphragms made of silicon nitride single layers and oxide/nitride bilayers, and applying comprehensive mechanical model that describes the mechanical response of the diaphragms under uniform differential pressure. The model is valid for thin films with arbitrary z-dependent plane-strain modulus and prestress, where z denotes the coordinate perpendicular to the diaphragm. It takes into account the bending rigidity and stretching stiffness of the layered materials and the compliance of the supporting edges. This enables the accurate computation of the load-deflection response and stress distribution throughout the composite diaphragm as a function of the load, in particular at the critical pressure leading to the fracture of the diaphragms. The method is applied to diaphragms made of single layers of 300-nm-thick silicon nitride deposited by low-pressure chemical vapor deposition and composite diaphragms of silicon nitride grown on top of thermal silicon oxide films produced by wet thermal oxidation at 950 degrees C and 1050 degrees C with target thicknesses of 500, 750, and 1000 mn. All films characterized have an amorphous structure. Plane-strain moduli E-ps and prestress levels sigma(0) of 304.8 +/- 12.2 GPa and 1132.3 +/- 34.4 MPa, respectively, are extracted for Si3N4, whereas E-ps = 49.1 +/- 7.4 GPa and sigma(0) = -258.6 +/- 23.1 MPa are obtained for SiO2 films. The fracture data are analyzed using the standardized form of the Weibull distribution. The Si3N4 films present relatively high values of maximum stress at fracture and Weibull moduli, i.e., sigma(max) = 7.89 +/- 0.23 GPa and m = 50.0 +/- 3.6, respectively, when compared to the thermal oxides (sigma(max) = 0.89 +/- 0.07 GPa and m = 12.1 +/- 0.5 for 507-nm-thick 950 degrees C layers). A marginal decrease of sigma(max) with thickness is observed for SiO2, with no significant differences between the films grown at 950 degrees C and 1050 degrees C. Weibull moduli of oxide thin films are found to lie between 4.5 +/- 1.2 and 19.8 +/- 4.2, depending on the oxidation temperature and film thickness.

Fracture properties of silicon carbide thin films by bulge test of long rectangular membrane

This paper reports the mechanical properties and fracture behavior of silicon carbide (3C-SiC) thin films grown on silicon substrates. Using bulge testing combined with a refined load-deflection model of long rectangular membranes, which takes into account the bending stiffness and prestress of the membrane material, the Young's modulus, prestress, and fracture strength for the 3C-SiC thin films with thicknesses of 0.40 and 1.42 mu m were extracted. The stress distribution in the membranes under a load was calculated analytically. The prestresses for the two films were 322 +/- 47 and 201 +/- 34 MPa, respectively. The thinner 3C-SiC film with a strong (111) orientation has a plane-gstrain moduli of 415 +/- 61 GPa, whereas the thicker film with a mixture of both (111) and (110) orientations exhibited a plane-strain moduli of 329 +/- 49 GPa. The corresponding fracture strengths for the two kinds of SiC films were 6.49 +/- 0.88 and 3.16 +/- 0.38 GPa, respectively. The reference stresses were computed by integrating the local stress of the membrane at the fracture over edge, surface, and volume of the specimens and were fitted with Weibull distribution function. For the 0.40-mu m-thick membranes, the surface integration has a better agreement between the data and the model, implying that the surface flaws are the dominant fracture origin. For the 1.42-mu m-thick membranes, the surface integration presented only a slightly better fitting quality than the other two, and therefore, it is difficult to rule out unambiguously the effects of the volume and edge flaws.

Bulge testing and fracture properties of plasma-enhanced chemical vapor deposited silicon nitride thin films

The mechanical properties and fracture behavior of silicon nitride (SiNx) thin film fabricated by plasma-enhanced chemical vapor deposition is reported. Plane-strain moduli, prestresses, and fracture strengths of silicon nitride thin film; deposited both oil a bare Si substrate and oil a thermally oxidized Si substrate were extracted using bulge testing combined with a refined load-deflection model of long rectangular membranes. The plane-strain modu i and prestresses of SiNx thin films have little dependence on the substrates, that is, for the bare Si substrate, they are 133 +/- 19 GPa and 178 +/- 22 MPa, respectively, while for the thermally oxidized substrate, they are 140 +/- 26 Gila and 194 +/- 34 MPa, respectively. However, the fracture strength values of SiNx films grown on the two substrates are quite different, i.e., 1.53 +/- 0.33 Gila and 3.08 +/- 0.79 GPa for the bare Si substrate a A the oxidized Si substrate, respectively. The reference stresses were computed by integrating the local stress of the membrane at the fracture over the edge, Surface, and volume of the specimens and fitted with the Weibull distribution function. For SiNx thin film produced oil the bare Si Substrate, the Volume integration gave a significantly better agreement between data and model, implying that the volume flaws re the dominant fracture origin. For SiNx thin film grown on the oxidized Si substrate, the fit quality of surface and edge integration was significantly better than the Volume integration, and the dominant surface and edge flaws could be caused by buffered HF attacking the SiNx layer during SiO2 removal. Crown Copyright (C) 2008 Published by Elsevier B.V. All rights reserved.

Fracture properties of PECVD silicon nitride thin films by long rectangular memrane bulge test

Bulge test combined with a refined load-deflection model for long rectangular membrane was applied to determine the mechanical and fracture properties of PECVD silicon nitride (SiNx) thin films. Plane-strain modulus E-ps prestress s(0), and fracture strength s(max) of SiNx thin films deposited both on bare Si substrate and on SiO2-topped Si substrate were extracted. The SiNx thin films on different substrates possess similar values of E-ps and s(0) but quite different values of s(max). The statistical analysis of fracture strengths were performed by Weibull distribution function and the fracture origins were further predicted.

Fracture properties of silicon carbide thin films charcterized by bulge test of long membranes

The mechanical properties and fracture behavior of silicon carbide (3C-SiC) thin films grown on silicon substrates were characterized using bulge testing combined with a refined load-deflection model for long rectangular membranes. Plane-strain modulus E-ps, prestress so, and fracture strength s(max) for 3C-SiC thin films with thickness of 0.40 mu m and 1.42 mu m were extracted. The E, values of SiC are strongly dependent on grain orientation. The thicker SIC film presents lower so than the thinner film due to stress relaxation. The s(max) values decrease with increasing film thickness. The statistical analysis of the fracture strength data were achieved by Weibull distribution function and the fracture origins were predicted.

Fractals in fracture of bulk metallic glass

We investigate the nanoscale periodic corrugation (NPC) structures on the dynamic fracture surface of a typical tough bulk metallic glass, submitted to high-velocity plate impact and scanned by atomic force microscopy (AFM). The detrended fluctuation analysis (DFA) of the recorded AFM profiles reveals that the valley landscapes of the NPC are nearly memoryless, characterized by Hurst parameter of 0.52 and exhibiting a self-similar fractal character with the dimension of about 1.48. Our findings confirm the existence of the “quasi-cleavage” fracture underpinned by tension transformation zones (TTZs) in metallic glasses.

Interface energy and its influence on interface fracture between metal and ceramic thin films in nanoscale

A theoretical model about the size-dependent interface energy between two thin films with different materials is developed by considering the chemical bonding contribution based on the thermodynamic expressions and the structure strain contribution based on the mechanical characteristics. The interface energy decreases with reducing thickness of thin films, and is determined by such available thermodynamic and mechanical parameters as the melting entropy, the melting enthalpy, the shear modulus of two materials, etc. The predicted interface energies of some metal/MgO and metal/Al2O3 interfaces based on the model are consistent with the results based on the molecular mechanics calculation. Furthermore, the interface fracture properties of Ag/MgO and Ni/Al2O3 based on the atomistic simulation are further compared with each other. The fracture strength and the toughness of the interface with the smaller structure interface energy are both found to be lower. The intrinsic relations among the interface energy, the interface strength, and the fracture toughness are discussed by introducing the related interface potential and the interface stress. The microscopic interface fracture toughness is found to equal the structure interface energy in nanoscale, and the microscopic fracture strength is proportional to the fracture toughness. (C) 2010 American Institute of Physics. [doi:10.1063/1.3501090]

A method to determine fracture toughness using cube-corner indentation

For the cube-corner indenter, an approximate linear relationship between the ratio of hardness (H) to reduced modulus (E-r) and the ratio of unloading work (W-u) to total loading work (W-t) is confirmed by finite-element calculations and by experiments. Based on this relationship a convenient method to determine the fracture toughness (K-IC) of brittle materials, especially for those at small scale, using cube-corner indentations is proposed. Finally, the method is calibrated by indentation experiments on a set of brittle materials. (C) 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Nano-size Effect of Interface Energy and Its Effect on Interface Fracture

An analytical model about size-dependent interface energy of metal/ceramic interfaces in nanoscale is developed by introducing both the chemical energy and the structure stain energy contributions. The dependence of interface energy on the interface thickness is determined by the melting enthalpy, the molar volume, and the shear modulus of two materials composing the interfaces, etc. The analytic prediction of the interface energy and the atomic scale simulation of the interface fracture strength are compared with each other for Ag/MgO and Ni/Al2O3 interfaces, the fracture strength of the interface with the lower chemical interface energy is found to be larger. The potential of Ag/MgO interface related to the interface energy is calculated, and the interface stress and the interface fracture strength are estimated further. The effect of the interface energy on the interface strength and the behind mechanism are discussed.

Fracture behavior of a Zr-metallic glass under dynamic compression

Dynamic planar compressive experiments on a typical tough Zr-BMG (Bulk Metallic Glass) were carried out under impact velocity of 500-600 m/sec and strain rate of 10(6)/s. The fracture surface of samples exhibits different fracture patterns at different parts of the sample. At a corner close to the front loading boundary, fracture patterns from the free edge toward the centre changed from equiaxial veins in microscale to periodic corrugations in nanoscale; in the middle of the sample, the fracture surface contains glazed zones laid out orderly along the same boundary. FEM simulation was performed to investigate the stress distributions in the impacted sample under a short duration impact loading. It has revealed that the fracture patterns changing from the free edge toward the centre were resulted from the fracture modes' changing from the tensile dominant fracture to the shear dominant fracture. Whereas at the middle part of the sample, fracture initiated from several parallel shear bands propagating close to the same boundary is due to a large strain or much higher shear stress in this area.

Fracture of colloidal single-crystal films fabricated by controlled vertical drying deposition

Controlled vertical drying deposition method was used to make high-quality single crystal close-packed colloidal films formed of different radii polystyrene latex spheres on glass substrates coming from a low concentration water suspension (0.1% volume fraction). Regardless of the spheres radii the film thickness was about 6.3 microns. However, cracks destroyed the crystalline film structure during the colloidal film growth. The effect of particle radius (85-215 nm range) on film cracking was systematically studied using in situ optical fracture monitoring. Primary parallel cracks run along the vertical growth direction, later followed by secondary branched cracks in-between the primary cracks due to residual water evaporation. Quantitative theoretical relationship between the cracks spacing and particles radius was derived and shows good agreement with experimental observations. Normalized cracks spacing is related to a reciprocal ratio of the dimensionless particle radius.

Effects of Fracture Seepage on the Stability of Landslide during Reservoir Water Level Fluctuation

The hydraulic conductivity function of fractures is a key scientific question to describe and reveal the process and the role of water seepage reasonably. In this paper, the generation technology of random fracture network and the latest numerical computation method for equivalent permeability tensor of fracture network are applied to analyze the landslide located at Wangjiayuanzi in Wanzhou District of Chongqing by simulating the changes of the seepage field caused by the running of the Three Gorges Reservoir. The influences of the fracture seepage on the seepage field and stability of the landslide were discussed with emphasis. The results show that the fractures existing in the soil increase the permeability coefficient of the landslide body and reduce the delay time of the underground water level in the landslide which fluctuates relative to the water level of reservoir，that causes the safe coefficient of the slope changes more gently than that of the same slope without fractures. It means, if only water level fluctuating condition is concerned, the fractures existing in the soil plays a positive role to the stability of slopes.

Effect of physical aging on fracture behavior of polyphenylquinoxaline films

The influence of physical aging on the tensile fracture behavior of notched Polyphenylquinoxaline (PPQ-E) samples has been studied. The dependence of fracture stress and strain on physical aging has been explained. The glass transition temperature (T-g) and the endothermic peak at the end of T-g transition with different physical aging were characterized using differential scanning calorimetry (DSC) and the results have also been explained. The morphology of fracture surface was observed by scanning electron microscopy (SEM). (C) 2000 John Wiley & Sons, Inc.