Pretreatment and Post-deposition Annealing for Nanocomposite Electrodeposition on AZ91D Magnesium Alloy

LI Zhi, HOU Jin, LIU Chongyu, LIU Guangke, WANG Zhen

Surface Technology ›› 2026, Vol. 55 ›› Issue (7) : 157-168.

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Surface Technology ›› 2026, Vol. 55 ›› Issue (7) : 157-168. DOI: 10.16490/j.cnki.issn.1001-3660.2026.07.013
Surface and Interface Strengthening Technology

Pretreatment and Post-deposition Annealing for Nanocomposite Electrodeposition on AZ91D Magnesium Alloy

  • LI Zhi1, HOU Jin1, LIU Chongyu2, LIU Guangke1, WANG Zhen1,*
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Abstract

This study focuses on the optimization of pre-treatment chemical pre-deposition process and post-treatment annealing process for electrodeposited Ni-ND-CNTs nanocomposite coatings on the surface of AZ91D magnesium alloy. Nanocomposite electrodeposition technology is used to prepare Ni-ND-CNTs nanocomposite coatings on magnesium alloy. The properties of the deposited coatings are characterized by microhardness tester, scratch tester, friction and wear tester, and electrochemical workstation. The microstructure of the deposited coatings is analyzed by metallographic microscope, scanning electron microscope (SEM), X-ray diffractometer (XRD), and atomic force microscope (AFM) to identify the optimal pre-treatment and post-treatment process parameters for enhancing the microhardness, wear resistance, and corrosion resistance of the magnesium alloy surface.
The pre-treatment process includes pickling, surface adjustment, activation, and a two-step chemical pre-deposition (the first step is alkaline, and the second step is acidic) to obtain a chemically pre-deposited Ni-P coating with a uniform surface and good corrosion resistance, which provides a stable bonding surface for the subsequent electrodeposition of the Ni-ND-CNTs nanocomposite coating. An orthogonal experiment is conducted, with the self-corrosion current density of the chemically pre-deposited Ni-P coating as the core evaluation index. The optimal pre-treatment process parameters are determined as follows: pickling time of 40 s, surface adjustment time of 150 s, activation time of 90 s, pH of the first-step deposition solution of 9.40, and pH of the second-step deposition solution of 6.20. The chemically pre-deposited Ni-P coating prepared under these process conditions has a uniform and smooth surface. Its microhardness is 824.2HV, which is 11.9 times higher than that of the magnesium alloy substrate. Its self-corrosion current density is 6.643×10‒8 A/cm², which is three orders of magnitude lower than that of the magnesium alloy substrate. A single-factor experiment is adopted for the optimization of post-treatment process. With the microhardness, friction coefficient, self-corrosion current density, and adhesion strength of the Ni-ND-CNTs nanocomposite coating as evaluation indexes, the optimal annealing process parameters are confirmed: heating temperature of 400 ℃ and holding time of 60 min. Under these process conditions, the performance of the Ni-ND-CNTs nanocomposite coating is improved significantly. Its microhardness reaches 1 335.2HV, which is about 40% higher than that before annealing. The friction coefficient decreases from 0.34 to 0.24, a 29% reduction compared with that before annealing. The self-corrosion current density decreases significantly to 7.540×10‒8 A/cm2, which is one order of magnitude lower than that before annealing. Under the optimal pre-treatment and post-treatment process conditions, the microhardness of the Ni-ND-CNTs nanocomposite coating is 19 times higher than that of the magnesium alloy substrate, and its self-corrosion current density is four orders of magnitude lower than that of the magnesium alloy substrate.
This study clarifies the priority of pre-treatment process parameters on the corrosion resistance of the chemically pre-deposited Ni-P coating on magnesium alloy surface: pickling time > activation time > pH of alkaline deposition solution > surface adjustment time > pH of acidic deposition solution. The heating temperature and holding time of post-treatment annealing significantly affect the microhardness and friction-wear performance of the electrodeposited nanocomposite coating, but have little impact on its corrosion resistance. Through the synergistic optimization of pre-treatment chemical pre-deposition and post-treatment annealing processes, the synergistic improvement of hardness, wear resistance, and corrosion resistance of the electrodeposited nanocomposite coating on magnesium alloy surface is realized. This solves the problems of poor corrosion resistance and low wear resistance of magnesium alloy, and provides basic data and technical support for the development of magnesium alloy surface treatment technology.

Key words

AZ91D magnesium alloy / nanocomposite electrodeposited layer / pretreatment / post-treatment annealing / comprehensive performance

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LI Zhi, HOU Jin, LIU Chongyu, LIU Guangke, WANG Zhen. Pretreatment and Post-deposition Annealing for Nanocomposite Electrodeposition on AZ91D Magnesium Alloy[J]. Surface Technology. 2026, 55(7): 157-168

References

[1] YANG J R, ZHU Z Q, HAN S J, et al.Evolution, Limitations, Advantages, and Future Challenges of Magnesium Alloys as Materials for Aerospace Applications[J]. Journal of Alloys and Compounds, 2024, 1008: 176707.
[2] HE Q, ZHANG D, HUANG Y L, et al.Recent Progress of Corrosion Prevention Method of Magnesium Alloy[J]. Steel Research International, 2025, 96(2): 2400376.
[3] ALIAS J, ALANG N A, AHMAD A H, et al.Emerging Progress of Chemical-Based Coating for the Corrosion Protection of Magnesium Alloys: A Review[J]. Journal of Adhesion Science and Technology, 2024, 38(8): 1125-1160.
[4] ZHANG L Y, GAO K, LIANG C A, et al.Trends and Advances in the Development of Nanodiamond-Graphene Core-Shell Materials in Heterogeneous Catalysis[J]. Journal of Energy Chemistry, 2025, 106: 398-426.
[5] SALEH M, GUL A, NASIR A, et al.Comprehensive Review of Carbon-Based Nanostructures: Properties, Synthesis, Characterization, and Cross-Disciplinary Applications[J]. Journal of Industrial and Engineering Chemistry, 2025, 146: 176-212.
[6] LIU Y N, YANG P, LI Y X, et al.Effect of Sodium Dodecyl Sulfate (SDS) on the Co-Deposition and Frictional Behavior of Carbon Nanotube/Nickel Composite Layer[J]. Materials Research Express, 2024, 11(4): 046508.
[7] SINGH C, TIWARI S K, SINGH R.Exploring Environment Friendly Nickel Electrodeposition on AZ91 Magnesium Alloy: Effect of Prior Surface Treatments and Temperature of the Bath on Corrosion Behaviour[J]. Corrosion Science, 2019, 151: 1-19.
[8] ZHANG Q Y.Effect of Zinc Phosphating Pretreatment on NiP Electroless Coating on AZ31B Magnesium Alloy Surface[J]. International Journal of Electrochemical Science, 2022, 17(6): 220664.
[9] GHAVIDEL N, ALLAHKARAM S R, NADERI R, et al.Corrosion and Wear Behavior of an Electroless Ni-P/Nano-SiC Coating on AZ31 Mg Alloy Obtained through Environmentally-Friendly Conversion Coating[J]. Surface and Coatings Technology, 2020, 382: 125156.
[10] YUAN J, LI P, YUAN R, et al.Influence of Pickling Time on Electroless Ni-P Coating on Magnesium Alloy[J]. Materials and Corrosion, 2021, 72(4): 642-651.
[11] SEIFZADEH D, RAJABALIZADEH Z, DIKICI B, et al.A Review of Pretreatment Techniques for Electroless Nickel-Phosphorus Plating on Magnesium Alloys with Enhanced Corrosion Resistance and Mechanical Properties[J]. Materials Today Communications, 2025, 44: 112171.
[12] XIE Z H, ZHUO Z, SHU Y, et al.Polysiloxane-Modified Porous Magnesium Hydroxide Pretreatment Film for Electroless Plating of Highly Corrosion-Resistant and Strongly Adhered Ni-P Coating on Magnesium Alloy[J]. Journal of Alloys and Compounds, 2024, 1008: 176680.
[13] KUMAR S, BANERJEE T, PATEL D. Structural, Mechanical, Tribological and Corrosion Characteristics of Dual Layer Ni-P/Sr-P Coating on AZ91D Mg Alloy through Environmentally-Friendly Chemical Conversion and Electroless Routes[J]. Surface and Coatings Technology, 2024, 485: 130922.
[14] YUAN J, LI P, YUAN R, et al.Fabrication and Corrosion Resistance of a Superhydrophobic Ni-P/Ni3(NO3)2(OH)4 Multilayer Protective Coating on Magnesium Alloy[J]. ACS Omega, 2020, 5(38): 24247-24255.
[15] XIE Z H, TENG Y H, HUANG Z F, et al.Corrosion- Resistant and Superhydrophobic Nickel-Based Composite Coating on Magnesium Alloy[J]. Surface and Coatings Technology, 2025, 496: 131638.
[16] LIU J P, SUN W C, LIU E Y, et al.Microstructure, Friction and Wear Behavior and Corrosion Resistance of Electroless Double-Layer Ni-P/Ni-Mo-P Coatings on AZ91D Magnesium Alloy[J]. Materials Research, 2024, 27: e20230379.
[17] XU Y K, LI W T, LIANG B J, et al.Enhancement of Wear and Corrosion Resistance of Pulsed Electrodeposited Ni-Mo Amorphous/Nanocrystalline Coatings by Heat Treatment[J]. Vacuum, 2024, 229: 113549.
[18] YANG J H, JI P F, YANG X M, et al.Relationship between Texture, Hydrogen Content, Residual Stress and Corrosion Resistance of Electrodeposited Chromium Coating: Influence of Heat Treatment[J]. Materials, 2024, 17(16): 4142.
[19] BISWAS P, DAS S K, SAHOO P.Tribological and Corrosion Performance of Duplex Electrodeposited Ni-P/Ni-W-P Coatings[J]. Physica Scripta, 2024, 99(11): 115018.
[20] BENATMANE A, DHIFLAOUI H, EWALD M, et al.Heat Treatment Effects on the Microstructural and Mechanical Properties of Electrodeposited Cu-Ni Coatings[J]. Journal of Materials Engineering and Performance, 2025, 34(16): 18260-18276.
[21] PETRIČEVIĆ A, KRSTAJIĆ PAJIĆ M N, ZABINSKI P, et al. Hydrogen Evolution Reaction on Electrodeposited Ni-MoOx Composite Coatings[J]. Electrochimica Acta, 2025, 519: 145825.
[22] CHAKAROVA V, MONEV M.Electrocatalytic Properties of Electroless Ni-P Coatings towards Hydrogen Evolution Reaction in Alkaline Solution: Ni-P Coatings Deposited on Steel Substrate at Different Concentrations of Sodium Hypophosphite[J]. Electrocatalysis, 2023, 14(2): 259-266.
[23] LI Y X, YANG P, XIAO Y, et al.Effect of Carbon Nanotube Content and Annealing Temperature on Corrosion Performance of Carbon Nanotube/Ni Composite Layer[J]. Materials Research Express, 2024, 11(4): 046503.
[24] BELTOWSKA-LEHMAN E, BIGOS A, SZCZERBA M J, et al.Heat Treatment of Ultrasonic Electrodeposited Ni-W/ZrO2 Nanocomposites[J]. Surface and Coatings Technology, 2020, 393: 125779.
[25] RAJA G, ELUMALAI A, UMA P, et al.Synthesis of Novel Bi2O3/ZnO Nanocomposite by Hydrothermal Method: A Sustainable Solution for Photocatalytic Malachite Green and Acid Blue 113 Dye Degradation[J]. Chemistry Africa, 2025, 8(10): 5823-5837.
[26] CUI G J, LIU Y P, LI S, et al.Nano-TiO2 Reinforced CoCr Matrix Wear Resistant Composites and High- Temperature Tribological Behaviors under Unlubricated Condition[J]. Scientific Reports, 2020, 10: 6816.
[27] KUMAR R, KUMAR R M, LAHIRI D, et al.Measurement of Bonding Strength of Thermally Reduced Graphene Oxide with Soda Lime Glass Using Nanoscratch Technique[J]. Materials Today: Proceedings, 2018, 5(8): 16338-16345.
[28] YANG P, WANG N, ZHANG J, et al.Investigation of the Microstructure and Tribological Properties of CNTS/Ni Composites Prepared by Electrodeposition[J]. Materials Research Express, 2022, 9(3): 036404.
[29] XIA F F, YAN P, MA C Y, et al.Effect of Different Heat-Treated Temperatures Upon Structural and Abrasive Performance of Ni-TiN Composite Nanocoatings[J]. Journal of Materials Research and Technology, 2023, 27: 2874-2881.

Funding

Liaoning Provincial Department of Education 'Challenge and Lead' Local Service Project (JYTMS20230371); Dalian University National College Student Innovation and Entrepreneurship Training Program Project (202511258013)
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