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An electrical technique was recently developed to measure the in situ contact area continuously during instrumented indentation by simultaneously monitoring electrical contact response between a conductive indenter tip and a conductive sample. This technique has the potential to overcome limitations of the Oliver-Pharr method caused by the lack of a direct contact area measurement. However, the electrical contact current-voltage (I-V) curves measured from the technique were nonlinear, posing a significant challenge to inferring accurate in situ contact areas. To overcome this challenge and extend the electrical technique to more applications, various I-V curve analysis methods were investigated for their abilities to infer in situ contact area and hardness. Annealed Cu was indented using both linear and exponential loading tests. When analyzing the resulting data, the feasibility of each method was evaluated and the optimal methods to calculate the in situ contact area and hardness were determined. It was found that a simple summation of the absolute values of area under I-V curves or the area under I-V curves at positive voltages yielded the most robust area measure, whereas error in the inferred contact area was systematic and primarily from velocity dependence of the I-V response.
The effect of electropulsing treatment (EPT) on the microstructure and mechanical properties of aged Mg-9Al-1Zn alloy strip was studied. EPT was found to accelerate tremendously the β phase spheroidization in the aged Mg-9Al-1Zn alloy. This improved microstructure exhibits excellent mechanical properties, that is, increasing elongation to failure significantly without loss of tensile strength. The spheroidization of the β phase during EPT was attributed to the reduction of the nucleation thermodynamic barrier and enhancement of atomic diffusion.
To investigate the microwave (MW) processing of Fe3O4, for which occurrence of decrystallization has been reported, the micro/nanostructures of MW-heated Fe3O4 powder were observed in this study. The specimens were irradiated by 2.45 GHz MW at the position of magnetic (H)-field maximum in a TE10 single mode applicator. The specimen was heated well above the Curie temperature in H-field. The heated specimen above 1000 °C revealed the glass-like surface with the diminished x-ray diffraction (XRD) peak intensities. They resemble the reported features of decrystallization in an earlier work performed at Penn State University. According to the XRD profiles of the MW-heated specimens, formation of FeO and shift of Fe3O4 peaks to the lower angle with the broadened width were observed. To account for the findings, a model is presented that phase separation occurred into FeO and Fe3O4 resulting in an increased lattice parameter due to the increased oxygen content. This activity is caused by local transport of oxygen in nanoscale. Considering the shape of the main XRD Fe3O4 peak with a shoulder and the existence of halo in nanobeam diffraction (NBD), amorphous phase areas exist. As a result of transmission electron microscopy observation, it was shown that they were in nanoscaled localized regions, and it was not confirmed that the glass-like morphologies (or decrystallized morphologies) are totally amorphous. The observed micro/nanostructures and mechanism of the amorphous phase formation were discussed considering the Fe-O phase diagram.
The remarkable progress in nonpolar and semipolar devices based on gallium nitride (GaN) in recent years has been driven by not only advancements in the epitaxial growth technique but also improvements in the quality of bulk nonpolar and semipolar GaN substrates. At present, high-quality nonpolar/semipolar substrates are only made by slicing thick bulk GaN crystals grown by hydride vapor-phase epitaxy (HVPE). Although HVPE is currently the most successful method for obtaining high-quality bulk GaN crystals, it is still difficult to obtain uniform crystals with large diameters and thicknesses. The size of the nonpolar/semipolar substrates has been limited by the growth thickness along the c-axis of bulk GaN crystals. Here we review the growth of bulk GaN crystals by HVPE to achieve high-quality and large-sized nonpolar and semipolar substrates.
Sol-gel-derived biocompatible titanium oxide–cerium oxide (TiO2–CeO2) nanocomposite film was deposited onto indium tin oxide (ITO)-coated glass substrate by the dip-coating method. This nanobiocomposite film has been characterized using x-ray diffraction, Fourier transform infrared, atomic force microscope, and electrochemical techniques, respectively. The particle size of the TiO2–CeO2 nanobiocomposite film was found to be 23 nm. The urea biosensor fabricated by immobilizing mixed enzyme [urease (Urs) and glutamate dehydrogenase (GLDH)] on this nanobiocomposite showed a response time of 10 s, sensitivity as 0.9165 μAcm−2mM−1, detection limit of 0.166 μM, and negligible effect due to interferants uric acid, cholesterol, glucose, and ascorbic acid. The value of Michaelis–Menten constant (Km) estimated using Lineweaver–Burke plot as 4.8 mM indicated enhancement in the affinity and/or activity of enzyme attached to their nanobiocomposite. This bioelectrode retained 95% of enzyme activity after 6 months at 4 °C.
Reverse atom transfer radical polymerization of methacrylonitrile (MAN) initiated by azobisisobutyronitrile (AIBN) was approached for the first time in the absence of any ligand in four novel ionic liquids, 1-methylimidazolium acetate ([mim][AT]), 1-methylimidazolium butyrate ([mim][BT]), 1-methylimidazolium caproate ([mim][CT]), and 1-methylimidazolium heptylate ([mim][HT]). The polymerization in [mim][AT] not only showed the best control of molecular weight and its distribution but also provided a more rapid reaction rate with the ratio of [MAN]:[FeCl3]:[AIBN] at 300:2:1. The block copolymer PMAN-b-PSt was obtained via a conventional ATRP process in [mim][AT] by using the resulting PMAN as a macroinitiator. After simple purification, [mim][AT] and FeCl3 could be easily recycled and reused and had no effect on the living nature of reverse atom transfer radical polymerization of MAN.
We have developed a soft lithography-based process to create microscale patterns of silica on a diverse array of substrates. A sacrificial polymer layer was first patterned using a micromolding technique. A peptide was adsorbed on the substrate and the sacrificial layer was removed. The patterned peptide template then catalyzed the deposition of silica from a silicic acid solution. With this procedure, we have created both continuous and discontinuous silica patterns on metallic, ceramic, and polymer substrates.
The results of positron lifetime and Doppler broadening spectrum of defects in the hydrogen charged non-heat treatable 5xxx Al alloys are presented in this work. The yield stress of the sample was reduced for about 20 MPa after hydrogen was charged. A similar trend was observed in positron lifetime measurement, as the average lifetime τav descended remarkably to almost the level of Al matrix. The change in coincidence Doppler broadening (CDB) spectroscopy was also significant, exhibited by the characteristic change in CDB radio curves of a sample before and after hydrogen was charged. After hydrogen charging, there is an obvious enhancement in the high momentum region compensating dehancement in the low momentum region. This indicates the existence of hydrogen filling effect. The vacancies around the Mg atoms should be preferential filling sites for hydrogen because Mg has a strong affinity for hydrogen. The formation of an Mg–H bond parallel to a grain boundary is an important factor in weakening the grain boundary cohesion.
Composite materials are those that contain two or more distinct constituent materials or phases, on a microscopic or macroscopic size scale larger than the atomic scale, and in which physical properties are significantly altered in comparison with those of a homogeneous material. In this vein, fiberglass and other fibrous materials are viewed as composites, but alloys, such as brass, are not. Semicrystalline polymers, such as polyethylene, have a heterogeneous structure, which can be treated via composite theory. Biological materials also have a heterogeneous structure and are known as natural composites. Composites may contain solid, liquid, and gas phases. For example, composites of gas and liquid include mist and foam; composites of solid and gas include foam and smoke. Composites with a structural role have several solid phases or a connected solid phase with gas or liquid in the interstices (structural foam and honeycomb).
Composite Structures and Properties
Ideal Structures
The properties of composites are greatly dependent upon microstructure. Composites differ from homogeneous materials in that considerable control can be exerted over the larger scale structure; and hence over the desired properties. In particular, the properties of a composite depend upon the shape of the heterogeneities, upon the volume fraction occupied by them, and upon the interface between the constituents. Volume fraction refers to the ratio of the volume of a constituent to the total volume of a composite specimen. The shape of the heterogeneities in a composite is classified as follows. The principal inclusion shape categories (Figure 9.1) are the particle, with no long dimension; the fiber, with one long dimension; and the platelet (flake, lamina), with two long dimensions.
The purpose of Chapter 7 is to present the viscoelastic behavior of representative real materials so that the reader can gain a sense of orders of magnitude of the effects. Engineers and scientists who deal with elastic behavior of materials are aware of the moduli of various common materials. Similarly, knowledge of the viscoelastic properties of particular materials is essential to rationally apply them. Further examples, with analysis of the physical causes of the viscoelasticity, are provided in Chapter 8. Materials presented here are classified as polymers, metals, ceramics, biological composites and synthetic composites (Chapter 9). In a survey, damping properties of metals, ceramics, and metal matrix composites are compared [1]. Structural metals tend to be low damping, with tan? on the order of 10−3 or less. Experimental results for the same material can differ substantially depending on purity and permanent deformation. Most ceramics also exhibit low damping at ambient temperature, but some exhibit modest damping at elevated temperature.
Overview: Some Common Materials
An overview of modulus and damping of selected classes of materials at small strain is shown in Figure 7.1. At high strain amplitude, some metals exhibit higher damping [2] in such maps.
The loss tangents of some well-known materials at various temperatures and frequencies are presented in Table 7.1. Most of the data are at room temperature, denoted rt in Table 7.1 except as noted, and at audio or subaudio frequencies.
For some applications of viscoelastic materials, it is sufficient to understand creep and relaxation properties. For example sometimes structural elements are maintained under steady load or constant extension. In other applications the response to an arbitrary load or strain history is required. To predict this response, constitutive equations that incorporate all possible responses are of use. Various mathematical tools are used in the development of these equations. The viscoelastic functions in the equations are obtained by experimentation.
Prediction of the Response of Linearly Viscoelastic Materials
Prediction of Recovery from Relaxation E(t)
The creep and relaxation properties described above in §1.3 permit one to predict the response of the material to a step function stress or strain. To predict the response of the material to any history of stress or strain (i.e., stress or strain as a function of time), constitutive equations are developed.
The following is restricted to isothermal deformation in one dimension. The symbol E is used to represent an elastic modulus, however, the analysis applies equally to shear deformation corresponding to a shear modulus G or volumetric deformation corresponding to a bulk modulus B, which is sometimes called K.
To develop the constitutive equation for linear materials, we use the Boltzmann superposition principle, which states that the effect of a compound cause is the sum of the effects of the individual causes. This principle is a statement of linearity. First, we consider the strain associated with a relaxation and recovery experiment, with the intention to use the idea of linearity as embodied in the Boltzmann superposition principle to predict the resulting stress history.
The treatment of viscoelasticity thus far has dealt with phenomena, measurement of material properties, prediction of response to various load histories, and stress analysis. In this chapter we consider the physical causes of viscoelastic response. Study of causal mechanisms is motivated by (1) the desire for scientific understanding; (2) the intention to gain ability to choose or tailor materials with specified viscoelastic properties; and (3) the utility of viscoelastic measurements as a probe of microphysical processes that are causally linked to viscoelasticity. The conceptually simplest of the causal mechanisms are developed in detail here. These processes can occur in crystalline materials including metals, ceramics as well as in polymers. Examples of damping due to fluid–solid interaction in porous materials according to the Biot theory are given in §7.5, biological tissue. Viscoelasticity in tissue also results from stress induced motion at the molecular scale. The treatment is intended to be introductory, not exhaustive.
Survey of Viscoelastic Mechanisms
There are many causal mechanisms [1–3] responsible for viscoelastic response; several of these are as follows. Mechanisms indicated by a * are called fundamental mechanisms because they occur even in an ideal perfect single crystal, and they are not removable, even in principle. Many effects are named for the person who discovered them or who provided a clear analysis of the physical processes responsible for them. The word relaxation is used in these names to refer to viscoelasticity in a general sense, not necessarily a specific stress relaxation experiment.
The response of viscoelastic materials to sinusoidal load is developed in this section, and this response is referred to as dynamic. Dynamic in this context has no connection with inertial terms or resonance. The dynamic behavior is of interest because viscoelastic materials are used in situations in which the damping of vibration or the absorption of sound is important. The results developed in this section have a bearing on applications of viscoelastic materials, on experimental methods for their characterization, and on the development of physical insight regarding viscoelasticity.
The frequency of the sinusoidal load on an object or structure may be so slow that inertial terms do not appear (the subresonant regime), or high enough that resonance of structures made of the material occurs. At a sufficiently high frequency, dynamic behavior is manifested as wave motion. This distinction between ranges of frequency does not appear in the classical continuum description of a homogeneous material, because the continuum view deals with differential elements of material.
Oscillatory stress and strain histories are represented by sinusoid functions. Suppose we have α(ωt) = α0sinωt, in which t is time, α0 is the amplitude, and ω is the angular frequency. The sine function repeats every 2π radians. So α(ωt + 2π) = α(ωt). The time T required for the sine function to complete one cycle is obtained from ωT = 2π, or T = 2π/ω. T is called the period, the number of seconds required for one cycle.
Experimental procedures for viscoelastic materials, as in other experiments in mechanics, make use of a method for applying force or torque, a method for measuring the same, and a method for determining displacement, strain, or angular displacement of a portion of the specimen. If the experimenter intends to explore a wide range of time, and/or frequencies, the requirements for performance of the instrumentation can be severe. Elementary creep procedures are discussed first, because they are the simplest. Methods for measurement and for load application are discussed separately, since many investigators choose to assemble their own equipment from components. Many procedures in viscoelastic characterization of materials have aspects in common with other mechanical testing. Therefore, study of known standard methods [1, 2] for mechanical characterization of materials is useful. As in other forms of mechanical characterization, it is important that the stress distribution in the specimen be well-defined. End conditions in the gripping of specimens are usually not well known. The experimenter often uses elongated specimens for tension, torsion, or bending, to appeal to Saint Venant's principle in using idealized stress distributions for the purpose of analysis. The determination of viscoelastic properties as a function of frequency is at times referred to as mechanical spectroscopy.
Frequency response is an important consideration for instruments used in viscoelasticity; the transducers [3] for force generation and measurement and for measurement of deformation must respond adequately at the frequencies of interest.