Showing papers in "Journal of Materials Research in 2002"

Paradox of strength and ductility in metals processed by severe plastic deformation

Abstract: It is well known that plastic deformation induced by conventional forming methodssuch as rolling, drawing or extrusion can significantly increase the strength of metalsHowever, this increase is usually accompanied by a loss of ductility. For example, Fig.1 shows that with increasing plastic deformation, the yield strength of Cu and Almonotonically increases while their elongation to failure (ductility) decreases. Thesame trend is also true for other metals and alloys. Here we report an extraordinarycombination of high strength and high ductility produced in metals subject to severeplastic deformation (SPD). We believe that this unusual mechanical behavior is causedby the unique nanostructures generated by SPD processing. The combination ofultrafine grain size and high-density dislocations appears to enable deformation by newmechanisms. This work demonstrates the possibility of tailoring the microstructures ofmetals and alloys by SPD to obtain both high strength and high ductility. Materialswith such desirable mechanical properties are very attractive for advanced structuralapplications.

Understanding nanoindentation unloading curves

Abstract: Experiments have shown that nanoindentation unloading curves obtained with Berkovich triangular pyramidal indenters are usually welldescribed by the power-law relation P = α(h − hf)m, where hf is the final depth after complete unloading and α and m are material constants. However, the power-law exponent is not fixed at an integral value, as would be the case for elastic contact by a conical indenter (m = 2) or a flat circular punch (m = 1), but varies from material to material in the range m = 1.2–1.6. A simple model is developed based on observations from finite element simulations of indentation of elastic–plastic materials by a rigid cone that provides a physical explanation for the behavior. The model, which is based on the concept of an indenter with an “effective shape” whose geometry is determined by the shape of the plastic hardness impression formed during indentation, provides a means by which the material constants in the power law relation can be related to more fundamental material properties such as the elastic modulus and hardness. Simple arguments are presented from which the effective indenter shape can be derived from the pressure distribution under the indenter.

Flame-made Ceria Nanoparticles

Abstract: Flame spray pyrolysis (FSP) has been used to synthesize high-surface-area ceria from cerium acetate in acetic acid solution. With the addition of an iso-octane/2-butanol mixture to that solution, homogeneous CeO2 nanoparticles were obtained. The specific surface area of the powders ranged from 240 to 101 m2/g by controlling the oxygen dispersion and liquid precursor flow rates through the flame. Furthermore, for production rates from 2 to 10 g/h a constant average primary particle size could be obtained at selected process parameters. The ceria showed high crystallinity and primary particles with a stepped surface. The powder exhibited good thermal stability and conserved up to 40% of its initial specific surface area when calcinated for 2 h at 900 °C. This shows the potential of FSP made ceria for high-temperature applications as in three-way catalysts or fuel cells.

Effects of Creep and Thermal Drift on Modulus Measurement Using Depth-sensing Indentation

Abstract: In modulus measurement by depth-sensing indentation, previous considerations assume elastic recovery to be the sole process during unloading, but in reality creep and thermal drift may also occur, causing serious errors in the measured modulus. In this work, the problem of indentation on a linear viscoelastic half-space is solved using the correspondence principle between elasticity and linear viscoelasticity. The correction term due to creep in the apparent contact compliance is found to be equal to the ratio of the indenter displacement rate at the end of the load hold to the unloading rate. A condition for nullifying the effect of thermal drift on modulus measurement is also proposed. With this condition satisfied, the effect of thermal drift on the calculated modulus is negligible irrespective of the magnitude of the drift rate.

C60 Nanowhiskers Formed by the Liquid–liquid Interfacial Precipitation Method

Abstract: Fine needlelike crystals of C60 have been formed by a liquid–liquid interfacial precipitation method which uses an interface of the concentrated toluene solution of C60/isopropyl alcohol. The needlelike crystals of C60 with a diameter of submicrons (“C60 nanowhiskers”) were found to be single crystalline and composed of thin slabswith a thickness of about 10 nm. The intermolecular distance of the C60 nanowhiskerswas found to be shortened along the growth axis as compared with the pristine C60crystals, indicating a formation of strong bonding between C60 molecules. TheC60 nanowhiskers are assumed to be polymerized via the “2 + 2” cycloaddition inthe close-packed [110]c direction.

Morphology, kinetics, and thermodynamics of solid-state aging of eutectic SnPb and Pb-free solders (Sn–3.5Ag, Sn–3.8Ag–0.7Cu and Sn–0.7Cu) on Cu

Abstract: Intermetallic compound (IMC) growth during solid-state aging at 125, 150, and 170 °C up to 1500 h for four solder alloys (eutectic SnPb, Sn–3.5Ag, Sn–3.8Ag–0.7Cu, and Sn–0.7Cu) on Cu under bump metallization was investigated. The samples were reflowed before aging. During the reflow, the solders were in the molten state and the formation of the IMC Cu6Sn5 in the cases of eutectic SnPb and Sn–3.5Ag had a round scallop-type morphology, but in Sn–0.7Cu and Sn–3.8Ag–0.7Cu the scallops of Cu6Sn5 were faceted. In solid-state aging, all these scallops changed to a layered-type morphology. In addition to the layered Cu6Sn5, the IMC Cu3Sn also grew as a layer and was as thick as the Cu6Sn5. The activation energy of intermetallic growth in solid-state aging is 0.94 eV for eutectic SnPb and about 1.05 eV for the Pb-free solders. The rate of intermetallic growth in solid-state aging is about 4 orders of magnitude slower than that during reflow. Ternary phase diagrams of Sn–Pb–Cu and Sn–Ag–Cu are used to discuss the reactions. These diagrams predict the first phase of IMC formation in the wetting reaction and the other phases formed in solid-state aging. Yet, the morphological change and the large difference in growth rates between the wetting reaction and solid-state aging cannot be predicted.

Superhard B–C–N materials synthesized in nanostructured bulks

Abstract: We report here the high-pressure synthesis of well-sintered millimeter-sized bulks of superhard BC2N and BC4N materials in the form of a nanocrystalline composite with diamond-like amorphous carbon grain boundaries. The nanostructured superhard B–C–N material bulks were synthesized under high P–T conditions from amorphous phases of the ball-milled molar mixtures. The synthetic B–C–N samples were characterized by synchrotron x-ray diffraction, high-resolution transmission electron microscope, electron energy-loss spectra, and indentation hardness measurements. These new high-pressure phases of B–C–N compound have extreme hardnesses, second only to diamond. Comparative studies of the high P–T synthetic products of BC2N, BC4N, and segregated phases of diamond + cBN composite confirm the existence of the single B–C–N ternary phases.

Ag3Sn plate formation in the solidification of near ternary eutectic Sn–Ag–Cu alloys

Abstract: Near-ternary eutectic Sn–Ag–Cu alloys are leading candidates for Pb-free solders. These alloys have three solid phases: β–Sn, Ag3Sn, and Cu6Sn5. Starting from the fully liquid state in solidifying near-eutectic Sn–Ag–Cu alloys, the equilibrium eutectic transformation is kinetically inhibited. The Ag3Sn phase nucleates with minimal undercooling, but the β–Sn phase requires a typical undercooling of 15 to 30 °C for nucleation. Because of this disparity in the required undercooling for nucleation, large, platelike Ag3Sn structures can grow rapidly within the liquid phase, before the final solidification of the solder joints. At lower cooling rates, the large Ag3Sn plates can subtend the entire cross section of solder joints and can significantly influence the mechanical deformation behavior of the solder joints under thermomechanical fatigue conditions. In this paper, it is demonstrated that the Ag3Sn plate formation can be inhibited, an important factor in assuring the reliability of solder joints composed of these alloys.

Viscoelastic effects during unloading in depth-sensing indentation

Abstract: With polypropylene as a prototype viscoelastic material at room temperature, it was found that a “nose” may appear in the unloading segment of the load–displacement curve during nanoindentation when the holding time at peak load is short and/or the unloading rate is small, and when the peak load is high enough. The load at which the nose appears was also found to decrease linearly with decreasing unloading rate. A linear viscoelasticity analysis was performed to interpret this effect. The analysis predicts a linear variation between the nose load and the unloading rate, and the slope of such a linear variation is also shown to be proportional to the viscosity parameter of the material. Thus, by measuring the slope of the nose-load versus unloading rate plot at a given temperature, the viscosity parameter of the specimen can be found. This is a new way of measuring the viscosity parameter of a material in addition to the existing method of force modulation and noting the frequency response of the displacement.

Novel titanium foam for bone tissue engineering

Abstract: Titanium foams fabricated by a new powder metallurgical process have bimodal pore distribution architecture (i.e., macropores and micropores), mimicking natural bone. The mechanical properties of the titanium foam with low relative densities of approximately 0.20-0.30 are close to those of human cancellous bone. Also, mechanical properties of the titanium foams with high relative densities of approximately 0.50-0.65 are close to those of human cortical bone. Furthermore, titanium foams exhibit good ability to form a bonelike apatite layer throughout the foams after pretreatment with a simple thermochemical process and then immersion in a simulated body fluid. The present study illustrates the feasibility of using the titanium foams as implant materials in bone tissue engineering applications, highlighting their excellent biomechanical properties and bioactivity.

Effect of Cu concentration on the interfacial reactions between Ni and Sn–Cu solders

Abstract: The eutectic 99.3Sn–0.7Cu solder (wt%, Sn–0.7Cu) is the most promising lead-free replacement for the eutectic Sn–Pb solder in wave-soldering applications. In this study, the effect of a small perturbation in the Cu concentration on the reaction between the Sn–0.7Cu solder and Ni was investigated. Specifically, four Sn–xCu solders (x = 0.2, 0.4, 0.7, and 1) were reacted with Ni at 250 °C. A slight variation in Cu concentration produced completely different reaction products. When the Cu concentration was low (x = 0.2), the reaction product was (Ni1–xCux)3Sn4. At high Cu concentrations (x = 0.7 and 1), the reaction product was (Cu1–yNiy)6Sn5. When the Cu concentration was in-between (x = 0.4), both (Ni1–xCux)3Sn4 and (Cu1–yNiy)6Sn5, formed. The above findings were rationalized using the Cu–Ni–Sn isotherm. The results of this study imply that the Cu concentration must be strictly controlled in industrial production to produce the desired intermetallic at the interface.

Deformation and Failure of Zr57Ti5Cu20Ni8Al10 Bulk Metallic Glass Under Quasi-static and Dynamic Compression

Abstract: We have examined the mechanical behavior of Zr57Ti5Cu20Ni8Al10 bulk metallic glass under uniaxial compression at strain rates from 10−4to 3 × 103 s−1. The failure stress decreases with increasing strain rate, and shear-band formation remains the dominant deformation mechanism. A consideration of basic properties of adiabatic shear bands makes it appear unlikely that shear bands formed under quasi-static loading are adiabatic; in the dynamic case, the time scales of deformation and thermal conduction are similar, indicating that a more sophisticated calculation is required. In the dynamic tests, however, high-speed cinematography reveals evidence that the mechanism of failure involves an adiabatic component.

Overview: Damage in brittle layer structures from concentrated loads

Abstract: In this article, we review recent advances in the understanding and analysis of damage initiation and evolution in laminate structures with brittle outerlayers and compliant sublayers in concentrated loading. The relevance of such damage to lifetime-limiting failures of engineering and biomechanical layer systems is emphasized. We describe the results of contact studies on monolayer, bilayer, trilayer, and multilayer test specimens that enable simple elucidation of fundamental damage mechanics and yet simulate essential function in a wide range of practical structures. Damage processes are observed using post mortem (“bonded-interface”) sectioning and direct in situ viewing during loading. The observations reveal a competition between damage modes in the brittle outerlayers—cone cracks or quasiplasticity at the top (near-contact) surfaces and laterally extending radial cracks at the lower surfaces. In metal or polymeric support layers, yield or viscoelasticity can become limiting factors. Analytical relations for the critical loads to initiate each damage mode are presented in terms of key system variables: geometrical (layer thickness and indenter radius); material (elastic modulus, strength and toughness of brittle components, hardness of deformable components). Such relations provide a sound physical basis for the design of brittle layer systems with optimal damage thresholds. Other elements of the damage process—damage evolution to failure, crack kinetics (and fatigue), flaw statistics, and complex (tangential) loading—are also considered.

Rate Dependence of Serrated Flow During Nanoindentation of a Bulk Metallic Glass

Abstract: Plastic deformation of Pd–40Ni–20P bulk metallic glass (BMG) was investigated by instrumented nanoindentation experiments over a broad range of indentation strain rates. At low rates, the load–displacement curves during indentation exhibited numerous serrations or pop-ins, but these serrations became less prominent as the indentation rate was increased. Using the tip velocity during pop-in as a gauge of serration activity, we found that serrated flow is only significant at indentation strain rates below about 1–10/s. This result suggests a transition in plastic flow behavior at high strain rates, in agreement with prior studies of BMGs under different modes of loading.

Characterization of Free Volume in a Bulk Metallic Glass Using Positron Annihilation Spectroscopy

Abstract: The free volume of metallic glasses has a significant effect on atomic relaxation processes, although a detailed understanding of the nature and distribution of free volume sites is currently lacking. Positron annihilation spectroscopy was employed to study free volume in a Zr–Ti–Ni–Cu–Be bulk metallic glass following plastic straining and cathodic charging with atomic hydrogen. Multiple techniques were used to show that strained samples had more open volume, while moderate hydrogen charging resulted in a free volume decrease. It was also shown that the free volume is associated with zirconium and titanium at the expense of nickel, copper, and beryllium. Plastic straining led to a slight chemical reordering.

Mechanisms of ceramic coating deposition in solution-precursor plasma spray

Abstract: The solution-precursor plasma spray (SPPS) method is a new process for depositing thick ceramic coatings, where solution feedstock (liquid) is injected into a plasma. This versatile method has several advantages over the conventional plasma spray method, and it can be used to deposit nanostructured, porous coatings of a wide variety of oxide and non-oxide ceramics for a myriad of possible applications. In an effort to understand the SPPS deposition process, key diagnostic and characterization experiments were performed on SPPS coatings in the Y2O3-stabilized ZrO2 (YSZ) system. The results from these experiments show that there are multiple pathways to SPPS coating formation. The atomized precursor droplets undergo rapid evaporation and breakup in the plasma. This is followed by precipitation, gelation, pyrolysis, and sintering. The different types of particles reach the substrate and are bonded to the substrate or the coating by sintering in the heat of the plasma. The precursor also reaches the substrate or the coating. This precursor pyrolyzes in situ on the substrate, either after it reaches a “cold” substrate or upon contact on a “hot” substrate and helps bond the particles. The coating microstructure evolves during SPPS deposition as the coating temperature reaches approximately 770 °C.

Surface Effects on Nanoindentation

Abstract: In this paper, we report on a study of the surface effect on nanoindentation and introduce the apparent surface stress that represents the energy dissipated per unit area of a solid surface in a nanoindentation test. The work done by an applied indentation load contains both bulk and surface work. Surface work, which is related to the apparent surface stress and the size and geometry of an indenter tip, is necessary in the deformation of a solid surface. Good agreement is found between theoretical first-order approximations and empirical data on depth-dependent hardness, indicating that the apparent surface stress plays an important role in depth-dependent hardness. In addition, we introduce a critical indentation depth. The surface deformation predominates if the indentation depth is shallower than the critical depth, while the bulk deformation predominates when the indentation depth is deeper than the critical depth.

Optimal and Manufacturable Two-dimensional, Kagomé-like Cellular Solids

Abstract: We used the topology optimization technique to obtain two-dimensional, isotropic cellular solids with optimal effective elastic moduli and effective conductivity. The overall aim was to obtain the best (simplest) manufacturable structures for these effective properties, i.e., single-length-scale structures. Three different but simple periodic structures arose due to the imposed geometric mirror symmetries: lattices with triangular-like cells, hexagonal-like cells, or Kagome-like cells. As a general rule, the structures with the Kagome-like cells provided the best performance over a wide range of densities, i.e., for 0 ≰ ф <0.6, where ф is the solid volume fraction (density). At high densities (ф < 0.6), Kagome-like structures were no longer possible, and lattices with hexagonal-like or triangular-like cells provide virtually the same optimal performance. The Kagome-like structures were found to be a new class of cellular solids with many useful features, including desirable transport and elastic properties, heat-dissipation characteristics, improved mechanical strength, and ease of fabrication.

Contact Deformation Regimes Around Sharp Indentations and the Concept of the Characteristic Strain

Abstract: Finite element simulations are performed to analyze the contact deformation regimes induced by a sharp indenter in elastic – power-law plastic solids. As the yield strength (σys) and strain hardening coefficient (n) decrease or, alternatively, as Young’s modulus (E) increases, the contact regime evolves from (i) an elastic–plastic transition, to (ii) a fully plastic contact response, and to (iii) a fully plastic regime where piling-up of material at the contact area prevails. In accordance with preliminary analyses by Johnson, it is found that Tabor’s equation, where hardness (H) = 2.7σr, applies within the fully plastic regime of elastic – power-law plastic materials. The results confirm the concept of the uniqueness of the characteristic strain, ∈r = 0.1, that is associated with the uniaxial stress, σr. A contact deformation map is constructed to provide bounds for the elastic–plastic transition and the fully plastic contact regimes for a wide range of values of σ ys, n, and E. Finally, the development of piling-up and sinking-in at the contact area is correlated with uniaxial mechanical properties. The present correlation holds exclusively within the fully plastic contact regime and provides a tool to estimate σ ys and n from indentation experiments.

Chemical mechanical polishing of thermal oxide films using silica particles coated with ceria

Abstract: Thermal oxide covered silicon wafers were polished with slurries containing either nano-sized ceria (CeO2) or newly prepared uniform colloidal silica particles coated with ceria. The polish rate of the latter was significantly higher than that of pure ceria. The experiments were carried out using different concentrations of the abrasives at pH 4 and 10. Little effect on the polishing rates was noted when the conditions of the slurries were varied, which was explained by the compensation of two opposite polishing mechanisms.

Microwave dielectric properties of MO–La2O3–TiO2 (M = Ca, Sr, Ba) ceramics

Abstract: Single-phase polycrystalline ceramics in the MO–La2O3–TiO2 (M = Ca, Sr, Ba) system, such as cation-deficient hexagonal perovskites CaLa4Ti4O15, SrLa4Ti4O15, BaLa4Ti4O15, and Ca2La4Ti5O18 and the orthorhombic phases CaLa4Ti5O17 and CaLa8Ti9O31, were prepared through the solid-state ceramic route. The phases and structure of the ceramics were analyzed through x-ray diffraction and scanning electron microscopy. The microwave dielectric properties of the ceramics were studied using a network analyzer. The investigated ceramics show high er in the range 42 to 54, high quality factors with Q ×f in the range 16,222 to 50,215 GHz, and low Tf in the range –25 to +6 ppm / °C. These high dielectric constant materials with high Q × f up to 50,215 GHz are suitable for applications where narrow bandwidth and extremely low insertion loss is necessary, especially at frequencies around 1.9 GHz.

Highly Ordered Nanoporous Alumina Films: Effect of Pore Size and Uniformity on Sensing Performance

Abstract: The effect of pore size and uniformity on the humidity response of nanoporous alumina, formed on aluminum thick films through an anodization process, is reported. Pore sizes examined range from approximately 13 to 45 nm, with a pore size standard deviations ranging from 2.6 to 7.8 nm. The response of the material to humidity is a strong function of pore size and operating frequency. At 5 kHz an alumina sensor with an average pore size of 13.6 nm (standard deviation 2.6 nm) exhibits a well-behaved change in impedance magnitude of 103 over 20% to 90% relative humidity. Increasing pore size decreases the humidity range over which the sensors have high sensitivity and shifts the operating range to higher humidity values. Cole–Cole plots of 5 to 13 MHz measured impedance spectra, modeled using equivalent circuits, are used to resolve the effects of water adsorption and ion migration within the adsorbed water layer. The presence of impurity ions within the highly ordered nano-dimensional pores, accumulated during the anodization process, appear highly beneficial for obtaining a substantial variation in measured impedance over a wide range of humidity values.

Thermal conductivity of ceramics in the ZrO2-GdO1.5system

Abstract: Low thermal conductivity ceramics in the ZrO2-GdO1.5 system have potential in structural (refractories, thermal barrier coatings, thermal protection) and nuclear applications. To that end, the thermal conductivities of hot-pressed xGdO1.5 ·(1 - x)ZrO2 (where x = 0.05, 0.15, 0.31, 0.50, 0.62, 0.75, 0.89, and 1.00) solid solutions were measured, for the first time, as a function of temperature in the range 25 to 700 °C. On the ZrO2-rich side, the thermal conductivity first decreased rapidly with increasing concentration of GdO1.5 and then reached a plateau. On the GdO1.5-rich side, the decrease in the thermal conductivity with increasing concentration of ZrO2 was less pronounced. The thermal conductivity was less sensitive to the composition with increasing temperature. The thermal conductivity of pyrochlore Gd2Zr2O7 (x = 0.5) was higher than that of surrounding compositions at all temperatures. A semiempirical phonon-scattering theory was used to analyze the experimental thermal conductivity data. In the case of pure ZrO2 and GdO1.5, the dependence of the thermal conductivity to the absolute temperature (T) was less than 1/T. Therefore, the minimum thermal conductivity theory was applied, which better described the temperature dependence of the thermal conductivity of pure ZrO2 and GdO1.5. In the case of solid solutions, phonon scattering by cation mass fluctuations and additional scattering by oxygen vacancies on the ZrO2-rich side and by gadolinium vacancies on the GdO1.5-side seemed to account for the composition and temperature dependence of the thermal conductivity.

Grain Growth, Stress, and Impurities in Electroplated Copper

Abstract: The widely observed secondary grain growth in electroplated Copper layers is shown to be incomplete after the sheet resistance and stress of the layer appear to have stabilized. Instead the layer is in an intermediate state with a grain size distribution that depends on the plating conditions. Further extensive annealing at high temperatures results in an additional considerable enlargement of the grain structure, accompanied by an additional decrease of the sheet resistance and desorption of impurities that were incorporated during plating.

Large-quantity production of high-yield boron nitride nanotubes

Abstract: A high quantity and Yield (up to 85%) of boron nitride (BN) nanotubes have been produced using a mechanothermal method. Elemental boron powders were first mechanically milled at room temperature in NH3 atmosphere and subsequently heated in N-2 gas at 1200 degreesC for up to 16 h. The BN nanotubes obtained have either multiwalled cylindrical or bamboolike structures, suggesting different growth processes. The high formation yield of BN nanotubes is due to a high density of nanostructured nuclei created by an extensive milling treatment.

Reactive Sputter Deposition of Highly Oriented AlN Films at Room Temperature

Abstract: Textured as well as epitaxial thin AlN films are of great interest for a wide range of electro-acoustic and optoelectronic applications. Reduction of the deposition temperature is of vital importance in a number of applications due to thermal budget limitations. In this work we systematically studied the influence of the process parameters on the film properties and identified the factors leading to improved film quality as well as reduced deposition temperature with pulsed direct current sputtering in an Ar/N2 atmosphere. We demonstrated that fully textured (0002) films can be grown under a wide range of conditions. At the same time the full width at half-maximum (FWHM) of the rocking curve of the (0002) XRD peak was found to vary systematically with process conditions—depostion rate, process pressure, gas composition, and substrate temperature. The best films showed a FWHM of 1.2°. We found that by far the most important factor is the arrival energy of the sputtered Al atoms, which is primarily controlled by the process pressure. We report for the first time that fully textured AlN films with a FWHM of under 2° can be grown at room temperature. Other important factors are the ion and electron bombardment of the films and substrate temperature as well as gas composition, although their influence is not as dramatic. Generally, the film quality increases with temperature. Bias and electron bombardment within a certain range also lead to better films.

Low-cost manufacturing process for nanostructured metals and alloys

Abstract: In spite of their interesting properties, nanostructured materials have found limited uses because of the cost of preparation and the limited range of materials that can be synthesized. It has been shown that most of these limitations can be overcome by subjecting a material to large-scale deformation, as occurs during common machining operations. The chips produced during lathe machining of a variety of pure metals, steels, and other alloys are shown to be nanostructured with grain (crystal) sizes between 100 and 800 nm. The hardness of the chips is found to be significantly greater than that of the bulk material.

Orientation imaging studies of Sn-based electronic solder joints

Abstract: Single shear lap specimens were subjected to creep, isothermal aging, and thermomechanical fatigue (TMF). Scanning electron microscopy micrographs of previously polished specimens revealed changes in surface morphology. Orientation imaging microscopy was carried out on the same specimens to study the microstructural evolution and crystal orientation changes. As-fabricated joints consistently show a preferred crystal orientation with a few minority orientations with highly preferred misorientations. Alloy additions caused an increase in the number of statistically significant crystal orientations and misorientations. The solidification microstructure was unchanged due to room-temperature creep. Aging caused development and motion of well-defined subgrain boundaries and removal of most minority orientations. TMF causes heterogeneous refinement of the microstructure that accounts for the localized grain boundary sliding in regions of high strain concentration. This study implies that the lead-free solder joints are not polycrystals, but multicrystals, so that deformation is very heterogeneous and sensitive to strain and temperature history.

Fracture toughness and adhesion energy of sol-gel coatings on glass

Abstract: The reliability of coatings that are used in industrial applications critically depends on their mechanical properties. Nanoindentation and scratch testing are well-established techniques to measure some of these properties, namely the elastic modulus and hardness of coatings. In this paper, we investigate the possibility of also assessing the coating fracture toughness and the energy of adhesion between the coating and the substrate using indentation and scratch testing. Various existing and new methods are discussed, and they are illustrated by measurements on particle-filled sol-gel coatings on glass. All methods are based on the occurrence of cracking, and they are therefore only applicable to coating systems that act like brittle materials and exhibit cracking during indentation and scratching. The methods for determining the fracture toughness give comparable results, but the values still differ to within about 50%. The values of the adhesion energy obtained from different measurements are consistent, but it remains uncertain to which extent the obtained values are quantitatively correct. The results show that the methods used are promising, but more research is needed to obtain reliable quantitative results.

Creep behavior of eutectic Sn–Ag lead-free solder alloy

Abstract: Precipitation-strengthened tin-based eutectic Sn–3.5 Ag alloy was investigated for its creep behavior at three temperatures ranging from 303 to 393 K, under the tensile stress range of σ/E = 10−4 to 10−3. The steady-state creep rates cover seven orders of magnitude (10−3 to 10−9 s−1). The initial microstructure was found to have Ag3Sn intermetallic compound finely dispersed in the matrix of β–Sn. By incorporation of a threshold stress, σth, into the analysis, the creep data of eutectic Sn–Ag at all temperatures can be fitted by a single straight line with a slope of seven after normalizing the steady-state creep rate and the effective stress, indicating that the creep rates are controlled by the dislocation-pipe diffusion in the Sn matrix. The steady-state creep rate, , can then be expressed as , where QC is the creep activation energy, G is the temperature-dependent shear modulus, b is Burger's vector, R is the universal gas constant, T is the absolute temperature, σ is the applied stress, A is a material-dependent constant, and , in which σOB is the Orowan bowing stress and kR is the relaxation factor.