William D. Nix

Indentation size effects in crystalline materials: A law for strain gradient plasticity

Abstract We show that the indentation size effect for crystalline materials can be accurately modeled using the concept of geometrically necessary dislocations. The model leads to the following characteristic form for the depth dependence of the hardness: H H 0 1+ h ∗ h where H is the hardness for a given depth of indentation, h, H0 is the hardness in the limit of infinite depth and h ∗ is a characteristic length that depends on the shape of the indenter, the shear modulus and H0. Indentation experiments on annealed (111) copper single crystals and cold worked polycrystalline copper show that this relation is well-obeyed. We also show that this relation describes the indentation size effect observed for single crystals of silver. We use this model to derive the following law for strain gradient plasticity: ( σ σ 0 ) 2 = 1 + l χ , where σ is the effective flow stress in the presence of a gradient, σ0 is the flow stress in the absence of a gradient, χ is the effective strain gradient and l a characteristic material length scale, which is, in turn, related to the flow stress of the material in the absence of a strain gradient, l ≈ b( μ σ 0 ) 2 . For materials characterized by the power law σ 0 = σ ref e 1 n , the above law can be recast in a form with a strain-independent material length scale l. ( builtσ σ ref ) 2 = e 2 n + l χ l = b( μ σ ref ) 2 = l ( σ 0 σ ref ) 2 . This law resembles the phenomenological law developed by Fleck and Hutchinson, with their phenomenological length scale interpreted in terms of measurable material parametersbl].

A method for interpreting the data from depth-sensing indentation instruments

Depth-sensing indentation instruments provide a means for studying the elastic and plastic properties of thin films. A method for obtaining hardness and Youngs modulus from the data obtained from these types of instruments is described. Elastic displacements are determined from the data obtained during unloading of the indentation. Youngs modulus can be calculated from these measurements. In addition, the elastic contribution to the total displacement can be removed in order to calculate hardness. Determination of the exact shape of the indenter at the tip is critical to the measurement of both hardness and elastic modulus for indentation depths less than a micron. Hardness is shown to depend on strain rate, especially when the hardness values are calculated from the data along the loading curves.

Mechanical properties of thin films

The mechanical properties of thin films on substrates are described and studied. It is shown that very large stresses may be present in the thin films that comprise integrated circuits and magnetic disks and that these stresses can cause deformation and fracture to occur. It is argued that the approaches that have proven useful in the study of bulk structural materials can be used to understand the mechanical behavior of thin film materials. Understanding the mechanical properties of thin films on substrates requires an understanding of the stresses in thin film structures as well as a knowledge of the mechanisms by which thin films deform. The fundamentals of these processes are reviewed. For a crystalline film on a nondeformable substrate, a key problem involves the movement of dislocations in the film. An analysis of this problem provides insight into both the formation of misfit dislocations in epitaxial thin films and the high strengths of thin metal films on substrates. It is demonstrated that the kinetics of dislocation motion at high temperatures are expecially important to the understanding of the formation of misfit dislocations in heteroepitaxial structures. The experimental study of mechanical properties of thin films requires the development and use of nontraditional mechanical testing techniques. Some of the techniques that have been developed recently are described. The measurement of substrate curvature by laser scanning is shown to be an effective way of measuring the biaxial stresses in thin films and studying the biaxial deformation properties at elevated temperatures. Submicron indentation testing techniques, which make use of the Nanoindenter, are also reviewed. The mechanical properties that can be studied using this instrument are described, including hardness, elastic modulus, and time-dependent deformation properties. Finally, a new testing technique involving the deflection of microbeam samples of thin film materials made by integrated circuit manufacturing methods is described. It is shown that both elastic and plastic properties of thin film materials can be measured using this technique.

Mechanism-based strain gradient plasticity : I. Theory

Abstract A mechanism-based theory of strain gradient plasticity (MSG) is proposed based on a multiscale framework linking the microscale notion of statistically stored and geometrically necessary dislocations to the mesoscale notion of plastic strain and strain gradient. This theory is motivated by our recent analysis of indentation experiments which strongly suggest a linear dependence of the square of plastic flow stress on strain gradient. While such linear dependence is predicted by the Taylor hardening model relating the flow stress to dislocation density, existing theories of strain gradient plasticity have failed to explain such behavior. We believe that a mesoscale theory of plasticity should not only be based on stress–strain behavior obtained from macroscopic mechanical tests, but should also draw information from micromechanical, gradient-dominant tests such as micro-indentation or nano-indentation. According to this viewpoint, we explore an alternative formulation of strain gradient plasticity in which the Taylor model is adopted as a founding principle. We distinguish the microscale at which dislocation interaction is considered from the mesoscale at which the plasticity theory is formulated. On the microscale, we assume that higher order stresses do not exist, that the square of flow stress increases linearly with the density of geometrically necessary dislocations, strictly following the Taylor model, and that the plastic flow retains the associative structure of conventional plasticity. On the mesoscale, the constitutive equations are constructed by averaging microscale plasticity laws over a representative cell. An expression for the effective strain gradient is obtained by considering models of geometrically necessary dislocations associated with bending, torsion and 2-D axisymmetric void growth. The new theory differs from all existing phenomenological theories in its mechanism-based guiding principles, although the mathematical structure is quite similar to the theory proposed by Fleck and Hutchinson. A detailed analysis of the new theory is presented in Part II of this paper.

Effects of the substrate on the determination of thin film mechanical properties by nanoindentation

We examine the effects of the substrate on the determination of mechanical properties of thin films by nanoindentation. The properties of aluminum and tungsten films on the following substrates have been studied: aluminum, glass, silicon and sapphire. By studying both soft films on hard substrates and hard films on soft substrates we are able to assess the effects of elastic and plastic inhomogeneity, as well as material pile-up, on the nanoindentation response. The data set includes Al/glass and W/sapphire, with the film and substrate having nearly the same elastic properties. These systems permit the true contact area and true hardness of the film to be determined from the measured contact stiffness, irrespective of the effects of pile-up or sink-in. Knowledge of the true hardness of the film permits a study of the effects of the elastic modulus mismatch on the nanoindentation properties, using the measured contact stiffness as a function of depth of indentation.

Interconnected silicon hollow nanospheres for lithium-ion battery anodes with long cycle life.

Silicon is a promising candidate for the anode material in lithium-ion batteries due to its high theoretical specific capacity. However, volume changes during cycling cause pulverization and capacity fade, and improving cycle life is a major research challenge. Here, we report a novel interconnected Si hollow nanosphere electrode that is capable of accommodating large volume changes without pulverization during cycling. We achieved the high initial discharge capacity of 2725 mAh g(-1) with less than 8% capacity degradation every hundred cycles for 700 total cycles. Si hollow sphere electrodes also show a Coulombic efficiency of 99.5% in later cycles. Superior rate capability is demonstrated and attributed to fast lithium diffusion in the interconnected Si hollow structure.

What is the Young's Modulus of Silicon?

The Youngs modulus (E) of a material is a key parameter for mechanical engineering design. Silicon, the most common single material used in microelectromechanical systems (MEMS), is an anisotropic crystalline material whose material properties depend on orientation relative to the crystal lattice. This fact means that the correct value of E for analyzing two different designs in silicon may differ by up to 45%. However, perhaps, because of the perceived complexity of the subject, many researchers oversimplify silicon elastic behavior and use inaccurate values for design and analysis. This paper presents the best known elasticity data for silicon, both in depth and in a summary form, so that it may be readily accessible to MEMS designers.

Determination of indenter tip geometry and indentation contact area for depth-sensing indentation experiments

The phenomena of pile-up and sink-in associated with nanoindentation have been found to have large effects on the measurements of the indentation modulus and hardness of copper. Pile-up (or sink-in) leads to contact areas that are greater than (or less than) the cross-sectional area of the indenter at a given depth. These effects lead to errors in the absolute measurement of mechanical properties by nanoindentation. To account for these effects, a new method of indenter tip shape calibration has been developed; it is based on measurements of contact compliance as well as direct SEM observations and measurements of the areas of large indentations. Application of this calibration technique to strain-hardened (pile-up) and annealed (sink-in) copper leads to a unique tip shape calibration for the diamond indenter itself, as well as to a material parameter, a, which characterizes the extent of pile-up or sink-in. Thus the shape of the indenter tip and nature of the material response are separated in this calibration method. Using this approach, it is possible to make accurate absolute measurements of hardness and indentation modulus by nanoindentation.

A new bulge test technique for the determination of Young's modulus and Poisson's ratio of thin films

A new analysis of the deflection of square and rectangular membranes of varying aspect ratio under the influence of a uniform pressure is presented. The influence of residual stresses on the deflection of membranes is examined. Expressions have been developed that allow one to measure residual stresses and Youngs moduli. By testing both square and rectangular membranes of the same film, it is possible to determine Poissons ratio of the film. Using standard micromachining techniques, free-standing films of LPCVD silicon nitride were fabricated and tested as a model system. The deflection of the silicon nitride films as a function of film aspect ratio is very well predicted by the new analysis. Youngs modulus of the silicon nitride films is 222 ± 3 GPa and Poissons ratio is 0.28 ± 0.05. The residual stress varies between 120 and 150 MPa. Youngs modulus and hardness of the films were also measured by means of nanoindentation, yielding values of 216 ± 10 GPa and 21.0 ± 0.9 GPa, respectively.

Measurement and Interpretation of stress in aluminum-based metallization as a function of thermal history

Mechanical stress in interconnections is a problem of growing importance in VLSI devices. The origins of this stress are discussed, and a measurement technique based on the determination of wafer curvature with a laser scanning device is described. The changes in stress observed during thermal cycles are interpreted quantitatively in terms of a simple model of elastic and plastic strain in the metal. The effects of changes in deposition conditions, film composition, and film structure are discussed.