大面积铝合金局部放电微弧氧化及热阻隔膜层制备
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摘要
随着航空、航天事业的发展,轻量化设计已成为发展趋势。铝合金因具有较高的比强度,现已在航空航天领域得到了广泛应用。然而随着飞行速度提升而带来的严重气动加热问题,使得通常作为飞行器结构材料的铝合金已无法承受过高的热载荷,因此必须对其进行热防护处理。微弧氧化技术作为阀金属表面陶瓷膜原位生长技术,可以实现高结合强度、优良热稳定性的膜层制备,在热阻隔膜层制备方面具有广阔的前景。但因高电压、大电流以及能量效率低等方面的不足,使其无法实现对大尺寸工件的处理,从而限制了该技术的工业化应用。为了实现对大面积工件的微弧氧化处理,本文首先在常规微弧氧化技术的前提下,研究了电极间距离对微弧氧化放电的影响,提出了栅网阴极微距微弧氧化方法,有效地降低了氧化电压,增大了微弧氧化技术的处理能力。在此基础上详细地研究了约束阴极微弧氧化的局部放电特性,通过此方法的采用成功地摆脱了待处理工件尺寸受电源功率输出的限制,实现了大尺寸工件的微弧氧化处理。同时针对约束阴极大面积微弧氧化技术所涉及的放电、成膜特点,进行了非同步、非连续微弧氧化成膜特性研究。此外,为了调控膜层结构,进而改善膜层热阻隔效果,本文基于K_2ZrF_6在碱性溶液中形成带负电颗粒的作用机理,实现了K_2ZrF_6对Na2SiO3-KOH溶液体系所制备膜层的组织及性能调制。并借助扫描电镜(SEM)、X射线衍射仪器(XRD)、X射线光电子能谱(XPS)、透射电子显微镜(TEM)等手段分析了膜层的组织和结构,利用同步热分析仪、热阻隔、高温氧化、热冲击及火焰烧蚀等测试研究了膜层的热物理性能。最终,提出了约束阴极大面积微弧氧化系统的设计与实施方案,为工业化应用提出了依据,并利用该装置在Na2SiO3-KOH-K_2ZrF_6溶液中,实现了尺寸为2000 mm×1000 mm×1 mm铝合金表面的热阻隔膜层制备。
电极距离变化对微弧氧化放电特性的影响研究表明,在击穿放电发生之前溶液压降所占比例较小(不足百分之十),但当电极表面击穿放电发生后,电极间溶液压降所占比例大幅增加。因此,在微弧氧化放电成膜时,减少电极间距离能够有效的降低溶液压降,提高氧化工作时的能量效率。通过栅网结构阴极的采用,解决了微小电极距离所引起的气体排放及溶液交换问题,最终使得微距微弧氧化得以实现,有效的降低了微弧氧化电压。同时,氧化电压随电极距离变化研究揭示了电压随电极距离减小的非线性降低变化规律,分析认为这主要是因随电极距离的减小电极间电场分布由发散变为均匀所致。
约束阴极微弧氧化放电行为研究结果表明,采用相对于阳极尺寸较小的阴极,能够使得电场较为集中的分布于临近阴极附近的阳极试样表面,且随电极间距离的减小,电场集中效果更为明显,从而很好的实现了大尺寸待处理工件表面的微弧氧化放电局部控制。阴极尺寸变化结果显示,随着阴极尺寸的增加,氧化电流随之增大,同时阴极下方成膜面积随之增大。但当电极间距离为5 mm阴极尺寸超过Φ20 mm时,由于“气罩效应”使得微小电极距离微弧氧化不能顺畅进行,而栅网结构阴极很好的解决了上述“气罩”问题,确保了约束阴极微距微弧氧化的实现。
针对约束阴极对大尺寸工件进行处理时涉及的不同区域不同时序的微弧氧化成膜特性,所进行的非同步微弧氧化试验研究表明,当处理电压、时间达到先氧化区域的成膜条件时,不同区域的膜层在厚度、结构及性能上能够达到统一,且不同时序成膜界面处并未出现断裂及分层等现象。针对约束阴极微弧氧化工件表面某一确定位置处膜层的生长并非一次性完成特点,所进行的非连续氧化研究表明,非连续工作模式对膜层生长的影响并不明显,且对膜层显微结构影响不大,非连续氧化模式所形成的膜层与连续成膜方式的耐磨、耐腐蚀性能随工作电压变化具有相同的变化规律,均随电压的增加而提高。
基于“K_2ZrF_6在碱性溶液中形成负电Zr(OH)4颗粒”的作用机理,通过K_2ZrF_6的添加,能够对Na2SiO3-KOH溶液中2024铝合金微弧氧化膜层的结构及性能进行调制。结果显示,K_2ZrF_6的引入增大了微弧氧化成膜速率,并对膜层结构产生了显著调制作用。含K_2ZrF_6溶液制得膜层的内外表面较为平整,膜层内大尺寸缺陷减少。EDX线扫描及XPS分析表明,添加K_2ZrF_6后所形成的膜层中有大量Zr元素出现,且其含量随距膜/基界面距离的增加而增加。XRD及TEM结果显示,K_2ZrF_6添加后制备的膜层中晶态氧化物含量降低、非晶态物质增多。膜层热分析测试表明,不同溶液中制备的膜层都具有很好的热稳定性,2024基体经微弧氧化处理后抗高温氧化性能都有所提高。隔热性能测试显示,经K_2ZrF_6调制后的膜层具有更加优良的热阻隔性能。
为验证微距约束阴极微弧氧化对大尺寸工件处理的实用性,设计并制造了一套适用于工业标准尺寸铝板的大面积微弧氧化处理系统,在Na2SiO3-KOH-K_2ZrF_6溶液中,实现了尺寸为2 mm×1 m、厚度为1 mm的2024铝合金板的表面热阻隔膜层制备,为工业化生产提供了技术依据。
With the development of space and aircraft industries, more and more aluminum alloys have been used in the manufacturing aerocrafts. With the increase of aerocrafts’speed, the service environment becomes more and more harsh and temperature rise and thermal shock on aerocrafts surface are big problems. Consequently, aluminum alloys as frequent aerocraft structural material can not endure so high temperature circumstance, which substantially limits further their applications. Microarc oxidation (MAO), as a relatively new surface treatment method to produce thick, thermal stability, thermal protection and adherent coatings on rectifying metals has been developed rapidly in recent years. MAO is an anodizing process during which microdischarges generate dielectric breakdown of the anodic oxide film under high electric field. As a result, it is difficult to process large-scale workpiece in the suggested electrical regime. In this paper, as a novel technique, confined cathode microarc oxidation with shorter distance (SD-CCMAO) has been proposed to process workpiece with large area. The discharge characteristics of the SD-CCMAO have been investigated. In addition, in order to modulate the microstructure and then improve the thermal-resistance of MAO coatings fabricated on 2024 alloy, K_2ZrF_6 additive has been introduced into Na2SiO3-KOH based electrolyte. The modulation effect of K_2ZrF_6 addition on microstructure has been investigated by SEM, XRD, XPS and TEM respectively. Meanwhile, the thermal properties of MAO coatings formed on 2024 aluminum alloy in different electrolytes have been studied. Ultimately, a MAO system for processing workpiece with a large area has been designed and developed.
A shorter electrode distance decreases the voltage drop, and eventually lowers the energy consumption. If the distance becomes too small, the MAO does not work. The novel technique using a grid cathode is employed to implement MAO with the shorter electrode distance. Both the voltage drop and the joule heat in the electrolyte are reduced. Consequently, the processing efficiency, from the viewpoint of energy consumption per unit coating volume, decreases by 25% if the electrode distance decreases from 50 mm to 5 mm. Meanwhile, the experimental result shows that the voltage changes non-linearly with the electrode distance. The non-linear behaviour is much dependent on relative dimension and electrode distance of anode-cathode system but slightly affected by applied anodizing current density and whether there is discharge on anode surface. This may be attributed to the divergence effect of electric field between two electrodes and well verified experimentally by the similar current density on the different parts of the anode if the distance is short. Our results also suggest that, a shorter electrode distance can reduce effectively anodizing voltage and, consequently, improve greatly the energy efficiency. This may speed up the industrial application of PEO technology.
Confined cathode microarc oxidation (CC-MAO) has been investigated in Na2SiO3-KOH solution with industrial pure aluminums substrate materials. The effects of the electrode distance (ED) on working current, potential distribution, arcing voltage and so on have been focused on. The energy efficiency as a function of ED has also been evaluated. The results show the working current decreases with increasing ED with the same exposure area of confined cathode and anode. However, the working current increases with increasing ED if only the cathode is confined. It is attributed to different electrical field on the anode surface. With increasing ED, the electrical field beneath the confined cathode decreases while that far from the cathode increases. This leads to a different total working current. The arcing voltage increases with increasing ED while the effective voltage on anode surface nearly keeps constant. The thickness of the ceramic coating produced with a small ED is much higher than that with a larger ED. The energy consumption per unit volume of oxides by CCMAO indicates that smaller ED leads to higher energy efficiency. The influences of MAO voltage and treatment time during asynchronous MAO process on the oxide current, coating thickness and surface morphology have been studied. Experimental results show that, when the voltage keeps constant, the difference of MAO current between the naked sample and the local oxided sample decreases with treatment time increasing. For the voltage varying, at the beginning of MAO treatment, the difference of MAO current between the naked sample and the local oxided sample increases with the increase in voltage, and then decreases with the increase in treatment time. When the voltage is higher, the thicknesses of different regions are easy to get identical. Scanning electron microscopy shows that longer treatment time and higher voltage will contribute to more identical surface morphology of MAO coatings.
Pure aluminum was treated by microarc oxidation in electrolyte containing Na2SiO3 and KOH at constant voltage mode. The effect of voltage on the properties of the coating prepared by discontinuous microarc oxidation was investigated. The phase composition and surface morphologies of MAO coatings were analyzed by XRD and SEM. The results show that, for the discontinuous MAO, the current drops to some extent at the interrupted point. MAO coatings fabricated by different modes show the similar thickness that increases with increasing oxide time. The processing mode has slight effect on the phase composition of MAO coatings, which are mainly composed ofγ-Al_2O_3 andα-Al_2O_3. The surface morphology of the MAO coatings is hardly affected by processing mode and no lamination is observed for the coatings prepared by discontinuous mode. The coatings fabricated by different modes possess the similar wear resistance and corrosion resistance. This discontinuous mode improves the control flexibility during micro-oxidation processes.
Zr(OH)4 particles can be formed and negatively charged in alkaline solution with K_2ZrF_6 addition. Based on this, Zr-containing ceramic coatings were fabricated on 2024 aluminum alloy by microarc oxidation (MAO) using K_2ZrF_6 as a special additive in Na2SiO3-KOH base electrolyte. The results show that the K_2ZrF_6 addition can increase the micro-arc oxidation rate and significantly alter the structure of MAO coatings. Both the top surface and inner surface of MAO coatings fabricated in Zr-containing electrolyte become relatively smooth. Compared with the coating formed in Zr-free electrolyte, a large amount of Zr element is found in the coating formed in electrolyte with K_2ZrF_6 addition. Two main phases,γ-Al_2O_3 andα-Al_2O_3, are contained in Zr-free coating. In contrast, more amorphous phase is found in Zr-containing coating with reduced amount of crystalline alumina. Experimental results also demonstrate that Zr-containing coating exhibits higher heat resistance.
To investigate the feasibility of industrial application, a MAO system for processing a 2024 alloy plate with the standard scale (2000 mm×1000 mm×1 mm) has been designed and manufactured. The Zr-containing coating on the whole large workpiece surface has been achieved successfully.
电极距离变化对微弧氧化放电特性的影响研究表明,在击穿放电发生之前溶液压降所占比例较小(不足百分之十),但当电极表面击穿放电发生后,电极间溶液压降所占比例大幅增加。因此,在微弧氧化放电成膜时,减少电极间距离能够有效的降低溶液压降,提高氧化工作时的能量效率。通过栅网结构阴极的采用,解决了微小电极距离所引起的气体排放及溶液交换问题,最终使得微距微弧氧化得以实现,有效的降低了微弧氧化电压。同时,氧化电压随电极距离变化研究揭示了电压随电极距离减小的非线性降低变化规律,分析认为这主要是因随电极距离的减小电极间电场分布由发散变为均匀所致。
约束阴极微弧氧化放电行为研究结果表明,采用相对于阳极尺寸较小的阴极,能够使得电场较为集中的分布于临近阴极附近的阳极试样表面,且随电极间距离的减小,电场集中效果更为明显,从而很好的实现了大尺寸待处理工件表面的微弧氧化放电局部控制。阴极尺寸变化结果显示,随着阴极尺寸的增加,氧化电流随之增大,同时阴极下方成膜面积随之增大。但当电极间距离为5 mm阴极尺寸超过Φ20 mm时,由于“气罩效应”使得微小电极距离微弧氧化不能顺畅进行,而栅网结构阴极很好的解决了上述“气罩”问题,确保了约束阴极微距微弧氧化的实现。
针对约束阴极对大尺寸工件进行处理时涉及的不同区域不同时序的微弧氧化成膜特性,所进行的非同步微弧氧化试验研究表明,当处理电压、时间达到先氧化区域的成膜条件时,不同区域的膜层在厚度、结构及性能上能够达到统一,且不同时序成膜界面处并未出现断裂及分层等现象。针对约束阴极微弧氧化工件表面某一确定位置处膜层的生长并非一次性完成特点,所进行的非连续氧化研究表明,非连续工作模式对膜层生长的影响并不明显,且对膜层显微结构影响不大,非连续氧化模式所形成的膜层与连续成膜方式的耐磨、耐腐蚀性能随工作电压变化具有相同的变化规律,均随电压的增加而提高。
基于“K_2ZrF_6在碱性溶液中形成负电Zr(OH)4颗粒”的作用机理,通过K_2ZrF_6的添加,能够对Na2SiO3-KOH溶液中2024铝合金微弧氧化膜层的结构及性能进行调制。结果显示,K_2ZrF_6的引入增大了微弧氧化成膜速率,并对膜层结构产生了显著调制作用。含K_2ZrF_6溶液制得膜层的内外表面较为平整,膜层内大尺寸缺陷减少。EDX线扫描及XPS分析表明,添加K_2ZrF_6后所形成的膜层中有大量Zr元素出现,且其含量随距膜/基界面距离的增加而增加。XRD及TEM结果显示,K_2ZrF_6添加后制备的膜层中晶态氧化物含量降低、非晶态物质增多。膜层热分析测试表明,不同溶液中制备的膜层都具有很好的热稳定性,2024基体经微弧氧化处理后抗高温氧化性能都有所提高。隔热性能测试显示,经K_2ZrF_6调制后的膜层具有更加优良的热阻隔性能。
为验证微距约束阴极微弧氧化对大尺寸工件处理的实用性,设计并制造了一套适用于工业标准尺寸铝板的大面积微弧氧化处理系统,在Na2SiO3-KOH-K_2ZrF_6溶液中,实现了尺寸为2 mm×1 m、厚度为1 mm的2024铝合金板的表面热阻隔膜层制备,为工业化生产提供了技术依据。
With the development of space and aircraft industries, more and more aluminum alloys have been used in the manufacturing aerocrafts. With the increase of aerocrafts’speed, the service environment becomes more and more harsh and temperature rise and thermal shock on aerocrafts surface are big problems. Consequently, aluminum alloys as frequent aerocraft structural material can not endure so high temperature circumstance, which substantially limits further their applications. Microarc oxidation (MAO), as a relatively new surface treatment method to produce thick, thermal stability, thermal protection and adherent coatings on rectifying metals has been developed rapidly in recent years. MAO is an anodizing process during which microdischarges generate dielectric breakdown of the anodic oxide film under high electric field. As a result, it is difficult to process large-scale workpiece in the suggested electrical regime. In this paper, as a novel technique, confined cathode microarc oxidation with shorter distance (SD-CCMAO) has been proposed to process workpiece with large area. The discharge characteristics of the SD-CCMAO have been investigated. In addition, in order to modulate the microstructure and then improve the thermal-resistance of MAO coatings fabricated on 2024 alloy, K_2ZrF_6 additive has been introduced into Na2SiO3-KOH based electrolyte. The modulation effect of K_2ZrF_6 addition on microstructure has been investigated by SEM, XRD, XPS and TEM respectively. Meanwhile, the thermal properties of MAO coatings formed on 2024 aluminum alloy in different electrolytes have been studied. Ultimately, a MAO system for processing workpiece with a large area has been designed and developed.
A shorter electrode distance decreases the voltage drop, and eventually lowers the energy consumption. If the distance becomes too small, the MAO does not work. The novel technique using a grid cathode is employed to implement MAO with the shorter electrode distance. Both the voltage drop and the joule heat in the electrolyte are reduced. Consequently, the processing efficiency, from the viewpoint of energy consumption per unit coating volume, decreases by 25% if the electrode distance decreases from 50 mm to 5 mm. Meanwhile, the experimental result shows that the voltage changes non-linearly with the electrode distance. The non-linear behaviour is much dependent on relative dimension and electrode distance of anode-cathode system but slightly affected by applied anodizing current density and whether there is discharge on anode surface. This may be attributed to the divergence effect of electric field between two electrodes and well verified experimentally by the similar current density on the different parts of the anode if the distance is short. Our results also suggest that, a shorter electrode distance can reduce effectively anodizing voltage and, consequently, improve greatly the energy efficiency. This may speed up the industrial application of PEO technology.
Confined cathode microarc oxidation (CC-MAO) has been investigated in Na2SiO3-KOH solution with industrial pure aluminums substrate materials. The effects of the electrode distance (ED) on working current, potential distribution, arcing voltage and so on have been focused on. The energy efficiency as a function of ED has also been evaluated. The results show the working current decreases with increasing ED with the same exposure area of confined cathode and anode. However, the working current increases with increasing ED if only the cathode is confined. It is attributed to different electrical field on the anode surface. With increasing ED, the electrical field beneath the confined cathode decreases while that far from the cathode increases. This leads to a different total working current. The arcing voltage increases with increasing ED while the effective voltage on anode surface nearly keeps constant. The thickness of the ceramic coating produced with a small ED is much higher than that with a larger ED. The energy consumption per unit volume of oxides by CCMAO indicates that smaller ED leads to higher energy efficiency. The influences of MAO voltage and treatment time during asynchronous MAO process on the oxide current, coating thickness and surface morphology have been studied. Experimental results show that, when the voltage keeps constant, the difference of MAO current between the naked sample and the local oxided sample decreases with treatment time increasing. For the voltage varying, at the beginning of MAO treatment, the difference of MAO current between the naked sample and the local oxided sample increases with the increase in voltage, and then decreases with the increase in treatment time. When the voltage is higher, the thicknesses of different regions are easy to get identical. Scanning electron microscopy shows that longer treatment time and higher voltage will contribute to more identical surface morphology of MAO coatings.
Pure aluminum was treated by microarc oxidation in electrolyte containing Na2SiO3 and KOH at constant voltage mode. The effect of voltage on the properties of the coating prepared by discontinuous microarc oxidation was investigated. The phase composition and surface morphologies of MAO coatings were analyzed by XRD and SEM. The results show that, for the discontinuous MAO, the current drops to some extent at the interrupted point. MAO coatings fabricated by different modes show the similar thickness that increases with increasing oxide time. The processing mode has slight effect on the phase composition of MAO coatings, which are mainly composed ofγ-Al_2O_3 andα-Al_2O_3. The surface morphology of the MAO coatings is hardly affected by processing mode and no lamination is observed for the coatings prepared by discontinuous mode. The coatings fabricated by different modes possess the similar wear resistance and corrosion resistance. This discontinuous mode improves the control flexibility during micro-oxidation processes.
Zr(OH)4 particles can be formed and negatively charged in alkaline solution with K_2ZrF_6 addition. Based on this, Zr-containing ceramic coatings were fabricated on 2024 aluminum alloy by microarc oxidation (MAO) using K_2ZrF_6 as a special additive in Na2SiO3-KOH base electrolyte. The results show that the K_2ZrF_6 addition can increase the micro-arc oxidation rate and significantly alter the structure of MAO coatings. Both the top surface and inner surface of MAO coatings fabricated in Zr-containing electrolyte become relatively smooth. Compared with the coating formed in Zr-free electrolyte, a large amount of Zr element is found in the coating formed in electrolyte with K_2ZrF_6 addition. Two main phases,γ-Al_2O_3 andα-Al_2O_3, are contained in Zr-free coating. In contrast, more amorphous phase is found in Zr-containing coating with reduced amount of crystalline alumina. Experimental results also demonstrate that Zr-containing coating exhibits higher heat resistance.
To investigate the feasibility of industrial application, a MAO system for processing a 2024 alloy plate with the standard scale (2000 mm×1000 mm×1 mm) has been designed and manufactured. The Zr-containing coating on the whole large workpiece surface has been achieved successfully.
引文
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