合金化镀锌板镀层抗粉化性能及相关工艺研究
摘要
钢铁材料工业上应用广泛,但在使用过程中,接触到大气、液态水、土壤及特种介质,会发生不同程度的腐蚀。为了防止钢铁材料腐蚀,常常采用涂镀保护层的方法将钢铁与其它腐蚀介质隔离开来。锌的最重要的应用是钢铁的防腐蚀,主要是以涂层的形式,因为涂锌的钢在自然环境中有出色的耐蚀性。最早采用电镀的方法,但电镀方法具有成本高,有逐渐为热镀锌取代的趋势。热镀锌是将金属产品浸入熔融锌液中从而获得锌镀层。
锌是比铁更为活泼的一种金属元素,更容易被氧化腐蚀。锌在干燥的空气中不起变化。但在潮湿空气的腐蚀环境中,锌的表面会生成一层致密的耐腐蚀的碳酸锌薄膜,它能保护锌内部不再受到腐蚀,从而延长材料使用寿命。
锌铁合金层电极电位(-0.59V--0.66V)介于铁和纯锌之间,所以电化学腐蚀速度比纯锌慢。锌铁合金通过在热浸镀后退火处理,镀层发生合金化形成多种合金相得到。另外,锌铁合金层具有更好的焊接性及涂装性,所以逐渐得到越来越广泛的应用。但其在冲压成型时,常常会出现粉化及脱落问题。镀层粉化及脱落降低镀层的耐蚀性能,影响涂装后的外观,而且因剥落的锌粉粘附于模具上,并在模具中积聚,影响模具的使用寿命。因此,提高合金化镀锌板镀层的抗粉化性能,一直是国内外镀锌学者的研究热点。而合金化镀锌板镀层的抗粉化性能,与镀层的相结构密切相关。
为了研究合金化镀锌板镀层的相结构,以提高某钢厂现有产品抗粉化及剥落性能,进行了系统的比较及模拟研究,主要工作及结论如下：
1)首次运用动态拉伸观察合金化镀锌板镀层在持续拉伸状态下的断裂演变过程。并通过扫描电镜及能谱仪分析,发现镀层和基板的剥离发生在基板/r相界面。r相断口呈锯齿状,约数百个纳米厚度。镀层厚度上主要为6相。
2)通过对镀层抗粉化性及附着力的分析,发现某钢厂早期生产的合金化热镀锌钢板(主要是DX54D+ZF)镀层的抗粉化性能不稳定,部分产品的粉化量偏大。通过辉光光谱分析发现,原因是合金化钢板镀层中r相的含量较其它几种合金化钢板中的r相的含量要多。用扫描电镜观对比观察了不同合金化镀层的表面形貌,发现DX54D+ZF镀层表面的相结构是比较单一柱状锌铁合金相,并且镀层表面较脆,未见明显光整压痕,镀层内部在变形前已经产成了大量的合金化预裂纹。在此分析基础上提出了改进方法。
3)通过对DX54D+ZF在不同温度、不同合金化时间下进行模拟合金化退火实验,并采用光学显微镜、扫描电镜、辉光光谱仪及XRD等方法揭示了DX54D+ZF抗粉化及剥落性能与相关工艺参数的对应规律：合金化温度在450℃时,在比较长的时间范围内,粉化量都比较小；合金化温度在500℃时,合金化温度在120s以内,粉化量随合金化时间的变化也不大；合金化温度超过550℃时,在极短的时间内,镀层的粉化量急剧增加。
4)通过对DX56D+ZF在不同温度、不同合金化时间下进行模拟合金化退火实验采用光学显微镜、扫描电镜、辉光光谱仪及XRD等方法揭示了DX56D+ZF抗粉化及剥落性能与相关工艺参数的对应规律：在480℃左右合金化时,镀层粉化量很小,且随合金化时间的延长,镀层粉化量变化很小；在480℃合金化且时间不超过25s时,Zn/Fe界面A1元素富集明显,有利于抑制脆性相的形成,镀层抗粉化性能较好,当合金化温度更高,合金化时间更长时,镀层中开始出现脆性相,并不断增厚,镀层抗粉化性能逐渐下降。
5)通过对H180BD+ZF在不同温度、不同合金化时间下进行模拟合金化退火实验采用光学显微镜、扫描电镜、辉光光谱仪及XRD等方法揭示了H180BD+ZF抗粉化及剥落性能与相关工艺参数的对应规律：合金化时间小于25s时,450℃、480℃合金化镀层的抗粉化性能均较好,较低温度450℃时效果更佳；大于25s时,480℃合金化镀层粉化量急剧增加；而450℃合金化镀层粉化量略有下降,当合金化时间超过30s时,镀层粉化量才开始较缓慢地增加；合金化温度为510℃及540℃时,即使合金化时间极短,粉化量也较大,且随合金化时间的延续,粉化量急剧增加。
6)不同镀锌板在合金化刚开始时A1元素均富集于镀层／基体界面,随着合金化时间的延长,A1元素逐渐向镀层表面扩散,最终均匀分布于镀层中。且合金化温度越高,这一过程越显著。
7)合金化温度越高,表面形貌变化也越显著,但当合金化完成后,增加合金化时间,表面形貌变化不明显。
The steel is used widely in industry, but it would be corroded often in some degree when it meets air, water, soil and other especial substance. In order to avoid corrosion, the steel is aften plated with protective layer to be insulated with corrosive substance. The most important use of Zinc is to mitigate corrosion by coating mainly, because it has excellent corrosion resisting property in nature environment. Electic plating method is used early, but the cost is very high and the hot galvanizing is replacing it gradually. Hot galvanizing is a method acquiring coating by immersing steel in the melting metal.
Zinc is a more active element than Fe which could be oxidated more easily. Zinc is unconveted in dry air. But in moist air its surface would generate dense zinc carbonate film which could protect internal zinc from corrosion sequentially prolong steel service life.
Electrode voltage of Zn-Fe alloy coating (-0.59V～-0.66V) is between the Zinc and Fe, so the corrosion rate of Zn-Fe alloy coating is more slowly than pure zinc. Galvannealed coatings are produced by a continuous hot dipping process followed by an in-line annealing cycle, during which alloying takes place and the different Fe-Zn phases are formed.Inadditon, it has excellent spot weldability and paintability,so Zn-Fe alloy coating is widely used gradually. But powdering and flaking of the coating often happen when the steel band is punched. Powdering and flaking make the coating's corrosion resisting property and appearance after painting worse and zinc powder hich comes from powdering and flaking adheres to the die would affect its life. So how to improve the powdering resisting property of coating is the research hotspot all along for galvannealed coating. The powdering resisting property of coating is correlative with the phase structure of galvannealed coating.
In order to research the phase structure of galvannealed coatings made by some steel plant and improve its powdering and flaking resisting property, systemic research are made as follows:
1) The fracture evolution of galvannealed coating is observed by dynamic tensility experiment in-situ SEM observation for the first time. It is thought that flaking takes place at the interface of substrate/Γ phase by SEM and EDX analysis. The Fracture of Γ phase is serrated and its thickness is hundreds of nano-metres.δphase is main in the coating.
2) The powdering resisting property of coatings and adhesive power is analysed and it is found that the performance of early galvannealed coating of galvannealed steel sheet(mainly DX54D+ZF) made in some steel plant is instable, the quantity of powdering is a little more than other products.It is found by Glow Discharge Spectrometer that Γ phase in the coating of DX54D+ZF is more than in other products coating.The surface topography of DX54D+ZF is simple columnar Zn-Fe Alloy phases in SEM and its surface is more brittle than others,no indentation by skin rolling could be found, there are many early cracks before deforming.Improved methods are brought forward.
3)Simulation annealing experiments are made to DX54D+ZF at different annealing temperatures and different annealing times and the powdering resisting property of coatings with different processing parameters is discovered by OM, SEM,GDS and XRD:The quantity of powdering is little in a long annealing time at the temperature of450℃. The quantity of powdering dose not change within120s at the temperature of500℃.The quantity of powdering increases quickly in a short time at the temperature of550℃.
4) Annealing experiments for simulating DX56D+ZF production are made at different annealing temperature and different annealing time and the powdering resisting property of coatings with different processing parameters is discovered by OM, SEM,GDS and XRD:The quantity of powdering is little for a long annealing time at the temperature of480℃. If the annealing time is no more than25s, Al is aggregate at the interface of coating/substrate and it is advantageous to inhibit brittle phase forming. When the annealing temperature is higher and the annealing time is longer, the brittle phases appears and its thickness become more and more thick, the powdering resisting property of coatings is descending.
5) Annealing experiments for simulating H180BD+ZF production are made at different annealing temperature and different annealing time and the powdering resisting property of coatings with different processing parameters is discovered by OM, SEM,GDS and XRD:The quantity of powdering is little for a less annealing time than20s at the temperature of450℃or480℃and the effect is better at the temperature of450℃. The quantity of powdering increases quickly when the annealing time is more than25s at the temperature of480℃, but at the same annealing time the quantity of powdering is descending a little at the temperature450℃and the quantity of powdering is increased slowly until the annealing time more than30s. The powdering resisting property of coatings increases fast at the temperature of510℃or540℃,even in a short annealing time.
6) In the beginning of annealing, Al enrichs interface of coating/substrate for all coatings of galvannealed steel sheets. With the time prolonged, Al diffuses to the surface of coating continuously and it would evenly distributed to the whole coating in the end.The process is more notable when the annealing temperature is higher.
7)The surface appearance of coatings would change remarkably when the annealing temperature is higher, but when the galvannealed coatings has formed, the surface appearance of coating would not change remarkably if the annealing time is increased.
锌是比铁更为活泼的一种金属元素,更容易被氧化腐蚀。锌在干燥的空气中不起变化。但在潮湿空气的腐蚀环境中,锌的表面会生成一层致密的耐腐蚀的碳酸锌薄膜,它能保护锌内部不再受到腐蚀,从而延长材料使用寿命。
锌铁合金层电极电位(-0.59V--0.66V)介于铁和纯锌之间,所以电化学腐蚀速度比纯锌慢。锌铁合金通过在热浸镀后退火处理,镀层发生合金化形成多种合金相得到。另外,锌铁合金层具有更好的焊接性及涂装性,所以逐渐得到越来越广泛的应用。但其在冲压成型时,常常会出现粉化及脱落问题。镀层粉化及脱落降低镀层的耐蚀性能,影响涂装后的外观,而且因剥落的锌粉粘附于模具上,并在模具中积聚,影响模具的使用寿命。因此,提高合金化镀锌板镀层的抗粉化性能,一直是国内外镀锌学者的研究热点。而合金化镀锌板镀层的抗粉化性能,与镀层的相结构密切相关。
为了研究合金化镀锌板镀层的相结构,以提高某钢厂现有产品抗粉化及剥落性能,进行了系统的比较及模拟研究,主要工作及结论如下：
1)首次运用动态拉伸观察合金化镀锌板镀层在持续拉伸状态下的断裂演变过程。并通过扫描电镜及能谱仪分析,发现镀层和基板的剥离发生在基板/r相界面。r相断口呈锯齿状,约数百个纳米厚度。镀层厚度上主要为6相。
2)通过对镀层抗粉化性及附着力的分析,发现某钢厂早期生产的合金化热镀锌钢板(主要是DX54D+ZF)镀层的抗粉化性能不稳定,部分产品的粉化量偏大。通过辉光光谱分析发现,原因是合金化钢板镀层中r相的含量较其它几种合金化钢板中的r相的含量要多。用扫描电镜观对比观察了不同合金化镀层的表面形貌,发现DX54D+ZF镀层表面的相结构是比较单一柱状锌铁合金相,并且镀层表面较脆,未见明显光整压痕,镀层内部在变形前已经产成了大量的合金化预裂纹。在此分析基础上提出了改进方法。
3)通过对DX54D+ZF在不同温度、不同合金化时间下进行模拟合金化退火实验,并采用光学显微镜、扫描电镜、辉光光谱仪及XRD等方法揭示了DX54D+ZF抗粉化及剥落性能与相关工艺参数的对应规律：合金化温度在450℃时,在比较长的时间范围内,粉化量都比较小；合金化温度在500℃时,合金化温度在120s以内,粉化量随合金化时间的变化也不大；合金化温度超过550℃时,在极短的时间内,镀层的粉化量急剧增加。
4)通过对DX56D+ZF在不同温度、不同合金化时间下进行模拟合金化退火实验采用光学显微镜、扫描电镜、辉光光谱仪及XRD等方法揭示了DX56D+ZF抗粉化及剥落性能与相关工艺参数的对应规律：在480℃左右合金化时,镀层粉化量很小,且随合金化时间的延长,镀层粉化量变化很小；在480℃合金化且时间不超过25s时,Zn/Fe界面A1元素富集明显,有利于抑制脆性相的形成,镀层抗粉化性能较好,当合金化温度更高,合金化时间更长时,镀层中开始出现脆性相,并不断增厚,镀层抗粉化性能逐渐下降。
5)通过对H180BD+ZF在不同温度、不同合金化时间下进行模拟合金化退火实验采用光学显微镜、扫描电镜、辉光光谱仪及XRD等方法揭示了H180BD+ZF抗粉化及剥落性能与相关工艺参数的对应规律：合金化时间小于25s时,450℃、480℃合金化镀层的抗粉化性能均较好,较低温度450℃时效果更佳；大于25s时,480℃合金化镀层粉化量急剧增加；而450℃合金化镀层粉化量略有下降,当合金化时间超过30s时,镀层粉化量才开始较缓慢地增加；合金化温度为510℃及540℃时,即使合金化时间极短,粉化量也较大,且随合金化时间的延续,粉化量急剧增加。
6)不同镀锌板在合金化刚开始时A1元素均富集于镀层／基体界面,随着合金化时间的延长,A1元素逐渐向镀层表面扩散,最终均匀分布于镀层中。且合金化温度越高,这一过程越显著。
7)合金化温度越高,表面形貌变化也越显著,但当合金化完成后,增加合金化时间,表面形貌变化不明显。
The steel is used widely in industry, but it would be corroded often in some degree when it meets air, water, soil and other especial substance. In order to avoid corrosion, the steel is aften plated with protective layer to be insulated with corrosive substance. The most important use of Zinc is to mitigate corrosion by coating mainly, because it has excellent corrosion resisting property in nature environment. Electic plating method is used early, but the cost is very high and the hot galvanizing is replacing it gradually. Hot galvanizing is a method acquiring coating by immersing steel in the melting metal.
Zinc is a more active element than Fe which could be oxidated more easily. Zinc is unconveted in dry air. But in moist air its surface would generate dense zinc carbonate film which could protect internal zinc from corrosion sequentially prolong steel service life.
Electrode voltage of Zn-Fe alloy coating (-0.59V～-0.66V) is between the Zinc and Fe, so the corrosion rate of Zn-Fe alloy coating is more slowly than pure zinc. Galvannealed coatings are produced by a continuous hot dipping process followed by an in-line annealing cycle, during which alloying takes place and the different Fe-Zn phases are formed.Inadditon, it has excellent spot weldability and paintability,so Zn-Fe alloy coating is widely used gradually. But powdering and flaking of the coating often happen when the steel band is punched. Powdering and flaking make the coating's corrosion resisting property and appearance after painting worse and zinc powder hich comes from powdering and flaking adheres to the die would affect its life. So how to improve the powdering resisting property of coating is the research hotspot all along for galvannealed coating. The powdering resisting property of coating is correlative with the phase structure of galvannealed coating.
In order to research the phase structure of galvannealed coatings made by some steel plant and improve its powdering and flaking resisting property, systemic research are made as follows:
1) The fracture evolution of galvannealed coating is observed by dynamic tensility experiment in-situ SEM observation for the first time. It is thought that flaking takes place at the interface of substrate/Γ phase by SEM and EDX analysis. The Fracture of Γ phase is serrated and its thickness is hundreds of nano-metres.δphase is main in the coating.
2) The powdering resisting property of coatings and adhesive power is analysed and it is found that the performance of early galvannealed coating of galvannealed steel sheet(mainly DX54D+ZF) made in some steel plant is instable, the quantity of powdering is a little more than other products.It is found by Glow Discharge Spectrometer that Γ phase in the coating of DX54D+ZF is more than in other products coating.The surface topography of DX54D+ZF is simple columnar Zn-Fe Alloy phases in SEM and its surface is more brittle than others,no indentation by skin rolling could be found, there are many early cracks before deforming.Improved methods are brought forward.
3)Simulation annealing experiments are made to DX54D+ZF at different annealing temperatures and different annealing times and the powdering resisting property of coatings with different processing parameters is discovered by OM, SEM,GDS and XRD:The quantity of powdering is little in a long annealing time at the temperature of450℃. The quantity of powdering dose not change within120s at the temperature of500℃.The quantity of powdering increases quickly in a short time at the temperature of550℃.
4) Annealing experiments for simulating DX56D+ZF production are made at different annealing temperature and different annealing time and the powdering resisting property of coatings with different processing parameters is discovered by OM, SEM,GDS and XRD:The quantity of powdering is little for a long annealing time at the temperature of480℃. If the annealing time is no more than25s, Al is aggregate at the interface of coating/substrate and it is advantageous to inhibit brittle phase forming. When the annealing temperature is higher and the annealing time is longer, the brittle phases appears and its thickness become more and more thick, the powdering resisting property of coatings is descending.
5) Annealing experiments for simulating H180BD+ZF production are made at different annealing temperature and different annealing time and the powdering resisting property of coatings with different processing parameters is discovered by OM, SEM,GDS and XRD:The quantity of powdering is little for a less annealing time than20s at the temperature of450℃or480℃and the effect is better at the temperature of450℃. The quantity of powdering increases quickly when the annealing time is more than25s at the temperature of480℃, but at the same annealing time the quantity of powdering is descending a little at the temperature450℃and the quantity of powdering is increased slowly until the annealing time more than30s. The powdering resisting property of coatings increases fast at the temperature of510℃or540℃,even in a short annealing time.
6) In the beginning of annealing, Al enrichs interface of coating/substrate for all coatings of galvannealed steel sheets. With the time prolonged, Al diffuses to the surface of coating continuously and it would evenly distributed to the whole coating in the end.The process is more notable when the annealing temperature is higher.
7)The surface appearance of coatings would change remarkably when the annealing temperature is higher, but when the galvannealed coatings has formed, the surface appearance of coating would not change remarkably if the annealing time is increased.
引文
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