D. F. Bahr

Non-linear deformation mechanisms during nanoindentation

Abstract Experiments involving the indentation of single crystals of both tungsten and an iron alloy show that the observed yield phenomena can be predicted using a superdislocation model driven by the change in shear stress between the elastically and fully plastic loading conditions. A low density of dislocation multiplication sites is required to support elastic loading which approaches applied shear stresses on the order of the theoretical shear strength of the material. Oxide film thickness and crystal orientation are examined as parameters in controlling the yield phenomena. A model based on activation of dislocation multiplication sources is suggested to explain the initiation of the yield point during indentation and the overall load–depth relationship during indentation.

Yield strength predictions from the plastic zone around nanocontacts

Abstract Using a simplified version of Johnson’s core model analysis of the plastic zone, one may determine the plastic zone size around a contact or, alternatively, determine the yield strength by measuring the plastic zone. The theoretical model contains three parameters: indentation load, yield strength and zone size so that knowing any two gives the third. This is experimentally demonstrated for a series of single crystals (Fe–3wt%Si, tungsten, zinc) and polycrystals (1100-0 Al, copper and 2024-T6 aluminum). In addition, two of these are evaluated in several work-hardened states. Plastic zone sizes are estimated principally by atomic force microscopy and Zygo interferometry imaging with some verification by transmission electron microscopy. On the theoretical side, verification of the relationship is obtained by elastic–plastic numerical analysis of a bi-material system based upon an Fe–3wt%Si single crystal with a thin oxide film. It is shown that in general predictions are reasonable down to nanometer level contacts except for two cases where an indentation size effect may dominate. The proposed relationship is suggested to be an alternative measure of yield strength compared to the often cited value of H /3, particularly at light contacts.

Plastic strain and strain gradients at very small indentation depths

Abstract Plastic strains and their respective strain gradients produced by nanoindentation have been theoretically interpreted and experimentally measured at shallow indentation depths. Existing data for 〈100〉 tungsten with four different conical tip radii varying from 85 to 5000 nm and new data for four conical tips (R=0.5 to 20 μm) into 〈100〉 aluminum are presented. Theoretical results based on geometrically necessary dislocations and semi-empirical experimental continuum calculations are compared for spherical and wedge indenters. For a sharp wedge, both experimental continuum based and theoretical geometrical approaches suggest strain gradient decreasing with the increasing indentation depth, δ. In contrast, theoretical geometrical analysis for a spherical contact yields a depth independent strain gradient proportional to 1/R and continuum calculations suggest a slight increase of a strain gradient proportional to δ1/4/R3/4. Both single crystals exhibit about a factor of two decrease in hardness with increasing depth, irrespective of either increasing or decreasing average strain gradients. Implications to strain gradient plasticity and indentation size effect interpretations at very shallow depths are discussed.

Elastic loading and elastoplastic unloading from nanometer level indentations for modulus determinations

A new method for evaluating modulus and hardness from nanoindentation load/ displacement curves is presented. As a spherical indenter penetrates an elastoplastic half-space, the elastic displacement above the contact line is presumed to diminish in proportion to the total elastic displacement under the indenter. Applying boundary conditions on the elastic and plastic displacements for elastic and rigid plastic contacts leads to an expression that can be best fit to the entire unloading curve to determine E*, the reduced modulus. Justification of the formulation is presented, followed by the results of a preliminary survey conducted on three predominantly isotropic materials: fused quartz, polycrystalline Al, and single crystal W. Diamond tips with radii ranging from 130 nm to 5 μm were used in combination with three different nanoindentation devices. Results indicate that the method gives property values consistent with accepted values for modulus and hardness. The importance of surface roughness and indentation depth are also considered.

Adhesion and acoustic emission analysis of failures in nitride films with a metal interlayer

Abstract Interfacial fracture has been induced between a tantalum nitride film with an aluminum interlayer on a sapphire substrate using nanoindentation. To identify failures for which a model calculation is valid a commercial acoustic emission sensor has been used to study the details of the failure event. The interfacial fracture energy of the system with an aluminum interlayer under the loading conditions at the crack tip is approximately 8 J/m2. Within narrow bounds, this toughness value is reproducible using three different theoretical approaches. The acoustic emission signal is used to determine a lower bound interfacial crack velocity of 5 m/s. The majority of the failure occurs at the aluminum-sapphire interface, suggesting that the fracture energy and crack velocity determined are related to the toughness of this interface and not the nitride-aluminum interface.

THE MECHANICAL BEHAVIOR OF A PASSIVATING SURFACE UNDER POTENTIOSTATIC CONTROL

Continuous microindentation has been carried out on an iron–3% silicon single crystal in 1 M sulfuric acid. The ability of the material to support elastic loading is directly linked to the presence of thermally grown oxide films and passive films applied through potentiostatic control of the sample. When the passive film is removed, either by chemical or electrochemical means, the iron alloy can no longer sustain pressures on the order of the theoretical shear strength of iron. Instead, the metal behaves in a traditional elastic-plastic manner when no film is present. The oxide film at the edges of the indentation can sustain applied tensile stresses up to 1.2 GPa prior to failure. Indentation in materials undergoing dissolution must account for the rate of material removal over the remote surface and the resulting plastic deformation around the contact of the indentation.

Characterization of d.c.jet CVD diamond films on molybdenum

Abstract Diamond films grown using a thermal plasma technique are characterized using a variety of techniques. The relationships between the chemistry, morphology, and mechanical properties are explored using microscopy, Raman spectroscopy, Auger electron spectroscopy, and X-ray photoelectron spectroscopy. The characteristics of films grown using two different nucleation enhancement techniques are shown. Films grown using high methane concentrations at the beginning of growth produce large grained columnar films, whereas films grown on substrates which have been treated with a diamond polishing step show nanocrystalline structures. Variations in sp3 and sp2 bonding and peak shifts are tracked through the thickness of the film, corresponding to variations in the methane concentration during growth. Stresses are measured using peak shifts and beam bending techniques. Adhesion is tested using indentations, and is shown to increase both as growth temperatures and surface roughness increase.

Effect of in and out of plane stresses during indentation of diamond films on metal substrates

Diamond films grown on molybdenum substrates are indented with conical diamond indenters to depths more than 5 times the thickness of the film. This causes delamination and spalling of the film. The effects of variations in indenter angle and film thickness are demonstrated. Using a radius of the delaminated area to the residual contact radius, sharper indenters are shown to cause a 10 to 20% change in that ratio. For films greater than 5 {micro}m thick, there is no apparent film thickness effect. Possibilities for this observation are cracking due to bending stresses or the interfacial crack kinking out of the interface to a reduction in compressive stresses, leading to mixed mode loading. The strain energy release rate of the interface for an 800 nm diamond film on molybdenum is between 2.4 and 7 J/m{sup 2}.

Adhesion evaluation of CVD diamond films and metal reinforced composite diamond films

Poor adhesion of diamond films limits the use of CVD diamond films as coatings for cutting tools. The adhesion of these films is limited by stresses in the film caused by thermal expansion mismatch between the substrate and the film and by voids present at the interface due to the morphology of the crystal growth. A three step process of making diamond composite films has been developed, involving nucleation of individual diamonds on the substrate, electroplating a metal binder in the voids between the crystals, and lastly growing a complete film over the composite layer. The metal binder acts both to fill the voids at the interface and to absorb energy during fracture processes at the interface. Diamond growth was performed in a DC Triple Torch reactor using a mixture of methane and hydrogen with a molybdenum substrate. Measurements to determine the amount of improvement of the film adhesion have been performed. These tests include indentations using conventional hardness testing equipment and four point bend tests with the film in tension and compression. A correlation is shown between the plastic zone of the substrate and the area of the film which delaminated during indentation. Bend tests with the film in tension did not delaminate the film, instead the film underwent intergranular fracture. Bend tests in compression act similarly to pile up around an indentation, and cause film delamination. Residual stress measurements in the single step film show a compressive stress of 650 MPa.