铝合金表面化学镀Ni-Mo-P镀层制备及性能研究
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摘要
本文采用酸性化学镀液在铝合金表面获得Ni-Mo-P合金镀层。利用X荧光光谱分析(XRF)、场发射扫描电镜(FESEM)、透射电镜(TEM)、X射线衍射分析(XRD)、能谱仪(EDS)和激光共聚焦显微镜(LSCM)、差示热扫描仪(DSC)等现代分析手段,探讨了Na_2MoO_4浓度和施镀温度对镀层中Mo含量、镀层形貌、沉积速度、显微硬度、结合力等性能的影响。研究了不同热处理温度对镀层的结构、结合力以及硬度的影响。
结果表明:以柠檬酸钠为络合剂的酸性化学镀镀液可很好的实现Ni、Mo、P的共沉积。XRF分析表明:在试验范围内,随着Na_2MoO_4浓度的增加,镀层中Mo含量增加,P含量降低,还原剂的消耗增加,镀层形成能力下降。最佳Na_2MoO_4浓度范围为0.5 g/L~0.6 g/L,温度为90℃。TEM分析证明:镀态镀层主要为非晶结构,随Na_2MoO_4浓度变化镀层中出现混晶态和纳米晶态两种微观结构。
此外研究表明:温度为90℃,Na_2MoO_4浓度为0.5 g/L左右时,镀层的沉积速率最大为9.5μm/h;镀层表面HV硬度最大为458.70;镀层结合力最高达30 N;表面粗糙度最小,Rz<3040。
化学镀机理研究表明:随着热处理温度的提高,Ni-Mo-P合金镀层大体上经历结构驰豫+晶态Ni的析出→Ni_3P相的析出→晶态Ni、Ni_3P的聚集长大等过程。热处理可使镀层的结合力有所增加。300℃保温1 h镀层的结合力达到最大,达到40 N以上;退火温度超过300℃后,镀层的结合力迅速下降;硬度随热处理温度升高而增加。400℃热处理后,Ni-Mo-P镀层横截面硬度为15.12 GPa,表面HV硬度为774.23。热处理温度超过400℃,Ni-Mo-P镀层镀层硬度开始下降。
In this thesis, Ni-Mo-P alloy coating was deposited by electreless plating using acidic plating solution on the substrate of aluminum alloy. The effects of bath temperature and concentration of Na_2MoO_4 on the composition, structure, properties, such as microhardness, deposition rate and adhesion of the Ni-Mo-P alloy deposits were studied by Thermal Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive Spectrometer (EDS), X-Ray Fluorescence (XRF), Transmission Electron Microscope (TEM), X-ray Diffractometer (XRD), Differential Scanning Calorimetry (DSC) and Laser Confocal Scanning Microscope (LCSM). The influence of heat treatment temperature on the structure, microhardness and adhesion of the Ni-Mo-P alloy deposits were also discussed.
The experimental results show that the Ni-Mo-P alloy coating could be obtained using the acidic plating solution in which the C6H5Na3O7·2H2O was used as the complex agent.XRF results indicate that the Mo contents and the deposition rate would be increased with the increase of MoO42- concentration, corresponding with the decrease of P contents in the bath solution. The key plating factors, bath temperature and the concentration of Na_2MoO_4 were around 90℃and in the range from 0.5 g/L to 0.6 g/L, respectively. It was found that the maximum deposition rate was 9.5μm/h, the maximum microhardness was 458.70 HV, the maximum adhesion was 30 N, the minimum surface roughness (Rz) was less than 3040 ? obtained at the bath temperature of 90℃, the Na_2MoO_4 concentration of 0.5 g/L.
TEM results demonstrate that amorphous structure was the main structure of Ni-Mo-P alloy coating. The microstructure of as plated coatings would be changed from amorphous to nanocrystalline and mix-crystalline structure with the change of the Na_2MoO_4 concentration.
After heat-treatment at differernt conditions, the structure of Ni-Mo-P alloy coating experience a series of transformations, such as structural relaxation, formation of Ni nanocrystal, bulk formation of Ni_3P nanoerystal, especially, the grain aggregation and growth of Ni and Ni_3P may be increased with the increase of heat treatment temperature. The adhesion strength of as-plated coating reaches its maximum value (40 N) after heat treatment at 300℃, 1 h. The microhardness determined at the conditions of 400℃and 1 h on the cross section and surface were about 15.12 GPa and 774.23 HV, respectively.
结果表明:以柠檬酸钠为络合剂的酸性化学镀镀液可很好的实现Ni、Mo、P的共沉积。XRF分析表明:在试验范围内,随着Na_2MoO_4浓度的增加,镀层中Mo含量增加,P含量降低,还原剂的消耗增加,镀层形成能力下降。最佳Na_2MoO_4浓度范围为0.5 g/L~0.6 g/L,温度为90℃。TEM分析证明:镀态镀层主要为非晶结构,随Na_2MoO_4浓度变化镀层中出现混晶态和纳米晶态两种微观结构。
此外研究表明:温度为90℃,Na_2MoO_4浓度为0.5 g/L左右时,镀层的沉积速率最大为9.5μm/h;镀层表面HV硬度最大为458.70;镀层结合力最高达30 N;表面粗糙度最小,Rz<3040。
化学镀机理研究表明:随着热处理温度的提高,Ni-Mo-P合金镀层大体上经历结构驰豫+晶态Ni的析出→Ni_3P相的析出→晶态Ni、Ni_3P的聚集长大等过程。热处理可使镀层的结合力有所增加。300℃保温1 h镀层的结合力达到最大,达到40 N以上;退火温度超过300℃后,镀层的结合力迅速下降;硬度随热处理温度升高而增加。400℃热处理后,Ni-Mo-P镀层横截面硬度为15.12 GPa,表面HV硬度为774.23。热处理温度超过400℃,Ni-Mo-P镀层镀层硬度开始下降。
In this thesis, Ni-Mo-P alloy coating was deposited by electreless plating using acidic plating solution on the substrate of aluminum alloy. The effects of bath temperature and concentration of Na_2MoO_4 on the composition, structure, properties, such as microhardness, deposition rate and adhesion of the Ni-Mo-P alloy deposits were studied by Thermal Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive Spectrometer (EDS), X-Ray Fluorescence (XRF), Transmission Electron Microscope (TEM), X-ray Diffractometer (XRD), Differential Scanning Calorimetry (DSC) and Laser Confocal Scanning Microscope (LCSM). The influence of heat treatment temperature on the structure, microhardness and adhesion of the Ni-Mo-P alloy deposits were also discussed.
The experimental results show that the Ni-Mo-P alloy coating could be obtained using the acidic plating solution in which the C6H5Na3O7·2H2O was used as the complex agent.XRF results indicate that the Mo contents and the deposition rate would be increased with the increase of MoO42- concentration, corresponding with the decrease of P contents in the bath solution. The key plating factors, bath temperature and the concentration of Na_2MoO_4 were around 90℃and in the range from 0.5 g/L to 0.6 g/L, respectively. It was found that the maximum deposition rate was 9.5μm/h, the maximum microhardness was 458.70 HV, the maximum adhesion was 30 N, the minimum surface roughness (Rz) was less than 3040 ? obtained at the bath temperature of 90℃, the Na_2MoO_4 concentration of 0.5 g/L.
TEM results demonstrate that amorphous structure was the main structure of Ni-Mo-P alloy coating. The microstructure of as plated coatings would be changed from amorphous to nanocrystalline and mix-crystalline structure with the change of the Na_2MoO_4 concentration.
After heat-treatment at differernt conditions, the structure of Ni-Mo-P alloy coating experience a series of transformations, such as structural relaxation, formation of Ni nanocrystal, bulk formation of Ni_3P nanoerystal, especially, the grain aggregation and growth of Ni and Ni_3P may be increased with the increase of heat treatment temperature. The adhesion strength of as-plated coating reaches its maximum value (40 N) after heat treatment at 300℃, 1 h. The microhardness determined at the conditions of 400℃and 1 h on the cross section and surface were about 15.12 GPa and 774.23 HV, respectively.
引文
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2 A.Wurtz, C. R. Seances. Acad. Sci. 1989, 12, 44(2): 702-705
3 H. Wang, S. Yao and S. Matsumura. Electrochemical pre-paration and characterization of Ni/SiC gradient deposit. Mater. Process. Technol. 2004, 9, 25(8): 299-311
4 B. A. Riddell, GE. Proc. Amer. Electropl, Soc. J. Res. NBS. 1947, (39): 385
5张敬尧. Ni-P基多元化学沉积及其镀层组织结构转变的研究.洛阳工学院. 2001: 50-60
6熊宽.铝合金表面Ni-Cu-P镀层的制备及其性能研究.西安电子科技大学. 2008: 3-9
7 G. Gutzeit, An outling of the chemistry involved in the process of catalytic nickel deposition from aqueous solution, plating. 1959(10): 1158-1164
8许姣姣,胡信国,余强.电化学沉积技术的新发展.南方金属. 2007, 02, 39(4): 33-38
9 M. Pavnovic, Electrochemical aspects of electroless deposition of metals, plating. 1968(12): 1161-1167
10 N. Feldstein. A new technique for investigating the electrochemical behavior of electroless plating bath and the mechanism of electroless nickel plating, J. Electrochem. Soc. 1971(118): 869-874
11白栓堂.化学镀镍合金及电子工业中的应用.电镀与环保. 1999, 19(5): 7-9
12郭慧林,司云森.低磷化学镀镍层性能的研究.电化学. 1996, 01, 35(4): 45-50
13赵文轸.材料表面工程导论.西安交通大学出版社. 1998: 2l-211
14 N. V. Mandich, G. A. Krulik. A novel biogenic nickel source for electroless nickel plating. Metal Finishing. 1992, 09, 12(3): 9-10
15贾韦,宣天鹏.化学镀镍在微电子领域的应用及发展前景.稀有金属快报. 2007, 03, 12(5): 11-14
16梅建庭,刘华. Ni-P-Sic化学复合镀层耐磨性与显微硬度的研究.电镀与涂饰.2004, 01, 33(5): 27-32
17高进.化学镀Ni-P合金在金属材料表面处理上的特殊应用.机械制造. 2000, 09, 24(1): 49-54
18夏传义.化学镀在电子工业中的应用.电镀与涂饰. 1999, 04, 31(4): 32-37
19黎永钧.化学镀镍合金在电子工业中的应用.电子工艺技术. 1998, 05, 14(2): 19-25
20贺英,桑文斌,王均安.化学镀工艺在微电子材料中的研究和应用.微纳电子技术. 2003, 05, 22(3): 49-54
21崔国峰,李宁,黎德育.化学镀镍和镍合金在微电子领域中的应用及展望.电镀与环保. 2003, 04, 21(6): 31-35
22俞世俊.化学镀镍磷及镍磷-碳化硅复合涂层的研究. 2003, 06: 26-31
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