AZ91D镁基体上冷喷涂Al及Al-Mg_(17)Al_(12)复合涂层的研究
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摘要
镁及镁合金是目前已经得到应用的密度最小的金属结构材料，在航空航天、交通运输、电子通讯和国防军工等领域已有多年的应用。但是镁的化学性质非常活泼，不仅能和很多气体发生反应，而且和其它工程用金属材料相比具有较低的电极电位，同时使用时将首先被腐蚀。提高镁合金表面耐腐蚀性能的方法很多，其中使用涂层把镁合金和外部介质隔绝开来无疑是比较经济，也是比较容易实现的方法。
考虑到镁合金的特殊性质，本文选用Al作为涂层的主要材料，有以下两个原因，首先，Al表面暴露在空气中能够形成致密的氧化物薄膜，可以有效阻止Al的进一步腐蚀，具有自修复功能；另外，在经常用到的金属材料中，Al和Mg的电极电位相差较小，它们之间一般不会形成严重的电偶腐蚀或者点蚀。在镁基体上制备Al涂层的方法很多，如电镀和化学镀、等离子喷涂、激光熔覆、热喷涂、气相沉积等等，但这些传统的制备方法都存在一些弊端，如耗能太高、沉积效率太低、或者制备过程存在严重污染等。同时值得注意的是Al化学性质比较活泼，采用高温热源(如热喷涂和激光熔覆等)容易导致Al粒子的氧化或者其内部晶粒的长大，从而恶化涂层的整体性能。在这种情况下，使用冷喷涂技术沉积Al涂层，制备的涂层不仅可以保留原材料粉末粒子的显微形貌，而且能够有效减少甚至避免由于高温而导致的各种缺陷。
本文在AZ91D镁合金基体上采用冷喷涂技术沉积了纯Al涂层、Al复合涂层和Al梯度涂层，并且以此为研究对象考察了热处理对纯Al涂层/Mg基体界面扩散形成的金属间化合物的影响，以及强化相粉末粒子在原材料粉末中的含量对复合涂层性能的影响等等，重点探讨了涂层组织和性能之间的关系。本文综合运用了多种材料研究方法，包括光学金相分析、X射线衍射分析、ICP成分分析、扫描和透射电子显微分析、显微硬度分析、涂层孔隙率和结合强度分析等等，系统地开展了原材料粉末制备、喷涂过程使用参数、涂层后续热处理等对涂层力学性能和耐腐蚀性能的影响，旨在为提高镁合金表面耐蚀性提供一种新的思路和必要的实验依据。
由于使用的纯Al粉末粒子的平均粒子直径较大(58.5μm)，并且具有较宽的粒径分布。为了提高涂层的整体性能，根据得到涂层的厚度和孔隙率含量为依据，对涂层制备工艺中的主要参数进行了优化，表明在使用He作为工作气体和载气，同时使用耐高温塑料喷枪的情况下，工作气体的温度为300°C，压力为0.98MPa，喷枪出口到基体表面的距离为10mm，其相对移动速度为2mm/s时，通过1个道次的沉积，即可在镁基体上沉积得到约400μm的涂层，并且其孔隙率含量低于0.5vol.%。对涂层进行的后续热处理表明，由于镁基体与铝涂层之间的原子互扩散导致在界面附近生成了两种金属间化合物，使得涂层与基体的结合方式由物理的机械咬合转变为冶金结合。但是扩散生成的金属间化合物硬度很高，塑性很差，在剪切应力的作用下，很容易发生脆性断裂，反而恶化了涂层的结合强度。虽然得到的Al涂层比较致密，具有较好的耐腐蚀性能，但是涂层内部的结合强度较低。
为了提高纯Al涂层的结合强度，在原材料纯Al粉末中加入了球形金属间化合物粉末Mg_(17)Al_(12)，并使用不锈钢喷枪对混合粉末进行了沉积，得到了Al基复合涂层，同时研究了原材料粉末中不同含量(50vol.%和75vol.%)的Mg_(17)Al_(12)对涂层性能的影响。结果表明，强化相粉末的加入不仅能够显著提高金属Al粉末的沉积效率，有效改善涂层与基体的结合强度，而且不会恶化涂层的耐腐蚀能力。涂层比较致密，同时在基体上没有发现Mg_(17)Al_(12)粒子，结合其它研究结果，可以看出球形强化相粒子的作用为去除基体和粒子表面的氧化物和污染物、提高基体表面的粗糙度以增大涂层与基体的接触面积、改善金属Al粉末的沉积效率、夯实已经发生粘接的粉末粒子以及清洗不锈钢喷枪内壁。
用冷喷涂逐层沉积的方法在镁基体表面沉积了两种Al-Mg_(17)Al_(12)梯度涂层，并观察了涂层的显微形貌，结果显示涂层和基体在界面处结合较好，没有明显的缺陷；成分不同的层与层之间的界面也无法分辨，表明梯度涂层整体具有较好的结合强度，没有出现明显的分层现象。其主要原因是Mg_(17)Al_(12)粒子在涂层中的含量很低。涂层的显微组织也从侧面反映出使用冷喷涂技术逐层沉积制备梯度材料的可行性。
Magnesium (Mg) and its alloys are considered as the lowest densitystructural metallic materials in the world. They have been used in aerospace,transportation, electronic communication devices, home appliances andmilitary components for many years. However, as everyone knows, Mg is akind of material with very active chemical properties. It can react with manykinds of gases, elements, solutions and compounds, even at room temperature.Compared to other industrial metallic materials, Mg alloys usually have arelative lower electrode potential which means they will be preferentiallyattacked in the corrosion medium and acted as a sacrificial anode. A fewmethods have been reported could be employed to improve the surfaceproperties for Mg alloys, but using a coating to protect Mg and its alloys isundoubtedly a simple and economic solution.
Considering the poor corrosion resistance of Mg, aluminum (Al) wasused as the principle component in the coating. Two reasons can be used toillustrate why Al was selected in this study. The first is that when exposed inthe air, Al can react with oxygen and generate a dense oxide film which willprevent the further oxidation, and then has a self-repair function. The secondis that no remarkable electrode potential difference was found between Al andMg, therefore, galvanic corrosion or pitting will not supposed to take placebetween these two metals. Various of techniques, such as electroplating,chemical plating, plasma spraying, laser cladding, thermal spray and vapordeposition, have been used for depositing Al on Mg for improving the surface properties. But these traditional coating fabrication methods usually havesome disadvantages, such as high power consumption, low depositionefficiency or environment unfriendliness. It is worthy to note that Al powderis also very active, so the deposition process (like thermal spray or lasercladding) which has high temperature heat resource should be avoid, becausethey will lead to the formation of oxide on the Al surface or the grain growth,which will undermine the comprehensive performances of the coating. Underthese circumstances, cold spray technique was employed to deposite coatingsin this study. The coatings produced using cold spray not only can retain theinitial microstructure of the feedstock, but also decrease or eliminate thedefects which attributed to the high processing temperature.
Pure Al coatings, Al composite coatings and Al gradient coatings weredeposited on AZ91D magnesium substrate using cold spray. The effects of thepost heat treatment on the properties of the diffusion-induced intermetallicswhich formed at the coating/substrate interface were investigated. Theinfluences of the volume fraction of the reinforcement particles in thefeedstock on the performances of the composite coatings and the relationshipbetween the coating microstructure and properties were also discussed.Several modern material testing methods were employed in this study,including optical microscopy, X-ray diffraction, ICP chemical compositionanalysis, scanning electro microscopy, transmission electro microscopy,microhardness test, porosity content and bonding strength test of the coating,et. al. The effects of the feedstock preparation, spraying parameters and postheat treatments on the mechanical performances and anticorrosionperformances of the coatings were systematically investigated and discussed,for the purpose of providing a new solution and some useful experimentalresults for improving the anticorrosion properties of Mg surface.
The pure Al powders used as feedstock have an average particle size of58.5μm and present a broad size distribution with a diameter ranging from6to170μm. For improving the comprehensive performances of the as-sprayedcoatings, the main parameters in the cold spray process were optimized according to the thickness and porosity content of the corresponding coatings.The results show that pure Al coatings can be deposited on Mg substratessuccessfully by a single pass with a thickness of approximately400μm and aporosity level less than0.5vol.%. Noted that helium was used as bothpropellent and powder carrier gas, thermoplastic nozzle was used as sprayinggun with a gas temperature and pressure of300°C and0.98MPa, respectively.The standoff distance was kept at10mm and the relative traverse velocitybetween the nozzle and the substrate was kept at2mm/s. Heat treated thecoated samples will result in the formation of two intermetallics near theinterface, and then the coating bonding mechanism will turn intometallurgical bonding, instead of physical mechanical bonding. Thediffusion-induced intermetallics have similar characteristics to ceramicswhich present a higher hardness and relative lower plasticity. They will beeasily cracked under shear load and then undermine the coating bondingstrength. The as-sprayed Al coatings which produced using these optimizedparameters have similar anticorrosion properties to the bulk Al, but they havean inferior cohesion strength.
In order to improve the bonding strength of the as-sprayed Al coatings,spherical Mg_(17)Al_(12)powders were used as reinforcement particles in the Alfeedstock. Al-Mg_(17)Al_(12)composite coatings were attained using a stainlesssteel nozzle and a powder mixture. The effects of the powder mixturecompositions on the coating performances were investigated. The resultsshow that with an addition of Mg_(17)Al_(12)particles into the original Al powders,the deposition efficiency of the Al particles was significantly increased andthe adhesion strength between the substrate and the coating was alsoimproved, without any remarkable degradation of the anticorrosion properties.The composite coatings are very dense and no reinforcement particles werefound at the interface. Compared to the results proposed by other researchers,it can be concluded that the main functions of the spherical reinforcementparticles are to remove the surface oxidations and contaminations of thesubstrate and particle, increase the substrate roughness and then increase the contact area, improve the deposition efficiency of the Al powders, tamp thepre-deposited coatings and clean the inner surface of the stainless steel nozzle.
Two Al-Mg_(17)Al_(12)gradient coatings were deposited layer-by-layer on Mgsubstrates using cold spray. By carefully examination of the coatingmicrostructure, it was found that the gradient coatings have a good bondingwith the substrate and no defects were found at the interface. Moreover, theinterface between different layers was undetectable and no delaminationswere took place which was attributed to the lower Mg_(17)Al_(12)content in thecoating as well as Al was the dominant ingredient. It implied that the gradientcoatings have an improved bonding strength. All the results demonstrated thatcold spray can be used as an alternative method for fabricating gradientcoatings.
考虑到镁合金的特殊性质，本文选用Al作为涂层的主要材料，有以下两个原因，首先，Al表面暴露在空气中能够形成致密的氧化物薄膜，可以有效阻止Al的进一步腐蚀，具有自修复功能；另外，在经常用到的金属材料中，Al和Mg的电极电位相差较小，它们之间一般不会形成严重的电偶腐蚀或者点蚀。在镁基体上制备Al涂层的方法很多，如电镀和化学镀、等离子喷涂、激光熔覆、热喷涂、气相沉积等等，但这些传统的制备方法都存在一些弊端，如耗能太高、沉积效率太低、或者制备过程存在严重污染等。同时值得注意的是Al化学性质比较活泼，采用高温热源(如热喷涂和激光熔覆等)容易导致Al粒子的氧化或者其内部晶粒的长大，从而恶化涂层的整体性能。在这种情况下，使用冷喷涂技术沉积Al涂层，制备的涂层不仅可以保留原材料粉末粒子的显微形貌，而且能够有效减少甚至避免由于高温而导致的各种缺陷。
本文在AZ91D镁合金基体上采用冷喷涂技术沉积了纯Al涂层、Al复合涂层和Al梯度涂层，并且以此为研究对象考察了热处理对纯Al涂层/Mg基体界面扩散形成的金属间化合物的影响，以及强化相粉末粒子在原材料粉末中的含量对复合涂层性能的影响等等，重点探讨了涂层组织和性能之间的关系。本文综合运用了多种材料研究方法，包括光学金相分析、X射线衍射分析、ICP成分分析、扫描和透射电子显微分析、显微硬度分析、涂层孔隙率和结合强度分析等等，系统地开展了原材料粉末制备、喷涂过程使用参数、涂层后续热处理等对涂层力学性能和耐腐蚀性能的影响，旨在为提高镁合金表面耐蚀性提供一种新的思路和必要的实验依据。
由于使用的纯Al粉末粒子的平均粒子直径较大(58.5μm)，并且具有较宽的粒径分布。为了提高涂层的整体性能，根据得到涂层的厚度和孔隙率含量为依据，对涂层制备工艺中的主要参数进行了优化，表明在使用He作为工作气体和载气，同时使用耐高温塑料喷枪的情况下，工作气体的温度为300°C，压力为0.98MPa，喷枪出口到基体表面的距离为10mm，其相对移动速度为2mm/s时，通过1个道次的沉积，即可在镁基体上沉积得到约400μm的涂层，并且其孔隙率含量低于0.5vol.%。对涂层进行的后续热处理表明，由于镁基体与铝涂层之间的原子互扩散导致在界面附近生成了两种金属间化合物，使得涂层与基体的结合方式由物理的机械咬合转变为冶金结合。但是扩散生成的金属间化合物硬度很高，塑性很差，在剪切应力的作用下，很容易发生脆性断裂，反而恶化了涂层的结合强度。虽然得到的Al涂层比较致密，具有较好的耐腐蚀性能，但是涂层内部的结合强度较低。
为了提高纯Al涂层的结合强度，在原材料纯Al粉末中加入了球形金属间化合物粉末Mg_(17)Al_(12)，并使用不锈钢喷枪对混合粉末进行了沉积，得到了Al基复合涂层，同时研究了原材料粉末中不同含量(50vol.%和75vol.%)的Mg_(17)Al_(12)对涂层性能的影响。结果表明，强化相粉末的加入不仅能够显著提高金属Al粉末的沉积效率，有效改善涂层与基体的结合强度，而且不会恶化涂层的耐腐蚀能力。涂层比较致密，同时在基体上没有发现Mg_(17)Al_(12)粒子，结合其它研究结果，可以看出球形强化相粒子的作用为去除基体和粒子表面的氧化物和污染物、提高基体表面的粗糙度以增大涂层与基体的接触面积、改善金属Al粉末的沉积效率、夯实已经发生粘接的粉末粒子以及清洗不锈钢喷枪内壁。
用冷喷涂逐层沉积的方法在镁基体表面沉积了两种Al-Mg_(17)Al_(12)梯度涂层，并观察了涂层的显微形貌，结果显示涂层和基体在界面处结合较好，没有明显的缺陷；成分不同的层与层之间的界面也无法分辨，表明梯度涂层整体具有较好的结合强度，没有出现明显的分层现象。其主要原因是Mg_(17)Al_(12)粒子在涂层中的含量很低。涂层的显微组织也从侧面反映出使用冷喷涂技术逐层沉积制备梯度材料的可行性。
Magnesium (Mg) and its alloys are considered as the lowest densitystructural metallic materials in the world. They have been used in aerospace,transportation, electronic communication devices, home appliances andmilitary components for many years. However, as everyone knows, Mg is akind of material with very active chemical properties. It can react with manykinds of gases, elements, solutions and compounds, even at room temperature.Compared to other industrial metallic materials, Mg alloys usually have arelative lower electrode potential which means they will be preferentiallyattacked in the corrosion medium and acted as a sacrificial anode. A fewmethods have been reported could be employed to improve the surfaceproperties for Mg alloys, but using a coating to protect Mg and its alloys isundoubtedly a simple and economic solution.
Considering the poor corrosion resistance of Mg, aluminum (Al) wasused as the principle component in the coating. Two reasons can be used toillustrate why Al was selected in this study. The first is that when exposed inthe air, Al can react with oxygen and generate a dense oxide film which willprevent the further oxidation, and then has a self-repair function. The secondis that no remarkable electrode potential difference was found between Al andMg, therefore, galvanic corrosion or pitting will not supposed to take placebetween these two metals. Various of techniques, such as electroplating,chemical plating, plasma spraying, laser cladding, thermal spray and vapordeposition, have been used for depositing Al on Mg for improving the surface properties. But these traditional coating fabrication methods usually havesome disadvantages, such as high power consumption, low depositionefficiency or environment unfriendliness. It is worthy to note that Al powderis also very active, so the deposition process (like thermal spray or lasercladding) which has high temperature heat resource should be avoid, becausethey will lead to the formation of oxide on the Al surface or the grain growth,which will undermine the comprehensive performances of the coating. Underthese circumstances, cold spray technique was employed to deposite coatingsin this study. The coatings produced using cold spray not only can retain theinitial microstructure of the feedstock, but also decrease or eliminate thedefects which attributed to the high processing temperature.
Pure Al coatings, Al composite coatings and Al gradient coatings weredeposited on AZ91D magnesium substrate using cold spray. The effects of thepost heat treatment on the properties of the diffusion-induced intermetallicswhich formed at the coating/substrate interface were investigated. Theinfluences of the volume fraction of the reinforcement particles in thefeedstock on the performances of the composite coatings and the relationshipbetween the coating microstructure and properties were also discussed.Several modern material testing methods were employed in this study,including optical microscopy, X-ray diffraction, ICP chemical compositionanalysis, scanning electro microscopy, transmission electro microscopy,microhardness test, porosity content and bonding strength test of the coating,et. al. The effects of the feedstock preparation, spraying parameters and postheat treatments on the mechanical performances and anticorrosionperformances of the coatings were systematically investigated and discussed,for the purpose of providing a new solution and some useful experimentalresults for improving the anticorrosion properties of Mg surface.
The pure Al powders used as feedstock have an average particle size of58.5μm and present a broad size distribution with a diameter ranging from6to170μm. For improving the comprehensive performances of the as-sprayedcoatings, the main parameters in the cold spray process were optimized according to the thickness and porosity content of the corresponding coatings.The results show that pure Al coatings can be deposited on Mg substratessuccessfully by a single pass with a thickness of approximately400μm and aporosity level less than0.5vol.%. Noted that helium was used as bothpropellent and powder carrier gas, thermoplastic nozzle was used as sprayinggun with a gas temperature and pressure of300°C and0.98MPa, respectively.The standoff distance was kept at10mm and the relative traverse velocitybetween the nozzle and the substrate was kept at2mm/s. Heat treated thecoated samples will result in the formation of two intermetallics near theinterface, and then the coating bonding mechanism will turn intometallurgical bonding, instead of physical mechanical bonding. Thediffusion-induced intermetallics have similar characteristics to ceramicswhich present a higher hardness and relative lower plasticity. They will beeasily cracked under shear load and then undermine the coating bondingstrength. The as-sprayed Al coatings which produced using these optimizedparameters have similar anticorrosion properties to the bulk Al, but they havean inferior cohesion strength.
In order to improve the bonding strength of the as-sprayed Al coatings,spherical Mg_(17)Al_(12)powders were used as reinforcement particles in the Alfeedstock. Al-Mg_(17)Al_(12)composite coatings were attained using a stainlesssteel nozzle and a powder mixture. The effects of the powder mixturecompositions on the coating performances were investigated. The resultsshow that with an addition of Mg_(17)Al_(12)particles into the original Al powders,the deposition efficiency of the Al particles was significantly increased andthe adhesion strength between the substrate and the coating was alsoimproved, without any remarkable degradation of the anticorrosion properties.The composite coatings are very dense and no reinforcement particles werefound at the interface. Compared to the results proposed by other researchers,it can be concluded that the main functions of the spherical reinforcementparticles are to remove the surface oxidations and contaminations of thesubstrate and particle, increase the substrate roughness and then increase the contact area, improve the deposition efficiency of the Al powders, tamp thepre-deposited coatings and clean the inner surface of the stainless steel nozzle.
Two Al-Mg_(17)Al_(12)gradient coatings were deposited layer-by-layer on Mgsubstrates using cold spray. By carefully examination of the coatingmicrostructure, it was found that the gradient coatings have a good bondingwith the substrate and no defects were found at the interface. Moreover, theinterface between different layers was undetectable and no delaminationswere took place which was attributed to the lower Mg_(17)Al_(12)content in thecoating as well as Al was the dominant ingredient. It implied that the gradientcoatings have an improved bonding strength. All the results demonstrated thatcold spray can be used as an alternative method for fabricating gradientcoatings.
引文
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