金属表面等离子电解沉积强化层制备及特性研究
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摘要
等离子体电解沉积是一类新颖而高效的表面处理技术,可在金属表面形成较厚的冶金结合强化层,因此,在金属表面强化与功能化改性方面具有广阔的应用前景。近些年来该技术得到了国内外材料研究领域的专家以及涉及金属产品表面强化与装饰的企业的广泛关注,发展很快。然而,在理论与工程技术等方面尚存许多问题需要研究解决。本文主要开展了以下几方面研究工作:1)铝表面等离子体电解氧化;2)铝表面等离子体电解氧化及其强化与刷镀;3)Q235钢表面间接等离子体电解氧化;4) Q235钢表面等离子体电解溶渗;5) W_9Mo_5Cr_4V_2高速钢ESD-PED复合表面改性。
在铝表面等离子体电解氧化方面系统研究了等离子体氧化过程中电学参量、陶瓷层的厚度、表面形貌特征、相组成等随时间的变化规律和微观机理,以及陶瓷层的耐磨耐蚀性能等。研究表明:等离子体电解氧化过程中处理液的组分也参与到反应当中,并成为陶瓷层的一部分;陶瓷层厚度主要与电流密度和处理时间有关,不同电流密度下存在不同的最佳处理时间,电流密度越小,最佳处理时间越短;陶瓷层内残留的放电通道尺寸随时间延长而增大,数目减少,并依此建立物理模型推导出放电通道处温度升高速率与工艺参数及材料常数的关系式。
在铝表面等离子体电解氧化及其强化与刷镀方面主要研究了几种添加剂,以及添加剂与超声波共同作用对陶瓷层的生长速度与性能的影响,提出并初步研究了刷镀等离子体电解氧化陶瓷层及其电绝缘特性。研究表明:电解液内添加重铬酸钾K_2Cr_2O_7后形成的陶瓷层很致密,有大理石质感,陶瓷层的成膜速率也有显著提高,而钨酸钠,氟化钾,硼砂和纳米氧化铝粉末等其它几种添加剂效果不明显,有的甚至产生负作用,如增大放电通道尺寸;超声波对等离子体电解氧化过程具有明显的促进作用,有效地提高了陶瓷层的生长速率、硬度、耐磨性与耐磨性;刷镀等离子体电解氧化具有不受电解槽的尺寸和电源功率限制,并且可以方便地对工件进行局部陶瓷化处理等优点;陶瓷层的击穿电压随陶瓷层厚度增加而升高,而击穿场强随厚度增加而下降。
在Q235钢复合等离子体电解氧化研究中分别开展了有关热浸镀铝层和经感应重熔的电弧喷铝层作为中介层进行等离子体电解氧化的模拟、试验与理论研究。研究表明,这两种复合强化技术均可在钢表面获得冶金结合的复合涂层,明显提高了钢表面耐蚀性和耐磨性。
在Q235钢等离子体电解溶渗研究中,系统研究了电解液、电压、处理时间、极间距等工艺规范的影响情况,研究表明:采用KCl-C_2H_5ONH_2电解液体系对Q255钢进行液相等离子体电解碳氮共渗处理,效果很显著,而采用KCl-HCONH_2 and KCl-CO(NH_2)2电解液体系未能获得明显有效的渗层或电解液发生快速分解失效。对采用KCl-C_2H_5ONH_2电解液体系进行液相等离子体电解碳氮共渗处理开展了系统研究工作,获得了一系列重要研究结果。
在W_9Mo_5Cr_4V_2高速钢PED-ESD复合表面改性研究中,以W_9Mo_5Cr_4V_2高速钢为基体,YG8硬质合金为电极,开展了工艺与组织性能试验研究工作。研究表明,新方法的成膜速率明显高于ESD技术,形成的金属陶瓷涂层耐磨性也明显优于ESD技术。
本文的主要创新点如下:在理论上,1)根据等离子体电解氧化陶瓷层表面形貌的进化过程建立物理模型,获得了放电通道温度升高速率公式,并据此计算了铝表面等离子体电解氧化放电通道瞬间温度;2)在现有感应重熔理论基础上,获得了对电弧喷涂层感应重熔过程具有指导意义的断面温度分布公式;3)在分析等离子体电解氧化机理基础上,提出击穿阻抗概念和诱发微缺陷促进等离子体电解氧化陶瓷层均匀化节能生长理论。在技术上,1)将热浸镀铝和热喷铝感应重熔作为预处理手段,成功地将等离子体电解氧化技术用于Q235钢表面陶瓷化处理;2)提出并研究极间相对运动等离子体电解氧化工艺,为大工件强化或局部强化提供条件;3)提出并采用超声波技术显著推动等离子体电解氧化过程;4)电解液中引入适量重铬酸钾显著提高了等离子体电解氧化陶瓷层的致密性和生长速度;5)提出并采用火花放电-等离子体电解复合技术在W_9Mo_5Cr_4V_2高速钢表面快速获得了高硬、耐磨金属陶瓷层。
Plasma electrolytic disposition (PED) is a kind of novel and effective surface engineering technique that can be used to prepare metallurgically bonded ceramic coatings on metals, so it possesses broad application prospects and has been given a wide attention by specialists in metal material researching field and enterprisers in metal product manufacturing field all over the world recent years, developing quickly. However, there are still plenty of projects to research no matter in theory and engineering technology. Main research aspects included in this dissertation are 1) Plasma electrolytic oxidation on aluminum surface; 2) Enhancement and brush plating of plasma electrolytic oxidation on aluminum surface; 3) Hybrid plasma electrolytic oxidation on Q235 steel surface; 4) Plasma electrolytic saturation on Q235 steel surface; 5) ESD-PED hybrid surface modification on W_9Mo_5Cr_4V_2 high speed steel.
In plasma electrolytic oxidation on aluminum surface, the evolution law and mechanism of electric parameters, coating thickness, surface micro-morphology, coating composition were investigated in order to understand the growth characteristics of PEO ceramic coatings. Wear and corrosion resistances were also evaluated. The results show that, species from the electrolyte also take part in the PEO process and can be one of elements making up the ceramic coatings; The thickness of the ceramic coatings is mainly dependent on PEO current density and treatment time, there are different optimum treatment times at different densities, and the lower the current density, the shorter the optimum time; The size of the remaining discharge channels in the coatings increases and population of the channels decreases with treatment time; A physical model was set up according to the evolution law above, and a formulation was derived from the physical model.
In the section on enhancement and brush plating of plasma electrolytic oxidation, effects of additives and ultrasonic wave on growth rate and properties of the ceramic coatings were investigated, and brush plating method of plasma electrolytic oxidation was proposed and electric isolation property of the ceramic coatings prepared with the new method was investigated. The results show that, density and growth rate of the ceramic coatings formed in the electrolyte with additive K_2Cr_2O_7 are improved very obviously, but Na_2WO_4, KF, Na_2B_4O_7, Al_2O_3 and some other additives did not play obvious positive roles, even played some negative roles, such as making discharge channels large; Ultrasonic wave has very obvious promotion influence on the plasma electrolytic oxidation process, so that the growth rate, hardness, wear resistance and corrosion resistance of the PEO coatings increase greatly under ultrasonic wave; The brush plating plasma electrolytic oxidation make the plasma electrolytic oxidation of large work-pieces not to be limited by size of the electrolyte tank and volume of the power supply; In addition, work-pieces can be treated partially with plasma electrolytic oxidation process; The breakdown voltage of the ceramic coatings prepared with brush plating plasma electrolytic oxidation increases with the thickness of the coatings, but breakdown strength of the coatings decreases with the thickness.
In the section on hybrid electrolytic oxidation on Q235 steel, hot-dipped aluminum coatings and arc sprayed aluminum coatings after inductively heated were prepared as medium coatings of the plasma electrolytic oxidation process, and relative simulation, experiment and theory researches were done. The results show that the plasma electrolytic oxidation process can be applied to prepare oxide ceramic coatings metallurgically bonded on Q235 steel substrates by means of hot dipping aluminum or arc spraying aluminum induction-heated before the PEO process; The coatings can increase significantly corrosion and wear resistances of the steel substrate surface.
In the section of plasma electrolytic saturation on Q235 steel, effects of some process factors such as electrolyte, voltage, treatment time, electrode distance on the process were investigated. The results show that, KCl-C_2H_5ONH_2 electrolyte is very effective to prepare ceramic coatings containing carbides and nitrides on Q235 steel with the plasma electrolytic saturation process, however, KCl-HCONH_2 and KCl-CO(NH_2)_2 electrolytes are not effective to do so. A series of excellent research results were obtained through some systematical investigations with KCl-C_2H_5ONH_2 electrolyte.
In the section of ESD-PED hybrid surface modification on W_9Mo_5Cr_4V_2 high speed steel, the microstructure and properties of the ceramic coatings prepared on the W_9Mo_5Cr_4V_2 substrate with the YG8 electrode rod and the hybrid surface modification process were investigated. The results show that the new process is much better than the ESD one in growth rate, wear resistance of the coatings.
Main new points in theory are as follows: 1) A physical model was set up and a formula was derived on temperature rising of discharge channels during plasma electrolytic oxidation process, and the instantaneous temperature of discharge channels in the plasma electrolytic oxidation coatings on aluminum was calculated; 2) Based on the previous induction re-melting theory, a temperature distribution formula was derived along the coating depth during the induction re-melting of the arc spraying aluminum coatings on steels; 3)A breakdown resistance concept and a theory on defect induction to promote energy saving growth and densification of plasma electrolytic oxidation coatings were proposed. Main new points in technology are as follows: 1) Hot dipping aluminum and arc spraying aluminum were used as pretreatment steps respectively and plasma electrolytic oxidation ceramic coatings were successfully formed on Q235 steel; 2)Plasma electrolytic oxidation process by relative movement between electrodes was proposed and some research work was carried out; 3)Ultrasonic wave vibration was adopted in the plasma electrolytic oxidation process, the process was driven notably; 4)K_2Cr_2O_7 added into the electrolyte played a rather great role in densification and growth rate of the plasma electrolytic oxidation coatings; 5)A ESD-PED process was proposed based on the idea for combining the advantages of both plasma electrolytic disposition (PED) and electric spark disposition (ESD), and a hard and wear resistant metal ceramic coating was formed on W_9Mo_5Cr_4V_2 high speed steel.
在铝表面等离子体电解氧化方面系统研究了等离子体氧化过程中电学参量、陶瓷层的厚度、表面形貌特征、相组成等随时间的变化规律和微观机理,以及陶瓷层的耐磨耐蚀性能等。研究表明:等离子体电解氧化过程中处理液的组分也参与到反应当中,并成为陶瓷层的一部分;陶瓷层厚度主要与电流密度和处理时间有关,不同电流密度下存在不同的最佳处理时间,电流密度越小,最佳处理时间越短;陶瓷层内残留的放电通道尺寸随时间延长而增大,数目减少,并依此建立物理模型推导出放电通道处温度升高速率与工艺参数及材料常数的关系式。
在铝表面等离子体电解氧化及其强化与刷镀方面主要研究了几种添加剂,以及添加剂与超声波共同作用对陶瓷层的生长速度与性能的影响,提出并初步研究了刷镀等离子体电解氧化陶瓷层及其电绝缘特性。研究表明:电解液内添加重铬酸钾K_2Cr_2O_7后形成的陶瓷层很致密,有大理石质感,陶瓷层的成膜速率也有显著提高,而钨酸钠,氟化钾,硼砂和纳米氧化铝粉末等其它几种添加剂效果不明显,有的甚至产生负作用,如增大放电通道尺寸;超声波对等离子体电解氧化过程具有明显的促进作用,有效地提高了陶瓷层的生长速率、硬度、耐磨性与耐磨性;刷镀等离子体电解氧化具有不受电解槽的尺寸和电源功率限制,并且可以方便地对工件进行局部陶瓷化处理等优点;陶瓷层的击穿电压随陶瓷层厚度增加而升高,而击穿场强随厚度增加而下降。
在Q235钢复合等离子体电解氧化研究中分别开展了有关热浸镀铝层和经感应重熔的电弧喷铝层作为中介层进行等离子体电解氧化的模拟、试验与理论研究。研究表明,这两种复合强化技术均可在钢表面获得冶金结合的复合涂层,明显提高了钢表面耐蚀性和耐磨性。
在Q235钢等离子体电解溶渗研究中,系统研究了电解液、电压、处理时间、极间距等工艺规范的影响情况,研究表明:采用KCl-C_2H_5ONH_2电解液体系对Q255钢进行液相等离子体电解碳氮共渗处理,效果很显著,而采用KCl-HCONH_2 and KCl-CO(NH_2)2电解液体系未能获得明显有效的渗层或电解液发生快速分解失效。对采用KCl-C_2H_5ONH_2电解液体系进行液相等离子体电解碳氮共渗处理开展了系统研究工作,获得了一系列重要研究结果。
在W_9Mo_5Cr_4V_2高速钢PED-ESD复合表面改性研究中,以W_9Mo_5Cr_4V_2高速钢为基体,YG8硬质合金为电极,开展了工艺与组织性能试验研究工作。研究表明,新方法的成膜速率明显高于ESD技术,形成的金属陶瓷涂层耐磨性也明显优于ESD技术。
本文的主要创新点如下:在理论上,1)根据等离子体电解氧化陶瓷层表面形貌的进化过程建立物理模型,获得了放电通道温度升高速率公式,并据此计算了铝表面等离子体电解氧化放电通道瞬间温度;2)在现有感应重熔理论基础上,获得了对电弧喷涂层感应重熔过程具有指导意义的断面温度分布公式;3)在分析等离子体电解氧化机理基础上,提出击穿阻抗概念和诱发微缺陷促进等离子体电解氧化陶瓷层均匀化节能生长理论。在技术上,1)将热浸镀铝和热喷铝感应重熔作为预处理手段,成功地将等离子体电解氧化技术用于Q235钢表面陶瓷化处理;2)提出并研究极间相对运动等离子体电解氧化工艺,为大工件强化或局部强化提供条件;3)提出并采用超声波技术显著推动等离子体电解氧化过程;4)电解液中引入适量重铬酸钾显著提高了等离子体电解氧化陶瓷层的致密性和生长速度;5)提出并采用火花放电-等离子体电解复合技术在W_9Mo_5Cr_4V_2高速钢表面快速获得了高硬、耐磨金属陶瓷层。
Plasma electrolytic disposition (PED) is a kind of novel and effective surface engineering technique that can be used to prepare metallurgically bonded ceramic coatings on metals, so it possesses broad application prospects and has been given a wide attention by specialists in metal material researching field and enterprisers in metal product manufacturing field all over the world recent years, developing quickly. However, there are still plenty of projects to research no matter in theory and engineering technology. Main research aspects included in this dissertation are 1) Plasma electrolytic oxidation on aluminum surface; 2) Enhancement and brush plating of plasma electrolytic oxidation on aluminum surface; 3) Hybrid plasma electrolytic oxidation on Q235 steel surface; 4) Plasma electrolytic saturation on Q235 steel surface; 5) ESD-PED hybrid surface modification on W_9Mo_5Cr_4V_2 high speed steel.
In plasma electrolytic oxidation on aluminum surface, the evolution law and mechanism of electric parameters, coating thickness, surface micro-morphology, coating composition were investigated in order to understand the growth characteristics of PEO ceramic coatings. Wear and corrosion resistances were also evaluated. The results show that, species from the electrolyte also take part in the PEO process and can be one of elements making up the ceramic coatings; The thickness of the ceramic coatings is mainly dependent on PEO current density and treatment time, there are different optimum treatment times at different densities, and the lower the current density, the shorter the optimum time; The size of the remaining discharge channels in the coatings increases and population of the channels decreases with treatment time; A physical model was set up according to the evolution law above, and a formulation was derived from the physical model.
In the section on enhancement and brush plating of plasma electrolytic oxidation, effects of additives and ultrasonic wave on growth rate and properties of the ceramic coatings were investigated, and brush plating method of plasma electrolytic oxidation was proposed and electric isolation property of the ceramic coatings prepared with the new method was investigated. The results show that, density and growth rate of the ceramic coatings formed in the electrolyte with additive K_2Cr_2O_7 are improved very obviously, but Na_2WO_4, KF, Na_2B_4O_7, Al_2O_3 and some other additives did not play obvious positive roles, even played some negative roles, such as making discharge channels large; Ultrasonic wave has very obvious promotion influence on the plasma electrolytic oxidation process, so that the growth rate, hardness, wear resistance and corrosion resistance of the PEO coatings increase greatly under ultrasonic wave; The brush plating plasma electrolytic oxidation make the plasma electrolytic oxidation of large work-pieces not to be limited by size of the electrolyte tank and volume of the power supply; In addition, work-pieces can be treated partially with plasma electrolytic oxidation process; The breakdown voltage of the ceramic coatings prepared with brush plating plasma electrolytic oxidation increases with the thickness of the coatings, but breakdown strength of the coatings decreases with the thickness.
In the section on hybrid electrolytic oxidation on Q235 steel, hot-dipped aluminum coatings and arc sprayed aluminum coatings after inductively heated were prepared as medium coatings of the plasma electrolytic oxidation process, and relative simulation, experiment and theory researches were done. The results show that the plasma electrolytic oxidation process can be applied to prepare oxide ceramic coatings metallurgically bonded on Q235 steel substrates by means of hot dipping aluminum or arc spraying aluminum induction-heated before the PEO process; The coatings can increase significantly corrosion and wear resistances of the steel substrate surface.
In the section of plasma electrolytic saturation on Q235 steel, effects of some process factors such as electrolyte, voltage, treatment time, electrode distance on the process were investigated. The results show that, KCl-C_2H_5ONH_2 electrolyte is very effective to prepare ceramic coatings containing carbides and nitrides on Q235 steel with the plasma electrolytic saturation process, however, KCl-HCONH_2 and KCl-CO(NH_2)_2 electrolytes are not effective to do so. A series of excellent research results were obtained through some systematical investigations with KCl-C_2H_5ONH_2 electrolyte.
In the section of ESD-PED hybrid surface modification on W_9Mo_5Cr_4V_2 high speed steel, the microstructure and properties of the ceramic coatings prepared on the W_9Mo_5Cr_4V_2 substrate with the YG8 electrode rod and the hybrid surface modification process were investigated. The results show that the new process is much better than the ESD one in growth rate, wear resistance of the coatings.
Main new points in theory are as follows: 1) A physical model was set up and a formula was derived on temperature rising of discharge channels during plasma electrolytic oxidation process, and the instantaneous temperature of discharge channels in the plasma electrolytic oxidation coatings on aluminum was calculated; 2) Based on the previous induction re-melting theory, a temperature distribution formula was derived along the coating depth during the induction re-melting of the arc spraying aluminum coatings on steels; 3)A breakdown resistance concept and a theory on defect induction to promote energy saving growth and densification of plasma electrolytic oxidation coatings were proposed. Main new points in technology are as follows: 1) Hot dipping aluminum and arc spraying aluminum were used as pretreatment steps respectively and plasma electrolytic oxidation ceramic coatings were successfully formed on Q235 steel; 2)Plasma electrolytic oxidation process by relative movement between electrodes was proposed and some research work was carried out; 3)Ultrasonic wave vibration was adopted in the plasma electrolytic oxidation process, the process was driven notably; 4)K_2Cr_2O_7 added into the electrolyte played a rather great role in densification and growth rate of the plasma electrolytic oxidation coatings; 5)A ESD-PED process was proposed based on the idea for combining the advantages of both plasma electrolytic disposition (PED) and electric spark disposition (ESD), and a hard and wear resistant metal ceramic coating was formed on W_9Mo_5Cr_4V_2 high speed steel.
引文
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