Acta Materialia 149 (2018) 19e28
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Acta Materialia
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Full length article Dislocation-based modeling of long-term creep behaviors of Grade 91 steels
* Jifeng Zhao a, , Jiadong Gong a, Abhinav Saboo a, David C. Dunand b, Gregory B. Olson a, b a QuesTek Innovations LLC, 1820 Ridge Avenue, Evanston, IL 60201, USA b Northwestern University, Dept. of Materials Science & Engineering, 2220 Campus Drive, Evanston, IL 60208, USA article info abstract
Article history: To meet the 30 years (~263,000 h) design lifetime of a typical thermal power plant, understanding and Received 29 September 2017 modeling of the long-term creep behaviors of the power plant structural steels are critical to prevent Received in revised form premature structural failure due to creep. The extremely long exposure to high operation temperature 27 January 2018 results in evolving microstructure during service, which cannot be observed in standard short-term (<1 Accepted 1 February 2018 year) creep tests. In fact, creep rupture life predictions based on short-term creep testing data often Available online 8 February 2018 overestimate the creep rupture times for long period of time, and are therefore insufficient to provide a reliable failure time prediction. In this article, a microstructure-sensitive, long-term creep model is Keywords: Grade 91 ferritic steel developed and validated against existing long-term creep experimental data (~80,000 h) for ferritic steel Creep modeling Grade 91 (Fe-8.7Cr-0.9Mo-0.22V-0.072Vb-0.28Ni in wt.%). The mechanistic creep model is based on Dislocation climb fundamental dislocation creep mechanisms e the particle bypass model based on dislocation climb from Dislocation detachment Arzt and Rosler€ [1] - that describe the steady state creep strain rate as a function of stress, temperature, Creep threshold stress and microstructure. In particular, the model incorporates the evolution of the particle size via coarsening Z phase into the dislocation climb theory, dislocation detachment mechanism and back-stress generated by Precipitation strengthening mechanism subgrain dislocation structures. Model inputs were obtained based on the microstructure information obtained from published literature from the National Institute of Material Science (NIMS, Japan) creep database. The model, which can be used on many types of alloys, shows excellent agreement with existing long-term creep experimental data (~80,000 h) of Grade 91 ferritic steel. © 2018 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
1. Introduction (1000e1050 F) or higher [6]. In the hottest part of the boiler and for components such as headers, tubes, and pipes, the hoop stress can The lifetime of a power plant can be in excess of 30 years be as high as 100 MPa [5]. Creep test data under these conditions (~263,000 h), which requires outstanding creep resistance of load- are essential to ensure a reliable power plant design that exceeds 30 bearing structural steels to prevent the premature power plant years in lifetime. However, laboratory-scale creep test data of Grade component failure. Grade 91 steels have been used as one of the 91 steels are not available up to 300,000 h. Fig. 1 shows one of the major structural steels for Advanced Ultra Supercritical (AUSC) [2] longest existing laboratory test data for creep rupture time as a power plants due to its outstanding high-temperature creep function of the applied stresses and temperature for both 9%Cr resistance [2], [3]. Components made of the Grade 91 ferritic steel (Grade 91) and 12%Cr (T122) steel, which are approaching (with 9 wt% Cr and 1 wt% Mo as major alloying elements, micro- 100,000 h creep rupture time (11.5 years). A “secondary-like” additions of V and Nb, 0.1 wt% C and a controlled nitrogen con- minimum creep rate, stable at 2 ± 1 10 7 h 1, is maintained over a tent [4]) are experiencing a wide array of internal stresses very long time span of 40,000 h. During this 4.5 year duration, the depending on the location and welds [5]. Typical supercritical fossil microstructure is evolving extremely slowly. Therefore, we assume fueled power stations operate at a steam pressure typically above a quasi steady-state condition (dislocation motion, diffusion pro- 24 MPa (3.5 ksi) with steam temperatures of 538e566 C cess) in the model derivation for this “secondary-like” creep. Nevertheless, when plotting creep rupture time vs. stress (Fig. 1(a)), accelerated reduction of creep rupture time occurs in the long-term > * Corresponding author. creep region ( 40,000 h), which has to be separated from the short- E-mail address: [email protected] (J. Zhao). term region and is represented by a steeper slope in a creep rupture https://doi.org/10.1016/j.actamat.2018.02.001 1359-6454/© 2018 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved. 20 J. Zhao et al. / Acta Materialia 149 (2018) 19e28
Fig. 1. (a) Double logarithmic plot of applied stress vs. time to rupture for ferritic steels with 9% Cr (Grade 91) (b) Semi-logarithmic plot of creep rate vs. time for steel Grade 91 at 600 C and 70 MPa, showing primary, secondary-like (~1e3x10 7 h 1) and tertiary creep regions (beyond ~40,000 h). Arrows indicate the times at which creep tests were interrupted to obtain the microstructure information by the replica technique (see Fig. 2). [22], [25][26][39].
time vs. stress regression plot such as Fig. 1(a). Consequently, dispersion-strengthened alloys, Arzt and Rosler€ [14] predicted a simple extrapolation from short-term creep rupture time over- threshold stress using a local climb theory, where new dislocation estimate the long-term creep rupture time, which necessitate line is created as the dislocation climbs around the matrix- more complex models [[7e10]] and motivates the development of a precipitate interface during the bypass process. However, the microstructure-based creep model capable of predicting premature local climb is an unstable process where the sharp bend of dislo- creep failure for the long-term creep regime. cation can be rapidly relaxed by vacancy diffusion leading to a more The low applied stress region (long-term creep) is characterized “general” climb process [14], [15]. Arzt and Rosler€ [14] calculated by high creep exponent in the classical power law relationship. For the detailed dislocation profiles based on the condition of mini- single-phase metals and alloys, minimum (secondary) strain rates ε_ mum energy, which leads to the combination of local and general can be written as a power law of the applied stress s: climb as the stable dislocation configurations. These authors [1] later suggested that a threshold stress can furthermore arise from DGb s napp ε_ ¼ A (1) an attractive interaction between the dislocation and incoherent kBT G dispersoid at the detachment side [16], which occurs after the dislocation has surmounted the obstacles by climb. In addition, where A is a constant, D is the vacancy diffusion coefficient, G the Dunand and coworkers proposed that the threshold stress due to shear modulus, b the Burgers vector, and n is the stress exponent climb is affected by the lattice strain induced by the lattice which is predicted to be 3e5 based on the classical dislocation parameter and the stiffness mismatches between matrix and climb and glide mechanisms. We use here the conventional ap- coherent precipitates, which changes the net forces on the climbing proaches of secondary, minimum creep rate in Eq (1) as an dislocation [17], [18]. Subgrains are dislocation networks with low approximation for the near-constant “secondary-like” minimum misorientation (1 or 2 angle) boundaries [19][20], in martensitic creep rates, which are stable over periods of years (Fig. 1(a)) but hierarchical structures whereas prior austenite grain boundaries nevertheless associated with very slow microstructure evolution. and martensitic block boundaries are high-angle grain boundaries. However precipitation-strengthened alloys usually exhibit a The coarsening of subgrain structures are observed to be detri- very high stress exponent, labelled the apparent stress exponent mental to the creep failure [21], [22]. It is supported by experi- napp when using Eq. (1), which is stress- and temperature- mental observations that subgrain structures create long-range dependent [11], [12]. According to NIMS published creep tests internal stresses that locally reduces the effective applied stress for database, when the applied stress is in the range of 70e130 MPa, both monotonic and cyclic loading [23], [24]. This effect can be Grade 91 has an apparent stress exponent napp ranging from 6 to leveraged by the introduction of threshold stress in Eq. (2). 12 at 600 C. This high stress sensitivities can be explained by These experimental observations and theories elucidate the s introducing a threshold stress th. interaction between dislocation and the nano-sized particles from which a steady state creep rate can be then calculated. Here, we DGb s s n € ε_ ¼ A th (2) follow Arzt and Rosler's approaches and derive a mathematical kBT G expression of creep strain rate based on the fundamental physics of dislocation climb mechanisms (around MX particles) for Grade 91 where n is the stress exponent of the matrix, which leads to arbi- steels. Back stress contributed from the evolving subgrain disloca- trarily high apparent stress exponent napp on the plot of tion structures is also accounted for in the model framework, as is ðε_Þ ðsÞ s log log near th. Electron microscopy observations and the evolving precipitation sizes and volume fractions during creep theories suggest that the threshold stress for precipitation- deformation. These two microstructure-sensitive mechanisms both strengthened alloys is due to the interactions between the matrix have been considered in a unified modeling framework. Necessary dislocations and the particles during climb bypass [13]. Many the- microstructure information are obtained from interrupted creep ories have been proposed to explain to the origin of the threshold tests performed by NIMS [25]e [27] as the model inputs. Model stress due to unshearable precipitates or dispersoids, including predictions of the steady-state strain rate of Grade 91 show excel- local and general climb theory, dislocation detachment theory, and lent agreement with experiments. back-stress induced by subgrain structures. For incoherent J. Zhao et al. / Acta Materialia 149 (2018) 19e28 21
2. Modeling approach goal of this work to achieve integrate microstructural evolution model for dissolution, coarsening and growth of precipitates into 2.1. Microstructure evolution models that consider interaction of dislocations with these pre- cipitates to predict macroscopic strain rates. The composition of the commercial Grade 91 steel is shown in Table 1. As processed Grade 91 steel has, before creep exposure, a 2.2. Creep modeling (Arzt and Rosler€ theory) tempered martensitic hierarchical microstructure. As illustrated by the schematics in Fig. 2(b), prior austenite grain boundaries (PAGB) Due to the very slow evolution of the microstructures occurring are divided into martensitic packets, which are aggregates of over a timescale of years, it is reasonable to assume a local steady- martensitic blocks on the same plane [28]. Therefore packets can be state condition in the “secondary-like” creep stage. The creep divided into martensitic blocks, which further contain subgrain model developed in this article follows the earlier approach by Arzt dislocation structures/lath structures. As both martensitic blocks and Rosler€ [1], [14]. Consider particles (MX) dispersed at a low and packets are bound by high-angle boundaries, they are generally volume fraction within a matrix. At high temperature, if shearing is referred to as “grains”. Subgrain-scale dislocation structures are not operational, such obstacles are bypassed by matrix dislocations bounded by low-angle boundaries [19], [29]. Excessive coarsening via a climb mechanism [14]. The particles are assumed to have a of subgrains has been observed during long term creep tests in simplified geometry with a rectangular cross section (Fig. 3). The Fig. 7 that contributes to the loss of creep resistance and dictates shear stress necessary for particle by-pass by athermal dislocation the final creep failure. Two types of precipitates are initially pre- bowing, given by the Orowan stress, is an upper bound. When the sent. First, M23C6 carbides with ~0.1 mm size [26], which are shear stress acting on the dislocation is below the Orowan stress, nucleated predominantly at the prior austenite grain boundaries, the dislocation glides until it become pinned by the particles. As and along martensite lath boundaries after tempering. Oruganti depicted in Fig. 3, the dislocation climbs up on the particle to po- [30] suggests that the existence of M23C6 particles effectively pin sition z0 aided by vacancy diffusions. The climbing face is inclined the subgrain boundaries, therefore providing creep resistance. at an angle b to the glide plane of the dislocation. Under the action fi Second, nano-sized MX carbonitride precipitates, which are nely of its line tension, a distance x0 of the dislocation line is unraveled distributed inside the matrix, provide significant resistance against out of the glide plane. dislocation motion. Both M23C6 and MX particles thus control long- According to the Orowan-Taylor equation, the steady state creep term creep deformation. rate ε_ can be written as a function of the average dislocation ve- In conventional creep theories, the microstructure is usually locity v as: assumed to be stable through the steady state creep period, which results in a constant strain rate in the secondary creep stage. l l ε_ ¼ rbv ¼ rb zrb (3) However the National Institute for Materials Science (NIMS, Japan) tc þ tg tc performed interrupted creep tests on steel Grade 91 and illustrated a very slowly evolving microstructure due to thermal exposure where b is the burger's vector, r is the mobile dislocation density, l during the very long testing times used, as shown in Fig. 2 [5]. is the particle spacing, tc is the time that dislocation climbs over a Microstructures are examined by both transmission electron mi- particle, tg is the time dislocation glides to the next particle. croscopy (TEM) and scanning TEM in conjunction with energy- Assuming that the dislocation climb is the rate-controlling process, dispersive X-ray analysis (STEM-EDX) at 200 kV. Thin foils for (i.e., the dislocation climb time tc[tg ), then the dislocation ve- € TEM study are prepared at the gauge section of crept samples after locity can then be simplified as v ¼ l=tc. Based on Artz and Rosler's creep test interruption. STEM-EDX is performed to determine the work, dislocation climb time is contributed by dislocation general composition of each precipitations. Micrographs in Fig. 2 (a)-(f) are climb, local climb and/or detachment mechanisms: taken at the times corresponding to the arrows in Fig. 1 (b). These ¼ þ þ observations elucidate that the microstructure is evolving during tc tgeneral tlocal tdetachment (4) the long creep experiments, spanning 10,000 to 81,000 h (1.1e9.2 years). First, the MX carbo-nitride precipitates which interact with dislocations are dissolving, thus reducing creep resistance. Second, the M23C6 precipitates at (sub)grain boundaries are coarsening, 2.2.1. Dislocation climb mechanism thus significantly decreasing the pinning forces for subgrain Fig. 4 depicts the projection of dislocation lines on the x-z plane, boundary migration and also decreasing to the creep resistance. where one or both related climbing modes co-exist, i.e., local climb Third, at a later stage during creep, Z-phase particles are formed and general climb. Local climb indicates that, when the dislocation and coarsen rapidly at the expense of the beneficial MX carboni- is climbing over the particles, the dislocation line is confined closely tride, which leads to reduced creep resistance and accelerated to the particle interface with sharp bending corners, which is a creep strain rate after long-term thermal exposure. Up to 10,000 h, preferred configuration at high applied stress (Fig. 4(a)). By the number density and radius of the MX precipitates are relatively contrast, general climb occurs at lower applied stresses with a stable in the short-term creep regime. Only after long-term creep lower strain rate, which allows for vacancy diffusion to relax the do the MX nitrides, with composition (V,Nb)N, transform into Z- dislocation profile to leave the particle interface and form a smooth phase nitride Cr(V,Nb)N by Cr diffusion into the precipitates. curve (Fig. 4(b)). Arzt and Rosler€ [14] calculated the equilibrium Therefore, the microstructure evolution is key to modeling the dislocation line profile subject to a condition of minimum energy. long-term creep behavior of the Grade 91 steel; it is the primary This work elucidates that the stress required for stable local climb is as high as Orowan looping stress. At an intermediate applied stress below the Orowan stress, the local climb is an energetically un- Table 1 stable process and therefore a “strictly” local climb process does not Composition (wt.%) of commercial Grade 91 steel [25]. occur.
CSiNbVN NiCrMoCu Instead, the two climb modes co-exist during the dislocation climbing process as shown in Fig. 4 (c). Arzt and Rosler's€ work is Grade 91 0.09 0.29 0.072 0.22 0.044 0.28 8.7 0.90 0.032 based on the assumption that line energy T of the dislocation 22 J. Zhao et al. / Acta Materialia 149 (2018) 19e28
Fig. 2. Micrograph showing microstructure evolution of Grade 91 steels during creep test at 600 C; under 70 MPa at (a) as tempered (b) 10,000 h (c) 30,000 h (d) 50,000 h (e)
70,000 h (f) 81,000 h (Figure (a)e(f) are taken from Ref. [5]). Evolution of the four types of precipitates are represented by different color codes. Red particles indicate the M23C6 particles, blue represents the VX carbonitride, green represents the NbX carbonitride, Z phase is represented by white color. The yellow dotted line indicates the prior austenite grain boundaries. (g) Schematic of the hierarchical microstructure that consists of prior austenite grain boundary, martensitic blocks and subgrain dislocation structures [29]. (For interpretation of the references to color in this figure legend, the reader is referred to the Web version of this article.)
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi " # = d t 2 x z t 1 z 9 4 ¼ 1 eff , 0 þ 0 , eff 1 þ 1 0 x0 tO z0 x0 tO tanb x0 (6)
where x0, z0 and b are defined in Fig. 4 (a) and (c), which describes fi t t the dislocation equilibrium pro le, O is the Orowan stress, eff is the local effective applied stress (modified by a back stress as in Eq. Fig. 3. Schematics of dislocation climb over non-shearable particles after [17][1], [14]. (15) due to the subgrain dislocation structures, as discussed in the next section). The solution of x0 at a given z0 cannot be explicitly written, since x0 and z0 are implicitly coupled together. Instead, Eq. segment residing in or near the particle-matrix interface Linterface is (6) can be solved numerically by using Brent's root finding method. reduced by a factor of k compared to the line energy of a dislocation As the dislocation climbs over a particle, both x0 and z0 are segment remote from the particle as L : ð * ; * Þ remote increasing until a critical position x0 z0 is reached. After this critical point, the local climb mode is switched on for a portion of the dislocation line segment as shown in Fig. 4 (c), which becomes ¼ the energetically favorable climb mode. The critical position Linterface kLremote (5) ð * ; * Þ x0 z0 can be calculated as [1]: The line energy reduction makes the particle-matrix interface rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi an energetically favorable place for the dislocation movement, 2 t 2 * 1 1 k þ eff tan2b z cosb tO which (i) stabilizes the local climb mode on a portion of dislocation 0 ¼ * t (7) segment and (ii) also introduces an attractive interaction between x k þ eff b 0 cosb t tan dislocation and particle on the departure side. At an intermediate O applied stress, the dislocation starts interacting with particles via The solutions for the dislocation profiles are illustrated in Fig. 5 the general climb. The equilibrium profile of the dislocation line for four different applied stresses. At lower applied stress, general was calculated based on the energy minimum: climb occurs throughout the climbing history. As the applied stress
Fig. 4. Schematic of dislocation climb mechanism (a) general climb (b) local climb (c) general þ local configuration for various times t1,t2,t3. J. Zhao et al. / Acta Materialia 149 (2018) 19e28 23
jmð ; ; l; tÞj dy ð ; Þ¼ x0 z0 x0 z0 Ci ð ; Þj (8) dt jdAABD=dy x0 z0
where AABD is the area under the climbing segment A-D projected in the direction Burger's vector and Ci is a kinetic constant pro- portional to the volume diffusivity Dv:
p ¼ 2 Dvd Ci (9) kBTb
where d is the particle diameter (d ¼ 2r). The chemical potential m can be written as a function of particles spacing l, applied stress t, fi ¼ : Fig. 5. Equilibrium dislocation pro le z0 and x0 at 600 C with k 0 85. Solid line and and the climb mode. More detailed discussions of Eqs. (6)e(8) can dashed line indicate the general and local climb respectively. The stresses displayed in t t be found in Refs. [1], [14]. The MX particle spacing can be calculated the legend are the total applied stress app instead of eff . as a function of the particle radius r and volume fraction f : increases, the dislocation line tends to bend over to a greater de- sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi ! gree, resulting in a smaller x0 at a given z0. As the applied stress pð1 1=3hÞ l ¼ r 1:23 2 (10) further increases, the local climb mode is achieved. The higher the f local stress is, the earlier this local climb mode is turned on, which is consistent with the physical understanding that local climb is where h is the particle aspect ratio taken here as unity, as the MX preferred as a higher stress. particles are assumed to be spherical Finally, the time needed for Following Arzt and Rosler€ [14], the climb rate is written as a the dislocation to climb and bypass the particle can be calculated by function of the chemical potential of the dislocation line m: integrating the climb rate over the climbing height:
Fig. 6. Dislocation detachment mechanisms, reprinted from Ref. [31] (a) TEM images of dislocation are attracted at the particle interface for dispersion-strengthened superalloy MA 6000 and (b) schematics of dislocation detachment mechanism.
Fig. 7. (aef) Dislocation substructure evolution during the same creep tests as in Fig. 2 obtained from Sawada [25]. (g) Subgrain boundary bowing between M23C6 particles under the influence of stress (from Oruganti [38]). 24 J. Zhao et al. / Acta Materialia 149 (2018) 19e28
contributes to strain and is thus detrimental to the creep life. It has * Zy Zr been shown that the creep strain acceleration is well correlated ¼ 1 þ 1 tc ð = Þ dt ð = Þ dt (11) with the subgrain dislocation coarsening based on NIMS creep tests dy dt gen dy dt local 0 y* and Rustam [28]. Bazazi [35] showed that the coarsening of the subgrains has a strong influence on the decrease of material Introducing Eq. (11) into the Orowan relation in Eq. (3), the hardness under creep conditions. Moreover, these subgrain steady-strain rate can then be calculated. boundaries are pinned by the M23C6 carbides and Nb-rich M(C, N) carbonitride that are precipitated on these boundaries. Therefore 2.2.2. Dislocation detachment mechanism the dissolution of MX particles and coarsening behaviors of pinning fl As discussed further by Arzt and Rosler€ [1], a direct consequence M23C6 carbides have a strong in uence of these subgrain bound- of the line energy reduction in Eq. (5) is that it leads to an attractive aries coarsening and must be modeled. particle-dislocation interaction, which results in a threshold stress It has been widely accepted that the subgrain boundaries net- behavior associated with the detachment process after the climb works (cells) create a long-range internal stress, i.e., a back stress, t bypass has been completed. The dislocation detachment mecha- for both cyclic and monotonic loading. The back stress back is nism has been widely accepted in the literature. Fig. 6 shows an interpreted as an internal material resistance due to subgrain example of a dislocation at the departure side of an oxide disperoid dislocation networks and it locally reduces the applied stress t in a nickel matrix, where the dislocation line is clearly pinned at the applied (resolved on the glide plane from the applied tensile stress): departure side of the particle-matrix interface as expected if an t ¼ t t attractive particle-dislocation interaction is present. A threshold eff applied back (15) stress is then required for the dislocation to complete the detach- The presence of significant levels of dynamic internal stresses ment process, below which the dislocation is trapped at the particle due to subgrain structures has been observed by Takeuchi [36] and and creep strain rate is thus negligible. The threshold stress t ðTÞ is d Argon [33] experimentally. Although a large of body of literature calculated as a fraction of the Orowan stress t in shear by Arzt and o has been dedicated to studying the subgrain dislocation structure, Rosler€ [1] as: the exact mechanism that causes these significant internal stresses sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi is still not completely understood and under active research. t ðTÞ 2k T ε_ 2 d ¼ 1 k þ B ln 0 (12) Mughrabi [23][37], advocated that the internal stress arises due to 2 to Gb d ε_ different yield stresses of subgrain walls (hard) and interior regions (soft). Since the hard and soft regions yield at different stresses, the Where T is the temperature, ε_ is the strain rate, ε_ is the refer- 0 “composite” therefore has a heterogeneous stress state upon ence strain rate (e.g., that of the particle-free material at the same loading, which leads to a non-zero internal stress even after the stress). The value ε_ =ε_ ¼ 1010 [31] is adopted in this work. It is 0 applied stress is removed and successfully explained the Bau- noted that the detachment process is considered to be a thermally- schinger effect in fatigue. However, this theory is less applicable in activated event, where the athermal threshold limit is found to be pffiffiffiffiffiffiffiffiffiffiffiffiffiffi creep since macroscale material yielding is unlikely to occur during t ¼ t 1 k2 at T ¼ 0K.Atafinite temperature, thermal activa- d o creep under very low applied stress. tion assists the detachment process from the particle, even if the Here, we adopt a theory which we believe to be more suitable stress is below the athermal threshold limit. for modeling creep deformation, as originally suggested by Argon When t > t ðTÞ, detachment barriers are overcome instantly eff d [33] and further modified by Oruganti [30] for ferritic steel. In creep therefore time for detachment to complete t ¼ 0. When detach deformation, the migration of subgrain boundaries is impeded by t < t ðTÞ, the detachment process is considered as a thermally- eff d pinning particles. Fig. 7 (g) shows a subgrain boundary in the activated event, whose kinetic can be described as: process of breaking away from a set of M23C6 particles. The h i 0 t 3=21 boundary is bowed between the particles, and dislocation debris is 2 ð Þ eff 3Dv Gb r 1 k 1 t ðTÞ observed around the particles from which the boundaries have t