Modeling in support of the development of steels for high-temperature applications

Oxide dispersion strengthened alloys are known for their better chemical and mechanical
properties affected by composition and microstructure, respectively. Oxide Dispersion
Strengthened (ODS) steels are potential candidates for high temperature applications such as
future fusion and nuclear reactor, chemical reactors, ultra supercritical steam turbines, etc in the
form of structural members. The addition of nano-size ODS particles enhances the high
temperature creep strength of these steels. In addition such steels require good oxidation
resistance, reduced activation when exposed to neutron irradiation, and long-term microstructure
stability at high temperatures as those expected during service life of component [1, 2, 3].
Radiation damage in materials is quantified by the displacement per atom (DPA). DPA
represents how many times an atom is displaced from its original atomic lattice position to a new
lattice position as a result of given radiation flux. Candidate materials intended for fusion
structural materials and plasma facing materials should consist of following elements for low or
reduced activation property of composition to meet low level waste criteria: Cr, Ti, V, Fe, W, Si,
and C. High temperature stability of microstructure is decided by the amount of recrystallization
occurring which in turn is affected by the amount of applied strain, particle volume fraction, size
distribution, and spacing between them. High temperature corrosion resistance is enhanced by
presence of Cr in steel; however, its content needs to be optimized in order to balance the
demerit of aging embrittlement while maintaining strength at high temperature [4]. Excess
oxygen (except for oxygen concentration in Y2O3) resulting from processing is considered
harmful for microstructure and mechanical properties of steel and hence needs to be controlled at
the initial stages of processing.
Dispersion of fine ODS particles cause zener drag and renders recrystallization sluggish.
Nano ODS particles of Y2O3 or Ti2Y2O7 are known to trap irradiation induced point defects and
diffusing atoms like Cr, Nb, Mo, V; at the particle-matrix interface, thereby suppressing aging
embrittlement [2]. Bimodal distribution of Y-containing ODS particles is present in reduced
activated ferritic steels (RAF) ODS steel wherein Ti is also found at the particles. Y2O3
dispersoid shows coarsening above 600 oC, however addition of Ti refines the size of
dispersoids, increases the number density and no significant dispersoid coarsening for Ti2Y2O7
particles was observed up to 1000 oC [3]. Hence steels with Y-Ti-O type nano particles exhibit
higher elevated temperature strength and improved creep and irradiation resistance. When Y/Ti
ratio is less than 1, the dispersoids are confirmed to be Ti2Y2O7. These particles are formed
homogeneously, in the grain interior as well as at the grain boundaries [5].
A minimum of 4 hrs milling of the atomized steel and Y2O3 powders is performed to get
optimum properties [3]. In RAF-ODS steel bimodal grain distribution is observed which may be
attributed to the hot isostatic pressing (HIP) processing parameters and needs to be studied
further [5]. With change in hot extrusion temperature from 1150 oC to 1200 oC, degradation in
creep and tensile strength was observed and needs to be investigated further [6].

A strong coherency between oxide lattice and matrix results in effective strengthening
due to oxide dispersion. In case of considerable differences in their lattice parameters, smaller
particles (< 5 nm) ensures better coherency with the matrix, resulting in superior high and low
temperature creep resistance with increased strength. S. Ohtsuka et. al. [6] has suggested that in a
9Cr ferritic-martensitic ODS steel, finer and denser particle precipitation is observed in presence
of elongated residual ferrite in the structure after annealing treatment. The fraction of elongated
ferrite grains is controlled through titanium, which in excess combines with carbon, and
resultantly increases the ferrite concentration. According to the theory on precipitate coarsening
[7, 8] oxide particle growth is controlled by the interfacial energy between an oxide particle and
matrix. If the lattice misfit between ferrite phase and oxide particles is smaller than that between
austenite phase and oxide particles, the enhanced and finer precipitation of oxide dispersion in
elongated residual ferrite can be interpreted in light of the above precipitation theory.
Oka et. al. [9] have observed an orientation relationship between the ODS particles and
matrix similar as in case of precipitates; <200>oxide // <111>matrix for Cr-NiODS (fcc structure)
and <111>oxide // <110>matrix for 12CrODS (bcc structure). AP-FIM analysis of ODS particles
showed inner and outer shell like structure with larger Ti-enriched region compared to Yenriched region, indicating Ti enrichment occurred at the outer region of the particles during
fabrication process at high temperature, as Ti was not contained in original Yttria powder. Under
electron irradiation particles less than 10 nm dissolved at lower temperature, whereas in case of
larger particles some amount of sputtering was observed on the surface of the particle including
the interface. Stability of ODS particles is commented to be dependent upon the composition and
purity (amount of Ex. O) of oxide particles. In lab scale studies irradiation environment such as
vacuum condition also plays a role in accurately determining irradiation damage in material.
Recovery is the dominant softening mechanism in these particles containing steels [3, 5]
whereas recrystallized grains are formed in the vicinity of the prior grain boundaries or coarse
precipitate particles due to particle stimulated nucleation (PSN). However, no significant
dispersoid coarsening for Ti2Y2O7 particles was observed up to 1000 oC and softening due to
grain coarsening is ruled out. During annealing, recrystallization occurs preferentially in grains
belonging to the -fiber texture component on account of their higher stored energy.
Electron backscattered diffraction (EBSD) has been successfully used to characterize the
grain boundaries up to 2o misorientation, however in order to study the nature of
particle/boundary interaction resulting in recovery/recrystallization, TEM is essential. EBSD has
also been used to study the microtexture evolution in differently strained components [5].
As can be seen, very fine oxide particles contribute strongly to the strength and creeprupture properties but are dissolved easily during electron irradiation. Stability of oxide particles
under irradiation conditions is reported to be dependent on its composition and purity. Numerous
sources reported refinement and dense formation of ODS particles in presence of Ti and is also
found to be dependent on the matrix phase and its orientation. High temperature service

conditions cause temperature-dependent softening phenomenon in material reducing its high

temperature strength as well as aging embrittlement causing premature failure. Recovery is the
most dominant while limited texture-dependent recrystallization is also observed. HRTEM
studies of the particle-matrix interface under irradiative and high temperature conditions forms
the major part of the project to study the softening mechanism, their kinetics, aging
embrittlement, and defect-sink phenomenon at particle interface. Hence for future development
of ODS steels, oxide particle composition, size, density and volume fraction needs to be
finalized. This configuration should be such to balance the strength and stability of
microstructure against irradiation damage, at intended high temperatures. For the purpose,
categorical effect of thermo-mechanical processing of ODS steel on development of oxide
particle composition, dispersion as well as textural changes in the matrix, needs to be simulated
physically and/or mathematically for next stage of development.
References
1. H. R. Z. Sandim, R. A. Renzetti, A. F. Padilha, A. Moslang, R. Lindau, and D. Raabe.
Annealing behavior of RAFM ODS-Eurofer steel. Fusion Science and Technology, Vol. 61,
2012, pp. 136.
2. H. R. Z. Sandim, R. A. Renzetti, A. F. Padilha, D. Raabe , M. Klimenkov, R. Lindau and A.
Moslang. Annealing behavior of ferritic-martensitic 9% Cr-ODS-Eurofer steel. Materials
Science and Engineering A, A 527, 2010, pp. 3602.
3. G. Sundararajan, R. Vijay, and A. V. Reddy. Development of 9Cr ferritic-martensitic and
18Cr ferritic oxide dispersion strengthened steels. Current Science, Vol. 105, No. 8, 2013,
pp. 1100.
4. S. Li, Z. Zhou, M. Wang, H. Hu, L. Zou, G. Zhang, and L. Zhang. Microstructure and
mechanical properties of 16 Cr-ODS ferritic steel for advanced nuclear energy system.
Journal of Physics: Conference Series, DOI: 10.1088/1742-6596/419/1/012036.
5. Ch. Ch. Eiselt, M. Klimenkov, R. Lindau, A. Moslang, H. R. Z. Sandim, A. F. Padilha, and
D. Raabe. High resolution transmission electron microscopy and electron backscatter
diffraction in nanoscaled ferritic and ferritic-martensitic oxide dispersion strengthened-steels.
Journal of Nuclear Materials, 385, 2009, pp. 231.
6. S. Ohtsuka, S. Ukai, M. Fujiwara, T. Kaito, and T. Narita. Improvement of creep strength of
9CrODS martensitic steel by controlling excess oxygen and titanium concentrations.
Materials Transactions, Vol. 46, No. 3, 2005, pp. 487.
7. D. A. Porter and K. E. Easterling. Phase transformations in metals and alloys, Stonely
Thrones Publishers Ltd., Cheltenham, 2000, pp. 314.
8. J. W. Martin and R. D. Doherty. Stability of microstructure in metallic systems, Cambridge
University Press, Cambridge, 1976, pp. 173.
9. K. Oka, S. Ohnuki, S. Yamashita, N. Akasaka, S. Ohtsuka, and H. Tanigawa. Structure of
nano-size oxides in ODS steels and its stability under electron irradiation. Materials
Transactions, Vol. 48, No. 10, 2007, pp. 2563.