Effect of graphene nanosheets on the properties of Ni-W-ZrO2 composite coating
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摘要: 为提高Ni-W-ZrO2复合镀层的显微硬度和耐蚀性，通过电沉积方法在7075铝合金上制备Ni-W-ZrO2-石墨烯纳米片(GNPs)复合镀层，利用GNPs来改善Ni-W-ZrO2复合镀层表面性能不足的问题。利用正交试验对实验工艺条件进行优选：电流密度为10 A/dm2，搅拌速度为250 r/min，温度为60℃。在优选工艺条件下，ZrO2纳米颗粒保持10 g/L，改变GNPs的含量(1、2、3、4 g/L)，寻求最佳GNPs添加量的Ni-W-10 g/L ZrO2-GNPs复合镀层。通过显微硬度计及旋转摩擦试验仪，研究显微硬度和耐磨性，通过SEM、EDS、XRD和AFM进行微观表征。通过电化学方法研究Ni-W-ZrO2-GNPs复合镀层在质量分数为3.5wt%NaCl溶液中的耐蚀性。结果表明：GNPs和ZrO2纳米颗粒均匀共沉积在镍钨镀层中，GNPs的掺入对Ni-W-ZrO2复合镀层微观形貌、晶粒大小、显微硬度、摩擦性能及耐蚀性均有显著影响，当GNPs添加量为3 g/L时，镍(钨)基体的晶粒尺寸最小，显微硬度(HV 942)最高，平均摩擦系数(0.1981)最小；当GNPs添加量为2 g/L时，Ni-W-ZrO2-GNPs复合镀层的耐蚀性(电荷转移电阻Rct：9532 Ω·cm2)相较Ni-W-ZrO2复合镀层的耐蚀性(Rct：1766 Ω·cm2)改善明显。Abstract: In order to improve the microhardness and corrosion resistance of Ni-W-ZrO2 composite coating, Ni-W-ZrO2-graphene nanosheets (GNPs) composite coating was prepared on 7075 aluminum alloy by electrodeposition method, and GNPs was used to improve the surface performance of Ni-W-ZrO2 composite coating. Orthogonal experiment was used to optimize the experimental process conditions: the current density was 10 A/dm2, the stirring speed was 250 r/min, and the temperature was 60℃. Under the optimal process conditions, ZrO2 nanoparticles maintain 10 g/L, change the content of GNPs (1, 2, 3, 4 g/L), and seek the best GNPs addition amount of Ni-W-10 g/L ZrO2-GNPs composite coating. The microhardness and abrasion resistance were studied by the microhardness tester and the rotating friction tester, and the microscopic characterization was carried out by SEM, EDS, XRD and AFM. The corrosion resistance of Ni-W-ZrO2-GNPs composite coating in 3.5wt%NaCl solution was studied by electrochemical method. The results show that GNPs and ZrO2 nanoparticles are uniformly co-deposited in the nickel-tungsten coating, and the incorporation of GNPs has a significant effect on the microscopic morphology, grain size, microhardness, friction performance and corrosion resistance of the Ni-W-ZrO2 composite coating. When the amount of GNPs added is 3 g/L, the grain size of the Ni (W) matrix is the smallest, the microhardness (HV 942) is the highest, and the average friction coefficient (0.1981) is the smallest. When the amount of GNPs is 2 g/L, the corrosion resistance of Ni-W-ZrO2-GNPs composite coating (Charge transfer resistance Rct: 9532 Ω·cm2) is significantly improved compared to Ni-W-ZrO2 composite coating (Rct: 1766 Ω·cm2).
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图 1 ZrO2纳米颗粒的TEM图像 (a) 和XRD图谱 (b)
Figure 1. TEM image and XRD pattern of ZrO2 nanoparticles
图 2 石墨烯纳米片(GNPs)的拉曼图谱
Figure 2. Raman spectra of graphene nanosheets (GNPs)
D—D band; G—G band
图 3 不同GNPs添加量下Ni-W-ZrO2-GNPs复合镀层的SEM图像
Figure 3. SEM images of Ni-W-ZrO2-GNPs composite coating with different GNPs addition amount
图 4 不同GNPs添加量下Ni-W-ZrO2-GNPs复合镀层的AFM图像
Figure 4. AFM images of Ni-W-ZrO2-GNPs composite coating with different GNPs addition amount
图 5 GNPs添加量对Ni-W-ZrO2-GNPs复合镀层中W、Zr、C含量的影响
Figure 5. Effect of GNPs addition on the contents of W, Zr and C in Ni-W-ZrO2-GNPs composite coating
图 6 Ni-W-10 g/L ZrO2-2 g/L GNPs复合镀层中Ni (a)、W (b)、C (c) 和Zr (d) 元素的EDS图谱
Figure 6. EDS spectras of Ni (a), W (b), C (c) and Zr (d) elements in Ni-W-10 g/L ZrO2-2 g/L GNPs composite coatings
图 7 不同GNPs添加量下Ni-W-ZrO2-GNPs复合镀层的截面微观形貌
Figure 7. Cross-sectional micro-morphologies of Ni-W-ZrO2-GNPs composite coatings with different GNPs additions
图 8 不同GNPs添加量下Ni-W-ZrO2-GNPs复合镀层的XRD图谱
Figure 8. XRD pattern of Ni-W-ZrO2-GNPs composite coatings with different GNPs additions
图 9 不同GNPs添加量对Ni-W-ZrO2-GNPs复合镀层晶粒尺寸的影响
Figure 9. Effect of different GNPs additions on grain size of Ni-W-ZrO2-GNPs composite coatings
图 10 不同GNPs添加量对Ni-W-ZrO2-GNPs复合镀层显微硬度及平均摩擦系数的影响
Figure 10. Effect of different GNPs addition on the microhardness and average friction coefficient of Ni-W-ZrO2-GNPs composite coating
图 11 干摩擦条件下Ni-W-ZrO2-GNPs复合镀层摩擦系数随时间的摩擦曲线
Figure 11. Friction curves of Ni-W-ZrO2-GNPs composite coatings with time under dry friction condition
图 12 不同GNPs添加量的Ni-W-ZrO2-GNPs复合镀层的阻抗谱 (a)和动电位极化曲线 (b)
Figure 12. Impedance spectrum (a) and potentio dynamic polarization curve (b) of Ni-W-ZrO2-GNPs composite coating with different GNPs addition amount
图 13 Ni-W-ZrO2-GNPs复合镀层等效电路模型
Figure 13. Equivalent electrical circuit model of Ni-W-ZrO2-GNPs composite coating
Rs—Solution resistance; CPE—Constant phase element; Rct—Electrochemical reaction charge transfer resistance
表 1 Ni-W-ZrO2-GNPs复合镀层正交试验结果
Table 1. Orthogonal experimental results of Ni-W-ZrO2-GNPs composite plating
Number Content of GNPs/
(g·L−1)Current density/
(A·dm−2)Temperature/
℃Stirring speed/
(r·min−1)Microhardness Average friction
coefficient1 0 6 40 150 659 0.5721 2 0 8 50 200 684 0.5437 3 0 10 60 250 710 0.4697 4 0 12 70 300 723 0.5042 5 1 6 50 250 734 0.3181 6 1 8 40 300 702 0.3469 7 1 10 70 150 746 0.2731 8 1 12 60 200 893 0.2661 9 2 6 60 300 801 0.2504 10 2 8 70 250 757 0.2573 11 2 10 40 200 785 0.2326 12 2 12 50 150 745 0.3006 13 3 6 70 200 768 0.2724 14 3 8 60 150 831 0.2520 15 3 10 50 300 821 0.2227 16 3 12 40 250 819 0.2533 
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表 2 Ni-W-ZrO2-GNPs复合镀层直接分析结果
Table 2. Direct analysis results of Ni-W-ZrO2-GNPs composite plating
Number Content of
GNPs/(g·L−1)Current density/
(A·dm−2)Temperature/
℃Stirring speed/
(r·min−1)Microhardness Average friction
coefficient1 3 12 60 200 876 0.2454 2 3 10 60 250 942 0.1981 3 3 10 50 300 821 0.2227
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表 3 Ni-W-ZrO2-GNPs复合镀层电化学阻抗数据
Table 3. Electrochemical impedance data of Ni-W-ZrO2-GNPs composite coating
Sample Rs/(Ω·cm2) Rct/(Ω·cm2) CPE-T/(Ω−1·cm−2·s−n) CPE-P/(Ω−1·cm−2·s−n) Ni-W-10 g/L ZrO2 8.254 1766 0.000104 0.81017 Ni-W-10 g/L ZrO2-1 g/L GNPs 7.411 3051 0.000136 0.82018 Ni-W-10 g/L ZrO2-2 g/L GNPs 8.877 9532 0.000042 0.92166 Ni-W-10 g/L ZrO2-3 g/L GNPs 7.672 7448 0.000068 0.85591 Ni-W-10 g/L ZrO2-4 g/L GNPs 9.783 2606 0.000111 0.83356 Note: CPE-T, CPE-P—Two parameters of CPE.
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