Observation of fatigue damage in structural steel by scanning atomic force microscopy

Fatigue slip bands and plastic deformation around fatigue microcracks were observed by scanning atomic force microscopy. In fatigue slip bands, extrusions were observed but intrusions were not detected. Large extrusions were found in slip bands whose traces at specimen surface were almost perpendicular to the loading axis. Microcracks propagated under mixed mode condition of Mode I, Mode II, and Mode III.     

Morphologies and characteristics of deformation induced martensite during low cycle fatigue behaviour of austenitic stainless steel

Quantification, formation and nucleation micro-mechanisms of deformation induced martensite during low cycle fatigue behaviour of austenitic stainless steel have been investigated at various strain amplitudes tested at ambient temperature. The evolutionary deformation induced martensite has been quantified through magnetic measurement technique. It has been found that as strain amplitude increases, the volume fraction of deformation induced martensite increases. Extensive analytical transmission electron microscopy studies showed more than one nucleation site for martensitic transformation and the transformation micro-mechanisms have been observed to be: γ (fcc) → ? (hcp), γ (fcc) → α′ (bcc), γ (fcc) → deformation twins → α′ (bcc) and γ (fcc) → ? (hcp) → α′ (bcc).     

Roughness determination of plasma-modified surface layers with atomic force microscopy

Graphite surfaces exposed to the deuterium plasma in the TEXTOR tokamak were characterized in detail by means of scanning probe microscopy, ion beam analysis and colorimetry methods. The aim is to study the composition and structure of thin layer deposits formed on surfaces subjected to the tokamak plasma. The surface roughness was measured and parametrized in terms of fractal dimension and scaling constant. Several different methods for the fractal analysis of plasma-exposed surfaces have been critically evaluated. The main emphasis of this paper is on the correlation between surface roughness (fractal parameters), the amount of deposited atoms and the layer thickness.     

Microstructural effects on the short crack behaviour of a stainless steel weld metal during low-cycle fatigue

An experimental study into microstructural effects on short fatigue crack behaviour of 19 stainless steel weld metal smooth specimens during low-cycle fatigue is performed by a so-called ‘effective short fatigue crack criterion’. This material has a mixed microstructure in which it is difficult to distinguish the grains and measure the grain diameter. The columnar grain structure is made up of matrix-rich δ ferrite bands, and the distance between the neighbouring rich δ ferrite bands is an appropriate measurement for characterizing this structure. Particularly, the effective short fatigue cracks (ESFCs) always initiate from the bands of δ ferrite in the matrix in the weakest zone on one of the specimen surface zones which is orientated in accordance with the inner or outer surface of welded pipe from which the specimens were machined. These cracks exhibit characteristics of the microstructural short crack (MSC) and the physically small crack (PSC) stages. The average length of the ESFCs at the transition between MSC and PSC behaviour is ≈40 μm, while the corresponding fatigue life fraction is ≈0.3 at this transition. Different from previous test observations, the growth rate of the dominant effective short fatigue crack in the MSC stage still shows a decrease with fatigue cycling under the present low-cycle fatigue loading levels. A statistical evolution analysis of the growth rates reveals that the short fatigue crack growth is a damage process that gradually evolves from a non-ordered (chaotic) to a perfectly independent stochastic process, and then to an ordered (history-dependent) stochastic state. Correspondingly, the microstructural effects gradually evolve from a weak effect to a strong one in the MSC stage, which maximizes at the transition point. In the PSC stage, the effects gradually evolve from a strong to weak state. This improves our understanding that the short crack behaviour in the PSC stage is mainly related to the loading levels rather than microstructural effects.     

Modelling the effects of surface finish on fatigue limit in austenitic stainless steels

Existing short fatigue crack models have been reviewed to determine the most suitable fatigue model to analyse the effect of the surface finish on the fatigue limit of Type 304 austenitic stainless steels. A mechanistic model firstly proposed by Navarro and Rios (N‐R model) was selected as the most suitable generic model, because the model can include the effects of surface finishing parameters such as surface roughness and residual stress depth profile on the fatigue limit. The N‐R model has been implemented for fatigue specimens with various surface finishing conditions, and the effect of the surface finish on the fatigue limit was simulated. The material/surface properties required for the implementation were fully characterized by experiments. The applicability of the model to this study was also discussed. It is concluded that a development of the model would be required for proper prediction of the surface effects on fatigue in austenitic stainless steels.     

原子力显微镜与X射线光电子能谱对ITO表面改性的研究

采用氧气等离子体(OP)处理对氧化铟锡(ITO)薄膜进行表面改性,通过原子力显微镜(AFM)、X射线光电子能谱(XPS)和四探针等测试手段对薄膜样品进行表征,研究了OP处理对ITO表面性质的影响.实验结果表明OP处理有效去除了ITO表面的污染物,优化了ITO表面的化学组分,降低了ITO表面的粗糙度和方块电阻,改善了ITO的表面形态.与此同时,通过XPS监测研究了OP处理后ITO表面化学组分随老化时间的变化,结果显示经过优化的化学组分随老化时间增加而逐渐退化.另外,以OP处理后经过不同老化时间的ITO样品作为空穴注入电极,制备了有机电致发光器件(OELD),通过测试器件的电压-电流-亮度特性,进一步研究了ITO表面性质对于OELD光电性能的影响.     

Nanoscopic fatigue and stress corrosion crack growth behaviour in a high-strength stainless steel visualized in situ by atomic force microscopy

In situ atomic force microscope (AFM) imaging of the fatigue and stress corrosion (SC) crack in a high‐strength stainless steel was performed, under both static and dynamic loading. The AFM systems used were (1) a newly developed AFM‐based system for analysing the nanoscopic topographies of environmentally induced damage under dynamic loads in a controlled environment and (2) an AFM system having a large sample stage together with a static in‐plane loading device. By using these systems, in situ serial clear AFM images of an environmentally induced crack under loading could be obtained in a controlled environment, such as in dry air for the fatigue and in an aqueous solution for the stress corrosion cracking (SCC). The intergranular static SC crack at the free corrosion had a sharp crack tip when it grew straight along a grain boundary. The in situ AFM observations showed that the fatigue crack grew in a steady manner on the order of sub‐micrometre. The same result was obtained for the static SC crack under the free corrosion, growing straight along a grain boundary. In these cases, the crack tip opening displacement (CTOD) remained constant. However, as the static SC crack was approaching a triple grain junction, the growth rate became smaller, the CTOD value increased and the hollow ahead of the crack tip became larger. After the crack passed through the triple grain junction, it grew faster with a lower CTOD value; the changes in the CTOD value agreed with those of the crack growth rate. At the cathodic potential, the static SC crack grew in a zigzag path and in an unsteady manner, showing crack growth acceleration and retardation. This unsteady crack growth was considered to be due to the changes in the local hydrogen content near the crack tip. The changes in the CTOD value also agreed with those of the crack growth rate. The CTOD value in the corrosive environment was influenced by the microstructure of the material and the local hydrogen content, showing a larger scatter band, whereas the CTOD value of the fatigue crack in dry air was determined by the applied stress intensity factor, with a smaller scatter band. In addition, the CTOD value in the corrosive environment under both static and dynamic loading was smaller than that of the fatigue crack; the environmentally induced crack had a sharper crack tip than the fatigue crack in dry air.     

Reverted austenite in PH 13-8 Mo maraging steels

The mechanical properties of maraging steels are strongly influenced by the presence of reverted austenite. In this study, the morphology and chemical composition of reverted austenite in a corrosion resistant maraging steel was characterized using transmission electron microscopy (TEM) and atom probe tomography (APT). Two types of austenite, i.e. granular and elongated, are present after aging at 575 °C, whereby the content of the latter increases during aging. The investigations revealed that the austenite phase is enriched in Ni, which prevents the transformation to martensite during cooling. Inside and next to the austenitc areas, Mo and Cr-rich carbides, which form during the aging treatment, were found. Various aging treatments were performed to obtain the activation energy for the formation of reverted austenite. Additionally, the experimental data are compared with thermodynamic and kinetic simulations. Based on these results and the chemical composition changes of the phases, a model for the formation of reverted austenite is presented. It is concluded that precipitation of B2-ordered NiAl and formation of reverted austenite take place simultaneously during aging and that dissolution of precipitates is not essential for the initial formation of reverted austenite.     

A comparative study of the fretting fatigue behavior of 4340 steel and PH 13-8 Mo stainless steel

The fretting fatigue behavior of two high strength structural steels, PH 13-8 Mo stainless steel and quenched and tempered 4340 steel, is investigated. Both were heat treated to a similar hardness (43-44 HRC), comparable to the condition used in structural components. Both materials experienced significant reductions in fatigue strength due to fretting, with PH 13-8 Mo stainless steel exhibiting a greater susceptibility to fretting than 4340 steel, when operating in the mixed fretting regime. The use of fretting pads with different surface profiles showed that contact geometry did not significantly influence the fretting fatigue behavior of either steel for the range of loading conditions considered. The fretting fatigue lives are discussed in light of the low cycle fatigue and crack growth rate behavior of these steels. The life trends in fretting fatigue correlate more closely to the low cycle fatigue behavior.     

Growth behaviour of small surface fatigue cracks in AISI 304 stainless steel

A series of axial tensile fatigue tests (R = 0.1) was carried out to investigate the initiation and the growth behaviours of very small surface fatigue cracks under two different surface conditions (viz. smooth and pitted surfaces) of AISI 304 stainless steel at room temperature. This paper deals with both of the two approaches regarding the analysis of fatigue: the approach based on the concept of fracture mechanics and low cycle fatigue. In particular, both the initiation and growth of cracks and the coalescence of small cracks by fatigue in the specimen have been investigated by the methods of surface replicas and photomicrographs. Quantitative information such as the initiation period, growth and coalescence behaviours of small cracks, and crack growth properties were systematically obtained. The results show that the accurate determination of these parameters is critical for the application of fracture mechanics to fatigue life assessment.     

Reformed austenite transformation during fatigue crack propagation of 13%Cr-4%Ni stainless steel

In the as-quenched state, 13%Cr-4%Ni martensitic stainless steels are essentially 100% martensitic. However, a certain amount of austenite is formed during the tempering of this alloy. This reformed austenite is thermally stable at room temperature but can transform to martensite under stress. This transformation is known to happen during impact testing but it has never been established if it occurs during fatigue crack propagation. This study presents the results of X-ray diffraction measurements of reformed austenite before and after crack growth testing. It has been found that reformed austenite does transform to martensite at the crack tip and that this transformation occurs even at a low stress intensity factor. Low-cycle fatigue tests were conducted to verify austenite transformation under cyclic straining. It was found that reformed austenite transforms only partially during the first strain reversal but that essentially all austenite has disappeared after 100 cycles. The relation between austenite transformation under low-cycle fatigue and its transformation during crack growth is also discussed.     

Fatigue of additively manufactured 316L stainless steel: The influence of porosity and surface roughness

The fatigue behaviour of additively manufactured (AM) 316L stainless steel is investigated with the main emphasis on internal porosity and surface roughness. A transition between two cases of failure are found: failure from defects in the surface region and failure from the internal defects. At low applied load level (and consequently a high number of cycles to failure), fatigue is initiating from defects in the surface region, while for high load levels, fatigue is initiating from internal defects. Porosities captured by X‐ray computed tomography (XCT) are compared with the defects initiating fatigue cracks, obtained from fractography. The fatigue data are synthesised using stress intensity factor (SIF) of the internal and surface defects on the fracture surface.     

Deformation and microstructure evolution of a duplex stainless steel under out-of-phase thermo-mechanical fatigue

Abstract

Thermo-mechanical fatigue (TMF) of the duplex stainless steel SAF2205 (X2CrNiMoN22-5-3) was studied in the temperature range of 100–350°C. The tests were carried out on the duplex steel and on single-phase ferritic (X6Cr17, AISI 430) and austenitic steels (X2CrNiMo18-14-3, AISI 316L) similar to the two phases of the duplex steel for comparison. The mechanical behaviour of the three steels is analysed and discussed together with microstructural investigations by scanning electron microscopy, including electron backscatter diffraction and electron channelling contrast imaging.     

Removing material using atomic force microscopy with single- and multiple-tip sources

Atomic force microscopy (AFM) has been an effective material removing tool for fabricating various nanostructures because of its sub-nanometer precision and simplicity in operation. AFM material removing techniques have evolved from a solely mechanical process to one in which the tip can be loaded by additional energy sources, such as thermal, electric, or chemical, to enhance its fabrication abilities. In this paper, these material removing techniques are reviewed with an emphasis on their capabilities and recent progress. The recent hardware and software developments are first presented to provide a general view on the current status of the technology to be assessed. Following an overview of the feasibility and effectiveness of using mechanical scratching for removing various types of soft and hard materials, the processes of a wide range of approaches using multiple tip sources are then assessed with a focus on their principles, versatilities, and potentials for future applications.     

Surface evaluation of whey protein films by atomic force microscopy and water vapour permeability analysis

The atomic force microscopy (AFM) technique is a powerful tool for studying surfaces and has been used to provide qualitative and quantitative information about nanometer‐scale matter properties that are often inaccessible by any other experimental technique. In this work AFM was used to evaluate the surfaces of edible films produced with whey protein concentrate (WPC). The morphology and the roughness of the films were analysed. The effects of WPC and plasticizer concentration were characterized in terms of water vapour permeability (WVP) and roughness parameters. Roughness was calculated through the images captured with AFM. AFM can be useful to identify structural changes of the film resulting from sample preparation. The results showed a relation between water vapour permeability and area roughness, through different sample preparation. The analyses of topography through roughness obtained with AFM, demonstrated the correlation between the morphology of the film, obtained with nanometer resolution and WVP. Copyright © 2004 John Wiley & Sons, Ltd.     

In Situ Observations of the Microstructural Evolution during Heat Treatment of a PH 13-8 Mo Maraging Steel

The standard heat treatment of PH 13-8 Mo maraging steels consists of solution annealing and subsequent aging. Herein, it is investigated how an additional intercritical annealing step prior to aging affects the microstructure, and, consequently, the mechanical properties of a PH 13-8 Mo maraging steel. In situ techniques by means of high-temperature electron backscatter diffraction and high-temperature X-ray diffraction are applied to study the microstructural changes during intercritical annealing and subsequent aging. In addition, high-resolution investigation methods, such as transmission electron microscopy and atom probe tomography supplemented by transmission Kikuchi diffraction, are used for an in-depth characterization of the microstructure. The results reveal that a diffusion-controlled martensite to austenite transformation accompanied by partitioning of the substitutional atoms Cr, Ni, and Mo takes place during intercritical annealing. As a result of partitioning during intercritical annealing, an inhomogeneous distribution of Ni remains in the microstructure after the martensitic transformation. Consequently, the formation of reverted austenite is facilitated during subsequent aging due to existing Ni-enriched zones in martensite. Since the fracture toughness is significantly enhanced compared to the standard heat treatment, it is suggested that this improvement is related to the increased phase fraction of reverted austenite.     

基于原子力显微镜技术的沥青与矿料表面粗糙度及黏附特性

采用原子力显微镜技术(AFM)的轻敲和力曲线模式,在微观尺度下对沥青与矿料表面的二维图像和三维形貌信息进行采集和分析,并测试和计算表征材料物理黏结特性的表面能。测试和分析结果显示,不同油源的沥青具有明显不同的化学组分和表面粗糙度,具有蜂形结构的沥青表面粗糙度更大。老化将明显减少沥青的表面粗糙度,降低其表面能,进而对沥青与矿料的黏附产生不利影响。结合宏观的黏附拉拔力学试验,对沥青和矿料表面粗糙度、表面能与宏观拉拔强度间的关联进行统计分析。结果表明,对于含蜂形结构的沥青,沥青和矿料表面粗糙度对黏附力学性能较为重要;而对于不含蜂形结构的沥青,其与矿料的黏附性更决定于所选材料的表面能,即两种材料间的物理黏结作用。     

Application of dynamic impedance spectroscopy to atomic force microscopy

Abstract

Atomic force microscopy (AFM) is a universal imaging technique, while impedance spectroscopy is a fundamental method of determining the electrical properties of materials. It is useful to combine those techniques to obtain the spatial distribution of an impedance vector. This paper proposes a new combining approach utilizing multifrequency scanning and simultaneous AFM scanning of an investigated surface.     

Effect of strain rate on high-temperature low-cycle fatigue of 17-4 PH stainless steels

The effect of strain rate (10⁻², 10⁻³ and 10⁻⁴ s⁻¹) on the low-cycle fatigue (LCF) behavior was investigated for 17-4 PH stainless steels in three different conditions at temperatures of 300–500 °C. The cyclic stress response (CSR) for Condition A tested at 300 and 400 °C showed cyclic hardening due to an influence of dynamic strain aging (DSA). An in situ precipitation-hardening effect was found to be partially responsible for the cyclic hardening in Condition A at 400 °C. For H900 and H1150 conditions tested at 300 and 400 °C, the CSR exhibited a stable stress level before a fast drop in load indicating no cyclic hardening or softening. At 500 °C, cyclic softening was observed for all given material conditions because of a thermal dislocation recovery mechanism. The cyclic softening behavior in Conditions A and H900 tested at 500 °C is attributed partially to coarsening of the Cu-rich precipitates. The LCF life for each material condition, tested at a given temperature, decreased with decreasing strain rate as a result of an enhanced DSA effect. At all given testing conditions, transgranular cracking was the common fatigue fracture mode.