高效连铸结晶器铜材表面涂层制备、性能表征及其机理研究
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摘要
钢铁行业在国民经济中占有举足轻重的作用,在该领域里,连铸工艺因流程短效率高的特点被广泛应用,其生产效率和可靠性直接决定钢铁冶金的质量和产量。结晶器是连铸机的关键部件,运用于结晶器中的铜合金内套质量和使用寿命直接影响着铸坯的质量、产量和生产效率。由于结晶器内套长期与钢液直接接触,服役条件苛刻,导致其成为水平连铸生产线上关键的易耗件,随着钢铁冶金的需求逐年递增,结晶器内套的使用量和报废量也逐年增加,每年国内冶金行业铜结晶器的消耗在20亿元以上。因此,选择合理高效的表面处理技术,对结晶器铜合金内套材料进行表面改性,提高其耐高温钢液侵蚀、高温摩擦磨损等性能,不仅可以提高铜合金内套的使用寿命保证生产可靠性,还能降低生产成本,节约资源,满足国民经济的可持续发展。
本文选择了耐蚀、耐疲劳、导热性良好的CuCo2Be合金作为结晶器内套的基体材料,并对其进行热处理；合理设计了多涂层结构,选用高温耐磨的Cr3C2-NiCr作为工作层,NiAl为打底层,来提高界面结合强度,以及过渡工作层与基体材料热膨胀系数差异；运用等离子喷涂技术,在基体试样表面分别制备了厚度大于0.3mm的Cr3C2-NiCr涂层、NiAl打底层、Cr3C2-NiCr/NiAl复合涂层。通过试验,优化了三种涂层的喷涂参数,运用SEM、EDS、XRD等系统分析研究了三种涂层的组成、显微结构、形貌、界面行为及成形机理；并对最佳工艺参数下制备的三种涂层进行高温热震试验,研究对比了Cr3C2-NiCr/NiAl复合涂层与Cr3C2-NiCr涂层冷热疲劳寿命的差异及涂层的失效机理；并通过摩擦磨损试验研究了涂层摩擦磨损性能与喷涂工艺参数之间的变化规律,以及涂层在不同温度下摩擦磨损失效机理。研究并建立了涂层的组织、性能、成形机理与喷涂工艺之间的关系规律,以期确定最佳的喷涂工艺制备高性能使用寿命长的涂层,本试验研究结果将对结晶器用铜材的表面改性及后续的服役条件控制提供科学依据。
通过研究得出如下结论：优化后的三种涂层的喷涂工艺为：Cr3C2-NiCr涂层喷涂工艺及因素影响规律：功率(20kw)>送粉速率(18g.min-1)>主气流量(58L·min-1)>喷涂距离(95mm),在此条件制备的涂层结合强度为：43MPa; NiAl涂层喷涂工艺及因素影响规律：功率(20kw)>喷涂距离(90mm)>送粉速率(25g·min-1)>主气流量(61L.min1)。在此工艺条件下制备的NiAl涂层的结合强度为：48MPa；Cr3C2-NiCr/NiAl复合涂层喷涂工艺及因素影响规律：功率(22kw)>喷涂距离(100mm)>主气流量(64L·mm1)>送粉速率30·min-1)。在此条件下制备的复合涂层的结合强度为：47MPa。通过DTA验证了NiAl复合粉末在600℃C至671.8℃发生两次放热反应,结合XRD分析得知在此温度涂层中生成了AlNi3、Al3Ni2、AINi相。通过SEM分析可知三种涂层界面结合紧密,涂层致密呈现连续层状分布,工作层中有Cr23C6,Cr7C3,Cr3C2硬质相,打底层中有角状镍铝化合物；XRD分析了三种涂层不同层深处的物相表明：Cr3C2-NiCr涂层主要由Cr23C6, Cr7C3, Cr3C2, NiCr非晶相组成；NiAl涂层外表面主要由镍、铝单相组成,接近界面处检测到Cu3Al2、Cu0.81Ni0.19、Al1.1Ni0.9等化合物相。Cr3C2-NiCr/NiAl工作层与打底层界面处生成了AlCr2, Cr3Ni2,在接近界面0.05mm处存在Al2Cu、Cu0.81Ni0.19、Al1.1Ni0.9等相,结合EDS分析可知三种涂层与基体的结合以机械锚合为主,而在打底层与基体、工作层与打底层之间存在一定的元素扩散形成了微冶金结合。
选择500℃、550℃、600℃、650℃对最佳工艺参数下制备的Cr3C2-NiCr/NiAl复合涂层、Cr3C2-NiCr涂层进行抗热震性能试验。500℃时,复合涂层完全失效的次数为235次,单一工作层平均119次,说明通过合理的涂层结构设计有效过渡了工作层与基体之间体积膨胀的差异,使得应力的分布更加平缓,提高了涂层的抗热震性能。在550-650℃温度范围内进行热震实验,复合涂层完全失效的次数从120次突然变少至1-2次,单一工作层完全失效的次数从83次突然变少至1-2次,这说明随着温度升高至600℃以后,涂层的抗热震性能迅速变弱。通过SEM、XRD、EDS分析表明失效的主要机制是涂层及界面存在空隙、缩松,易吸入大量氧发生氧化,以及打底层与工作层之间存在热应力,这些因素共同作用导致涂层脱落。在500℃对最佳工艺参数下制备的NiAl打底涂层进行抗热震性能试验,发现Ni/Al涂层在冷热循环350次后涂层未开裂,说明NiAl涂层在500℃时具有非常良好的抗热震性能。对Cr3C2-NiCr/NiAl复合涂层进行摩擦磨损试验,确立了喷涂工艺与涂层摩擦磨损性能之间的关系。研究结果表明：室温时,其摩擦磨损机制为以磨粒磨损为主,粘着摩擦、刮擦摩擦为辅；高温时,磨损机制为粘着磨损。在不同温度下,由于摩擦磨损机制不同,摩擦系数的变化出现不同情况。常温时,摩擦副还没有进入摩擦副磨合区,摩擦系数是比较高的,而且不稳定,当进入磨合区之后,摩擦系数降低而且比较稳定。涂层高温摩擦磨损试验时由于摩擦副很快磨合,很快进入粘着摩擦区,摩擦系数上升到一定程度便稳定在一定数值,说明基体的耐摩擦磨损的性能低于涂层。
The iron and steel industry played an important role in national economy. Because of its short process and high efficiency, the continuous casting process was widely used in steel metallurgy. Quality and output of the iron and steel metallurgy depended on the efficiency and reliability of continuous casting. Crystallizer was the key component of continuous caster. Copper alloy was used in crystallizer's inner sleeve, its quality and service life directly affected the quality, yield and production efficiency of continuous casting. Due to the crystallizer's inner sleeve directly contacting liquid steel for a long time and tough serving conditions, Crystallizer became a key consumable in the process line of horizontal continuous casting. With the increasing demand of iron and steel metallurgy, amount of scrap crystallizer inner sleeve also increasing year by year, the domestic annual consumption of copper crystallizer was more than2billion Yuan in metallurgical industry. So the surface treatment technology and the modified material of crystallizer's inner sleeve copper alloy were important. Improving inner sleeve's copper alloy performance of erosion resistance on high temperature liquid steel, friction and wear resistance, it not only could improve the service life of crystallizer that ensure the production reliability, also could reduce the cost of production, save resources that meet the needs of national economy sustainable development.
CuCo2Be alloy was chose as the base material of crystallizer inner sleeve in this paper, because it had good thermal conductivity, corrosion resistance and fatigue resistance. Then it was set heat treatment. The multilayer structure of coating was designed reasonable. Cr3C2-NiCr was used as working layer because of its good performance of high temperature wear resistance. NiAl was used as bonding layer, it not only can improve the interface bonding strength, but also reduce the thermal expansion difference about transition layer and the substrate material; Plasma spraying technology was used to prepare Cr3C2-NiCr coating, NiAl bonding coating and Cr3C2-NiCr/NiAl multilayer coating on the sample surface respectively, the thickness of those coating was more than0.3mm.Through a series of spray test, three kinds spraying parameters of coatings was optimized. Using SEM, EDS, XRD and other means, we studied three kinds of coating's microstructure, morphology, interfacial behavior, the element and the forming mechanism. And then, the three kinds of coating prepared by optimum parameters was tes under high temperature thermal shock, the differences of cold and hot fatigue life and failure mechanism of the coating were studied and compared between Cr3C2-NiCr/NiAl composite coating and Cr3d-NiCr coating at high temperature. And through friction and wear test, the change rule between coating wear performance and spraying process parameters were studied, and the wear failure mechanism of coating was also studied under different temperature. The relationship between spraying process and organization, performance, forming mechanism of the coating, was studied and established, in order to determine the best preparation of high performance and long working life spraying coating, the test results will provide a scientific basis for improving the crystallization used copper surface and subsequent production use.
The following conclusions were drawn through studing:the optimized spraying process parameters of three coating:the spraying process parameters and influence law of Cr3C2-NiCr coating:Power (kw)20> feeding rate (18g·min-1)> main gas flow (58L·min-1)> spraying distance (95mm), bond strength of Cr3C2-NiCr coatings under preparation for this condition:43Mpa; The spraying process parameters and influence law of NiAl coating: Power (20kw)> spraying distance (90mm)> feeding rate (25g·min-1)>main gas flow (61L·min-1), bond strength of NiAl coatings under preparation for this condition:48MPa; The spraying process parameters and influence law of Cr3C2-NiCr/NiAl composite coating: Power (22kw)>spraying distance (100mm)> main gas flow (64L·min-1)> feeding rate (30g·min-1). bond strength of the composite coatings under preparation for this condition:47MPa; Two exothermic reaction of NiAl composite powder were verified by means of DTA in600℃to671.8℃, it was proved that coating generated AlNi3, Al3N12, AlNi phase in this temperature range by means of XRD. Through SEM it was analysed three coating interface combined closely, coating present continuous layer, there were undeformed Cr23C6, Cr7C3, Cr3C2hard phase in working layer, there was angular nickel aluminum compound in bonding layer; through XRD analysis of the phase of three different kinds of coating layer in the depth, it was showed that:Cr3C2-NiCr coating was mainly composed of Cr23C6, Cr7C3, Cr3C2, NiCr amorphous phase composition; External surface of the NiAl coating was mainly composed of nickel, aluminum single phase, Cu3Al2, Cu0.81Ni0.19, Al1.1Ni0.9compounds such as phase were detected at close to interface. The interface of Cr3C2-NiCr/NiAl working layer and bottom layer generated AlCr2, Cr3Ni2, there were Al2Cu, Cu0.81Ni0.19, Al1.1Ni0.9phase near the interface about0.05mm, EDS analysis showed the substrate bonding three kinds of coating and matrix was the machinery anchor-based bonding, between bottom layer and base, coating and bottom layer, metallurgical bonding was formed because of element diffusion.
Cr3C2-NiCr/NiAl composite coating, Cr3C2-NiCr coating prepared by optimum process parameters was chose to be carried out the thermal shock experiment in500℃,550℃,600℃,650℃.When500℃, the composite coating complete failure times was235, single working layer times was average119. It can be concluded that through the reasonable structure design of the coating, the difference of volume expansion between working layer and matrix was effectively buffered, the stress distribution was more litter, the thermal shock resistance of the coating was improved. Thermal shock test was carried out in550-650℃complete failure times of composite coating suddenly from120times to1-2times, the complete failure number of single working layer suddenly from83times to1-2times, it showed that as the temperature up to600℃, thermal shock resistance of the coating declined rapidly. Through SEM, XRD, EDS analysis it was concluded that the main failure mechanism was coating and interface had gap and shrinkage, they were easy inhalation of much oxygen and oxidizing, and the existence of thermal stress between bottom layer and working layer, all of these factors together caused coating peeling. NiAl bottom coating prepared by optimum process parameters was choosed to be carried out the thermal shock experiment in500℃, it was found that Ni/Al coating was not cracking after hot-cold cycle350times, we can conclude NiAl coating had very good thermal shock resistance. To establish the relationship between the friction and wear performance and coating spraying process, Cr3C2-NiCr/NiAl composite coating was carried out friction and wear test. Results showed:when room temperature, the friction and wear mechanism was mainly abrasive wear, adhesive friction and scratches friction were complementary, and the high temperature, wear mechanism was adhesive wear. Because the friction and wear mechanism was different at the different temperature, the coefficient of friction of changes would occur. At the room temperature, friction pair had not yet entered the friction pair in area, the friction coefficient was relatively high and unstable, After entering in pair area, coefficient was reduced and relatively stable.When high temperature friction and wear test was going on, the friction pair entered the friction pair in area soon and fast entered into the sticky friction area, and then friction coefficient was up to a certain degree of stability, so it was showed friction and wear resistance of matrix was lower than the coating.
本文选择了耐蚀、耐疲劳、导热性良好的CuCo2Be合金作为结晶器内套的基体材料,并对其进行热处理；合理设计了多涂层结构,选用高温耐磨的Cr3C2-NiCr作为工作层,NiAl为打底层,来提高界面结合强度,以及过渡工作层与基体材料热膨胀系数差异；运用等离子喷涂技术,在基体试样表面分别制备了厚度大于0.3mm的Cr3C2-NiCr涂层、NiAl打底层、Cr3C2-NiCr/NiAl复合涂层。通过试验,优化了三种涂层的喷涂参数,运用SEM、EDS、XRD等系统分析研究了三种涂层的组成、显微结构、形貌、界面行为及成形机理；并对最佳工艺参数下制备的三种涂层进行高温热震试验,研究对比了Cr3C2-NiCr/NiAl复合涂层与Cr3C2-NiCr涂层冷热疲劳寿命的差异及涂层的失效机理；并通过摩擦磨损试验研究了涂层摩擦磨损性能与喷涂工艺参数之间的变化规律,以及涂层在不同温度下摩擦磨损失效机理。研究并建立了涂层的组织、性能、成形机理与喷涂工艺之间的关系规律,以期确定最佳的喷涂工艺制备高性能使用寿命长的涂层,本试验研究结果将对结晶器用铜材的表面改性及后续的服役条件控制提供科学依据。
通过研究得出如下结论：优化后的三种涂层的喷涂工艺为：Cr3C2-NiCr涂层喷涂工艺及因素影响规律：功率(20kw)>送粉速率(18g.min-1)>主气流量(58L·min-1)>喷涂距离(95mm),在此条件制备的涂层结合强度为：43MPa; NiAl涂层喷涂工艺及因素影响规律：功率(20kw)>喷涂距离(90mm)>送粉速率(25g·min-1)>主气流量(61L.min1)。在此工艺条件下制备的NiAl涂层的结合强度为：48MPa；Cr3C2-NiCr/NiAl复合涂层喷涂工艺及因素影响规律：功率(22kw)>喷涂距离(100mm)>主气流量(64L·mm1)>送粉速率30·min-1)。在此条件下制备的复合涂层的结合强度为：47MPa。通过DTA验证了NiAl复合粉末在600℃C至671.8℃发生两次放热反应,结合XRD分析得知在此温度涂层中生成了AlNi3、Al3Ni2、AINi相。通过SEM分析可知三种涂层界面结合紧密,涂层致密呈现连续层状分布,工作层中有Cr23C6,Cr7C3,Cr3C2硬质相,打底层中有角状镍铝化合物；XRD分析了三种涂层不同层深处的物相表明：Cr3C2-NiCr涂层主要由Cr23C6, Cr7C3, Cr3C2, NiCr非晶相组成；NiAl涂层外表面主要由镍、铝单相组成,接近界面处检测到Cu3Al2、Cu0.81Ni0.19、Al1.1Ni0.9等化合物相。Cr3C2-NiCr/NiAl工作层与打底层界面处生成了AlCr2, Cr3Ni2,在接近界面0.05mm处存在Al2Cu、Cu0.81Ni0.19、Al1.1Ni0.9等相,结合EDS分析可知三种涂层与基体的结合以机械锚合为主,而在打底层与基体、工作层与打底层之间存在一定的元素扩散形成了微冶金结合。
选择500℃、550℃、600℃、650℃对最佳工艺参数下制备的Cr3C2-NiCr/NiAl复合涂层、Cr3C2-NiCr涂层进行抗热震性能试验。500℃时,复合涂层完全失效的次数为235次,单一工作层平均119次,说明通过合理的涂层结构设计有效过渡了工作层与基体之间体积膨胀的差异,使得应力的分布更加平缓,提高了涂层的抗热震性能。在550-650℃温度范围内进行热震实验,复合涂层完全失效的次数从120次突然变少至1-2次,单一工作层完全失效的次数从83次突然变少至1-2次,这说明随着温度升高至600℃以后,涂层的抗热震性能迅速变弱。通过SEM、XRD、EDS分析表明失效的主要机制是涂层及界面存在空隙、缩松,易吸入大量氧发生氧化,以及打底层与工作层之间存在热应力,这些因素共同作用导致涂层脱落。在500℃对最佳工艺参数下制备的NiAl打底涂层进行抗热震性能试验,发现Ni/Al涂层在冷热循环350次后涂层未开裂,说明NiAl涂层在500℃时具有非常良好的抗热震性能。对Cr3C2-NiCr/NiAl复合涂层进行摩擦磨损试验,确立了喷涂工艺与涂层摩擦磨损性能之间的关系。研究结果表明：室温时,其摩擦磨损机制为以磨粒磨损为主,粘着摩擦、刮擦摩擦为辅；高温时,磨损机制为粘着磨损。在不同温度下,由于摩擦磨损机制不同,摩擦系数的变化出现不同情况。常温时,摩擦副还没有进入摩擦副磨合区,摩擦系数是比较高的,而且不稳定,当进入磨合区之后,摩擦系数降低而且比较稳定。涂层高温摩擦磨损试验时由于摩擦副很快磨合,很快进入粘着摩擦区,摩擦系数上升到一定程度便稳定在一定数值,说明基体的耐摩擦磨损的性能低于涂层。
The iron and steel industry played an important role in national economy. Because of its short process and high efficiency, the continuous casting process was widely used in steel metallurgy. Quality and output of the iron and steel metallurgy depended on the efficiency and reliability of continuous casting. Crystallizer was the key component of continuous caster. Copper alloy was used in crystallizer's inner sleeve, its quality and service life directly affected the quality, yield and production efficiency of continuous casting. Due to the crystallizer's inner sleeve directly contacting liquid steel for a long time and tough serving conditions, Crystallizer became a key consumable in the process line of horizontal continuous casting. With the increasing demand of iron and steel metallurgy, amount of scrap crystallizer inner sleeve also increasing year by year, the domestic annual consumption of copper crystallizer was more than2billion Yuan in metallurgical industry. So the surface treatment technology and the modified material of crystallizer's inner sleeve copper alloy were important. Improving inner sleeve's copper alloy performance of erosion resistance on high temperature liquid steel, friction and wear resistance, it not only could improve the service life of crystallizer that ensure the production reliability, also could reduce the cost of production, save resources that meet the needs of national economy sustainable development.
CuCo2Be alloy was chose as the base material of crystallizer inner sleeve in this paper, because it had good thermal conductivity, corrosion resistance and fatigue resistance. Then it was set heat treatment. The multilayer structure of coating was designed reasonable. Cr3C2-NiCr was used as working layer because of its good performance of high temperature wear resistance. NiAl was used as bonding layer, it not only can improve the interface bonding strength, but also reduce the thermal expansion difference about transition layer and the substrate material; Plasma spraying technology was used to prepare Cr3C2-NiCr coating, NiAl bonding coating and Cr3C2-NiCr/NiAl multilayer coating on the sample surface respectively, the thickness of those coating was more than0.3mm.Through a series of spray test, three kinds spraying parameters of coatings was optimized. Using SEM, EDS, XRD and other means, we studied three kinds of coating's microstructure, morphology, interfacial behavior, the element and the forming mechanism. And then, the three kinds of coating prepared by optimum parameters was tes under high temperature thermal shock, the differences of cold and hot fatigue life and failure mechanism of the coating were studied and compared between Cr3C2-NiCr/NiAl composite coating and Cr3d-NiCr coating at high temperature. And through friction and wear test, the change rule between coating wear performance and spraying process parameters were studied, and the wear failure mechanism of coating was also studied under different temperature. The relationship between spraying process and organization, performance, forming mechanism of the coating, was studied and established, in order to determine the best preparation of high performance and long working life spraying coating, the test results will provide a scientific basis for improving the crystallization used copper surface and subsequent production use.
The following conclusions were drawn through studing:the optimized spraying process parameters of three coating:the spraying process parameters and influence law of Cr3C2-NiCr coating:Power (kw)20> feeding rate (18g·min-1)> main gas flow (58L·min-1)> spraying distance (95mm), bond strength of Cr3C2-NiCr coatings under preparation for this condition:43Mpa; The spraying process parameters and influence law of NiAl coating: Power (20kw)> spraying distance (90mm)> feeding rate (25g·min-1)>main gas flow (61L·min-1), bond strength of NiAl coatings under preparation for this condition:48MPa; The spraying process parameters and influence law of Cr3C2-NiCr/NiAl composite coating: Power (22kw)>spraying distance (100mm)> main gas flow (64L·min-1)> feeding rate (30g·min-1). bond strength of the composite coatings under preparation for this condition:47MPa; Two exothermic reaction of NiAl composite powder were verified by means of DTA in600℃to671.8℃, it was proved that coating generated AlNi3, Al3N12, AlNi phase in this temperature range by means of XRD. Through SEM it was analysed three coating interface combined closely, coating present continuous layer, there were undeformed Cr23C6, Cr7C3, Cr3C2hard phase in working layer, there was angular nickel aluminum compound in bonding layer; through XRD analysis of the phase of three different kinds of coating layer in the depth, it was showed that:Cr3C2-NiCr coating was mainly composed of Cr23C6, Cr7C3, Cr3C2, NiCr amorphous phase composition; External surface of the NiAl coating was mainly composed of nickel, aluminum single phase, Cu3Al2, Cu0.81Ni0.19, Al1.1Ni0.9compounds such as phase were detected at close to interface. The interface of Cr3C2-NiCr/NiAl working layer and bottom layer generated AlCr2, Cr3Ni2, there were Al2Cu, Cu0.81Ni0.19, Al1.1Ni0.9phase near the interface about0.05mm, EDS analysis showed the substrate bonding three kinds of coating and matrix was the machinery anchor-based bonding, between bottom layer and base, coating and bottom layer, metallurgical bonding was formed because of element diffusion.
Cr3C2-NiCr/NiAl composite coating, Cr3C2-NiCr coating prepared by optimum process parameters was chose to be carried out the thermal shock experiment in500℃,550℃,600℃,650℃.When500℃, the composite coating complete failure times was235, single working layer times was average119. It can be concluded that through the reasonable structure design of the coating, the difference of volume expansion between working layer and matrix was effectively buffered, the stress distribution was more litter, the thermal shock resistance of the coating was improved. Thermal shock test was carried out in550-650℃complete failure times of composite coating suddenly from120times to1-2times, the complete failure number of single working layer suddenly from83times to1-2times, it showed that as the temperature up to600℃, thermal shock resistance of the coating declined rapidly. Through SEM, XRD, EDS analysis it was concluded that the main failure mechanism was coating and interface had gap and shrinkage, they were easy inhalation of much oxygen and oxidizing, and the existence of thermal stress between bottom layer and working layer, all of these factors together caused coating peeling. NiAl bottom coating prepared by optimum process parameters was choosed to be carried out the thermal shock experiment in500℃, it was found that Ni/Al coating was not cracking after hot-cold cycle350times, we can conclude NiAl coating had very good thermal shock resistance. To establish the relationship between the friction and wear performance and coating spraying process, Cr3C2-NiCr/NiAl composite coating was carried out friction and wear test. Results showed:when room temperature, the friction and wear mechanism was mainly abrasive wear, adhesive friction and scratches friction were complementary, and the high temperature, wear mechanism was adhesive wear. Because the friction and wear mechanism was different at the different temperature, the coefficient of friction of changes would occur. At the room temperature, friction pair had not yet entered the friction pair in area, the friction coefficient was relatively high and unstable, After entering in pair area, coefficient was reduced and relatively stable.When high temperature friction and wear test was going on, the friction pair entered the friction pair in area soon and fast entered into the sticky friction area, and then friction coefficient was up to a certain degree of stability, so it was showed friction and wear resistance of matrix was lower than the coating.
引文
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