低能耗镁合金微弧氧化电解液设计及添加剂作用机制研究
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摘要
镁合金以其密度小、比刚比强度高等优点在航空航天、汽车、电子等领域应用前景广阔。但镁合金耐磨耐蚀性能差限制了其应用范围的进一步扩大。因此对镁合金进行表面改性处理意义重大。微弧氧化以工艺简单环保、膜层性能好等特点在镁合金表面改性方面具有很大优势，但同时微弧氧化属于高电压、大电流密度的工作过程，能耗高限制了其工业化应用进程。发展低能耗微弧氧化技术是解决该问题的关键。本文提出了一种低能耗微弧氧化电解液的设计方法。为选择适当的添加剂，提出了一种基于阳极极化曲线判断微弧氧化起弧电压的方法，以指导选择具有低起弧电压的成膜促进剂；提出了Na_2CO_3诱导析气反应调制膜层结构的反应机制，提高膜层孔隙率进行，降低微弧氧化的工作电压；通过(NaPO_3)_6的络合增厚机制提高了膜层生长的速率。最终本文实现了镁合金低能耗微弧氧化过程并制备了微弧氧化膜层，借助于扫描电镜（SEM）、X射线衍射仪（XRD）、透射电子显微镜（TEM）等手段对膜层的组织和结构进行了分析，利用摩擦磨损试验、腐蚀试验等测试对膜层的性能进行了测试。最后本文在镁合金低能耗电解液中以低于1kW的功率成功实现了一次性对12dm2的镁合金进行微弧氧化处理，以小功率实现了对较大面积试件的处理，体现了低能耗微弧氧化的技术优势。
镁合金低能耗电解液的设计方法研究表明，选用适当的主盐和pH调节剂，在电解液中引入可以降低微弧氧化起弧电压的成膜促进剂、适量的可以提高膜层表面孔隙率的膜层结构调制剂以及适当的络合增厚剂，可以实现镁合金低能耗微弧氧化。对于镁合金，选用碱性磷酸盐体系作为基础溶液体系，引入成膜促进剂NaF、膜层结构调制剂Na_2CO_3和络合增厚剂(NaPO_3)_6作为低能耗微弧氧化电解液添加剂。
阳极极化行为对镁合金微弧氧化放电特性指导方法的研究结果表明，阳极极化曲线可以作为判断微弧氧化放电特性的依据，进而选择利于降低微弧氧化起弧电压的成膜促进剂。在金属的阳极极化行为中不能发生钝化现象的，则金属在相应电解液不能发生微弧氧化行为；对于可以使金属前期形成氧化膜的电解液，阳极极化行为中曲线上对应的钝化区间宽度越大，则微弧氧化容易在低电压发生放电；在钝化区间宽度相近的情况下，钝化膜层失稳前极化电流越小则微弧氧化起弧电压越低。Na_2CO_3诱导阳极区CO2析气调制膜层结构的反应机制研究表明，Na_2CO_3添加剂对微弧氧化膜层结构的调制是通过二级析气反应完成的。CO_3~(2-)在电场作用下进入阳极区与Mg元素作用生成MgCO_3，MgCO_3在微弧氧化放电瞬间高温作用下发生分解CO2逸出，熔融的氧化物来不及回填气泡逸出时在膜层留下的大量孔隙，提高了膜层内部孔隙率，气体逸出时留下的通道增加了微弧氧化膜层表面的孔隙率，由此实现对微弧氧化膜层结构的调制。(NaPO_3)_6络合增厚机制研究表明，(NaPO_3)_6通过水解产物络合微弧氧化过程中溶解到电解液的镁元素，络合离子团在电场作用下重新进入阳极区参与反应可提高膜层生长速率。
单一添加剂及添加剂复合作用对微弧放电特性的影响研究表明，NaF添加剂既可以降低微弧氧化的工作电压，又能有效提高微弧氧化膜层的成膜速率；Na_2CO_3可以有效降低微弧氧化的工作电压；(NaPO_3)_6添加剂对于提高膜层的生长速率具有积极作用。三种添加剂通过这些不同方式都可降低微弧氧化膜层的单位能耗。在镁合金微弧氧化电解液中同时引入NaF、Na_2CO_3以及(NaPO_3)_6三种添加剂可以起到良好的降低微弧氧化膜层单位能耗的效果。采用50g/LNa_3PO_4+2g/L KOH+30g/L NaF+10g/L Na_2CO_3+30g/L (NaPO_3)_6作为AZ31镁合金微弧氧化电解液时，微弧氧化膜层能耗可以低至4.71kJ/dm2·μm。低能耗微弧氧化过程中弧斑燃烧时间极短，并且氧化过程中参与等离子放电种类较常规微弧氧化少。
添加剂对微弧氧化膜层组织结构及性能的影响研究结果表明，NaF添加剂的引入会使膜层中出现MgF2相，另外会使膜层内部缺陷减少，膜层变致密；适量NaF添加剂的引入有利于提高微弧氧化膜层耐腐蚀性能。Na_2CO_3添加剂的引入能够提高膜层表面和内部孔隙率，但不会改变膜层的组织结构和成分。适当剂量的Na_2CO_3可以提高膜层的耐腐蚀性能，剂量较大时会降低膜层的耐腐蚀性能。(NaPO_3)_6添加剂对微弧氧化膜层形貌有影响，但不降低膜层的致密性；(NaPO_3)_6的引入会在膜层中引入P元素，但不以晶体相形式存在；(NaPO_3)_6添加剂能够提高膜层的电化学腐蚀和耐盐雾腐蚀性能。
基于对低能耗微弧氧化电解液的研究，本文在AZ31镁合金上制备了低能耗微弧氧化膜层。XRD、FT-IR和TEM等分析结果表明，镁合金低能耗微弧氧化膜层主要为非晶MgO组成。膜层具有与常规微弧氧化膜层相当的耐磨耐蚀性能以及优于常规微弧氧化膜层的可弯折性能。在镁合金低能耗微弧氧化电解液中，以1kW以下功率实现了微弧氧化处理过程，大大扩大现有电源的可处理面积，使得低能耗微弧氧化处理实现了其现实意义。
Magnesium alloys present a great potential in the field of aerospace,automobile, electronic and others for excellent properties such as low density, highspecific strength and specific rigidity. However, low hardness and poor corrosionresistance limit their further applications. So it is necessary for magnesium alloys tohave surface modification treatment. Micro-arc oxidation has been developedrapidly in recent years. However MAO is an anodizing process during which micro-discharges generate dielectric breakdown of the anodic oxide film under highelectric field. The question of high energy consumption limits its further applicationin industrial field. Developing low energy consumption MAO technology is the onlyway to solve the question. In this paper an idea of designing low energyconsumption electrolyte was brought out. A new method on predicting arc-initiatingof micro-arc oxidation by anodic polarization curve was given so as to choose theadditves which could lower the arcing voltage. The mechanism of reaction inducedby sodium carbonate additive to release carbon dioxide to modulate coatingformation was studied and the working voltage could be lowered.Coating formingvelocity was increased by complex reaction induced by sodium hexametahposphate.MAO coating was fabricated on magnesium alloys with low energy consumptionand the microstructure has been investigated by SEM, XRD, and TEM respectively.Meanwhile, the properties of MAO coatings formed on AZ31magnesium alloy havebeen studied. Ultimately a large-scale (12dm2) MAO coating with power less than1kW has been fabricated and the advantage of MAO with lower energy consumptionis demonstrated.
It can be proposed from the method of designing low energy consumptionelectrolyte that the introduction of additives with the ability to lower the arcingvoltage or additives with modulation effect on increasing the porosity of the coatingis beneficial for lowering the energy consumption. And additives with complexeffect to increase the forming velocity of MAO coating is needed. Phosphate alkaliis suitable to be the basic electrolyte of low energy consumption electrolyte. Andsodium fluoride is chosen to lower the arcing voltage and sodium carbonate isutilized to modulate the structure of the coating. Sodium hexametahposphate isemployed to increase coating velocity.
A new method on predicting arc igniting of micro-arc oxidation on magnesiumalloy by anodic polarization curve was proposed to choose additives to lower thearcing voltage. The results show that arcing voltage is much dependent on thestability of passivating films formed during anodic polarization process. The arcing voltage is higher with a larger passivation region of the polarization curve. Whenthe stability of passivating films is at about the same level, the arcing voltagebecomes lower in the solution possessing a smaller polarization current at the latersection of passivation curves. Microstructure of the MAO coating can be modulatedby gas evolution on anodes during micro arc oxidation process. The modulatationprocessed with a two-step reaction. Carbonate ions combine with magnesiumelement and then magnesium carbonate decomposes under the high temperature.Carbon dioxide escapes and micropores generate in the coating. Sodiumhexametahposphate is easy to hydrolyze to have hydroniums with complex ability inthe solution. During MAO process some Mg~(2+)cations dissolved could becomplexed and the complex ions could return to anode region in the electrical fieldand take part in the reaction. And it is beneficial to the thickening of the coating.
Effect of the three additives on MAO discharge has been studied. NaF hasadvantage in lowering the working voltage and increasing coating velocity. Thevoltage could be lowered with the introduction of sodium carbonate with themodulation effect on microstructure of coating and the coating formation velocitycoule be increased with sodium hexametahposphate introduced. Although the modeof reaction is different, the ECPUV could be lowered with introduction of the threeadditives. MAO process with low energy consumption coule be realized with all thethree additives in the electrolyte. In the electrolyte (50g/L Na_3PO_4+2g/L KOH+30g/L NaF+10g/L Na_2CO_3+30g/L (NaPO_3)_6) the ECPUV could be lowered to4.71kJ/dm2·μm. During lower energy consumption MAO a microarc lasts onlyhudrends of microseconds and fewer species of particles take part in the plasmadischarge compared to normal MAO.
Magnesium fluoride generates with sodium fluoride introduced into theelectrolyte and the coatings become compact. It is beneficial for the corrosionresistance of the coating with a right amount of sodium fluoride in the electrolyte.The porosity of the coating increase without change the phase and composition ofthe coating when sodium carbonate is introduced into the electrolyte. It is beneficialfor the corrosion resistance of the coatings with a certain amount of sodiumcarbonate in the electrolyte and the corrosion resistance becomes weak when theamount is too large. Surface morphology will change with introducing sodiumhexametahposphate into the electrolyte but it has no negative effect on thecompactness of the coating. Phosphorus element is found in the coating formed inelectrolyte with sodium hexametahposphate addition. The coatings fabricated inelectrolyte exhibita good corrosion resistance.
MAO coatings have been fabricated on magnesium alloys in the low energyconsumption electrolyte. The l coatings mainly are composed of MgO amorphousphase. Experimental results also demonstrate that the performance of the coatings is as good as that of the normal MAO coatings. Even the abending ability of thesample treated by MAO with low energy consumption is better than that treated bynormal MAO process.
To investigate the feasibility of industrial application of ow energyconsumption MAO, a AZ31magnesium alloy plate with the area of12dm~2has beentreated by MAO process with power less than1kW. This promotion the treatingability of the MAO power equipment and industrialization of this technology maybe realized.
镁合金低能耗电解液的设计方法研究表明，选用适当的主盐和pH调节剂，在电解液中引入可以降低微弧氧化起弧电压的成膜促进剂、适量的可以提高膜层表面孔隙率的膜层结构调制剂以及适当的络合增厚剂，可以实现镁合金低能耗微弧氧化。对于镁合金，选用碱性磷酸盐体系作为基础溶液体系，引入成膜促进剂NaF、膜层结构调制剂Na_2CO_3和络合增厚剂(NaPO_3)_6作为低能耗微弧氧化电解液添加剂。
阳极极化行为对镁合金微弧氧化放电特性指导方法的研究结果表明，阳极极化曲线可以作为判断微弧氧化放电特性的依据，进而选择利于降低微弧氧化起弧电压的成膜促进剂。在金属的阳极极化行为中不能发生钝化现象的，则金属在相应电解液不能发生微弧氧化行为；对于可以使金属前期形成氧化膜的电解液，阳极极化行为中曲线上对应的钝化区间宽度越大，则微弧氧化容易在低电压发生放电；在钝化区间宽度相近的情况下，钝化膜层失稳前极化电流越小则微弧氧化起弧电压越低。Na_2CO_3诱导阳极区CO2析气调制膜层结构的反应机制研究表明，Na_2CO_3添加剂对微弧氧化膜层结构的调制是通过二级析气反应完成的。CO_3~(2-)在电场作用下进入阳极区与Mg元素作用生成MgCO_3，MgCO_3在微弧氧化放电瞬间高温作用下发生分解CO2逸出，熔融的氧化物来不及回填气泡逸出时在膜层留下的大量孔隙，提高了膜层内部孔隙率，气体逸出时留下的通道增加了微弧氧化膜层表面的孔隙率，由此实现对微弧氧化膜层结构的调制。(NaPO_3)_6络合增厚机制研究表明，(NaPO_3)_6通过水解产物络合微弧氧化过程中溶解到电解液的镁元素，络合离子团在电场作用下重新进入阳极区参与反应可提高膜层生长速率。
单一添加剂及添加剂复合作用对微弧放电特性的影响研究表明，NaF添加剂既可以降低微弧氧化的工作电压，又能有效提高微弧氧化膜层的成膜速率；Na_2CO_3可以有效降低微弧氧化的工作电压；(NaPO_3)_6添加剂对于提高膜层的生长速率具有积极作用。三种添加剂通过这些不同方式都可降低微弧氧化膜层的单位能耗。在镁合金微弧氧化电解液中同时引入NaF、Na_2CO_3以及(NaPO_3)_6三种添加剂可以起到良好的降低微弧氧化膜层单位能耗的效果。采用50g/LNa_3PO_4+2g/L KOH+30g/L NaF+10g/L Na_2CO_3+30g/L (NaPO_3)_6作为AZ31镁合金微弧氧化电解液时，微弧氧化膜层能耗可以低至4.71kJ/dm2·μm。低能耗微弧氧化过程中弧斑燃烧时间极短，并且氧化过程中参与等离子放电种类较常规微弧氧化少。
添加剂对微弧氧化膜层组织结构及性能的影响研究结果表明，NaF添加剂的引入会使膜层中出现MgF2相，另外会使膜层内部缺陷减少，膜层变致密；适量NaF添加剂的引入有利于提高微弧氧化膜层耐腐蚀性能。Na_2CO_3添加剂的引入能够提高膜层表面和内部孔隙率，但不会改变膜层的组织结构和成分。适当剂量的Na_2CO_3可以提高膜层的耐腐蚀性能，剂量较大时会降低膜层的耐腐蚀性能。(NaPO_3)_6添加剂对微弧氧化膜层形貌有影响，但不降低膜层的致密性；(NaPO_3)_6的引入会在膜层中引入P元素，但不以晶体相形式存在；(NaPO_3)_6添加剂能够提高膜层的电化学腐蚀和耐盐雾腐蚀性能。
基于对低能耗微弧氧化电解液的研究，本文在AZ31镁合金上制备了低能耗微弧氧化膜层。XRD、FT-IR和TEM等分析结果表明，镁合金低能耗微弧氧化膜层主要为非晶MgO组成。膜层具有与常规微弧氧化膜层相当的耐磨耐蚀性能以及优于常规微弧氧化膜层的可弯折性能。在镁合金低能耗微弧氧化电解液中，以1kW以下功率实现了微弧氧化处理过程，大大扩大现有电源的可处理面积，使得低能耗微弧氧化处理实现了其现实意义。
Magnesium alloys present a great potential in the field of aerospace,automobile, electronic and others for excellent properties such as low density, highspecific strength and specific rigidity. However, low hardness and poor corrosionresistance limit their further applications. So it is necessary for magnesium alloys tohave surface modification treatment. Micro-arc oxidation has been developedrapidly in recent years. However MAO is an anodizing process during which micro-discharges generate dielectric breakdown of the anodic oxide film under highelectric field. The question of high energy consumption limits its further applicationin industrial field. Developing low energy consumption MAO technology is the onlyway to solve the question. In this paper an idea of designing low energyconsumption electrolyte was brought out. A new method on predicting arc-initiatingof micro-arc oxidation by anodic polarization curve was given so as to choose theadditves which could lower the arcing voltage. The mechanism of reaction inducedby sodium carbonate additive to release carbon dioxide to modulate coatingformation was studied and the working voltage could be lowered.Coating formingvelocity was increased by complex reaction induced by sodium hexametahposphate.MAO coating was fabricated on magnesium alloys with low energy consumptionand the microstructure has been investigated by SEM, XRD, and TEM respectively.Meanwhile, the properties of MAO coatings formed on AZ31magnesium alloy havebeen studied. Ultimately a large-scale (12dm2) MAO coating with power less than1kW has been fabricated and the advantage of MAO with lower energy consumptionis demonstrated.
It can be proposed from the method of designing low energy consumptionelectrolyte that the introduction of additives with the ability to lower the arcingvoltage or additives with modulation effect on increasing the porosity of the coatingis beneficial for lowering the energy consumption. And additives with complexeffect to increase the forming velocity of MAO coating is needed. Phosphate alkaliis suitable to be the basic electrolyte of low energy consumption electrolyte. Andsodium fluoride is chosen to lower the arcing voltage and sodium carbonate isutilized to modulate the structure of the coating. Sodium hexametahposphate isemployed to increase coating velocity.
A new method on predicting arc igniting of micro-arc oxidation on magnesiumalloy by anodic polarization curve was proposed to choose additives to lower thearcing voltage. The results show that arcing voltage is much dependent on thestability of passivating films formed during anodic polarization process. The arcing voltage is higher with a larger passivation region of the polarization curve. Whenthe stability of passivating films is at about the same level, the arcing voltagebecomes lower in the solution possessing a smaller polarization current at the latersection of passivation curves. Microstructure of the MAO coating can be modulatedby gas evolution on anodes during micro arc oxidation process. The modulatationprocessed with a two-step reaction. Carbonate ions combine with magnesiumelement and then magnesium carbonate decomposes under the high temperature.Carbon dioxide escapes and micropores generate in the coating. Sodiumhexametahposphate is easy to hydrolyze to have hydroniums with complex ability inthe solution. During MAO process some Mg~(2+)cations dissolved could becomplexed and the complex ions could return to anode region in the electrical fieldand take part in the reaction. And it is beneficial to the thickening of the coating.
Effect of the three additives on MAO discharge has been studied. NaF hasadvantage in lowering the working voltage and increasing coating velocity. Thevoltage could be lowered with the introduction of sodium carbonate with themodulation effect on microstructure of coating and the coating formation velocitycoule be increased with sodium hexametahposphate introduced. Although the modeof reaction is different, the ECPUV could be lowered with introduction of the threeadditives. MAO process with low energy consumption coule be realized with all thethree additives in the electrolyte. In the electrolyte (50g/L Na_3PO_4+2g/L KOH+30g/L NaF+10g/L Na_2CO_3+30g/L (NaPO_3)_6) the ECPUV could be lowered to4.71kJ/dm2·μm. During lower energy consumption MAO a microarc lasts onlyhudrends of microseconds and fewer species of particles take part in the plasmadischarge compared to normal MAO.
Magnesium fluoride generates with sodium fluoride introduced into theelectrolyte and the coatings become compact. It is beneficial for the corrosionresistance of the coating with a right amount of sodium fluoride in the electrolyte.The porosity of the coating increase without change the phase and composition ofthe coating when sodium carbonate is introduced into the electrolyte. It is beneficialfor the corrosion resistance of the coatings with a certain amount of sodiumcarbonate in the electrolyte and the corrosion resistance becomes weak when theamount is too large. Surface morphology will change with introducing sodiumhexametahposphate into the electrolyte but it has no negative effect on thecompactness of the coating. Phosphorus element is found in the coating formed inelectrolyte with sodium hexametahposphate addition. The coatings fabricated inelectrolyte exhibita good corrosion resistance.
MAO coatings have been fabricated on magnesium alloys in the low energyconsumption electrolyte. The l coatings mainly are composed of MgO amorphousphase. Experimental results also demonstrate that the performance of the coatings is as good as that of the normal MAO coatings. Even the abending ability of thesample treated by MAO with low energy consumption is better than that treated bynormal MAO process.
To investigate the feasibility of industrial application of ow energyconsumption MAO, a AZ31magnesium alloy plate with the area of12dm~2has beentreated by MAO process with power less than1kW. This promotion the treatingability of the MAO power equipment and industrialization of this technology maybe realized.
引文
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