Dealloying corrosion of anodic and nanometric Mg41Nd5 in solid solution-treated Mg-3Nd-1Li-0.2Zn alloy

doi:10.1016/j.jmst.2020.12.049

Abstract

Abstract:

The microstructure and chemical compositions of the solid solution-treated Mg-3Nd-1Li-0.2Zn alloy were characterized using optical microscope, scanning electron microscope (SEM), transmission electron microscope (TEM), electron probe micro-analyzer (EPMA) and X-ray photoelectron spectroscopy (XPS). The corrosion behaviour of the alloy was investigated via electrochemical polarization, electrochemical impedance spectroscopy (EIS), hydrogen evolution test and scanning Kelvin probe (SKP). The results showed that the microstructure of the as-extruded Mg-3Nd-1Li-0.2Zn alloy contained α-Mg matrix and nanometric second phase Mg₄₁Nd₅. The grain size of the alloy increased significantly with the increase in the heat-treatment duration, whereas the volume fraction of the second phase decreased after the solid solution treatment. The surface film was composed of oxides (Nd₂O₃, MgO, Li₂O and ZnO) and carbonates (MgCO₃ and Li₂CO₃), in addition to Nd. The as-extruded alloy exhibited the best corrosion resistance after an initial soaking of 10 min, whereas the alloy with 4h-solution-treatment possessed the lowest corrosion rate after a longer immersion (1 h). This can be attributed to the formation of Nd-containing oxide film on the alloys and a dense corrosion product layer. The dealloying corrosion of the second phase was related to the anodic Mg₄₁Nd₅ with a more negative Volta potential relative to α-Mg phase. The preferential corrosion of Mg41Nd5 is proven by in-situ observation and SEM. The solid solution treatment of Mg-3Nd-1Li-0.2Zn alloy led to a shift in corrosion type from pitting corrosion to uniform corrosion under long-term exposure.

Key words: Magnesium alloy, Corrosion, Second phase, Rare metal, Dealloying

Gui-Jia Gao, Mei-Qi Zeng, En-Liang Zhang, Rong-Chang Zeng, Lan-Yue Cui, Dao-kui Xu, Feng-Qin Wang, M. Bobby Kannan. Dealloying corrosion of anodic and nanometric Mg₄₁Nd₅ in solid solution-treated Mg-3Nd-1Li-0.2Zn alloy[J]. J. Mater. Sci. Technol., 2021, 83: 161-178.

Figures/Tables 23

Table 1 Treatment of the samples at T4 state.

Samples	#1	#2	#3	#4	#5
Heating time (h)	0	2	4	8	12

Fig. 1. Optical microstructure (a-e), SEM (a1-e1), EPMA images (a2-e2) and corresponding element energy spectrums (Mg (a3-e3), Nd (a4-e4) and Zn (a5-e5)) of samples #1, 2, 3, 4 and 5.

Fig. 2. Grain size and volume fraction of the secondary phase of the alloys at T4 treatment.

Fig. 3. (a) EPMA images of nanometric Mg41Nd5 particles, (b) corresponding EDS mapping of point 1-6 of sample 1 and (c) XRD pattern of samples #1-5.

Fig. 4. (a), (b) TEM morphology of nanometric Mg41Nd5 particles, (c) the atomic percentage in corresponding EDS results and (d) selected area diffraction patterns of Mg41Nd5.

Fig. 5. XPS survey of samples (a) #1, (b) #2, (c) #3, (d) #4 and (e) #5.

Fig. 6. High resolution XPS for Mg1 s, Nd3d, Li1 s, Zn2p and O1 s signals on the surface of samples (a) #1, (b) #2, (c) #3, (d) #4 and (e) #5.

Table 2 Chemical compositions of oxide films of samples #1-5 after solution heat treatment, at. %.

Sample	C	Li	Nd	Mg	O	Zn
#1	70.77	1.72	0.62	3.12	23.66	0.12
#2	53.53	1.21	1.23	5.89	37.98	0.17
#3	50.06	2.39	1.17	4.25	41.97	0.20
#4	34.00	6.51	1.33	9.04	48.91	0.21
#5	45.70	3.11	1.04	7.14	42.89	0.13

Fig. 7. HERs of samples (1) #1, (2) #2, (3) #3, (4) #4 and (5) #5 during (a) 0-13 h, (b) 0-158 h and (c) 50-160 h of soaking in 3.5 wt.% NaCl solution.

Fig. 8. Macroscopic corrosion morphology of samples (a) #1, (b) #2, (c) #3, (d) #4 and (e) #5 after immersion in 3.5 wt.% NaCl solution for 158 h.

Fig. 9. Corrosion morphologies with corrosion products of (a) #1, (b) #2, (c) #3, (d) #4, dealloying of second phases Mg41Nd5 emerged as the arrows, and (e) #5 samples at low magnification; and (f) #1, (g) #2, (h) #3, (i) #4 and (j) #5 samples at high magnification; corrosion morphology after removing corrosion products of (k) #1, (l) #2, (m) #3, (n) #4 and (o) #5 samples at low magnification; and (p) #1, (q) #2, (r) #3, (s) #4 and (t) #5 samples at high magnification.

Fig. 10. (a) Corresponding atomic percentage of the points in the SEM image of Fig. 9 via EDS and (b) XRD patterns of samples #1-5 after soaking in 3.5 wt. % NaCl solution for 158 h.

Fig. 11. SEM image of the Mg41Nd5 phase after soaking for (a) 0 h, (b) 1 h and (c) 2 h in 3.5 wt. % NaCl solution.

Fig. 12. (a) SEM image of Mg41Nd5 phase at high magnification after soaking for 1 h in 3.5 wt. % NaCl solution and (b), (c), (d), (e) and (f) EDS mapping images.

Fig. 13. In-situ observation of Mg41Nd5 soaked in 3.5 wt. % NaCl solution for (a) 0 h, (b) 1 h, (c) 3 h, (d) 5 h, (e) 7 h and (f) corrosion products removal of (e).

Fig. 14. Cross-sectional EPMA images of (a) #1, (b) #2, (c) #3, (d) #4 and (e) #5 after soaking for three days in 3.5 wt. % NaCl solution; (f) #1, (g) #2, (h) #3, (i) #4 and (j) #5 after soaking for five days and (k) #1, (l) #2, (m) #3, (n) #4 and (o) #5 after soaking for seven days.

Fig. 15. (a) Surface Volta potential map of #1, (b) OCP as a function of immersion time of (1) #1, (2) #2, (3) #3, (4) #4 and (5) #5 samples, (c) potentiodynamic polarization curves of (1) #1, (2) #2, (3) #3, (4) #4 and (5) #5 samples after the immersion in 3.5 wt.% NaCl solution for 10 min and (d) 1 h and (e) corresponding current density line chart.

Fig. 16. (a) Nyquist diagrams, (b) Bode plots of Zmod and (c) Bode plots of phase angle of (1) #1, (2) #2, (3) #3, (4) #4 and (5) #5 after the immersion in 3.5 wt.% NaCl solution for 10 min; (d) Nyquist diagrams, (e) Bode plots of Zmod and (f) Bode plots of phase angle of (1) #1, (2) #2, (3) #3, (4) #4 and (5) #5 after immersed in 3.5 wt.% NaCl solution for 1 h; (g) Equivalent circuits of samples #1-5 after immersion for 10 min, (h) sample #1 and (i) sample #2-5 after immersion for 1 h.

Table 3 Electrochemical data obtained by equivalent circuit fitting EIS curves of the samples after immersed for 10 min.

Samples	R_s (Ω cm²)	CPE₁ (Ω^-1·Sⁿ cm²)	n₁	R_ct (Ω cm²)	CPE₂ (Ω^-1·Sⁿ cm²)	n₂	R₂ (Ω cm²)	L (H cm²)	R_{L Mg}²⁺ (Ω cm²)
#1	19.20 ± 0.86	(1.64 ± 0.12)×10^-5	0.93 ± 0.03	548 ± 12	(3.97 ± 0.22)×10^-3	0.61 ± 0.02	235 ± 10	(7.82 ± 1.12)×10⁴	2124 ± 72
#2	19.69 ± 0.72	(1.80 ± 0.23)×10^-5	0.94 ± 0.03	357 ± 8	(5.13 ± 0.35)×10^-3	0.37 ± 0.03	231 ± 13	(3.54 ± 1.98)×10⁴	817 ± 35
#3	19.32 ± 1.06	(1.93 ± 0.32)×10^-5	0.94 ± 0.05	343 ± 5	(5.86 ± 0.18)×10^-3	0.56 ± 0.07	239 ± 18	(1.90 ± 1.88 × 10⁴	1052 ± 50
#4	19.68 ± 1.43	(1.75 ± 0.19)×10^-5	0.94 ± 0.08	327 ± 6	(7.46 ± 0.46)×10^-3	0.38 ± 0.04	274 ± 29	(2.32 ± 0.92)×10⁴	1414 ± 44
#5	19.30 ± 0.43	(1.71 ± 0.18)×10^-5	0.94 ± 0.06	244 ± 15	(8.36 ± 0.44)×10^-3	0.40 ± 0.06	252 ± 15	(1.27 ± 1.06)×10⁴	948 ± 25

Table 4 Electrochemical data obtained by equivalent circuit fitting EIS curves of the samples after immersing for 1 h.

Samples	R_s (Ω cm²)	CPE₄(Ω^-1·Sⁿ cm²)	n₁	R_ct (Ω cm²)	CPE₃(Ω^-1·Sⁿ cm²)	n₂	R₃ (Ω cm²)	L_Mg+ (H cm²)	R_{L Mg}²⁺ (Ω cm²)	L (H cm²)	R_L (Ω cm²)
#1	17.62 ± 0.36	(1.75 ± 0.13)×10^-5	0.90 ± 0.01	314 ± 7				(1.15 ± 0.88)×10³	61 ± 10	68 ± 16	2353 ± 398
#2	18.02 ± 0.44	(2.56 ± 0.15)×10^-5	0.89 ± 0.03	346 ± 12	(5.24 ± 0.22)×10^-3	0.45 ± 0.02	424 ± 19	(1.2 ± 0.13)×10⁴	865 ± 33	—	—
#3	21.74 ± 0.52	(1.98 ± 0.22)×10^-5	0.91 ± 0.02	500 ± 24	(5.08 ± 0.32)×10^-3	0.60 ± 0.04	549 ± 36	(3.32 ± 1.23)×10⁴	1182 ± 56	—	—
#4	17.56 ± 0.13	(2.18 ± 0.41)×10^-5	0.89 ± 0.03	419 ± 16	(5.24 ± 0.43)×10^-3	0.73 ± 0.08	401 ± 17	(1.74 ± 1.56)×10⁴	1205 ± 92	—	—
#5	21.34 ± 0.24	(2.18 ± 0.36)×10^-5	0.90 ± 0.03	362 ± 27	(5.87 ± 0.56 × 10^-3	0.61 ± 1.02	316 ± 22	(2.71 ± 0.98)×10⁴	1552 ± 78	—	—

Fig. 17. (a) Simplified corrosion polarization diagram (anodic 1 for Mg, anodic 2 for Nd) and (b) schematic diagram of the dealloying mechanism of anodic Mg41Nd5 phase.

Fig. 18. Schematic illustration for bubble growth mechanism of sample #3.

Fig. 19. Relationship between corrosion current density and grain sizes of (a) immersion for 10 min and (b) after the immersion for 1 h.

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Dealloying corrosion of anodic and nanometric Mg₄₁Nd₅ in solid solution-treated Mg-3Nd-1Li-0.2Zn alloy

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