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Extraction Replicas of Common Engineering Alloys for Analysis of Small PrecipitatesRolinska, Monika January 2020 (has links)
Characterization of small precipitates is important for development of new alloys. One inherent difficulty in characterisation of small precipitates with electron microscopy techniques while the particles are embedded in the matrix, is that the surrounding bulk material will contribute to the analysed signal- limiting, for example, the quantification of the composition of particles. In order to avoid the matrix contribution, the extraction replica technique was developed in the 1950's. Extraction replicas are made by extracting only the particles from a material onto a thin film for further analysis by scanning or transmission electron microscopy. Different types of particles can be examined by this technique, including various carbides, nitrides, oxides and borides, as well as many intermetallic phases. In this work, direct replication techniques were compared to two-stage replication for low-alloyed steel, concluding that both are suitable for qualitative analysis, but direct replication is preferred for quantitative analysis. Successful replication of the zirconium-based Zirlo and the stainless steel 254 SMO was performed, where the precipitated phases were isolated and the composition quantified. Particle extraction was successful also for the zirconium-based Zircaloy-2 and two types of aluminium alloys, but no quantification of composition could be made due to different problems associated with etching of each alloy, showing that properchoice of etchant is crucial for the quality of the replicas. / Karaktärisering av små utskiljningar är viktigt för utveckling av nya legeringar. En svårighet vid karaktärisering av små utskiljningar med elektronmikroskopi när partiklarna sitter kvar i matrisen är att matrisen kommer ge ett bidrag till den analyserade signalen, därför är t.ex. möjligheterna för kvantifiering av sammansättning begränsade. För att undvika bidraget från matrisen utvecklades extraktionsrepliker på 1950-talet. Extraktionsrepliker tillverkas genom att extrahera partiklar från ett material till en tunn film som sedan kan analyseras med hjälp av svep- eller transmissionselektronmikroskopi. Olika sorters partiklar kan undersökas med hjälp av denna metod. Dessa inkluderar olika typer av karbider, nitrider, borider, oxider och många olika sorters intermetalliska partiklar. I detta arbete jämfördes direkta metoder med tvåstegsrepliker på låglegerat stål. Slutsatsen blev att båda metoderna lämpar sig för kvalitativ analys av små partiklar, men direkta metoder är att föredra för kvantitativ analys. Lyckade repliker tillverkades även av zirkoniumlegeringen Zirlo och det rostfria stålet 254 SMO, där utskiljningarna kunde isoleras och sammansättningen kvantifieras. Extraktion av partiklar var lyckad även för zirkoniumlegeringen Zircaloy-2 samt två typer av aluminiumlegeringar, men ingen kvantifiering av sammansättningen kunde göras på grund av olika problem relaterade till den valda etsmetoden för varje legering, vilket visar att valet av etsmedel ar avgörande för kvaliteten av replikerna.
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Evaluation of the η (Eta) nitride with three laboratory meltsLind, Martin, Johansson, Cecilia January 2015 (has links)
η (eta) nitride, Cr3Ni2SiN, is a precipitate found in high temperature austenitic stainless steel and is not yet included in Thermo-Calc steel database TCFE7. The aim of this thesis is to collect thermodynamic data to enable the addition of η nitride in the databases. Three laboratory melts with varying levels of silicon, chromium and nickel have been aged at 700-1000 °C for 75 h, 300 h and 1200 h and examined by Light Optical Microscopy, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, Wavelength Dispersive Spectroscopy, Electron Backscattered Diffraction and X-ray Powder Diffraction. η nitride is in the studied alloys an equilibrium phase stabilized with nitrogen. Presence of η nitride was confirmed by Energy Dispersive Spectroscopy and X-ray Powder Diffraction. It was found to precipitate in four different ways, at primary grain boundaries, intragranularly, as a "skeleton-like" precipitate and as a border around the occurring Cr2N precipitates. The area fraction of η nitrides increases with longer aging times and is favored by silicon and nickel. The composition of η nitride is not changing regardless of material composition, aging temperature and aging time. The composition of η nitride in all three materials are 8.7-9.7 wt.% silicon, 47-54 wt.% chromium, 1.4-4.1 wt.% iron and 33-36 wt.% nickel. The nitrogen content 2 determined by Wavelength Dispersive Spectroscopy is 2.8-3.2 wt.%. No complete equilibrium was achieved and together with incomplete mixing of the alloying elements during melting, the microstructure is difficult to evaluate. Other precipitates found are Cr2N, π nitride, σ phase and two unidentified phases, M and N. Of these phases at least Cr2N is not an equilibrium phase as it dissolves during aging. Further aging to achieve complete equilibrium is necessary.
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