Influence of Crystallographic Orientation on Helium Bubble and
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Influence of Crystallographic Orientation on Helium Bubble and
Influence of Crystallographic Orientation on Bubble and Fuzz Structure Formation in Tungsten Exposed to Helium Plasma . Ohno, Y. Hirahata, S. Kajita, T. Saeki, M. Yamagiwa agoya University, Japan . Yoshihara, N. Yoshida yushu University, Japan M. Tokitani IFS, Japan 19th International Conference on Plasma Surface Interactions May 24-28 2008, San Diego, USA 1 Background and Purpose NAGDIS Background - Bubble and nanostructure formation (fuzz) in W caused by He plasma exposure → bubble and nanostructure formation reduces the durability to heat load, leading to the release of great amount of tungsten impurity. - Understanding the formation mechanism is one of key issues in case of application of W as plasma-facing components in fusion devices. However, the mechanism of the nanostructure formation has been not fully understood yet. Purpose -Investigate the effect of Crystal Orientation on bubble and nanostructure formation especially at initial phase (transition from bubble to protrusion) by using ITER reference W (Recrystallized), Single Crystal W (100), (110) Summary of bubble and fuzz formation condition NAGDIS NAGDIS •Closed markers with nanostructure •Open markers without nanostructure Surface Temp: 1000 K < T < 2000 K Ion Incident Energy>20 eV Kajita et al. NF2009 [4] M. Baldwin NF (2008). [7] W. Sakaguchi JNM (2009) [8] S. Kajita, NF (2007). [9] S. Kajita, NF (2009). [11] S. Kajita, J. Appl. Phys. (2006). [12] W. Sakaguchi, Proc. 18th Int. Toki Conf. (2008). [13] D. Nishijima, JNM (2004). [14] D. Nishijima, JNM (2003). [15] D. Nishijima, NF (2005). 3 Summary of bubble and fuzz formation condition NAGDIS NAGDIS Dr. Iwakiri (Kyusyu univ.) •Closed markers with nanostructure •open markers without nanostructure Surface Temp: 1000 K < T < 2000 K Ion Incident Energy>20 eV Kajita et al. NF2009 [4] M. Baldwin NF (2008). [7] W. Sakaguchi JNM (2009) [8] S. Kajita, NF (2007). [9] S. Kajita, NF (2009). [11] S. Kajita, J. Appl. Phys. (2006). [12] W. Sakaguchi, Proc. 18th Int. Toki Conf. (2008). [13] D. Nishijima, JNM (2004). [14] D. Nishijima, JNM (2003). [15] D. Nishijima, NF (2005). 4 Development of W nanostructure NAGDIS PM-W 1400K 50eV-He plasma Bubble Pinhole Protrusions Swelling &Digging NanoStructure (Fuzz) TEM (FIB) SEM S. Kajita, et al. NF20009 5 Initial phase of W nanostructure formation PM-W 1400K, 50eV-He plasma, 6x1024He+/m2 (375 s) NAGDIS NAGDIS Bubbles (~ 50nm) in the swelling and under the surface (100nm) Shape of bubble:sphere 100nm 100nm Initial phase of W nanostructure formation PM-W 1400K, 50eV-He plasma, 6x1024He+/m2 (375 s) NAGDIS NAGDIS Bubbles (~ 50nm) in the swelling and under the surface (100nm) Shape of bubble:sphere Bubbles?? 100nm 100nm Difference in bubble and fuzz formation for each grain NAGDIS NAGDIS 26 + 2 ITER reference-W 1800K 30eV-He plasma 7.2x10 He /m (36000 s) Large grains grow due to high surface temperature 500 500μm μm - Surface modification is quite different for each grain - black region -- flat terrace-like structure - white region – bumpy 50 50μm μm 5μm 55μm 5μm μm 8 Grain with wider terrace has few protrusions NAGDIS NAGDIS ITER reference-W 1800K 30eV-He plasma 7.2x1026He+/m2 (36000 s) 55μm μm 55μm μm 55μm μm 55μm μm TEM observation of boundary between grains NAGDIS with terraces and protrusions NAGDIS ITER reference-W 1800K 30eV-He plasma 7.2x1026He+/m2 (36000 s) Sample Area milled by FIB 10μm 10μm TEM observation of boundary between grains with terrace and protrusions (2) NAGDIS NAGDIS In the grain having the terrace, many bubbles, but no protrusions In the grain with protrusions, the surface goes down 600nm from original surface The depth of the hole becomes deeper along grain boundary Development of “terrace” structure development of nano-structure projection f ac e original sur face retreat of sur G.B. Area milled by FIB 10μm 10μm <113> <113> 1μm Bubble shape in grain having few protrusions NAGDIS ITER reference-W 1800K 30eV 7.2x1026He+/m2 Polygon shape bubbles with a diameter above 300nm surrounded by (110) surface → Gas pressure inside bubbles is relatively small → Few flaking → Few pinholes on the surface 101 200nm 200nm He plasma exposure to single crystal W NAGDIS Specimens: Single crystal W (0.5mm thickness) (110) : closed-packed plane W(bcc) → split plane (100) : - Cutting disks from single crystal tungsten rods - Mirror finish by mechanical polishing - Remove disordered surface layer by (100) using electrolytic polisher (110) XRD (100) He plasma (100) (110) PM-W 13 Surface modification on single crystal W(100) NAGDIS 1600K 64eV 1.0x1025He+/m2 - Slow growth of protrusions - Protrusion starts to grow at edge of pinhole (burr) - Once a protrusion appears, it grows rapidly. Surface modification on single crystal W(110) NAGDIS 1600K 64eV 1.0x1025He+/m2 Tilt 45º 1μm 1μm 1μm 1μm Tilt 60º -Strange wavy structure to be extended in one direction like a mountain range -Fewer pinholes -Fewer protrusions 1μm 1μm Surface modification on single crystal W(110) NAGDIS 1600K 64eV 1.0x1025He+/m2 200nm 200nm 200nm 200nm <001> Sample Sample area area by by FIB FIB 1μm - Cross section of wavy structure is almost triangle having planes with (010) and (001) - Wavy structure expands along (001) - Protrusion formation is very slow - It takes a time for (110) surface to be changed to (100) Summary -1 Conclusions NAGDIS NAGDIS - Investigate the effect of crystallographic orientation on formation of bubble and nanostructure At re-crystallized ITER reference W crystal grains with terrace and flat structure (113) have fewer protrusions even they have a lot of bubbles formed under the surface. Typical shape of bubbles is polygon. At the single crystal W (100) a protrusion starts to grow from edges of flaked bubbles. At the single crystal W (110) strange wavy structure having surfaces with (010) and (001) was formed. Fewer pinholes → Fewer protrusions → Slow nanostructure formation. W(110), (100), (113) slow growth, but fast growth grain?? Future works Re-crystallized W with large grain by only heating → Orientation of all grains is analyzed before He plasma exposure. 17 NAGDIS Appendix 18 SIM images of terrace region sputtered by FIB NAGDIS many bubbles under the surface 30度傾斜 30度傾斜 He flux and fluence in ITER NAGDIS ITPA presentation by Y. Ueda 20 He bubble and hole formation at bulky W (2) NAGDIS Threshold of incident ion energy as low as 6 eV D. Nishijima, M. Y.Ye, N. Ohno, S. Takamura Journal of Nuclear Materials, Vol.313-316, 2003, pp.97-101 21 He bubble and hole formation at bulky W (3) NAGDIS Threshold of surface temperature and fluence Hole Formation Nano Structure 22 Orientation of grains A:001 C:111 100μm 100μm B:101 Results B:(101) A:(001) 0.5μm C:(111) 0.5μm 0.5μm SCW(100) SCW(110) PM 5μm 5μm 5μm 2μm 2μm 2μm SEM micrograph 照射時間300s 入射イオンエネルギー69.8eV フラックス1.9×1022m-2s-1 フルエンス0.6×1025m-2 試料温度 1568 [K] 照射時間720s 入射イオンエネルギー64.4eV フラックス2.0×1022m-2s-1 フルエンス1×1025m-2 照射時間1080s 入射イオンエネルギー66.4eV フラックス1.5×1022m-2s-1 フルエンス1.6×1025m-2 試料温度 1599 [K] 試料温度 1519 [K] (100) 2μm 2μm 試料温度 1554 [K] 2μm 試料温度 1598 [K] 2μm 試料温度 1483 [K] (110) 2μm 試料温度 1544 [K] 2μm 2μm 試料温度 1579 [K] 2μm 2μm 試料温度 1499 [K] PM 2μm 2μm 2μm 2μm 2μm 2μm