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Acta Metall Sin  2025, Vol. 61 Issue (3): 509-520    DOI: 10.11900/0412.1961.2024.00324
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Effect of Hot Rolling Process on Mechanical Property and Corrosion Behavior of Rapidly Degrading Mg-Li Alloy
PANG Mengyao1, WU Ruizhi1(), MA Xiaochun1(), JIN Siyuan1, YU Zhe1, Boris Krit2
1 Key Laboratory of Superlight Materials & Surface Technology, Ministry of Education, Harbin Engineering University, Harbin 150001, China
2 Moscow Aviation Institute, National Research University, Moscow 125993, Russia
Cite this article: 

PANG Mengyao, WU Ruizhi, MA Xiaochun, JIN Siyuan, YU Zhe, Boris Krit. Effect of Hot Rolling Process on Mechanical Property and Corrosion Behavior of Rapidly Degrading Mg-Li Alloy. Acta Metall Sin, 2025, 61(3): 509-520.

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Abstract  

Oil and gas resources have become strategic assets, highlighting the need to improve production efficiency. Segmented fracturing technology effectively addresses the challenge of low fracturing efficiency and is widely used in oil and gas extraction. Therefore, the demand for degradable fracturing materials has increased rapidly to enhance oil and gas production efficiency. Rapidly degradable fracturing materials must achieve high degradation rates, while maintaining strong mechanical properties to ensure effective petroleum fracturing operations. Building on previous research on as-cast Mg-8Li-4Gd-1.5Ni alloys that are known for their high corrosion rates, this study performed hot rolling at 250 oC, with deformations of 30%, 50%, 70%, and 90%. Further, SEM, TEM, tensile mechanical performance testing, electrochemical testing, and hydrogen evolution measurements were used to examine the microstructure, mechanical properties, and corrosion behavior of the alloys. Results indicated that the microstructure underwent continuous elongation during rolling, and the networked long-period stacking ordered (LPSO) phases gradually transformed into parallel fibrous structures. At a deformation of 90%, the elongated fibrous LPSO phases were fractured into shorter segments, accompanied by an increase in the size and number of gaps between the LPSO phases. Recrystallized structures developed during hot rolling, accompanied by the refinement of GdNi3 particles and an increase in the dislocation density. As the deformation increased, the tensile strength of the alloy initially increased and then decreased. The alloy exhibited the highest tensile strength of 217 MPa and an elongation of 17% at a deformation of 70%. In a 3%KCl solution, the mass loss rate, hydrogen evolution volume, and hydrogen evolution rate of the alloy increased steadily, as the deformation increased. At a deformation of 90%, the alloy exhibited the highest corrosion rates at 25 and 93 oC, with mass loss rates of 0.47 and 3.63 mg/(cm2·min), respectively. Compared with the as-cast alloy, the weight loss rate of the hot-rolled alloy at 25 oC increased by 30.55%, whereas at 93 oC, it was 7.72 times greater than at 25 oC. The corrosion current density reached a maximum of 5.34 mA/cm2 at 25 oC. The corrosion began with pitting and gradually transitioned to filiform corrosion. The corrosion extended along the rolling direction at higher deformations. The parallel distribution of LPSO phases inhibited alloy corrosion. However, at a deformation of 90%, the fracture of the LPSO phases increased the number of galvanic corrosion sites. This fracture and the larger gaps between the LPSO phases reduced the protective effect. In addition, the bending of the LPSO phases, fragmentation of the secondary phases, recrystallization, and increased dislocation density enhanced the chemical reactivity of the alloy, resulting in a gradual increase in the corrosion rate. Hot rolling increased the dislocation density, reduced the grain size, and induced recrystallization in the alloy. These microstructural modifications resulted in work hardening and grain refinement, thereby improving the mechanical properties of the alloy.

Key words:  Mg-Li alloy      fracturing      rolling      corrosion behavior      mechanical property     
Received:  12 September 2024     
ZTFLH:  TG146.2  
Fund: National Natural Science Foundation of China(52261135538);National Natural Science Foundation of China(U21A2049);National Natural Science Foundation of China(52271098);National Natural Science Foundation of China(U23A20541);Russian Science Foundation(23-49-00098);China Postdoctoral Science Foundation(GZC20233424);Heilongjiang Postdoctoral Foundation(LBH-Z23116)
Corresponding Authors:  WU Ruizhi, professor, Tel: (0451)83519890, E-mail: rzwu@hrbeu.edu.cn;
MA Xiaochun, Tel: (0451)83519890, E-mail: maxiaochun@hrbeu.edu.cn

URL: 

https://www.ams.org.cn/EN/10.11900/0412.1961.2024.00324     OR     https://www.ams.org.cn/EN/Y2025/V61/I3/509

Fig.1  SEM images of as-cast (a) and rolled Mg-8Li-4Gd-1.5Ni alloy with deformations of 30% (b), 50% (c), 70% (d), and 90% (e) at 250 oC (Circles in Figs.1d and e show the α-Mg. LPSO—long-period stacking ordered)
Fig.2  TEM images of rolled Mg-8Li-4Gd-1.5Ni alloy with 90% deformation at 250 oC
(a) striated structure (b) recrystallized grain (c) dislocation
Fig.3  TEM images and corresponding EDS element maps of rolled Mg-8Li-4Gd-1.5Ni alloy with 90% deformation at 250 oC
(a) GdNi3 (b) LPSO phase (Inset in Fig.3b show the selected area electron diffraction pattern)
Fig.4  Engineering stress-strain curves of rolled Mg-8Li-4Gd-1.5Ni alloy with different deformations at 250 oC
Fig.5  Fracture morphologies of rolled Mg-8Li-4Gd-1.5Ni alloy with deformations of 30% (a), 50% (b), 70% (c), and 90% (d) at 250 oC
Fig.6  Mass loss rates (a), hydrogen evolution volumes (b), and hydrogen evolution rates (c) of rolled Mg-8Li-4Gd-1.5Ni alloy with different deformations at 250 oC after soaking in 3%KCl solution
Fig.7  RD-ND surface SEM images of rolled Mg-8Li-4Gd-1.5Ni alloy with deformations of 30% (a, e), 50% (b, f), 70% (c, g), and 90% (d, h) at 250 oC after soaking in 3%KCl solution for 2 s (a-d) and 30 s (e-h), corrosion products EDS line scaning results along arrows in Figs.7e-h (i-l), and surface SEM images after removal of corrosion products after soaking in 3%KCl solution for 30 s (m-p) (RD—rolling direction, ND—normal direction. Lines in Figs.7m-p show the corrosion regions)
Fig.8  RD-TD surface SEM images of rolled Mg-8Li-4Gd-1.5Ni alloy with deformations of 30% (a, e), 50% (b, f), 70% (c, g), and 90% (d, h) at 250 oC after soaking in 3%KCl solution for 2 s (a-d) and 30 s (e-h), and surface SEM images after removal of corrosion products after soaking in 3%KCl solution for 30 s (i-l) (TD—transverse direction)
Fig.9  RD-ND surface SEM images and corresponding EDS element maps of rolled Mg-8Li-4Gd-1.5Ni alloy with deformations of 30% (a), 50% (b), 70% (c), and 90% (d) at 250 oC after soaking in 3%KCl solution for 1 h (Yellow arrows show the area where LPSO phase prevents corrosion, red arrows indicate that the corrosion is spreading further, blue arrow represents bulk LPSO phase)
Fig.10  Polarization curves of rolled Mg-8Li-4Gd-1.5Ni alloy at 250 oC with different deformations (a) and fitting results (b) (SCE—saturated calomel electrode, Ecorr—corrosion potential, icorr—corrosion current density)
Fig.11  Electrochemical impedance spectroscopy (EIS) (a-c) and equivalent circuit (d) of rolled Mg-8Li-4Gd-1.5Ni alloy with different deformations at 250 oC after soaking in 3.0%KCl solution
(a) Nyquist curves (Z'—real part of the impedance, Z"—imaginary part of the impedance)
(b) Bode angle plots (f—frequency)
(c) Bode impedance plots (|Z|—mode of impedance)
(d) equivalent circuit (Rs—solution resistance, CPE1—a constant phase element representing the surface film capacitance, Rf—surface film resistance mainly determined by the film porosity and the solution conductivity in the film pores, CPE2—a constant phase element related to the double layer capacitance, Rct—charge transfer resistance at film/substrate interface, L—inductance meaning the collapse of partial protective film)

Deformation

%

Rs

Ω·cm2

CPE1

sn1·Ω-1·cm-2

n1

Rf

Ω·cm2

CPE2

sn2·Ω-1·cm-2

n2

Rct

Ω·cm2

L

H

3032.944.84 × 10-40.633.227.06 × 10-50.965.952.31
5031.246.05 × 10-50.823.281.07 × 10-40.925.462.17
7031.461.11 × 10-40.802.671.01 × 10-40.773.941.61
9031.426.57 × 10-20.831.331.13 × 10-40.992.711.37
Table 1  EIS fitting results of rolled Mg-8Li-4Gd-1.5Ni alloy with different deformations at 250 oC after soaking in 3.0%KCl solution
Fig.12  Corrosion mechanisms of rolled Mg-8Li-4Gd-1.5Ni alloy with deformations of 30% (a), 50% (b), 70% (c), and 90% (d) at 250 oC after soaking in 3.0%KCl solution
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