高速电弧喷涂FeMnCrAl/碳化物系涂层组织与性能及其机理研究
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摘要
国内外火力发电厂燃煤锅炉管道(水冷壁、过热器、再热器、省煤器管)存在严重冲蚀磨损、腐蚀现象以及由此造成的重大经济损失的现实问题。因此,针对燃煤锅炉管道的冲蚀磨损和腐蚀问题,立项研究并解决燃煤电厂锅炉管道表面的高温腐蚀和冲蚀磨损问题对于提高燃煤锅炉的发电能力,降低运行成本都有着非常重要的现实意义。本论文研究采用高速电弧喷涂粉芯丝材技术,选取低碳钢带作为表皮材料,选取适量配比的Mn粉、Cr粉、Al粉、Cr3C2粉、Ni包覆WC粉和Ni包覆Cr3C2粉等作为芯粉,成功制备了用于锅炉管道表面防护的低成本FeMnCrAl/碳化物系涂层。本文从影响冲蚀和热腐蚀的关键因素—材料出发,研制具有良好性价比的燃煤锅炉管道用新型电弧喷涂新材料,是一个节能防护课题,具有很大的实际应用价值和重要的学术意义。
本论文首先采用高速电弧喷涂技术成功制备了FeMnCr/Cr3C2涂层、FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层。涂层呈典型的层状显微组织结构,由金属结晶相、氧化物相、未熔颗粒和孔隙组成。与FeMnCr/Cr3C2涂层相比,FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层具有明显较少的未熔颗粒、氧化物含量和孔隙,组织致密度更高,涂层与基体的界面结合状况更好。
本论文研究了FeMnCr/Cr3C2涂层、FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层的显微硬度、结合强度和内聚强度,并对拉伸断口形貌进行电镜分析。研究发现,FeMnCr/Cr3C2涂层和FeMnCrAl/Cr3C2涂层具有较高的显微硬度值,为20钢的2-3倍；FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层结合强度较高,高于FeMnCr/Cr3C2涂层；FeMnCrAl/Cr3C2涂层的内聚强度高于其它对比涂层,达到174.5MPa；涂层的拉伸断口具有结晶相的准解理断裂、氧化物相的脆性断裂、“叠层”间分离脱开、未熔颗粒与“叠层”分离甚至被整体拔出等形貌特征。
通过抗热震性能试验发现：与FeMnCr/Cr3C2和FeNiCr/Cr3C2涂层相比,FeMnCrAl/Cr3C2-Ni9Al涂层抗热震性能最好,32次循环后仍然无脱落现象。涂层热震失效过程包括裂纹在氧化物区域和孔隙处的萌生和扩展；涂层中的孔洞会阻碍裂纹扩展,但是,如果孔洞形状不规则,则热震会使裂纹在孔洞的大曲率尖端处激活继续扩展,形成二次裂纹并扩展。裂纹是氧向涂层内扩散的“快速通道”,氧还会沿着孔洞、凝片间隙向内扩散,导致高温氧化在整个涂层中发生。当氧渗入到涂层与基体的结合界面时,造成界面氧化现象,涂层与基体的结合状态恶化,最终导致涂层脱落失效。
本文研究了FeMnCrAl/碳化物系涂层的高温氧化和热腐蚀性能,发现各涂层体系均具有良好的抗氧化性和耐热腐蚀性能,明显优于20钢,其中FeMnCrAl/Cr3C2涂层的抗腐蚀性能最好,约为20钢的1/10。
冲蚀磨损性能试验表明,FeMnCr/Cr3C2涂层和FeMnCrAl/Cr3C2涂层的冲蚀率都明显低于20钢基材,尤以FeMnCrAl/Cr3C2涂层的抗冲蚀磨损性能为最佳。涂层的冲蚀磨损机理为：低冲击角下以犁耕和切削作用为主,伴随着二次冲击的塑性变形和脆性脱落；高冲击角下发生表面材料挤压、脆性裂纹生成和脱落以及过度塑性变形后的疲劳开裂和脱落。
为改善陶瓷粉体在金属基涂层中浸润性和结合状态,本论文创新性地发明对WC和Cr3C2粉末进行化学镀Ni预处理的方法。该方法不需要贵金属敏化活化处理,预处理后的粉体可以保证后期镀Ni效果,镀层均匀。Ni颗粒的形核、长大和聚集的过程为：1)、化学镀溶液中的反应物在具有催化活性的表面缺陷上吸附,发生氧化-还原反应沉积出Ni颗粒。2)、Ni颗粒形核后长大成膜,其长大成膜过程为：Ni核依附“线条状”突起以“线型”方式长大、弯曲、分叉和聚集,而后缠绕成“胞状”结构,犹如生活中“缠毛线团”。“胞状”结构Ni颗粒不断长大聚集,最后成膜。与FeMnCrAl/WC涂层和FeMnCrAl/Cr3C2涂层相比,添加了Ni包覆陶瓷相的涂层结合强度和内聚强度平均值得到提高,其平均显微硬度值与原涂层相当。Ni包覆WC相改善了涂层抗冲蚀磨损性能,涂层的冲蚀机理基本相似。添加Ni包覆WC陶瓷相和Ni包覆Cr3C2陶瓷相的两种涂层的平均显微硬度值与未添加包覆陶瓷相的涂层相当。
FeMnCrAl/碳化物系涂层已经应用于水冷壁和屏过等部分受热面管道高温防腐和防磨中,经过半年多时间运行检测发现,防护效果非常理想,预计该涂层可以使用2年以上。
According to actual problems that there were serious erosion, corrosion and resulting in major economic losses caused on the boiler tubes (water wall,superheater, reheater, economizer tube) of coal-fired thermal power plants at home and abroad, low-cost FeMnCrAl/carbide series coatings have been studied to resolve the surface temperature corrosion and erosion problems using high velocity arc spraying process in this paper. In this study, low-cost FeMnCrAl/carbide series coatings were successfully prepared using Mn, Cr, Al, Cr3C2, Ni-coated WC, Ni-coated Cr3C2, etc cored wires together with high velocity arc spraying for surface protection of the boiler tubes. New arc-spraying materials with good cost-effective development of coal-fired boiler tubes were studied. This study content is an energy-saving protection issues, having great practical value and academic significance.
FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating were deposited on 20 steel substrates by the high velocity arc spraying. The coatings characteristically consisted of successive layers contained metal crystalline phases, oxide phases, un-melted particles and pores. Compared with that of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating significantly had less un-melted particles, oxide content and porosity, possessed good interfacial bonding and microstructure between coatings and substrate, no coarse pores and cracks.
Hardness, bond strength, cohesive strength and morphology of tensile fracture of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating have been studied. The results show that compared with that of 20 steel, FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating possess high average hardness,2-3 times than that of 20 steel. FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating exhibit higher bonding strength between coatings and substrate than that of FeMnCr/Cr3C2 coating. The average cohesive strength of FeMnCrAl/Cr3C2 coating is 174.5MPa, higher than that of FeMnCr/Cr3C2 coating.Characteristics of tensile fracture of coating are characteristics of quasi-cleavage fracture of metal crystalline phases and brittle fracture of oxide phases, characteristics of separation and disengagement of "laminations" and characteristics of un-melted particles integral putout.
Thermal shock resistances of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9A1 coating have been analyzed. Compared with that of FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating, FeMnCrAl/Cr3C2-Ni9Al coating possesses the best thermal shock resistance, being no exfoliation phenomenon after the number of thermal shock cycles 32. Failure mechanism of thermal shock of arc-sprayed coatings includes cracks initiating and propagating along the oxide phases and pores. Cracks, pores and interfaces between "laminations" are "fast track" of oxygen diffusion within coatings, leading to high temperature oxidation occurred in the coating, and secondary cracks formed and propagated in the new sites of coatings. Pores in the coatings may hinder crack propagation. However, if the shape of pores was irregular, cracks would be activated and propagated along the large curvature of pore tip. On the other hand, oxygen penetrating to the combination interface of coatings and substrate caused oxidation during thermal shock test, leading to coating failure.
High temperature oxidation and hot corrosion contrast tests of arc-sprayed coatings have been studied. The results show that FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating have better oxidation resistance and hot corrosion resistance than that of 20 steel. FeMnCrAl/Cr3C2 coating possess the best oxidation resistance and hot corrosion resistance.
Erosion tests of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and 20 steel were performed in an erosion tester at different impact angles. Compared with that of 20 steel, FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating possess lower average erosive rate than that of 20 steel, and FeMnCrAl/Cr3C2 coating exhibiting the best erosion resistance under all impact angles. Erosion mechanisms of the coatings as follows:Failure mode at low impact angles is ploughing and cutting, accompanying with plastic deformation and brittle desquamation under secondary impacting. Failure mode at high impact angles is indenting, brittle cracks and desquamation, accompanying with fatigue cracking off and desquamation after excessive plastic deformation. Failure mode at intermediate impact angles is multi-transition status.
In order to improve wettability and binding between carbide and metal matrix crystalline phases, Ni-coated WC and Ni-coated Cr3C2 powder were prepared by ultrasonic-assisted electroless plating process without conventional sensitization and activation treatments at room temperature. WC and Cr3C2 powders were first pretreated by immersing into an aqueous solution of hydrofluoric acid (HF) and ammonium fluoride (NH4F). The Ni layers on the powders had cell structure with dense, uniform distribution. The nucleation. growth and aggregation mechanisms of Ni layers as follows:1) the reactants in the plating solution were adsorbed on catalytic activity surfaces of powders and happened oxidation-reduction reaction.2) The growth and aggregation mechanisms of Ni particles after nucleation are "stripy" Ni-cells grew up, bend, bifurcated, and aggregated through "linear" approach, then wounding into a "cellular" structure, like "wrapping wool clusters" in the life. Finally "cellular" structure Ni particles grew up and merged into a layer. Compared with that of FeMnCrAl/WC coating and FeMnCrAl/Cr3C2 coating, Ni coated WC and Cr3C2 powders improve the bond strength and cohesive strength of coatings. Hardness of FeMnCrAl/Ni-coated WC coating and FeMnCrAl/Ni-coated Cr3C2 coating are similar to those of FeMnCrAl/WC coating and FeMnCrAl/Cr3C2 coating. Ni coated WC powder improves the erosion wear resistance of FeMnCrAl/Ni-coated WC coating. Erosion mechanism of FeMnCrAl/Ni-coated WC coating is similar to that of FeMnCrAl/WC coating.
FeMnCrAl/carbide series coatings had been used to heat surfaces of water wall and the screen tubes as protective coatings.After more than six months to run, the tests results show that FeMnCrAl/carbide series coatings play very good protective effects. The coatings may be expected to use more than 2 years.
本论文首先采用高速电弧喷涂技术成功制备了FeMnCr/Cr3C2涂层、FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层。涂层呈典型的层状显微组织结构,由金属结晶相、氧化物相、未熔颗粒和孔隙组成。与FeMnCr/Cr3C2涂层相比,FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层具有明显较少的未熔颗粒、氧化物含量和孔隙,组织致密度更高,涂层与基体的界面结合状况更好。
本论文研究了FeMnCr/Cr3C2涂层、FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层的显微硬度、结合强度和内聚强度,并对拉伸断口形貌进行电镜分析。研究发现,FeMnCr/Cr3C2涂层和FeMnCrAl/Cr3C2涂层具有较高的显微硬度值,为20钢的2-3倍；FeMnCrAl/Cr3C2涂层和FeMnCrAl/Cr3C2-Ni9Al涂层结合强度较高,高于FeMnCr/Cr3C2涂层；FeMnCrAl/Cr3C2涂层的内聚强度高于其它对比涂层,达到174.5MPa；涂层的拉伸断口具有结晶相的准解理断裂、氧化物相的脆性断裂、“叠层”间分离脱开、未熔颗粒与“叠层”分离甚至被整体拔出等形貌特征。
通过抗热震性能试验发现：与FeMnCr/Cr3C2和FeNiCr/Cr3C2涂层相比,FeMnCrAl/Cr3C2-Ni9Al涂层抗热震性能最好,32次循环后仍然无脱落现象。涂层热震失效过程包括裂纹在氧化物区域和孔隙处的萌生和扩展；涂层中的孔洞会阻碍裂纹扩展,但是,如果孔洞形状不规则,则热震会使裂纹在孔洞的大曲率尖端处激活继续扩展,形成二次裂纹并扩展。裂纹是氧向涂层内扩散的“快速通道”,氧还会沿着孔洞、凝片间隙向内扩散,导致高温氧化在整个涂层中发生。当氧渗入到涂层与基体的结合界面时,造成界面氧化现象,涂层与基体的结合状态恶化,最终导致涂层脱落失效。
本文研究了FeMnCrAl/碳化物系涂层的高温氧化和热腐蚀性能,发现各涂层体系均具有良好的抗氧化性和耐热腐蚀性能,明显优于20钢,其中FeMnCrAl/Cr3C2涂层的抗腐蚀性能最好,约为20钢的1/10。
冲蚀磨损性能试验表明,FeMnCr/Cr3C2涂层和FeMnCrAl/Cr3C2涂层的冲蚀率都明显低于20钢基材,尤以FeMnCrAl/Cr3C2涂层的抗冲蚀磨损性能为最佳。涂层的冲蚀磨损机理为：低冲击角下以犁耕和切削作用为主,伴随着二次冲击的塑性变形和脆性脱落；高冲击角下发生表面材料挤压、脆性裂纹生成和脱落以及过度塑性变形后的疲劳开裂和脱落。
为改善陶瓷粉体在金属基涂层中浸润性和结合状态,本论文创新性地发明对WC和Cr3C2粉末进行化学镀Ni预处理的方法。该方法不需要贵金属敏化活化处理,预处理后的粉体可以保证后期镀Ni效果,镀层均匀。Ni颗粒的形核、长大和聚集的过程为：1)、化学镀溶液中的反应物在具有催化活性的表面缺陷上吸附,发生氧化-还原反应沉积出Ni颗粒。2)、Ni颗粒形核后长大成膜,其长大成膜过程为：Ni核依附“线条状”突起以“线型”方式长大、弯曲、分叉和聚集,而后缠绕成“胞状”结构,犹如生活中“缠毛线团”。“胞状”结构Ni颗粒不断长大聚集,最后成膜。与FeMnCrAl/WC涂层和FeMnCrAl/Cr3C2涂层相比,添加了Ni包覆陶瓷相的涂层结合强度和内聚强度平均值得到提高,其平均显微硬度值与原涂层相当。Ni包覆WC相改善了涂层抗冲蚀磨损性能,涂层的冲蚀机理基本相似。添加Ni包覆WC陶瓷相和Ni包覆Cr3C2陶瓷相的两种涂层的平均显微硬度值与未添加包覆陶瓷相的涂层相当。
FeMnCrAl/碳化物系涂层已经应用于水冷壁和屏过等部分受热面管道高温防腐和防磨中,经过半年多时间运行检测发现,防护效果非常理想,预计该涂层可以使用2年以上。
According to actual problems that there were serious erosion, corrosion and resulting in major economic losses caused on the boiler tubes (water wall,superheater, reheater, economizer tube) of coal-fired thermal power plants at home and abroad, low-cost FeMnCrAl/carbide series coatings have been studied to resolve the surface temperature corrosion and erosion problems using high velocity arc spraying process in this paper. In this study, low-cost FeMnCrAl/carbide series coatings were successfully prepared using Mn, Cr, Al, Cr3C2, Ni-coated WC, Ni-coated Cr3C2, etc cored wires together with high velocity arc spraying for surface protection of the boiler tubes. New arc-spraying materials with good cost-effective development of coal-fired boiler tubes were studied. This study content is an energy-saving protection issues, having great practical value and academic significance.
FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating were deposited on 20 steel substrates by the high velocity arc spraying. The coatings characteristically consisted of successive layers contained metal crystalline phases, oxide phases, un-melted particles and pores. Compared with that of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating significantly had less un-melted particles, oxide content and porosity, possessed good interfacial bonding and microstructure between coatings and substrate, no coarse pores and cracks.
Hardness, bond strength, cohesive strength and morphology of tensile fracture of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating have been studied. The results show that compared with that of 20 steel, FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating possess high average hardness,2-3 times than that of 20 steel. FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9Al coating exhibit higher bonding strength between coatings and substrate than that of FeMnCr/Cr3C2 coating. The average cohesive strength of FeMnCrAl/Cr3C2 coating is 174.5MPa, higher than that of FeMnCr/Cr3C2 coating.Characteristics of tensile fracture of coating are characteristics of quasi-cleavage fracture of metal crystalline phases and brittle fracture of oxide phases, characteristics of separation and disengagement of "laminations" and characteristics of un-melted particles integral putout.
Thermal shock resistances of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and FeMnCrAl/Cr3C2-Ni9A1 coating have been analyzed. Compared with that of FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating, FeMnCrAl/Cr3C2-Ni9Al coating possesses the best thermal shock resistance, being no exfoliation phenomenon after the number of thermal shock cycles 32. Failure mechanism of thermal shock of arc-sprayed coatings includes cracks initiating and propagating along the oxide phases and pores. Cracks, pores and interfaces between "laminations" are "fast track" of oxygen diffusion within coatings, leading to high temperature oxidation occurred in the coating, and secondary cracks formed and propagated in the new sites of coatings. Pores in the coatings may hinder crack propagation. However, if the shape of pores was irregular, cracks would be activated and propagated along the large curvature of pore tip. On the other hand, oxygen penetrating to the combination interface of coatings and substrate caused oxidation during thermal shock test, leading to coating failure.
High temperature oxidation and hot corrosion contrast tests of arc-sprayed coatings have been studied. The results show that FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating have better oxidation resistance and hot corrosion resistance than that of 20 steel. FeMnCrAl/Cr3C2 coating possess the best oxidation resistance and hot corrosion resistance.
Erosion tests of FeMnCr/Cr3C2 coating, FeMnCrAl/Cr3C2 coating and 20 steel were performed in an erosion tester at different impact angles. Compared with that of 20 steel, FeMnCr/Cr3C2 coating and FeMnCrAl/Cr3C2 coating possess lower average erosive rate than that of 20 steel, and FeMnCrAl/Cr3C2 coating exhibiting the best erosion resistance under all impact angles. Erosion mechanisms of the coatings as follows:Failure mode at low impact angles is ploughing and cutting, accompanying with plastic deformation and brittle desquamation under secondary impacting. Failure mode at high impact angles is indenting, brittle cracks and desquamation, accompanying with fatigue cracking off and desquamation after excessive plastic deformation. Failure mode at intermediate impact angles is multi-transition status.
In order to improve wettability and binding between carbide and metal matrix crystalline phases, Ni-coated WC and Ni-coated Cr3C2 powder were prepared by ultrasonic-assisted electroless plating process without conventional sensitization and activation treatments at room temperature. WC and Cr3C2 powders were first pretreated by immersing into an aqueous solution of hydrofluoric acid (HF) and ammonium fluoride (NH4F). The Ni layers on the powders had cell structure with dense, uniform distribution. The nucleation. growth and aggregation mechanisms of Ni layers as follows:1) the reactants in the plating solution were adsorbed on catalytic activity surfaces of powders and happened oxidation-reduction reaction.2) The growth and aggregation mechanisms of Ni particles after nucleation are "stripy" Ni-cells grew up, bend, bifurcated, and aggregated through "linear" approach, then wounding into a "cellular" structure, like "wrapping wool clusters" in the life. Finally "cellular" structure Ni particles grew up and merged into a layer. Compared with that of FeMnCrAl/WC coating and FeMnCrAl/Cr3C2 coating, Ni coated WC and Cr3C2 powders improve the bond strength and cohesive strength of coatings. Hardness of FeMnCrAl/Ni-coated WC coating and FeMnCrAl/Ni-coated Cr3C2 coating are similar to those of FeMnCrAl/WC coating and FeMnCrAl/Cr3C2 coating. Ni coated WC powder improves the erosion wear resistance of FeMnCrAl/Ni-coated WC coating. Erosion mechanism of FeMnCrAl/Ni-coated WC coating is similar to that of FeMnCrAl/WC coating.
FeMnCrAl/carbide series coatings had been used to heat surfaces of water wall and the screen tubes as protective coatings.After more than six months to run, the tests results show that FeMnCrAl/carbide series coatings play very good protective effects. The coatings may be expected to use more than 2 years.
引文
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