The Effect of Mechanical Pretreatment on the Electrochemical Characteristics of PEO Coatings Prepared on Magnesium Alloy AZ80.

The main objective of this article is to provide new information on the effects of mechanical pretreatment of AZ80 magnesium alloy ground with SiC emery papers of different grain sizes on the plasma electrolytic oxidation (PEO) process and corrosion properties of AZ80 in 0.1 M NaCl solution. Then, the roughness of the coated samples was measured by confocal microscopy. The corrosion properties of the ground and coated surfaces were determined by potentiodynamic polarization (PDP) within 1 h of exposure, and electrochemical impedance spectroscopy (EIS) was performed during 168 h of exposure at laboratory temperature. Consequently, the obtained results of the PDP measurements were evaluated by the Tafel analysis and the EIS evaluation was performed by the equivalent circuit analysis through Nyquist diagrams. The morphology and structure of PEO coatings were observed by scanning electron microscopy (SEM) through the secondary imaging technology, and the presence of certain elements in PEO coatings was analyzed by EDS analysis.

High Pressure Torsion of Copper; Effect of Processing Temperature on Structural Features, Microhardness and Electric Conductivity.

By optimizing the fabrication method, copper components featuring (typically contradicting) advantageous electric conductivity and favorable mechanical properties can be acquired. In this study, we subjected conventional electroconductive copper to a single revolution of high pressure torsion (HPT) at room temperature (RT), searched for the conditions which would yield comparable structure characteristics (grain size) when deformed at a cryogenic temperature, and finally compared the mechanical and electric behaviors to assess specific differences and correlate them with the (sub)structural development. 180° revolution of cryo-HPT imparted structure refinement comparable to 360° revolution of room temperature HPT, i.e., the average grain size at the periphery of both the specimens was ~7 µm. The 360° RT HPT specimen exhibited preferential (111)||SD (shear direction) texture fiber in all the examined regions, whereas the 180° cryo-HPT specimen exhibited more or less randomly oriented grains of equiaxed shapes featuring substantial substructure development of a relatively homogeneous character and massive occurrence of (nano)twins. These structural features resulted in the increase in microhardness to the average value of 118.2 HV0.2 and the increase in the electric conductivity to 59.66 MS·m-1 (compared to 105 HV0.2 and 59.14 MS·m-1 acquired for the 360° RT HPT specimen). The deformation under the cryogenic conditions also imparted higher homogeneity of microhardness distribution when compared to RT processing.

Residual stress determination by the layer removal and X-ray diffraction measurement - correction method.

Very often a manufacturing process is followed by some surface treatment. Such a process induces residual stress into the manufactured component. Compressive residual stress is desirable for enhancing the fatigue properties of the component. The residual stress is often measured only at the surface, if at all. However, residual stress is equilibrating in the whole component. Therefore, compressive residual stress at the surface induces undesirable tensile stress inside in the component. Knowledge of the residual stress distribution in a body can be very useful in engineering applications. The authors found this knowledge necessary for a proper description of fatigue crack propagation in railway axles described in the original paper [1]. With the onset of modern surface treating technologies, e.g. induction hardening, which can affect the entire cross-section of the component, the residual stress determination is even more critical. The presented paper aims to describe a procedure developed for proper residual stress determination. The procedure can be easily used e.g. in R&D centers, where X-ray diffraction residual stress measurement is already in use. The procedure is suitable for the residual stress determination in sizable cylindrical bodies or components, e.g. railway axles. It uses X-ray diffraction residual stress surface measurement and layer removal by machining. Results experimentally obtained are corrected by a general procedure developed in MATLAB software in order to obtain the original residual stress state in the cylindrical body.•More accurate procedure for a residual stress determination in cylindrical bodies.

Characterising Correlations between Electric Conductivity and Structural Features in Rotary Swaged Al/Cu Laminated Conductors.

This study aims to characterize the correlations between electric characteristics and selected structural features of newly designed Al/Cu laminated conductors manufactured via room temperature rotary swaging. After swaging, the laminates with diameters of 15 mm were subjected to two different post-process annealing treatments. Structure analyses performed to evaluate the effects of thermomechanical processing were performed via scanning and transmission electron microscopies. Electric conductivity and resistivity of the laminates were experimentally measured and numerically simulated using models designed according to the real conditions. The results showed that the electric resistivity was affected by the grain size, bimodal grains' distribution (where observed), the presence of twins, and, last but not least, dislocation density. Among the influencing factors were the area fractions of Al and Cu at the cross-sections of the of the laminated conductors, too. The results revealed that fabrication of the laminate via the technology of rotary swaging introduced more advantageous combinations of electric and mechanical properties than fabrication by conventional manufacturing techniques. The lowest specific electric resistivity of 20.6 Ωm × 10-9 was measured for the laminated conductor subjected to the post-process annealing treatment at 350 °C, which imparted significant structure restoration (confirmed by the presence of fine, equiaxed, randomly oriented grains).

Influence of (Sub) Structure Development within Rotary Swaged Al-Cu Clad Conductors on Skin Effect during Transfer of Alternating Current.

The nature of alternating current transfer via metallic materials is specific, since the current density tends to be inhomogeneous across the cross-section of the conductor and the skin effect tends to occur. However, the influence of this effect on the behaviour of the conductor can be optimized via the design and fabrication procedures. The study presents innovative design of an Al-Cu clad conductor, which is supposed to affect favourably the influence of the skin effect. The clad conductors of various diameters (20 mm, 15 mm, and 10 mm) were fabricated via rotary swaging at room temperature, and their electric characteristics were subsequently examined both experimentally and via numerical simulations. Structure analyses performed to document the effects of the swaging technology on the development of substructure and characteristic structural features were carried out by scanning electron microscopy (electron backscatter diffraction analyses), and transmission electron microscopy. The results showed that the design of the composite has a favourable effect on decreasing the power losses during alternating current transfer and that the substructure development affected favourably the electric resistance of the conductor. The highest electric resistance was measured for the composite conductor with the diameter of 20 mm (1.8% increase compared to electric resistance during transfer of direct current). This value then decreased to 0.6%, and 0.1% after swaging down to the diameters of 15 mm, and 10 mm; the 10 mm composite featured the finest grains, partially restored structure, and texture randomization compared to the 20 mm and 15 mm composites. Manufacturing of the clad composite via rotary swaging imparted advantageous combinations of both the electric and mechanical properties, as swaging also introduced increased microhardness.

Structural Factors Inducing Cracking of Brass Fittings.

Cu-Zn-Pb brasses are popular materials, from which numerous industrially and commercially used components are fabricated. These alloys are typically subjected to multiple-step processing-involving casting, extrusion, hot forming, and machining-which can introduce various defects to the final product. The present study focuses on the detailed characterization of the structure of a brass fitting-i.e., a pre-shaped medical gas valve, produced by hot die forging-and attempts to assess the factors beyond local cracking occurring during processing. The analyses involved characterization of plastic flow via optical microscopy, and investigations of the phenomena in the vicinity of the crack, for which we used scanning and transmission electron microscopy. Numerical simulation was implemented not only to characterize the plastic flow more in detail, but primarily to investigate the probability of the occurrence of cracking based on the presence of stress. Last, but not least, microhardness in specific locations of the fitting were examined. The results reveal that the cracking occurring in the location with the highest probability of the occurrence of defects was most likely induced by differences in the chemical composition; the location the crack in which developed exhibited local changes not only in chemical composition-which manifested as the presence of brittle precipitates-but also in beta phase depletion. Moreover, as a result of the presence of oxidic precipitates and the hard and brittle alpha phase, the vicinity of the crack exhibited an increase in microhardness, which contributed to local brittleness.

Effect of Underload Cycles on Oxide-Induced Crack Closure Development in Cr-Mo Low-Alloy Steel.

Underload cycles with small load amplitudes below the fatigue crack growth threshold are dominantly considered as insignificant cycles without any influence on fatigue lifespan of engineering structural components. However, this paper shows that in some cases these underload cycles can retard the consequent crack propagation quite significantly. This phenomenon is a consequence of oxide-induced crack closure development during cyclic loading below the threshold. The experimentally described effect of fatigue crack growth retardation was supported by measurement of the width and the thickness of the oxide debris layer using the EDS technique and localized FIB cuts, respectively. Both the retardation effect and the amount of oxide debris were larger for higher number and larger amplitudes of the applied underload cycles. Crack closure measurement revealed a gradual increase of the closure level during underload cycling. Specimens tested in low air humidity, as well as specimens left with the crack open for the same time as that needed for application of the underload cycles, revealed no retardation effect. The results can improve our understanding of environmental effects on fatigue crack propagation and understanding the differences between the results of laboratory testing and the fatigue lives of components in service.

Effect of Solution Annealing on Fatigue Crack Propagation in the AISI 304L TRIP Steel.

Fatigue crack propagation in near-threshold regime was studied in the 304L austenitic stainless steel in two microstructural states: as-received (AR) with finer microstructure and low susceptibility to the transformation-induced plasticity (TRIP) effect, and solution-annealed (SA) with coarser microstructure and higher susceptibility to TRIP. At the load ratio R = 0.1 the threshold was higher in the SA state than in the AR state due to coarser grains and possibly the TRIP effect. In order to clarify the role of crack closure, experiments at R = 0.7 were done. The threshold in the SA state was still higher by 1 MPa·m0.5. This effect was identified as crack tip shielding induced by phase transformation, an example of a non-closure shielding effect. Higher resistance to crack growth in the SA state was attributed to promoted martensitic transformation in non-favorable oriented grain families rather than thicker martensite layers in the crack path area. The conclusions were verified by experiments at R = 0.7 and temperature 150 °C > Ms which did not reveal any notable difference in thresholds. However, the threshold values were affected by the load-shedding gradient C = -dΔK/da, which had to be equalized in both experimental setups inside and outside the furnace.

Ultrasonic Fatigue Testing in the Tension-Compression Mode.

Ultrasonic fatigue testing is one of a few methods which allow investigating fatigue properties in the ultra-high cycle region. The method is based on exposing the specimen to longitudinal vibrations on its resonance frequency close to 20 kHz. With use of this method, it is possible to significantly decrease the time required for the test, when compared to conventional testing devices usually working at frequencies under 200 Hz. It is also used to simulate loading of material during operation in high speed conditions, such as those experienced by components of jet engines or car turbo pumps. It is necessary to operate only in the high and ultra-high cycle region, due to the possibility of extremely high deformation rates, which can have a significant influence on the test results. Specimen shape and dimensions have to be carefully selected and calculated to fulfill the resonance condition of the ultrasonic system; thus, it is not possible to test the full components or specimens of arbitrary shape. Before each test, it is necessary to harmonize the specimen with the frequency of the ultrasonic system to compensate for deviations of the real shape from the ideal one. It is not possible to run a test until a total fracture of the specimen, since the test is automatically terminated after initiation and propagation of the crack to a certain length, when the stiffness of the system changes enough to shift the system out of the resonance frequency. This manuscript describes the process of evaluation of materials' fatigue properties at high-frequency ultrasonic fatigue loading with use of mechanical resonance at a frequency close to 20 kHz. The protocol includes a detailed description of all steps required for a correct test, including specimen design, stress calculation, harmonizing with the resonance frequency, performing the test, and final static fracture.

Chemiluminescence determination of antibacterial drug trimethoprim by automated sequential injection technique with permanganate and hexametaphosphate as reagents.

Antibacterial drug trimethoprim [2,4-diamino-5-(3,4,5-trimethoxybenzyl)-pyrimidine] (I) was determined in pharmaceutical formulations by using a lab-made PC-controlled SIA analyser linked to conventional HPLC fluorimetric detector equipped with a chemiluminescence module. The chemical principle is the oxidation of I by KMnO(4) in acid medium; the reaction is accompanied by the emission of chemiluminescence, which is enhanced in the presence of hexametaphosphate (HMP). The optimum sequence and the flow parameters and concentrations and volumes of reagents aspirated optimised by a computer-aided simplex method were, 100 mul of 5 mM HMP, 40 mul of a test solution of I, 2 mul of 0.5 M H(2)SO(4) and 20 mul of 1 mM KMnO(4); the luminescing zone was pushed into the detector at a flow rate of 49 mul s(-1). The calibration graph relating the intensity of luminescence to concentration of I was parabolic (r=0.9994) in the range 0.5-100 mug ml(-1) of I with rectilinear part (r=0.9999) in the range 20-100 mug ml(-1) of I; the limit of detection was 0.1 mug ml(-1) of I. The method was used for the assay of Triprim(R) tablets (with nominal content 100 or 200 mg of I) for the active substance as well as for content uniformity tests; the R.S.D. values did not exceed 1% (n=5). The SIA results did not show statistical difference from those obtained by pharmacopoeial acidimetric titration in non-aqueous medium; the excipients such as microcrystalline cellulose, maze starch, povidone, talc, magnesium stearate and gelatin did not interfere.