AZ91D镁合金表面磁控溅射Al、Ti-Al-N、Al/Ti-Al-N膜及其组织与性能研究
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摘要
镁合金是目前实际应用中最轻的金属结构材料,具有密度小,比强度、比刚度高,另外还具有优良的减震性以及电磁屏蔽能力,因此被广泛应用于汽车工业、航空航天以及电子产品等诸多领域。但由于镁合金耐腐蚀性较差,其应用受到了阻碍。目前主要应用于镁合金防腐蚀的表面处理方法有:化学转化、阳极氧化、化学镀、气相沉积等。磁控溅射技术具有沉积速率较其他气相沉积方法高、工艺简单、薄膜质量好、对环境友好等优点,成为薄膜工业化应用的重要方法之一。
本文采用磁控溅射镀膜方法,在AZ91D镁合金表面按照预定实验方案分别制备了Al、Ti-Al-N单层膜,并且在制备Al、Ti-Al-N单层膜实验的基础上,选择较优参数制备Al/Ti-Al-N双层膜。本论文主要研究了基材温度、负偏压以及N2/Ar分压比等磁控溅射实验参数对膜层组织和性能的影响。
研究结果表明:制备Al单层膜时,基材温度和负偏压对Al膜组织和性能有很大影响,基材温度为150℃时,晶粒细小且大小均匀,膜层致密度最好,膜层自腐蚀电流最小,自腐蚀电位较高,负偏压为-60V时,膜层致密度高,且自腐蚀电流最小;制备Ti-Al-N单层膜时,N2/Ar分压比和负偏压对Ti-Al-N膜层组织和性能有很大影响,N2/Ar分压比为1.5:10时,膜层显微硬度、憎水性较高,并具有较高的电化学阻抗,拥有较好的腐蚀防护性能,负偏压为-20V时,膜层具有较高的显微硬度、最高的憎水性以及最大的电化学阻抗,拥有最好的腐蚀防护性能。
最后利用制备Al、Ti-Al-N单层膜的最优参数,即在AZ91D镁合金基材温度为150℃,负偏压为-60V磁控溅射工艺参数下制备Al膜作为过渡层,过渡层制备完毕后保持Ar气流量10sccm不变,通入N2气流量为1.5sccm,AZ91D镁合金基材温度仍保持为150℃,负偏压为-20V在Al膜基础上沉积Ti-Al-N膜,制备得到Al/Ti-Al-N双层膜。比较了Ti-Al-N单层膜和Al/Ti-Al-N双层膜的组织与性能差异,对比分析了两种膜层的亲水性和电化学性能的不同,得出双层膜具有更好的腐蚀防护性能。
Magnesium alloy is the lightest metal structure material which is practical used, with excellent properties, such as low density, high specific strength and stiffness, good shock absorption ability, electromagnetic shielding ability, etc.. So, the magnesium alloy is widely used in the automotive industry, aerospace industry, microelectronics and many other fields. However, its poor corrosion resistance have hindered the wider use of magnesium alloy. At present, the surface treatment used for magnesium alloy are: chemical conversion, anodicoxidation treatment, chemical plating, vapor deposition and so on. Magnetron sputtering is one of the important methods for industrial application owing to its high deposition rate compared with other vapor deposition methods, simple process, good film quality and environmentally friendly.
In this thesis, the author deposited Al、Ti-Al-N monolayer films respectively on AZ91D magnesium alloy by magnetron sputtering. On the basis of Al、Ti-Al-N monolayer films preparation experiments, the author selected the optimum parameters to deposite Al/Ti-Al-N bilayer films. This thesis mainly studied the effects of magnetron sputtering parameters, such as substrate temperature, bias voltage and partial pressure ratio of N2/Ar, on the microstructure and properties of the films.
The results show that, substrate temperature and negative bias voltage had great influence on the microstructure and properties of Al monolayer films, while the substrate temperature was 150℃, the films with small but uniform grain size had high density, relatively high corrosion potential and lowest corrosion current; while the negative bias voltage was -60V, the films with high density had lowest corrosion current. Partial pressure ratio of N2/Ar and negative bias voltage had great influence on the microstructure and properties of Ti-Al-N monolayer films, while the partial pressure ratio of N2/Ar was 1.5:10, the films with high microhardness and hydrophobicity had high electrochemical impedance, and had better performance of anticorrosion; while the negative bias voltage was -20V, the films with relatively high microhardness and highest hydrophobicity had highest electrochemical impedance, and had best performance of anticorrosion
Last, the author deposited Al monolayer film as buffer layer first, and then deposited Ti-Al-N film using the optimum parameters by magnetron sputtering to prepare Al/Ti-Al-N bilayer film. The author studied the differences of microstructure and properties between Ti-Al-N monolayer films and Al/Ti-Al-N bilayer films, and got the result that the Al/Ti-Al-N bilayer films had more excellent anticorrosion ability by comparing the hydrophilicity and electrochemical property between this two kinds of films.
本文采用磁控溅射镀膜方法,在AZ91D镁合金表面按照预定实验方案分别制备了Al、Ti-Al-N单层膜,并且在制备Al、Ti-Al-N单层膜实验的基础上,选择较优参数制备Al/Ti-Al-N双层膜。本论文主要研究了基材温度、负偏压以及N2/Ar分压比等磁控溅射实验参数对膜层组织和性能的影响。
研究结果表明:制备Al单层膜时,基材温度和负偏压对Al膜组织和性能有很大影响,基材温度为150℃时,晶粒细小且大小均匀,膜层致密度最好,膜层自腐蚀电流最小,自腐蚀电位较高,负偏压为-60V时,膜层致密度高,且自腐蚀电流最小;制备Ti-Al-N单层膜时,N2/Ar分压比和负偏压对Ti-Al-N膜层组织和性能有很大影响,N2/Ar分压比为1.5:10时,膜层显微硬度、憎水性较高,并具有较高的电化学阻抗,拥有较好的腐蚀防护性能,负偏压为-20V时,膜层具有较高的显微硬度、最高的憎水性以及最大的电化学阻抗,拥有最好的腐蚀防护性能。
最后利用制备Al、Ti-Al-N单层膜的最优参数,即在AZ91D镁合金基材温度为150℃,负偏压为-60V磁控溅射工艺参数下制备Al膜作为过渡层,过渡层制备完毕后保持Ar气流量10sccm不变,通入N2气流量为1.5sccm,AZ91D镁合金基材温度仍保持为150℃,负偏压为-20V在Al膜基础上沉积Ti-Al-N膜,制备得到Al/Ti-Al-N双层膜。比较了Ti-Al-N单层膜和Al/Ti-Al-N双层膜的组织与性能差异,对比分析了两种膜层的亲水性和电化学性能的不同,得出双层膜具有更好的腐蚀防护性能。
Magnesium alloy is the lightest metal structure material which is practical used, with excellent properties, such as low density, high specific strength and stiffness, good shock absorption ability, electromagnetic shielding ability, etc.. So, the magnesium alloy is widely used in the automotive industry, aerospace industry, microelectronics and many other fields. However, its poor corrosion resistance have hindered the wider use of magnesium alloy. At present, the surface treatment used for magnesium alloy are: chemical conversion, anodicoxidation treatment, chemical plating, vapor deposition and so on. Magnetron sputtering is one of the important methods for industrial application owing to its high deposition rate compared with other vapor deposition methods, simple process, good film quality and environmentally friendly.
In this thesis, the author deposited Al、Ti-Al-N monolayer films respectively on AZ91D magnesium alloy by magnetron sputtering. On the basis of Al、Ti-Al-N monolayer films preparation experiments, the author selected the optimum parameters to deposite Al/Ti-Al-N bilayer films. This thesis mainly studied the effects of magnetron sputtering parameters, such as substrate temperature, bias voltage and partial pressure ratio of N2/Ar, on the microstructure and properties of the films.
The results show that, substrate temperature and negative bias voltage had great influence on the microstructure and properties of Al monolayer films, while the substrate temperature was 150℃, the films with small but uniform grain size had high density, relatively high corrosion potential and lowest corrosion current; while the negative bias voltage was -60V, the films with high density had lowest corrosion current. Partial pressure ratio of N2/Ar and negative bias voltage had great influence on the microstructure and properties of Ti-Al-N monolayer films, while the partial pressure ratio of N2/Ar was 1.5:10, the films with high microhardness and hydrophobicity had high electrochemical impedance, and had better performance of anticorrosion; while the negative bias voltage was -20V, the films with relatively high microhardness and highest hydrophobicity had highest electrochemical impedance, and had best performance of anticorrosion
Last, the author deposited Al monolayer film as buffer layer first, and then deposited Ti-Al-N film using the optimum parameters by magnetron sputtering to prepare Al/Ti-Al-N bilayer film. The author studied the differences of microstructure and properties between Ti-Al-N monolayer films and Al/Ti-Al-N bilayer films, and got the result that the Al/Ti-Al-N bilayer films had more excellent anticorrosion ability by comparing the hydrophilicity and electrochemical property between this two kinds of films.
引文
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