Lenka Klakurková

Gravity-flow open tubular cation chromatography

We describe ion chromatography (IC) on open tubular cation exchange columns with a controllable capacity multilayered stationary phase architecture. The columns of relatively large bore (75 microm id) are fabricated by coating fused-silica capillaries with multiple layers of poly(butadiene-maleic acid) (PBMA) copolymer and crosslinking the deposited layers by thermally initiated radical polymerisation. Column capacity increases in a predictable manner with increase in the number of successively coated layers. Gravity flow with a modest head (< 2 m) can provide the desired separations within a reasonable period. We provide a minimalist configuration where no suppression is used, the sample is injected hydrodynamically as in CE, and detection is accomplished by an inexpensive homebuilt contactless conductivity detector or a capacitance to voltage digital converter. A 1 m long 75 microm bore column coated with two layers of PBMA allows gravity-flow open tubular IC to separate four alkali cations in < 10 min with a 1 mM tartaric acid (TA) eluent. Simultaneous separation of alkali and alkaline earth metal cations can be accomplished in less than 25 min using 1.75 mM pyridinedicarboxylic acid as an eluent. Contactless conductometric detection (C(4)D) allows LODs down to 150 nmol/L, corresponding to 30 fmol injections. Analysis of real water samples is demonstrated.

Diffusion in Al-Ni and Al-NiCr Interfaces at Moderate Temperatures

The diffusion couples for experimental study were prepared by HVOF spraying of nickel and nickel with 20 wt.% of chromium powders onto an aluminium sheet surface. The interfaces with sharp gradients of chemical concentration of these elements were prepared. Annealing at temperatures of 600°C and 630°C, close to the Al + Al3Ni eutectic melting point (639.9°C), with different dwell times were used. During annealing, the reactants diffuse and form layers of Al3Ni2 and Al3Ni intermediate phase compositions. Moreover, nickel without the assistance of chromium diffuses preferably along the grain boundaries into aluminium substrate and produces the strengthening of the substrate by stable Al3Ni and metastable Al9Ni2 particles. The microstructures were obtained by scanning electron microscopy. Layer thickness measurements were realized by means of image analyses. Chemical composition was estimated by energy dispersive microanalysis measurements. According to the results of the analyses performed the average chemical interdiffusion coefficients and Wagner’s integral interdiffusion coefficients were calculated.

QUALITY OF ALUMINIUM ALLOY SURFACE AFTER WEDM

e-mail: mouralova@fme.vutbr.cz Efficient machining using wire electrical discharge machining (WEDM) technology is a compromise between cutting speed and resulting surface quality. Typical morphology of the surface machined by WEDM shows a plenty of craters caused by electrospark discharges produced during the cutting process. This work is focused on assessing the impact of machine setting parameters on quantitative and qualitative evaluation of the workpiece surface of aluminium alloy AlZn6Mg2Cu. Using metallography, the surface effects arisen during the process of wire spark erosion on cross-sections of preparations were studied. Using local spot EDX microanalysis, the chemical composition of the surfaces of the samples was studied. The attention was also paid to the highest height of profile of the craters, which were studied using 3D filtered images.

Use of the Powder Liquid Method for Aluminide Diffusion Coatings Formation on Inconel 713LC Nickel-Based Superalloy

Powder liquid method was used for aluminides diffusion coatings formation on the Inconel 713LC nickel-based superalloy. Two different powder mixtures (Al and Al + Si) in organic binder solution were prepared. Coatings deposition onto the substrate surface was realized by spraying. Two-stage heat treatment under the argon-flow atmosphere was designed. First stage at 200°C was used to decompose organic binder. In the second stage at 1000°C the elements from the coating interact with the substrate. Protective intermetallic layer and an interaction zone between the layer and substrate start to form. Elements interaction and phase transformations during annealing at 1000°C up to 600 min were studied. For this study the light microscopy, scanning electron microscopy, energy dispersive microanalysis, x-ray diffraction phase analysis, microhardness measurement, and image analysis methods were used.

Effect of Width of Kerf on Machining Accuracy and Subsurface Layer After WEDM

Wire electrical discharge machining is an unconventional machining technology that applies physical principles to material removal. The material is removed by a series of recurring current discharges between the workpiece and the tool electrode, and a ‘kerf’ is created between the wire and the material being machined. The width of the kerf is directly dependent not only on the diameter of the wire used, but also on the machine parameter settings and, in particular, on the set of mechanical and physical properties of the material being machined. To ensure precise machining, it is important to have the width of the kerf as small as possible. The present study deals with the evaluation of the width of the kerf for four different metallic materials (some of which were subsequently heat treated using several methods) with different machine parameter settings. The kerf is investigated on metallographic cross sections using light and electron microscopy.

Tricalcium Phosphate - Magnesium Interface: Microstructure and Properties

The fabrication of a composite material based on magnesium (Mg) and tricalcium phosphate is reported in this work. Rods of β-tricalcium phosphate (β-TCP) were processed and consolidated together with pure Mg powder through spark plasma sintering (SPS). The microstructure at the interface, the chemical composition and transformation of the components and the microhardness were analysed. The microstructure of the composite shows two zones with well-defined and continuous interface between them: a ceramic zone composed by β-TCP filled with Mg and the metallic zone constituted by Mg and Mg rich eutectic. Vickers hardness shows the excellent mechanical interaction between the two zones.

Critical Weak Points of Atmospheric Plasma Sprayed Thermal Barrier Coatings

The 8 wt. % yttria stabilized zirconia top coat (TC) and the CoNiCrAlY bond coat (BC) were sprayed onto the surface of newly developed fine-grained cast polycrystalline nickel-based superalloy Inconel 713LC by means of atmospheric plasma spraying (APS). As-prepared samples were isothermally exposed at the temperature of 1050 °C for 200 hours in an ambient atmosphere. Structural changes in the thermal barrier coatings (TBC) system after thermal exposure were studied by means of scanning electron microscope equipped with an energy dispersive microanalyzer. Critical weak points were identified on both the substrate-bond coat and bond coat-top coat interfaces.

Comparative Analysis of Hard Anodized Layer on Aluminium Alloy

Hard anodized layers were produced by two different manufacturers on the same type of aluminium alloy on a vacuum pump part of complex shape. The sulphuric acid/water solution was used to produce alumina layers, which were subsequently sealed in demineralized water. A comparative analysis based on metallographic methodology, with the aim to control the stability of alumina formation process and to identify its defects, was performed by means of light and scanning electron microscopy, surface profilometry and microhardness measurements. To determine the thickness of alumina layers, the image analysis was also used.

Application of sacrificial coatings and effect of composition on Al-Al3Ni ultrafine eutectic formation

This paper introduces an unconventional method designed for forming hypereutectic alloys via coating deposition onto the substrate surface and subsequent heat treatment of such systems. The coating was produced from 99.7 wt% nickel powder by means of high velocity oxyfuel (HVOF) spraying onto the surface of 99.999 wt% aluminium sheet. The specimens were manufactured immediately after the spraying. Specimens were heat-treated using a differential thermal analysis (DTA) apparatus up to a temperature of 900°C and then cooled down to the room temperature in an argon atmosphere with constant heating and cooling rates, under which the NiAl3 intermetallic phase formed within the initial substrate. Two different alloy microstructures consisting of a coarse eutectic and an ultrafine well-dispersed eutectic were produced. The formation processes and resultant microstructures were studied by means of differential thermal analysis, metallography, scanning electron microscopy, energy dispersive microanalysis, and image analysis techniques.

Analysis of Causes of Fractures of Terminal Board Bolts

The paper sums up the results of a complex analysis, using metallographic, microfractograpic and other methods, with the aim of establishing the cause of fractures appearing in bolts of a terminal board. The analysis has shown unambiguously that the bolt failure was a synergic effect of inadequately performed heat treatment and hydrogenation that occurred in course of surface treatment via pickling and subsequent zinc plating.