Influence of grinding operations on surface integrity and chloride induced stress corrosion cracking of stainless steels

Stainless steels were developed in the early 20th century and are used where both the mechanical properties of steels and corrosion resistance are required. There is continuous research to allow stainless steel components to be produced in a more economical way and be used in more harsh environments. A necessary component in this effort is to correlate the service performance with the production processes. The central theme of this thesis is the mechanical grinding process.  This is commonly used for producing stainless steel components, and results in varied surface properties that will strongly affect their service life. The influence of grinding parameters including abrasive grit size, machine power and grinding lubricant were studied for 304L austenitic stainless steel (Paper II) and 2304 duplex stainless steel (Paper I). Surface integrity was proved to vary significantly with different grinding parameters. Abrasive grit size was found to have the largest influence. Surface defects (deep grooves, smearing, adhesive/cold welding chips and indentations), a highly deformed surface layer up to a few microns in thickness and the generation of high level tensile residual stresses in the surface layer along the grinding direction were observed as the main types of damage when grinding stainless steels. A large degree of residual stress anisotropy is interpreted as being due to mechanical effects dominating over thermal effects. The effect of grinding on stress corrosion cracking behaviour of 304L austenitic stainless steel in a chloride environment was also investigated (Paper III). Depending on the surface conditions, the actual loading by four-point bend was found to deviate from the calculated value using the formula according to ASTM G39 by different amounts. Grinding-induced surface tensile residual stress was suggested as the main factor to cause micro-cracks initiation on the ground surfaces. Grinding along the loading direction was proved to increase the susceptibility to chloride-induced SCC, while grinding perpendicular to the loading direction improved SCC resistance. The knowledge obtained from this work can provide a reference for choosing appropriate grinding parameters when fabricating stainless steel components; and can also be used to help understanding the failure mechanism of ground stainless steel components during service.

Intergranular Corrosion and Stress Corrosion Cracking of Extruded AA6005A

A research program focused on understanding the intergranular corrosion (IGC) and stress corrosion cracking (SCC) behavior of AA6005A aluminum extrusions is presented in this dissertation. The relationship between IGC and SCC susceptibility and the mechanisms of SCC in AA6005A extrusions were studied by examining two primary hypotheses. IGC susceptibility of the elongated grain structure in AA6005A exposed to low pH saltwater was found to depend primarily on the morphology of Cu-containing precipitates adjacent to the grain boundaries in the elongated grain structure. IGC susceptibility was observed when a continuous (or semi-continuous) film of Cu-containing phase was present along the grain boundaries. When this film coarsened to form discrete Cu-rich precipitates, no IGC was observed. The morphology of the Cu-rich phase depended on post-extrusion heat treatment. The rate of IGC penetration in the elongated grain structure of AA6005A-T4 and AA6005A-T6 extrusions was found to be anisotropic with IGC propagating most rapidly along the extrusion direction, and least rapidly along the through thickness direction. A simple 3-dimensional geometric model of the elongated grain structure was accurately described the observed IGC anisotropy, therefore it was concluded that the anisotropic IGC susceptibility in the elongated grain structure was primarily due to geometric elongation of the grains. The velocity of IGC penetration along all directions in AA6005A-T6 decreased with exposure time. Characterization of the local environment within simulated corrosion paths revealed that a pH gradient existed between the tip of the IGC path and the external environment. Knowledge of the local environment within an IGC path allowed development of a simple model based on Fick's first law that considered diffusion of Al3+ away from the tip of the IGC path. The predicted IGC velocity agreed well with the observed IGC velocity, therefore it was determined that diffusion of Al3+ was the primary factor in determining the velocity of IGC penetration. The velocity of crack growth in compact tensile (CT) specimens of AA6005A-T6 extrusion exposed to 3.5% NaCl at pH = 1.5 was nearly constant over a range of applied stress intensities, exposure times, and crack lengths. The crack growth behavior of CT specimens of AA6005A-T6 extrusion exposed to a solution of 3.5% NaCl at pH = 2.0 exhibited similar behavior, but the crack velocity was ~10.5X smaller than that those exposed to a solution at pH =1.5. Analysis of the local stress state and polarization behavior at the crack tip predicted that increasing the pH of the bulk solution from 1.5 to 2.0 would decrease the corrosion current density at the crack tip by approximately 11.8X. This predicted decrease in corrosion current density was in reasonable agreement with the observed decrease in SCC velocity associated with increasing the solution pH from 1.5 to 2.0. The agreement between the predicted and observed SCC velocities suggested that the electrochemical reactions controlling SCC in AA6005A-T6 extrusions are ultimately controlled by the pH gradient that exists between the crack tip and external environment.

Stress corrosion crack propagation in AerMet 100

Fracture mechanics tests were carried out for AerMet 100 in distilled water and NaCl (3.5 and 35 gl(-1)). The initiation period at higher values of the stress intensity factor indicated that load application in the stress corrosion cracking (SCC) environment is a necessary but not sufficient factor for SCC and that time is needed for some other factor (e.g., the local hydrogen concentration) to reach an appropriate value. The threshold stress intensity factor, K-ISSC, was found to increase with decreasing NaCl concentration. The plateau stress corrosion crack velocity was 2 x 10(-8) ms(-1) for NaCl (3.5 and 35 gl(-1)). The fracture mode was transgranular with small areas of an intergranular nature. (C) 1998 Chapman & Hall.

Effects of hydrogen assisted stress corrosion on damage tolerance of a high-strength duplex stainless steel wire for prestressing concrete

The study brings new insights on the hydrogen assisted stress corrosion on damage tolerance of a high-strength duplex stainless steel wire which concerns its potential use as active reinforcement for concrete prestressing. The adopted procedure was to experimentally state the effect of hydrogen on the damage tolerance of cylindrical smooth and precracked wire specimens exposed to stress corrosion cracking using the aggressive medium of the standard test developed by FIP (International Prestressing Federation). Stress corrosion testing, mechanical fracture tests and scanning electron microscopy analysis allowed the damage assessment, and explain the synergy between mechanical loading and environment action on the failure sequence of the wire. In presence of previous damage, hydrogen affects the wire behavior in a qualitative sense, consistently to the fracture anisotropy attributable to cold drawing, but it does not produce quantitative changes since the steel fully preserves its damage tolerance.

Stress crrosion cracking fracture mechanisms in rock bolts

Rock bolts have failed by Stress Corrosion Cracking (SCC). This paper presents a detailed examination of the fracture surfaces in an attempt to understand the SCC fracture mechanism. The SCC fracture surfaces, studied using Scanning Electron Microscopy (SEM), contained the following different surfaces: Tearing Topography Surface (TTS), Corrugated Irregular Surface (CIS) and Micro Void Coalescence (MVC). TTS was characterised by a ridge pattern independent of the pearlite microstructure, but having a spacing only slightly coarser than the pearlite spacing. CIS was characterised as porous irregular corrugated surfaces joined by rough slopes. MVC found in the studied rock bolts was different to that in samples failed in a pure ductile manner. The MVC observed in rock bolts was more flat and regular than the pure MVC, being attributed to hydrogen embrittling the ductile material near the crack tip. The interface between the different fracture surfaces revealed no evidence of a third mechanism involved in the transition between fracture mechanisms. The microstructure had no effect on the diffusion of hydrogen nor on the fracture mechanisms. The following SCC mechanism is consistent with the fracture surfaces. Hydrogen diffused into the material, reaching a critical concentration level. The thus embrittled material allowed a crack to propagate through the brittle region. The crack was arrested once it propagated outside the brittle region. Once the new crack was formed, corrosion reactions started producing hydrogen that diffused into the material once again. (C) 2003 Kluwer Academic Publishers.

Linearly-increasing-stress testing of carbon steel in 4 N NaNO3 and in Bayer liquor

This paper reports the application of linearly increasing stress testing (LIST) to the study of stress corrosion cracking (SCC) of carbon steel in 4 N NaNO3 and in Bayer liquor. LIST is similar to the constant extension-rate testing (CERT) methodology with the essential difference that the LIST is load controlled whereas the CERT is displacement controlled. The main conclusion is that LIST is suitable for the study of the SCC of carbon steels in 4 N NaNO3 and in Bayer liquor. The low crack velocity in Bayer liquor and a measured maximum stress close to that of the reference specimen in air both indicate that a low applied stress rate is required to study SCC in this system. (C) 1998 Chapman & Hall.

EFFECT OF THE ADDITION OF CR AND NB ON THE MICROSTRUCTURE AND ELECTROCHEMICAL CORROSION OF HEAT-TREATABLE AL-ZN-MG ALLOYS

The effect of the addition of Cr and Nb on the microstructure and the electrochemical corrosion of the weldable, high-strength and stress corrosion cracking (SCC) resistant Al-5%Zn-1.67%Mg-0.23%Cu alloy (H) has been studied. Combined additions of the alloying elements, J (with Nb), L (with Cr) and O (with Cr and Nb) and different heat treatments, ST (cold-rolled), A (annealed), F (quenched), B (quenched and aged) and C (quenched in two steps and aged), to obtain different microstructures and hardness have been performed. To correlate the electrochemical corrosion with the microstructure of the specimens, corrosion potential (E(cor)) measurements in different chloride solutions were performed and optical microscopy, SEM, TEM and EDX were applied. In chloride solutions containing dissolved O-2 or H2O2, the present alloys were polarized up to the pitting attack. It was shown that the E(cor) measurements were very sensitive to the alloy composition and heat treatment, increasing in the order H < J < L < O < Al (for a given heat treatment) and F < A approximate to ST < B < C (for a given alloy). The MgZn2 precipitates of the annealed (A) and cold-rolled (ST) specimens were dissolved in chloride solutions containing oxidizing agents and pitting attack was shown to develop in the cavities where the precipitates were present. In the specimens B and C, the compositions of the precipitate free zones was found to be equal to that of the matrix solid solution and preferential intergranular attack was not evident, this being in agreement with their SCC resistance. The addition of Cr and Nb increased the pitting corrosion resistance. The effects of Cr and Nb were additive, that of Cr being predominant, either, in the E(cor) shift or in the increase in the pitting corrosion resistance.

Fracture propagation and stress corrosion in the case of dissimilar laser hybrid welded joints

The paper addresses the fracture propagation and stress corrosion behaviour of laser hybrid welds achieved between low carbon steel and stainless steel thin sheets. The crack propagation within these overmatched in strength welds was investigated by crack tip opening displacement (CTOD) on CT specimens notched transverse to the weld. A Digital Image Correlation System was used to qualify and estimate the initial crack length obtained by fatigue. The results are associated with the fractographic examinations of various regions of laser hybrid joints. Stress corrosion behaviour of the joint is also discussed.

Corrosion mechanisms of duplex stainless steels in the petrochemical industry

The recent search for new sources of hydrocarbons has led to production from very severe environments which can contain considerable amounts of carbon dioxide, hydrogen sulphide, and chloride ions, combined with temperatures which can exceed 100°C. Oil and gas production from such wells requires highly corrosion-resistant materials. The traditional solution of using carbon steel with additional protection is generally inadequate in these very-aggressive environments. Duplex stainless steels (DSS) are attractive candidates because of their high strength, good general corrosion resistance, excellent resistance to chloride-induced stress corrosion cracking, and good weldability. Although duplex stainless steels have a very good reputation in both subsea and topsides pipework, it is recognized that the tolerance of these materials to variations in microstructure and chemical composition are still not fully understood. The object of this paper is to review the corrosion behaviour of duplex stainless steels in the petrochemical industry, with particular emphasis on microstructures and the effect of changes in chemical composition.

ESEM observations of SCC initiation for 4340 high strength steel in distilled water

The stress corrosion cracking (SCC) initiation process for 4340 high strength steel in distilled water at room temperature was studied using a new kind of instrument: an environmental scanning electron microscope (ESEM). It was found that the applied stress accelerated oxide film formation which has an important influence on the subsequent SCC initiation. SCC was observed to initiate in the following circumstances: (1) cracking of a thick oxide film leading to SCC initiation along metal grain boundaries, (2) the initiation of pits initiating SCC in the metal and (3) SCC initiating from the edge of the specimen. All these three SCC initiation circumstances are consistent with the following model which couples SCC initiation with cracking of a surface protective oxide. There is a dynamic interaction between oxide formation, the applied stress, oxide cracking, pitting and the initiation of SCC. An aspect of the dynamic interaction is cracks forming in a protective surface oxide because of the applied stress, exposing to the water bare metal at the oxide crack tip, and oxidation of the bare metal causing crack healing. Oxide crack healing would be competing with the initiation of intergranular SCC if an oxide crack meets the metal surface at a grain boundary. If the intergranular SCC penetration is sufficiently fast along the metal grain boundary, then the crack yaws open preventing healing of the oxide crack. If intergranular SCC penetration is not sufficiently fast, then the oxidation process could produce sufficient oxide to fill both the stress corrosion crack and the oxide crack; in this case there would be initiation of SCC but only limited propagation of SCC. Stress-induced cracks in very thin oxide can induce pits which initiate SCC, and under some conditions such stress induced cracks in a thin oxide can directly initiate SCC.

Measurement of grain boundary composition for X52 pipeline steel

Analytical electron microscopy was used to measure the composition of grain boundaries (GBs) and interconstituent boundaries (IBs) of X52 pipeline steel using specimens about 40-60 nm in thickness. All elements of interest were examined with the exception of carbon. With this caveat; there was no segregation at proeutectoid ferrite GBs. This indicated that the commonly expected species S and P are not responsible for preferential corrosion of GBs during intergranular stress corrosion cracking of pipeline steels. Manganese was the only species measured to segregate at the IBs. Manganese segregated to the IBs between proeutectoid ferrite and pearlitic cementite, and desegregated from IBs between proeutectoid ferrite and pearlitic ferrite. The pearlitic cementite was Mn rich. There was no Mn segregation at the IBs between pearlitic ferrite and pearlitic cementite. The pattern of Mn segregation could be explained in terms of diffusion in the process zone ahead of the pearlite during the austenite to pearlite transformation and diffusion in the IBs between the proeutectoid ferrite and pearlite. (C) 1998 Acta Metallurgica Inc. Published by Elsevier Science Ltd. All rights reserved.

The crack tip strain field of AISI 4340 - Part I - Measurement technique

This is the first paper in a study on the influence of the environment on the crack tip strain field for AISI 4340. A stressing stage for the environmental scanning electron microscope (ESEM) was constructed which was capable of applying loads up to 60 kN to fracture-mechanics samples. The measurement of the crack tip strain field required preparation (by electron lithography or chemical etching) of a system of reference points spaced at similar to 5 mu m intervals on the sample surface, loading the sample inside an electron microscope, image processing procedures to measure the displacement at each reference point and calculation of the strain field. Two algorithms to calculate strain were evaluated. Possible sources of errors were calculation errors due to the algorithm, errors inherent in the image processing procedure and errors due to the limited precision of the displacement measurements. Estimation of the contribution of each source of error was performed. The technique allows measurement of the crack tip strain field over an area of 50 x 40 mu m with a strain precision better than +/- 0.02 at distances larger than 5 mu m from the crack tip. (C) 1999 Kluwer Academic Publishers.

The crack tip strain field of AISI 4340 - Part II - Experimental measurements

Crack tip strain maps have been measured for AISI 4340 high strength steel. No significant creep was observed. The measured values of CTOD were greater than expected from the HRR model. Crack tip branching was observed in every experiment. The direction of crack branching was in the same direction as a major ridge'' of epsilon(yy) strain, which in turn was in the same direction as predicted by the HRR model. Furthermore, the measured magnitudes of the epsilon(y)y strain in this same direction were in general greater than the values predicted by the HRR model. This indicates more plasticity in the crack tip region than expected from the HRR model. This greater plasticity could be related to the larger than expected CTOD values. The following discrepancies between the measured strain fields for AISI 4340 and the HRR predictions are noteworthy: (1) The crack branching. (2) Values of CTOD significantly higher than predicted by HRR. (3) The major ridge'' of epsilon(yy) strain an angle of about 60 degrees with the direction of overall propagation of the fatigue precrack, in which the measured magnitudes of the epsilon(yy) strain were greater than the values predicted by the HRR model. (4) Asymmetric shape of the plastic zone as measured by the epsilon(yy) strain. (5) Values of shear strain gamma(xy) significantly higher than predicted by the HRR model. (C) 1999 Kluwer Academic Publishers.

Implications of specimen preparation and of surface contamination for the measurement of the grain boundary carbon concentration of steels using x-ray microanalysis in an UHVFESTEM

The purpose of the present investigation was to gain an understanding of the nature of the carbon contamination on the surface of standard steel transmission electron spectroscopy (TEM) specimens, the effect of exposure of a clean specimen to normal laboratory air, and the efficacy of plasma-cleaning treatments. This knowledge is a necessary prerequisite to the development of appropriate specimen preparation and/or specimen cleaning methods. X-ray photoelectron spectroscopy in combination with argon ion beam profiling was used to characterize the specimen surfaces of X65 steel and 316 stainless steel. The only clean carbon-free surface obtained was that during argon etching of the sample in the surface analysis chamber. Any exposure of a previously cleaned sample to laboratory air resulted in a rapid carbon (hydrocarbon) contamination of the sample surface and the development of surface oxidation, Plasma cleaning with subsequent exposure of the specimen to the laboratory air also resulted in a carbon-contaminated surface. This suggests that procedures of preparation of TEM specimens of steels outside an ultrahigh vacuum chamber are unlikely to result in the lowering of contamination rates on specimens to levels where measurements for carbon in the grain boundaries are possible. What is needed is a cleaning system as an integral part of the specimen insertion system into the field-emission scanning transmission electron microscope. This cleaning could be carried out by argon ion etching. Copyright (C) 2000 John Wiley & Sons, Ltd.