Title page for ETD etd-06122010-223138


Document Type Doctoral Thesis
Author Sello, Maitse P
Email maitse_s@hotmail.com
URN etd-06122010-223138
Document Title The laves phase embrittlement of ferritic stainless steel type aisi 441
Degree PhD
Department Materials Science and Metallurgical Engineering
Supervisor
Advisor Name Title
Prof W E Stumpf Supervisor
Keywords
  • titanium niobium carbonitrides (Ti.Nb)(C.N)
  • Cottrell approach to grain size
  • Smith model of brittle grain boundary phases
  • ductile-to brittle transition temperature (DBTT)
  • grain size
  • impact embrittlement
  • laves phase (Fe2Nb)
  • Laves phase transformation kinetics
  • Thermo- Calc®
Date 2010-04-21
Availability unrestricted
Abstract
The effect of Laves phase (Fe2Nb) formation on the Charpy impact toughness of the ferritic stainless steel type AISI 441 was investigated. The steel exhibits good toughness after solution treatment at 850°C, but above and below this treatment temperature the impact toughness decreases sharply. With heat treatment below 850°C the presence of the Laves phase on grain boundaries and dislocations plays a significant role in embrittlement of the steel whereas above that temperature, an increase in the grain size from grain growth plays a major role in the impact embrittlement of this alloy. The toughness results agree with the phase equilibrium calculations made using Thermo–Calc® whereby it was observed that a decrease in the Laves phase volume fraction with increasing temperature corresponds to an increase in the impact toughness of the steel. Annealing above 900°C where no Laves phase exists, grain growth is found which similarly has a very negative influence on the steel’s impact properties. Where both a large grain size as well as Laves phase is present, it appears that the grain size may be the dominant embrittlement mechanism. Both the Laves phase and grain growth, therefore, have a significant influence on the impact properties of the steel, while the Laves phase’s precipitation behaviour has also been investigated with reference to the plant’s manufacturing process, particularly the cooling rate after a solution treatment.

The microstructural analysis of the grain size shows that there is a steady increase in grain size up to about 950°C, but between 950°C and 1000°C there is a sudden and rapid 60 % increase in the grain size. The TEM analysis of the sample that was annealed at 900°C shows that the Laves phase had already completely dissolved and cannot, therefore, be responsible for “unpinning of grain boundaries” at temperatures of 900°C and higher where this “sudden” increase in grain size was found. The most plausible explanation appears to be one of Nb solute drag that loses its effectiveness within this temperature range, but this probably requires some further study to fully prove this effect.

During isothermal annealing within the temperature range of 600 to 850°C, the time – temperature – precipitation (TTP) diagram for the Laves phase as determined from the transformation kinetic curves, shows two classical C noses on the transformation curves. The first one occurring at the higher temperatures of about 750 to 825°C and the second one at much lower temperatures, estimated to possibly be in the range of about 650 to 675°C. The transmission electron microscopy (TEM) analyses show that there are two independent nucleation mechanisms that are occurring within these two temperature ranges. At lower temperatures of about 600°C, the pertaining nucleation mechanism is on dislocations and as the temperature is increased to above 750°C, grain boundary nucleation becomes more dominant. Also, the morphology of the particles and the mis-orientation with the matrix changes with temperature. At lower temperatures the particles are more needle-like in shape, but as the temperature is increased the shape becomes more spheroidal.

The effect of the steel’s composition on the Laves phase transformation kinetics shows that by lowering the Nb content in these type 441 stainless steels, had no significance effect on the kinetics on precipitation of the Laves phase. However, a Mo addition and a larger grain size of the steel, retard the formation of the Laves phase, although the optimum values of both parameters still need further quantification.

The calculation made for the transformation kinetics of the Laves phase, using the number density of nucleation sites No and the interfacial energy, as the fitting parameters in this work, demonstrated a reasonable agreement with experimental results.

© 2009, University of Pretoria. All rights reserved. The copyright in this work vests in the University of Pretoria. No part of this work may be reproduced or transmitted in any form or by any means, without the prior written permission of the University of Pretoria.

Please cite as follows:

Sello, MP 2009, The laves phase embrittlement of ferritic stainless steel type aisi 441, PhD thesis, University of Pretoria, Pretoria, viewed yymmdd < http://upetd.up.ac.za/thesis/available/etd-06122010-223138/ >

D10/437/ag

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