Fracture Testing at Small-Length Scales: From Plasticity in Si to Brittleness in Pt

The field of micro-/nano-mechanics of materials has been driven, on the one hand by the development of ever smaller structures in devices, and, on the other, by the need to map property variations in large systems that are microstructurally graded. Observations of `smaller is stronger' have also brought in questions of accompanying fracture property changes in the materials. In the wake of scattered articles on micro-scale fracture testing of various material classes, this review attempts to provide a holistic picture of the current state of the art. In the process, various reliable micro-scale geometries are shown, challenges with respect to instrumentation to probe ever smaller length scales are discussed and examples from recent literature are put together to exhibit the expanse of unusual fracture response of materials, from ductility in Si to brittleness in Pt. Outstanding issues related to fracture mechanics of small structures are critically examined for plausible solutions.

Relationship between Laves phase and the impact brittleness of P92 steel reevaluated

Laves phase has been widely accepted to cause the impact brittleness of 9–12Cr martensitic heat-resistant steels after long time aging at elevated temperatures. However, in the present research, the impact toughness of the already brittle P92 steel aged at 600 °C for 2035 h could be restored to the original level by reheating at 700 °C for 1 h, with Laves phase barely changed. This interesting result strongly indicated that the presence of Laves phase might not be the real reason for the impact brittleness.

Relationship between elastic and mechanical properties of dental ceramics and their index of brittleness

The purpose of the study was to verify the effects of a number of materials' parameters (crystalline content; Young's modulus, E; biaxial flexure strength, sigma(i); Vickers hardness, VH; fracture toughness, K-Ic; fracture surface energy, gamma(f); and index of brittleness, B) on the brittleness of dental ceramics. Five commercial dental ceramics with different contents of glass phase and crystalline particles were studied: a vitreous porcelain (VM7/V), a porcelain with 16 vol% leucite particles (d.Sign/D), a glass-ceramic with 29 vol% leucite particles (Empress/E1), a glass-ceramic with 58 vol% lithium-disilicate needle-like particles (Empress 2/E2), and a glass-infiltrated alumina composite with 65 vol% crystals (In-Ceram Alumina/IC). Discs were constructed according to manufacturers' instructions, ground and polished to final dimensions (12 mm x 1.1 mm). Elastic constants were determined by ultrasonic pulse-echo method. sigma(i) was determined by piston-on-3-balls method in inert condition. VH was determined using 19.6 N load and K-Ic was determined by indentation strength method. gamma(f) was calculated from the Griffith-Irwin relation and B by the ratio of HV to K-Ic. IC and E2 showed higher values of sigma(i), E, K-Ic and gamma(f), and lower values of B compared to leucite-based glass-ceramic and porcelains. Positive correlations were observed for sigma(i) versus K-Ic, and K-Ic versus E-1/2, however, E did not show relationship with HV and B. The increase of crystalline phase content is beneficial to decrease the brittleness of dental ceramics by means of both an increase in fracture surface energy and a lowering in index of brittleness. (C) 2012 Elsevier Ltd and Techna Group Sri. All rights reserved.

Evaluation of the indirect measures of rock brittleness and fracture toughness in rock cutting

Performance prediction models for partial face mechanical excavators, when developed in laboratory conditions, depend on relating the results of a set of rock property tests and indices to specific cutting energy (SE) for various rock types. There exist some studies in the literature aiming to correlate the geotechnical properties of intact rocks with the SE, especially for massive and widely jointed rock environments. However, those including direct and/or indirect measures of rock fracture parameters such as rock brittleness and fracture toughness, along with the other rock parameters expressing different aspects of rock behavior under drag tools (picks), are rather limited. With this study, it was aimed to investigate the relationships between the indirect measures of rock brittleness and fracture toughness and the SE depending on the results of a new and two previous linear rock cutting programmes. Relationships between the SE, rock strength parameters, and the rock index tests have also been investigated in this study. Sandstone samples taken from the different fields around Ankara, Turkey were used in the new testing programme. Detailed mineralogical analyses, petrographic studies, and rock mechanics and rock cutting tests were performed on these selected sandstone specimens. The assessment of rock cuttability was based on the SE. Three different brittleness indices (B1, B2, and B4) were calculated for sandstones samples, whereas a toughness index (T-i), being developed by Atkinson et al.(1), was employed to represent the indirect rock fracture toughness. The relationships between the SE and the large amounts of new data obtained from the mineralogical analyses, petrographic studies, rock mechanics, and linear rock cutting tests were evaluated by using bivariate correlation and curve fitting techniques, variance analysis, and Student's t-test. Rock cutting and rock property testing data that came from well-known studies of McFeat-Smith and Fowell(2) and Roxborough and Philips(3) have also been employed in statistical analyses together with the new data. Laboratory tests and subsequent analyses revealed that there were close correlations between the SE and B4 whereas no statistically significant correlation has been found between the SE and T-i. Uniaxial compressive and Brazilian tensile strengths and Shore scleroscope hardness of sandstones also exhibited strong relationships with the SE. NCB cone indenter test had the greatest influence on the SE among the other engineering properties of rocks, confirming the previous studies in rock cutting and mechanical excavation. Therefore, it was recommended to employ easy-to-use index tests of NCB cone indenter and Shore scleroscope in the estimation of laboratory SE of sandstones ranging from very low to high strengths in the absence of a rock cutting rig to measure it until the easy-to-use universal measures of the rock brittleness and especially the rock fracture toughness, being an intrinsic rock property, are developed.

Structure–property relationships of silk-modified mesoporous bioglass scaffolds

Porous mesopore-bioglass (MBG) scaffolds have been proposed as a new class of bone regeneration materials due to their apatite-formation and drug-delivery properties; however, the material’s inherent brittleness and high degradation and surface instability are major disadvantages, which compromise its mechanical strength and cytocompatibility as a biological scaffold. Silk, on the other hand, is a native biomaterial and is well characterized with respect to biocompatibility and tensile strength. In this study we set out to investigate what effects blending silk with MBG had on the physiochemical, drug-delivery and biological properties of MBG scaffolds with a view to bone tissue engineering applications. Transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were the methods used to analyze the inner microstructure, pore size and morphology, and composition of MBG scaffolds, before and after addition of silk. The effect of silk modification on the mechanical property of MBG scaffolds was determined by testing the compressive strength of the scaffolds and also compressive strength after degradation over time. The drug-delivery potential was evaluated by the release of dexamethasone (DEX) from the scaffolds. Finally, the cytocompatibility of silk-modified scaffolds was investigated by the attachment, morphology, proliferation, differentiation and bone-relative gene expression of bone marrow stromal cells (BMSCs). The results showed that silk modification improved the uniformity and continuity of pore network of MBG scaffolds, and maintained high porosity (94%) and large-pore size (200–400 mm). There was a significant improvement in mechanical strength, mechanical stability, and control of burst release of DEX in silkmodified MBG scaffolds. Silk modification also appeared to provide a better environment for BMSC attachment, spreading, proliferation, and osteogenic differentiation on MBG scaffolds.

Mesoporous bioglass/silk composite scaffolds for bone tissue engineering

In the past 20 years, mesoporous materials have been attracted great attention due to their significant feature of large surface area, ordered mesoporous structure, tunable pore size and volume, and well-defined surface property. They have many potential applications, such as catalysis, adsorption/separation, biomedicine, etc. [1]. Recently, the studies of the applications of mesoporous materials have been expanded into the field of biomaterials science. A new class of bioactive glass, referred to as mesoporous bioactive glass (MBG), was first developed in 2004. This material has a highly ordered mesopore channel structure with a pore size ranging from 5–20 nm [1]. Compared to non-mesopore bioactive glass (BG), MBG possesses a more optimal surface area, pore volume and improved in vitro apatite mineralization in simulated body fluids [1,2]. Vallet-Regí et al. has systematically investigated the in vitro apatite formation of different types of mesoporous materials, and they demonstrated that an apatite-like layer can be formed on the surfaces of Mobil Composition of Matters (MCM)-48, hexagonal mesoporous silica (SBA-15), phosphorous-doped MCM-41, bioglass-containing MCM-41 and ordered mesoporous MBG, allowing their use in biomedical engineering for tissue regeneration [2-4]. Chang et al. has found that MBG particles can be used for a bioactive drug-delivery system [5,6]. Our study has shown that MBG powders, when incorporated into a poly (lactide-co-glycolide) (PLGA) film, significantly enhance the apatite-mineralization ability and cell response of PLGA films. compared to BG [7]. These studies suggest that MBG is a very promising bioactive material with respect to bone regeneration. It is known that for bone defect repair, tissue engineering represents an optional method by creating three-dimensional (3D) porous scaffolds which will have more advantages than powders or granules as 3D scaffolds will provide an interconnected macroporous network to allow cell migration, nutrient delivery, bone ingrowth, and eventually vascularization [8]. For this reason, we try to apply MBG for bone tissue engineering by developing MBG scaffolds. However, one of the main disadvantages of MBG scaffolds is their low mechanical strength and high brittleness; the other issue is that they have very quick degradation, which leads to an unstable surface for bone cell growth limiting their applications. Silk fibroin, as a new family of native biomaterials, has been widely studied for bone and cartilage repair applications in the form of pure silk or its composite scaffolds [9-14]. Compared to traditional synthetic polymer materials, such as PLGA and poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV), the chief advantage of silk fibroin is its water-soluble nature, which eliminates the need for organic solvents, that tend to be highly cytotoxic in the process of scaffold preparation [15]. Other advantages of silk scaffolds are their excellent mechanical properties, controllable biodegradability and cytocompatibility [15-17]. However, for the purposes of bone tissue engineering, the osteoconductivity of pure silk scaffolds is suboptimal. It is expected that combining MBG with silk to produce MBG/silk composite scaffolds would greatly improve their physiochemical and osteogenic properties for bone tissue engineering application. Therefore, in this chapter, we will introduce the research development of MBG/silk scaffolds for bone tissue engineering.

Three-dimensional printing of hierarchical and tough mesoporous bioactive glass scaffolds with a controllable pore architecture, excellent mechanical strength and mineralization ability

New-generation biomaterials for bone regenerations should be highly bioactive, resorbable and mechanically strong. Mesoporous bioactive glass (MBG), as a novel bioactive material, has been used for the study of bone regeneration due to its excellent bioactivity, degradation and drug-delivery ability; however, how to construct a 3D MBG scaffold (including other bioactive inorganic scaffolds) for bone regeneration still maintains a significant challenge due to its/their inherit brittleness and low strength. In this brief communication, we reported a new facile method to prepare hierarchical and multifunctional MBG scaffolds with controllable pore architecture, excellent mechanical strength and mineralization ability for bone regeneration application by a modified 3D-printing technique using polyvinylalcohol (PVA), as a binder. The method provides a new way to solve the commonly existing issues for inorganic scaffold materials, for example, uncontrollable pore architecture, low strength, high brittleness and the requirement for the second sintering at high temperature. The obtained 3D-printing MBG scaffolds possess a high mechanical strength which is about 200 times for that of traditional polyurethane foam template-resulted MBG scaffolds. They have highly controllable pore architecture, excellent apatite-mineralization ability and sustained drug-delivery property. Our study indicates that the 3D-printed MBG scaffolds may be an excellent candidate for bone regeneration.

Chitosan adhesive for laser tissue repair: In vitro characterization

Background and Objectives Laser tissue repair usually relies on hemoderivate protein solders, based on serum albumin. These solders have intrinsic limitations that impair their widespread use, such as limited tensile strength of repaired tissue, poor solder solubility, and brittleness prior to laser denaturation. Furthermore, the required activation temperature of albumin solders (between 65 and 70°C) can induce significant thermal damage to tissue. In this study, we report on the design of a new polysaccharide adhesive for tissue repair that overcomes some of the shortcomings of traditional solders. Study Design/Materials and Methods Flexible and insoluble strips of chitosan adhesive (elastic modulus ~6.8 Mpa, surface area ~34 mm2, thickness ~20 µm) were bonded onto rectangular sections of sheep intestine using a diode laser (continuous mode, 120 ± 10 mW, = λ 808 nm) through a multimode optical fiber with an irradiance of ~15 W/cm2. The adhesive was based on chitosan and also included indocyanin green dye (IG). The temperature between tissue and adhesive was measured using a small thermocouple (diameter ~0.25 mm) during laser irradiation. The repaired tissue was tested for tensile strength by a calibrated tensiometer. Murine fibroblasts were cultured in extracted media from chitosan adhesive to assess cytotoxicity via cell growth inhibition in a 48 hours period. Results Chitosan adhesive successfully repaired intestine tissue, achieving a tensile strength of 14.7 ± 4.7 kPa (mean ± SD, n = 30) at a temperature of 60-65°C. Media extracted from chitosan adhesive showed negligible toxicity to fibroblast cells under the culture conditions examined here. Conclusion A novel chitosan-based adhesive has been developed, which is insoluble, flexible, and adheres firmly to tissue upon infrared laser activation.

Flexible Ag electrode for use in organic photovoltaics

High efficiency organic photovoltaic cells discussed in literature are normally restricted to devices fabricated on glass substrates. This is a consequence of the extreme brittleness and inflexibility of the commonly used transparent conductive oxide electrode, indium tin oxide (ITO). This shortcoming of ITO along with other concerns such as increasing scarcity of indium, migration of indium to organic layer, etc. makes it imperative to move away from ITO. Here we demonstrate a highly flexible Ag electrode that possesses low sheet resistances even in ultra-thin layers. It retains its conductivity under severe bending stresses where ITO fails completely. A P3HT:PCBM blend organic solar cell fabricated on this highly flexible electrode gives an efficiency of 2.3%.

Organic photovoltaics using thin gold film as an alternative anode to indium tin oxide

Indium Tin Oxide (ITO) is the most commonly used anode as a transparent electrode and more recently as an anode for organic photovoltaics (OPVs). However, there are significant drawbacks in using ITO which include high material costs, mechanical instability including brittleness and poor electrical properties which limit its use in low-cost flexible devices. We present initial results of poly(3-hexylthiophene): phenyl-C61-butyric acid methyl ester OPVs showing that an efficiency of 1.9% (short-circuit current 7.01 mA/cm2, open-circuit voltage 0.55 V, fill factor 0.49) can be attained using an ultra thin film of gold coated glass as the device anode. The initial I-V characteristics demonstrate that using high work function metals when the thin film is kept ultra thin can be used as a replacement to ITO due to their greater stability and better morphological control.

A generic design environment for the rural industry knowledge acquisition

This paper describes a new knowledge acquisition method using a generic design environment where context-sensitive knowledge is used to build specific DSS for rural business. Although standard knowledge acquisition methods have been applied in rural business applications, uptake remains low and familiar weaknesses such as obsolescence and brittleness apply. We describe a decision support system (DSS) building environment where contextual factors relevant to the end users are directly taken into consideration. This "end user enabled design environment" (EUEDE) engages both domain experts in creating an expert knowledge base and business operators/end users (such as farmers) in using this knowledge for building their specific DSS. We document the knowledge organisation for the problem domain, namely a dairy industry application. This development involved a case-study research approach used to explore dairy operational knowledge. In this system end users can tailor their decision-making requirements using their own judgement to build specific DSSs. In a specific end user's farming context, each specific DSS provides expert suggestions to assist farmers in improving their farming practice. The paper also shows the environment's generic capability.

Role of heat treatment in the processing and quality of oat flakes

This thesis reports on investigations into the influence of heat treatment on the manufacturing of oat flakes. Sources of variation in the oat flake quality are reviewed, including the whole chain from the farm to the consumer. The most important quality parameters of oat flakes are the absence of lipid hydrolysing enzymes, specific weight, thickness, breakage (fines), water absorption. Flavour, colour and pasting properties are also important, but were not included in the experimental part of this study. Of particular interest was the role of heat processing. The first possible heat treatment may occur already during grain drying, which in Finland generally happens at the farm. At the mill, oats are often kilned to stabilise the product by inactivating lipid hydrolysing enzymes. Almost invariably steaming is used during flaking, to soften the groats and reduce flake breakage. This thesis presents the use of a material science approach to investigating a complex system, typical of food processes. A combination of fundamental and empirical rheological measurements was used together with a laboratory scale process to simulate industrial processing. The results were verified by means of industrial trials. Industrially produced flakes at three thickness levels (nominally 0.75, 0.85 and 0.90 mm) were produced from kilned and unkilned oat groats, and the flake strength was measured at different moisture contents. Kilning was not found to significantly affect the force required to puncture a flake with a 2mm cylindrical probe, which was taken as a measure of flake strength. To further investigate how heat processing contributes to flake quality, dynamic mechanical analysis was used to characterise the effect of heat on the mechanical properties of oats. A marked stiffening of the groat, of up to about 50% increase in storage modulus, was observed during first heating at around 36 to 57°C. This was also observed in tablets prepared from ground groats and extracted oat starch. This stiffening was thus attributed to increased adhesion between starch granules. Groats were steamed in a laboratory steamer and were tempered in an oven at 80 110°C for 30 90 min. The maximum force required to compress the steamed groats to 50% strain increased from 50.7 N to 57.5 N as the tempering temperature was increased from 80 to 110°C. Tempering conditions also affected water absorption. A significantly higher moisture content was observed for kilned (18.9%) compared to unkilned (17.1%) groats, but otherwise had no effect on groat height, maximum force or final force after a 5 s relaxation time. Flakes were produced from the tempered groats using a laboratory flaking machine, using a roll gap of 0.4 mm. Apart from specific weight, flake properties were not influenced by kilning. Tempering conditions however had significant effects on the specific weight, thickness and water absorption of the flakes, as well as on the amount of fine material (<2 mm) produced during flaking. Flake strength correlated significantly with groat strength and flake thickness. Trial flaking at a commercial mill confirmed that groat temperature after tempering influenced water absorption. Variation in flake strength was observed , but at the groat temperatures required to inactivate lipase, it was rather small. Cold flaking of groats resulted in soft, floury flakes. The results presented in this thesis suggest that heating increased the adhesion between starch granules. This resulted in an increase in the stiffness and brittleness of the groat. Brittle fracture, rather than plastic flow, during flaking could result in flaws and cracks in the flake. These would be expected to increase water absorption. This was indeed observed as tempering temperature increased. Industrial trials, conducted with different groat temperatures, confirmed the main findings of the laboratory experiments. The approach used in the present study allowed the systematic study of the effect of interacting process parameters on product quality. There have been few scientific studies of oat processing, and these results can be used to understand the complex effects of process variables on flake quality. They also offer an insight into what happens as the oat groat is deformed into a flake.

Prediction of fatigue strength in plain and reinforced concrete beams

A fatigue crack propagation model for concrete is proposed based on the concepts of fracture mechanics. This model takes into account the loading history, frequency of applied load, and size, effect parameters. Using this model, a method is described based on linear elastic fracture mechanics to assess the residual strength of cracked plain and reinforced concrete (RC) beams. This could be used to predict the residual strength (load carrying capacity) of cracked or damaged plain and reinforced concrete beams at a given level of damage. It has been seen that the fatigue crack propagation rate increases as. the size of plain concrete, beam increases indicating an increase in brittleness. In reinforced concrete (RC) beams, the fracture process becomes stable only when the beam is sufficiently reinforced.

Nonlinear fracture properties of concrete-concrete interfaces

The fracture properties of different concrete-concrete interfaces are determined using the Bazant's size effect model. The size effect on fracture properties are analyzed using the boundary effect model proposed by Wittmann and his co-workers. The interface properties at micro-level are analyzed through depth sensing micro-indentation and scanning electron microscopy. Geometrically similar beam specimens of different sizes having a transverse interface between two different strengths of concrete are tested under three-point bending in a closed loop servo-controlled machine with crack mouth opening displacement control. The fracture properties such as, fracture energy (G(f)), length of process zone (c(f)), brittleness number (beta), critical mode I stress intensity factor (K-ic), critical crack tip opening displacement CTODc (delta(c)), transitional ligament length to free boundary (a(j)), crack growth resistance curve and micro-hardness are determined. It is seen that the above fracture properties decrease as the difference between the compressive strength of concrete on either side of the interface increases. (C) 2010 Elsevier Ltd. All rights reserved.

Research on laser welding of cast Ni-based superalloy K418 turbo disk and alloy steel 42CrMo shaft

Exploratory experiments of laser welding cast Ni-based superalloy K418 turbo disk and alloy steel 42CrMo shaft were conducted. Microstructure of the welded seam was characterized by optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD), energy-dispersive spectrometer (EDS). Mechanical properties of the welded seam were evaluated by microhardness and tensile strength testing. The corresponding mechanisms were discussed in detail. Results showed that the laser-welded seam had non-equilibrium solidified microstructures consisting of FeCr0.29Ni0.16C0.06 austenite solid solution dendrites as the dominant and some fine and dispersed Ni3Al gamma' phase and Laves particles as well as little amount of MC short stick or particle-like carbides distributed in the interdendritic regions. The average microhardness of the welded seam was relatively uniform and lower than that of the base metal due to partial dissolution and suppression of the strengthening phase gamma' to some extent. About 88.5% tensile strength of the base metal was achieved in the welded joint because of a non-full penetration welding and the fracture mechanism was a mixture of ductility and brittleness. The existence of some Laves particles in the welded seam also facilitated the initiation and propagation of the microcracks and microvoids and hence, the detrimental effects of the tensile strength of the welded joint. The present results stimulate further investigation on this field. (c) 2006 Elsevier B.V. All rights reserved.