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Mechanical Characterization of W-armoured Plasma Facing Components after Thermal Fatigue D. Serret*, M. Richou M. Missirlian, and T. Loarer * [email protected] CEA, IRFM, F-13108 Saint Paul-lez-Durance, France PACS reference : 46.50 +a 62.20 me 81.40 Np 81.40 Gh 81.70 –q Abstract: The future fusion device ITER aims at demonstrating the scientific and technical feasibility of fusion power. Tens of thousands of W-armoured Plasma Facing Components (PFCs) will be installed in the vertical targets of the ITER divertor and submitted to high heat flux. The purpose of this paper is to present results on mechanical and microstructural characterizations of tungsten PFCs after thermal fatigue tests. On each component Vickers hardness measurements are performed. In parallel, the mean grain diameter in the corresponding zone of tungsten material is determined. The empirical Hall-Petch relation was adapted to experimental data. However, due to the plateau effect on recrystallization hardness, this relation does not seem to be relevant once recrystallization is complete: a new approach is proposed to predict the margin to the tungsten melting onset. 1 1. Introduction The future fusion device ITER aims at demonstrating the scientific and technical feasibility of fusion power. In the domain of the ITER Plasma Facing Component (PFC) design, monoblock geometry has been chosen to sustain high heat flux loads on the vertical targets of the divertor component. The current ITER Baseline foresees the use of carbon and tungsten in the strikepoint and baffle region of divertor, respectively, for the initial non-active phase of operation with hydrogen and helium plasmas. Thereafter a full tungsten divertor is considered for the nuclear phase with deuterium and deuterium-tritium (D-T) plasmas. High heat flux tests were performed on W components with a monoblock-type geometry consistent with the ITER divertor one. The results show that 10 MW/m² is currently the limit without any degradation observed on the heat load and removal capabilities [1-2]. Beyond, embrittlement of the W armour near the loaded surfaces occurs (roughening, cracking) at 15 MW/m². Finally, after several hundreds of cycles at 20 MW/m², cyclic fatigue induced damages result in higher and higher surface temperature up to the appearance of melted W droplets [3-4]. So far, current numerical simulation tools cannot predict correctly these experimental results. A better characterization of structural damage of W armour material, due to fatigue experiments, is required for a better understanding and prediction of fatigue lifetime related to W-armoured components. The purpose of this paper is to present the first results on mechanical and microstructural characterizations of tungsten armoured actively cooled PFCs after thermal fatigue tests. Among several tested samples, a study is carried out focused on 3 samples that endured 3000 cycles at 10 MW/m² followed by 500 cycles at 20 MW/m². On each 2 component Vickers hardness measurements are performed. In parallel, the mean diameter of the tungsten grains in the related area is determined. Furthermore a comparison with an empirical relation correlating grain diameter and Vickers hardness is discussed whilst an analysis of tungsten PFCs is proposed for its use in future fusion devices. 2. Experimental and numerical descriptions 2.1. Monoblock PFC geometry The geometry of PFCs used in the present work is presented in figure 1. The design is similar to the one used in the ITER Divertor. Each component is 36 mm high, 28 mm wide and 12 mm thick. The minimum tungsten thickness, corresponding to the minimum distance from the loaded surface to the copper heat sink structure, is 5 mm. In order to assess the maximal acceptable defect size (i.e allowing steady state operations without tungsten melting at the surface under heat flux exposure), some calibrated defects were artificially implemented inside the monoblocks. The individual tungsten blocks are made from tungsten sheet material. Pure copper casting technology and hot radial pressing were used to assemble the CuCrZr cooling tube to the Cu compliance layer and the Cu to the tungsten monoblock, respectively. 2.2. Fatigue test campaign A fatigue test campaign was performed on W monoblock PFCs using High Heat Flux (HHF) loads in the electron beam facility FE200 [5]. The purpose of this campaign was to study the detection and the evolution of artificially implemented and calibrated defects under thermal fatigue [1]. Each component was actively cooled with a pressurized (P=33 bar) and thermal controlled (Tinlet =120°C) water flow. During the 3 HHF test campaign, the surface temperature of each component was monitored via an infrared camera. The testing protocol included two phases: a first cycling step of 3000 cycles at 10 MW/m², and a second one of around 500 cycles at 20 MW/m². At 20 MW/m², several phenomena appeared: erosion and vertical cracks at the tungsten surface, initiation of new defects or propagation of artificial defects at the W/Cu interface. These last defects lead to a drop in the cooling efficiency resulting in a surface overheating, and eventually to tungsten melting. Three W-monoblocks were selected on the basis of the maximal surface temperature reached during the tests in order to estimate the fatigue influence on their mechanical properties. It is worth noting that these samples have sustained successfully 500 cycles at 20 MW/m². These monoblocks are considered at a safe state since no apparent damage occurred during fatigue tests. Due to different interface defect size, each component reached various maximal surface temperature monitored by the infrared camera taking into account the low emissivity value (0.28) of tungsten material [9]: Sample 1: Tmax surf = 2500°C Sample 2: Tmax surf = 2900°C Sample 3: Tmax surf = 3200°C 2.3. Mechanical and microstructural measurement set-ups In order to estimate the fatigue influence on the mechanical properties of tungsten monoblock, Vickers hardness measurement is carried out. The set-up is an AVK-CO model of Mitutoyo. This test consists in applying during 30 s a controlled mechanical load (294 N) with a diamond indenter and in correlating the diagonal size of the indentation mark to the Vickers Hardness HV30/30. 4 In parallel to this mechanical characterization, the local microstructure is analyzed based on the NF ISO 643 norm [6]. Among several possibilities for determining the mean tungsten grain diameter, counting the number of grain joint intersections with a 750 µm circle diameter is used. This method slightly overestimates the grain diameter measurement [6]. However, since the average grain diameter defines the recrystallization level that is correlated to the hardness value, this method is relevant for the characterisation of the recrystallization. Vickers hardness measurement and tungsten grain diameter can be linked by the Hall-Petch relation [7-8] which is written in the form: HV a b (kg.mm-2) D grain (1) In the case of the tungsten material at the delivery (from single crystalline material to nanometer polycrystalline grain made material), a and b equal 350 kg.mm-2 and 10 kg.mm-3/2 [9], respectively, and Dgrain represents the diameter of the grain. 2.4. Thermal numerical simulation Because of different evolution of artificial calibrated defects, monoblock overheating induced different surface temperature exceeding sometimes the tungsten melting point (≈ 3500°C). A correlation between number of cycles and the temperature reached by tungsten is used as a reference for defining the fatigue status of the monoblock. In order to estimate the temperature reached by tungsten at each Vickers Hardness and grain diameter measurements, a thermal numerical simulation of the realistic geometry has been performed taking machined defects at W/Cu or Cu/CuCrZr interfaces into account. Uniform heat flux (20 MW/m²) is applied on the top of the monoblock and the Sieder-Tate correlation [10] is used to estimate the convective 5 heat transfer coefficient in the CuCrZr tube. All these simulations are performed with the ANSYS code whilst the thermo mechanical properties are taken from [11]. 3. Results For sample 2 (Tmax = 2900°C), several hardness profiles at different depth in the direction parallel to the surface exposed to the heat flux are plotted in figure 2. These point out the evolution of the tungsten hardness from around 365 HV30/30 in the vicinity of the heated surface to 465 HV30/30 at a depth of 12 mm. At a depth of 6 mm from the heated surface, the hardness value of the non-recrystallized material is similar to the delivered one (HVnon-recrist = 460 HV30/30 [12]). It is worth noting that the experimental hardness measurement on the recrystallized material (365 HV30/30) is comparable to the theoretical value (HVrecrist = 360 HV30/30 [12]) and that the hardness profile does not depend on the direction perpendicular to the heat flux. Steady-state temperature field inside sample 2 is shown in figure 3-a for 20 MW/m² of heat flux deposition. During the HHF tests, once stationary conditions are reached, a constant thermal gradient is established within the monoblock from the heated surface to the cooling tube. The thermal gradient is mainly vertical which is in agreement with hardness profile measurements. This numerical simulation allows defining the recrystallization zone limit (Trecryst = 1350°C [12]). By comparing the numerical results to the tungsten material state in terms of recrystallization, a qualitative agreement is found as shown on figure 3-b. As the tungsten grain size is linked to the cyclic thermal load undergone during HHF tests, we aim at determining a quantitative correlation between grain size and Vickers hardness for the maximal surface temperature of a component. The original HallPetch relation (1) and the experimental data of the sample 2 are presented on the 6 figure 4-a, and it can be observed that the adapted theoretical relation does not fit at all to the experimental results. As a consequence, an adaption of the Hall-Petch relation by fitting the experimental data has been carried out, leading to a reassessment of parameters ‘a’ and ‘b’ at 65.5 and 70.4, respectively. Based on the original Hall-Petch relation, the grain diameter in the non-recrystallized area is estimated at 8 µm whereas the average experimental one is equal to 30 µm. The discrepancy may be explained by the overestimation of the grain diameter measurement technique, and/or the effect of the manufacturing process changing the tungsten grade. In figure 4-b the Vickers hardness is displayed as a function of the grain diameter and the corresponding Hall-Petch fitting curves for the three samples which endured different thermal gradients. Sample 1 reached a lower and sample 3 a higher maximal surface temperature than sample 2. These fitted curves are defined in the hardness range of 360-460 HV 30/30. These correlations are strongly dependent on the maximal surface temperature. The higher is the tungsten maximal surface temperature, the higher will be the maximal grain diameter. Whatever the thermal gradient and the maximal surface temperature of the component: tungsten grains close to the cooling tube will never or slightly be recrystallized. Otherwise copper fusion temperature (1080°C) may be exceeded. Once Vickers hardness has reached the recrystallization one (360 HV30/30), no evolution of the tungsten microstructure may be identified by this single measurement. Here is the highlighted limitation of this non-destructive examination method applied on a recrystallizing metal. In order to predict the effect of the surface temperature of the tungsten PFC on the margin to the melting onset, a new correlation is proposed using adimensional hardness ( HV ) and adimensional grain diameter ( Dgrain ). Using adimensional 7 variables defined in equation (2) and (3) allows adapting and testing the relation to other tungsten grade materials. HV HV HV recryst HV non recryst HV recryst D grain Where Dgrain 0 (2) D grain D grain0 (3) D grainLimit D grain0 is the non-recrystallized tungsten grain size and Dgrain Limit is the maximal grain size before tungsten melting measured during post mortem analysis (0.12 mm). Dgrain and HV are plotted on figure 5. Results for each component are fitted by an exponential function which is written in the form: HV c exp( d Dgrain ) e (4) Interceptions of the Dgrain fitted curves with HV 0 are estimated ( Dgrain ( HV 0) and plotted in figure 6 as a function of the maximal surface temperature. The margin to the tungsten melting onset is defined by the gap to the value Dgrain ( HV 0) 1 and is reduced by increasing the surface temperature. Because of the cyclic recrystallization process occurrence, tungsten grains keep growing. Therefore, in the case of additional fatigue cycles realized with the same maximal surface temperature, grains will be increasingly large implying that the margin to the onset of melting is reduced by the vertical displacement in the figure 6. This reasoning can be applied in the case of coupled additional cycles and increasing surface temperature: slanting displacement from curve to curve with increasing cycle number. To complete the knowledge for the endured thermal cycling, more monoblocks with several maximal surface temperatures are required. This data base will be progressively filled in by tungsten PFCs that endured other fatigue cycle numbers. 8 4. Conclusion Tungsten Plasma Facing Components will be installed in the ITER divertor and exposed to high heat flux. Their design has also to integrate the induced thermal fatigue resulting from cycling. Vickers hardness and microstructure measurements show the fatigue influence through the spatial grain diameter modification. This evolution is well correlated to the thermal gradient in the monoblock. A relation between Vickers hardness and grain diameter via the Hall-Petch one was also tested and adapted to experimental data. However, due to the non evolution of recrystallization hardness in function of the grain diameter, this relation does not seem to be relevant once recrystallization is complete. A new approach is proposed to predict the margin to the tungsten melting onset in the case of tungsten PFC. 9 References [1] Escourbiac F. et al. 2009 Fusion Eng. Des. 84 747 [2] Missirlian M. et al. 2010 Consequences of Fatigue on Heat Flux Removal Capabilities of W Actively Cooled Plasma-Facing Components 23th International Atomic Energy Agency Conference, Daejon, South Korea [3] Missirlian M. et al. 2011 Fatigue Lifetime and Power Handling Capability of Actively Cooled Plasma Facing Components for ITER Divertor 13th International Workshop on Plasma-Facing Materials and Components for Fusion Applications, Rosenheim, Germany [4] Gavila P. et al. 2010 High Heat Flux Testing of Mock-ups for full Tungsten Divertor 26th Symposium on Fusion Technology, Porto, Portugal [5] Bobin Vastra I. et al., Fusion Eng. Des., 2005, 75-79, 357 [6] NF ISO 643 Détermination micrographique de la grosseur de grain apparente, 2003 [7] Hall H.O. 1951 Proc. Phys. Soc. B 64 747 [8] Petch N.J. 1953 J. Iron Steel Inst. 174 25 [9] Lassner E. and Schubert W.-D. 1999 Tungsten: Properties, Chemistry, Technology of the Element, Alloys, and Chemical Compounds (Springer) [10] Sieder E.N. and Tate G.E. 1936 Ind. Eng. Chem. 28 1429 [11] ITER Material Properties Handbook, ITER Doc. No. 574 MA 2 [12] Tungsten Material Properties and Applications, Plansee Brochure 2000. 10 Figure 1: Geometry sketch of tungsten monoblock 11 Figure 2: Dependence of the Vickers hardness on the position in sample 2 (x=0 is on the outer edge, see figures 1 and 3b). 12 Figure 3: Numerical-experimental qualitative comparison of the recrystallization area on sample 2 a) Results of numerical simulation for sample 2 at 20 MW/m² b) Qualitative representation of recrystallized area based on Vickers hardness measurements a) b) Recrystallisation limit 13 Figure 4: Effect of the fatigue test on the relation between tungsten grain diameter and Vickers hardness measurement a) Comparison of the original Hall-Petch relation to experimental data obtained after HHF test (Sample 2) b) Effect of the maximal surface temperature on the relation between grain diameter and tungsten Vickers Hardness a) 14 b) Figure 5: Plot between adimensional Vickers hardness and grain diameter 15 Figure 6: Estimation of the margin to melting onset as function of the surface temperature after 3000 cycles at 10 MW/m² and 500 cycles at 20 MW/m² 16