In-situ TEM investigation of dislocation loop reaction and irradiation hardening in H2+-He+ dual-beam irradiated Mo

doi:10.1016/j.jmst.2021.07.040

Abstract

Abstract:

Through in-situ TEM observation during 30 keV H₂⁺-He⁺ dual-beam irradiation at 723 K, the reaction and transformation of dislocation loops in pure Mo were investigated, especially for <100> loops. Irradiation could directly cause the formation of 1/2<111> loops and <100> loops, but 1/2<111> loops were dominant. In-situ observation confirmed the formation mechanism of <100> loops, including direct irradiation induced mechanism, 1/2<111> loop direct conversion mechanism, and reaction mechanism of two 1/2<111> loops. Meanwhile, the reaction of two 1/2<111> loops to produce <100> loop should not require the strict size similarity condition. The reaction between 1/2<111> loops could also produce 1/2<111> loop, which was essentially a process in which one loop absorbed another one. The yield strength increment caused by irradiation-induced loops was analyzed, and its saturation value reached 0.48 GPa at 0.06 dpa. Compared with single He⁺ irradiation, the number density and average diameter of loops increased significantly and more serious damage was caused under the synergistic effect of hydrogen and helium. The mechanism based on in-situ experimental observation was discussed in depth.

Key words: In-situ TEM observation, Dislocation loop, Hydrogen helium irradiation, Molybdenum, Irradiation hardening

Yipeng Li, Guang Ran, Xinyi Liu, Qing Han, Xiuyin Huang, Yifan Ding. In-situ TEM investigation of dislocation loop reaction and irradiation hardening in H₂⁺-He⁺ dual-beam irradiated Mo[J]. J. Mater. Sci. Technol., 2022, 107: 14-25.

Figures/Tables 11

Fig. 1. (a) Depth profiles of displacement damage and injected H & He concentrations in pure Mo irradiated by 30 keV H2+ & He+ due beam with the fluence of 4.75 × 1015 H2+/cm2 and 3.96 × 1015 He+/cm2; (b) Time profiles of displacement damage, injected He & H concentrations in the in-situ monitored region (approximately 100 nm).

Table 1 The ion fluences and corresponding injected H-He concentrations and irradiation damage at the monitored region under 30 keV H2+-He+ dual-beam irradiation.

Ion fluence (ions/cm²)	4.75 × 10¹⁴ H₂⁺ + 3.96 × 10¹⁴ He⁺	1.19 × 10¹⁵ H₂⁺ + 9.90 × 10¹⁴ He⁺	1.90 × 10¹⁵ H₂⁺ + 1.58 × 10¹⁵ He⁺	2.38 × 10¹⁵ H₂⁺ + 1.98 × 10¹⁵ He⁺	3.56 × 10¹⁵ H₂⁺ + 2.97 × 10¹⁵ He⁺	4.75 × 10¹⁵ H₂⁺ + 3.96 × 10¹⁵ He⁺
Injected H₂⁺ concentration, appm	170	410	660	830	1240	1660
Injected He⁺ concentration, appm	280	690	1110	1390	2080	2780
Irradiation damage, dpa	0.008	0.02	0.03	0.04	0.06	0.08

Table 2 Type criterion of dislocation loops near the [001] zone axis.

g·b	1/2[111]	1/2[11$\bar{1}$]	1/2[$\bar{1}$11]	1/2[1$\bar{1}$1]	[100]	[010]	[001]
1 1 0	√	√	ⅹ	ⅹ	√	√	ⅹ
1$\bar{1}$0	ⅹ	ⅹ	√	√	√	√	ⅹ
0 2 0	√	√	√	√	ⅹ	√	ⅹ
Category	B	B	C	C	D	E	/

Fig. 2. Bright field TEM images taken under different diffraction conditions near [001] zone axis showing showing the formation of <100> loops. (a1-a3) g = 1$\bar{1}$0; (b1-b3) g = 110; and (c1-c3) g = 020. The irradiation fluences: (a1-c1) 1.19 × 1015 H2+/cm2 and 9.9 × 1014 He+/cm2; (a2-c2) 1.9 × 1015 H2+/cm2 and 1.58 × 1015 He+/cm2; and (a3-c3) 3.56 × 1015 H2+/cm2 and 2.97 × 1015 He+/cm2. Red and purple circles represent <100> loops, while blue and yellow circles represent 1/2<111> loops. Solid circles and dashed circles represent visibility and invisibility loops, respectively.

Fig. 3. Loop reactions are shown in the bright field TEM images taken at g =1$\bar{1}$0, 020 and 110 near [001] zone axis. (a1-a3) g =1$\bar{1}$0; (b1-b3) g =110; and (c1-c3) g =020. The irradiation fluences: (a1-c1) 2.38 × 1015 H2+/cm2 and 1.98 × 1015 He+/cm2; (a2-c2) 3.56 × 1015 H2+/cm2 and 2.97×1015 He+/cm2; (a3-c3) 4.75 × 1015 H2+/cm2 and 3.96 × 1015 He+/cm2. Red circles represent <100> loops, while blue and yellow circles represent 1/2<111> loops. Solid circles and dashed circles represent visibility and invisibility loops, respectively. All images have same scale bar.

Fig. 4. Loop reactions are shown in the bright field TEM images taken at g =1$\bar{1}$0, 020 and 110 near [001] zone axis. (a1) and (a2) g =1$\bar{1}$0; (b1) and (b2) g = 110; (c1) and (c2) g = 020. The irradiation fluences: (a1-c1) 2.38 × 1015 H2+/cm2 and 1.98 × 1015 He+/cm2; (a2-c2) 3.56×1015 H2+/cm2 and 2.97 × 1015 He+/cm2. Red circles represent <100> loops, while blue and yellow circles represent 1/2<111> loops. Solid circles and dashed circles represent visibility and invisibility loops, respectively.

Fig. 5. (a) The relationship between the ratio of <100> loops and irradiation dose; (b) The size and number density of <100> loops as a function of irradiation dose.

Fig. 6. (a) Volume number density and (b) average size of all dislocation loops as a function of irradiation dose at g =1$\bar{1}$0, 110 and 020 near [001] zone axis.

Fig. 7. Bright field TEM images taken at g =1$\bar{1}$0 close to [001] zone axis (indicated by black arrows in (a)) showing the evolution of dislocation loops in the Mo. Irradiation fluences are: (a) 4.75 × 1014 H2+/cm2 and 3.96 × 1014 He+/cm2; (b) 1.19 × 1015 H2+/cm2 and 9.9 × 1014 He+/cm2; (c) 1.9 × 1015 H2+/cm2 and 1.58 × 1015 He+/cm2; (d) 2.38 × 1015 H2+/cm2 and 1.98 × 1015 He+/cm2; (e) 3.56 × 1015 H2+/cm2 and 2.97 × 1015 He+/cm2; and (f) 4.75 × 1015 H2+/cm2 and 3.96 × 1015 He+/cm2. The scale bar in (a) applies to all images.

Fig. 8. Schematics showing the reaction process of two 1/2<111> loops after collision to form <100> loop or 1/2<111> loop. The two 1/2<111> loops (loop A and B) are located on different {111} habit planes. The black arrows represent the diffusion direction of interstitial atoms on the habit plane of the corresponding loop.

Fig.9. Irradiation hardening (Δσloop) and total damage (loop density × loop area) as a function of irradiation damage (dpa) for the in-situ 30 keV H2+-He+ dual-beam irradiated Mo sample at 723 K.

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In-situ TEM investigation of dislocation loop reaction and irradiation hardening in H₂⁺-He⁺ dual-beam irradiated Mo

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