Ti-60合金表面电弧离子镀Ti-Al-Cr高温防护涂层研究
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摘要
Ti-60属于Ti-Al-Zr-Mo-Si-Sn系近α型高温钛合金,使用温度已经达到600℃。但是,在高温使用时Ti-60合金的氧化和氧脆成为影响其热稳定性的主要因素,一方面表层氧化形成多孔的TiO_2膜,保护性能差;另一方面由于Ti与O的亲和性,氧渗透到基体中形成富氧层使合金塑性明显下降,这两个因素限制了Ti-60合金在高温下的应用。在高温下使用钛合金的困难在于必须提高抗氧化性能并满足对力学性能的要求。能提高某种性能的措施通常会降低另外一种性能。由于氧化破坏主要限于零件的外层或表层区域,而力学性能是由零件的整个截面决定的,因此同时获得最佳力学性能和抗氧化性能的一种有希望的方法是采用表面改性技术,特别是涂层技术。
本文主要研究了两方面的内容:一方面是Ti-60合金的氧化;另一方面对电弧离子镀技术制备Ti-Al-Cr型高温防护涂层的组织结构、高温抗氧化性能、高温抗腐蚀性能、热冲击性能、涂层与基体之间的相互作用等方面进行了深入的研究。
研究结果表明,Ti-60合金在650℃和750℃遵循晶粒尺寸正效应原则,即晶粒尺寸越小,氧化速率越小。Ti-60合金在600℃时的氧化增质较少,700℃时略高,800℃时发生失稳氧化。
电弧离子镀方法沉积的沉积态涂层呈明显的层状生长,涂层的XRD衍射峰出现明显的宽化。真空退火后的涂层内部明显的层状结构消失,涂层内部结合的更加致密,XRD衍射峰明显变窄。退火后Ti-48Al(原子分数,%)涂层由γ-TiAl相和少量的Ti_3Al相、TiAl_3相组成;而Ti-48Al-12Cr(原子分数,%)涂层退火后则由γ-TiAl相、Laves相、Ti_3Al相和TiAl_3相组成,TiAl_3相的含量高于Ti-48Al涂层。
在800℃等温氧化及循环氧化过程中,Ti-48Al和Ti-48Al-12Cr涂层样品表面氧化层保持完整,未发生剥落。两种涂层在800℃均能有效地保护Ti-60合金且与基体之间的结合力良好。在900℃氧化过程中,Ti-48Al涂层样品发生严重的剥落,不能有效地保护Ti-60合金,而Ti-48Al-12Cr涂层的表面生成大量的Al_2O_3,可以有效地保护Ti-60合金,说明12%Cr的加入可以有效的提高涂层的抗氧化性能。
采用电弧离子镀制备的Ti-Al-Cr-(Si,Y)涂层在800℃和850℃的硫酸盐腐蚀介质中,可以有效地保护Ti-60合金免受腐蚀破坏。Ti-Al-Cr-Si和Ti-Al-Cr-Si-Y涂层在硫酸盐中抗热腐蚀性能优于Ti-Al-Cr涂层,原因在于Y元素促进涂层表面Al_2O_3的生成,使涂层表面生成的Al_2O_3的量大于其在硫酸盐中的溶解量,延长了带涂层材料的热腐蚀孕育期;Si和Y元素还能细化氧化物颗粒,使氧化层致密,SO_4~(2-)和O元素通过致密的氧化层扩散比较困难,从而很好地保护了合金基材,改善了Ti-Al-Cr涂层体系的抗热腐蚀性能。此外,Ti-60合金及Ti-Al-Cr-(Si,Y)涂层在75%Na_2SO_4+25%K_2SO_4中的腐蚀比在纯硫酸钠中剧烈。
热冲击实验中,900℃和950℃实验温度下,电弧离子镀沉积的Ti-48Al-12Cr涂层表现出良好的抗热冲击性能,分别经过80个和30个周期的热冲击的实验后,涂层并没有发生明显的剥落;而Ti-48Al-5Cr涂层在900℃和950℃两种温度的热冲击下,氧化层和涂层发生了大量的剥落,产生了失重的现象。这是由于5%Cr元素的加入增加了Ti-48Al涂层中TiO_2中氧离子空位浓度,使原子扩散系数增大,提高了生成TiO_2的速率,使生成的氧化层较厚,易发生剥落。而12%Cr的加入从热力学和动力学上促进了保护性Al_2O_3氧化膜的形成,并且生成的Al_2O_3薄膜较薄,提高了带涂层材料的抗热冲击性能。此外,热冲击实验加速了氧化膜的剥落和破坏,因此也加速了内氧化的发生和裂纹的扩展。
Ti-60与Ti-Al-Cr涂层之间的扩散实验表明扩散层的厚度与时间和温度两个因素相关,其中与温度的关系最为密切。在800℃、850℃和900℃,Ti-60与Ti-48Al-12Cr涂层之间的扩散层的生长是由扩散控制的,大致遵循抛物线规律。Ti-60与Ti-48Al-12Cr涂层之间扩散层的生长激活能为113.71kJ/mol。
Ti-60 alloy is a near-αhigh temperature titanium alloy belonging to Ti-Al-Zr-Mo-Si-Sn system.It can be used stably up to 600℃.However,when Ti-60 was used at high temperatures,oxidation and oxygen brittleness were the main reasons that affected heat stability of Ti-60 alloys.On the one hand,surface oxidation formed porous TiO_2 which had no protection;on the other hand,for titanium alloy had a good affinity towards oxygen at elevated temperatures in air,thereby oxygen penetrated into titanium alloys and formed oxygen-enriched layer which decreased the alloy's plasticity obviously. Thoese two factors severely limited the application of Ti-60 at high temperatures.Measures to improve one property often leaded to degradation of the other.Since oxidation attack was mainly limited to the outer region of a component,and mechanical properties were determined by the entire cross-section,hence,a promising approach to obtain both the best mechanical property and oxidation resistance was the use of surface modification technologies,particularly coating techniques.
This thesis mainly concerns on two aspects,one is the oxidation behavior of Ti-60,and the other aspect,high temperature properties,hot corrosion behaviors,thermal shock cycling behaviors of the Ti-Al-Cr coatings deposited by arc ion plating(AIP) and interaction between coatings and Ti-60 base alloy were also investigated.
The results showed that Ti-60 alloys followed positive effect rules of grain size at 650℃and 750℃,i.e.the smaller a grain size was,the lower oxidation rate was.The weight increased smallest for the Ti-60 alloy exposed at 600℃,slightly heavy at 700℃,and at 800℃destabilizing oxidation occurred.
The as-deposited coatings prepared in AIP grew in layer and the peak of XRD diffraction pattern was obviously widened.After vacuum annealing,the layered microstructure disappeared and the inner of coatings became much denser.The peak of XRD diffraction patterns became narrow.Annealed Ti-48Al(atomic fraction,%) coatings were composed ofγphase,Ti_3Al phase and TiAl_3 phase;the amount of Ti_3Al phase and TiAl_3 phase were small.Annealed Ti-48Al-12Cr(atomic fraction,%) coatings were composed ofγphase,Laves phase,Ti_3Al phase and TiAl_3 phase;the amount of TiAl_3 phase was larger than that in Ti-48Al coatings.
The oxide layer of Ti-48Al coatings and Ti-48Al-12Cr coatings remained intact and no spalling occurred in the process of isothermal oxidation and cycling oxidation at 800℃. Both of the two coatings could protect Ti-60 alloys effectively and keep a good binding force with matrixes at 800℃.In the process of oxidation at 900℃,Ti-48Al coatings spalled seriously,which could not protect Ti-60 matrix.While Ti-48Al-12Cr coatings formed lots of Al_2O_3 which could protect Ti-60 matrix effectively.This demonstrated that the addition of 12%Cr element could improve oxidation resistance of coatings effectively.
Ti-Al-Cr-(Si,Y) coatings prepared in AIP could keep Ti-60 matrix from corrosion effectively in sulfate at 800℃and 850℃.Ti-Al-Cr-Si and Ti-Al-Cr-Si-Y coatings had better hot corrosion resistance than Ti-Al-Cr coatings in sulfate due to Y element could promote Al_2O_3 to form on the surface of the coatings;this could form more Al_2O_3 on the surface of coatings than that dissolved in sulfate,extend the hot corrosion incubation period of coatings.Si and Y elements could also make oxidation particles thinner which made the oxide layer denser and thus SO_4~(2-) and O diffused through the dense oxide layer difficultly. Therefore,the Ti-Al-Cr-Si and Ti-Al-Cr-Si-Y coatings could protect Ti-60 matrix effectively and improve the hot corrosion resistance of Ti-Al-Cr coatings.In addition to that, Ti-60 alloys and Ti-Al-Cr(Si,Y) coatings experienced more serious corrosion in 75% Na_2SO_4+25%K_2SO_4(weight fraction,%) than in pure Na_2SO_4.
The AIP Ti-48Al-12Cr coatings provided excellent thermal shock protection on Ti-60 alloys at 900℃and 950℃.No obvious coatings spallings were found after 900℃/80 cycles and 950℃/30 cycles.While a large amount of coatings and oxidation layers were found to spall when Ti-48Al-5Cr coatings were thermal shocked at 900℃and 950℃,hence induced weight change curve descended.As 5%Cr was added into Ti-48Al coatings,it increased vacancies of oxygen in TiO_2;enhanced the atomic diffusion coefficient;promoted the growing rate of forming of TiO_2;oxide layers thicker and spalling occurred easily.12%Cr elements promoted the formation of Al_2O_3 oxidation layers in thermodynamics and kinetics points.Al_2O_3 was very thin and dense improved the thermal shock resistance of Ti-60 with coatings.Besides,thermal shock cycling experiments accelerated the oxides spalling and breakdown thereby they accelerated internal oxidation,crack forming and crack propagation.
Diffusion experience between Ti-60 and Ti-48Al-12Cr coatings showed the relationship between the thicknesses of diffusion layers with time and temperatures, especially with temperatures.At 800℃,850℃and 900℃,the growth of diffusion layer between Ti-60 and Ti-48Al-12Cr coatings was controlled by diffusion,which followed parabolic rule.Growth activation energy of the diffusion layers between Ti-60 and Ti-48Al-12Cr coating was 113.71kJ/mol.
本文主要研究了两方面的内容:一方面是Ti-60合金的氧化;另一方面对电弧离子镀技术制备Ti-Al-Cr型高温防护涂层的组织结构、高温抗氧化性能、高温抗腐蚀性能、热冲击性能、涂层与基体之间的相互作用等方面进行了深入的研究。
研究结果表明,Ti-60合金在650℃和750℃遵循晶粒尺寸正效应原则,即晶粒尺寸越小,氧化速率越小。Ti-60合金在600℃时的氧化增质较少,700℃时略高,800℃时发生失稳氧化。
电弧离子镀方法沉积的沉积态涂层呈明显的层状生长,涂层的XRD衍射峰出现明显的宽化。真空退火后的涂层内部明显的层状结构消失,涂层内部结合的更加致密,XRD衍射峰明显变窄。退火后Ti-48Al(原子分数,%)涂层由γ-TiAl相和少量的Ti_3Al相、TiAl_3相组成;而Ti-48Al-12Cr(原子分数,%)涂层退火后则由γ-TiAl相、Laves相、Ti_3Al相和TiAl_3相组成,TiAl_3相的含量高于Ti-48Al涂层。
在800℃等温氧化及循环氧化过程中,Ti-48Al和Ti-48Al-12Cr涂层样品表面氧化层保持完整,未发生剥落。两种涂层在800℃均能有效地保护Ti-60合金且与基体之间的结合力良好。在900℃氧化过程中,Ti-48Al涂层样品发生严重的剥落,不能有效地保护Ti-60合金,而Ti-48Al-12Cr涂层的表面生成大量的Al_2O_3,可以有效地保护Ti-60合金,说明12%Cr的加入可以有效的提高涂层的抗氧化性能。
采用电弧离子镀制备的Ti-Al-Cr-(Si,Y)涂层在800℃和850℃的硫酸盐腐蚀介质中,可以有效地保护Ti-60合金免受腐蚀破坏。Ti-Al-Cr-Si和Ti-Al-Cr-Si-Y涂层在硫酸盐中抗热腐蚀性能优于Ti-Al-Cr涂层,原因在于Y元素促进涂层表面Al_2O_3的生成,使涂层表面生成的Al_2O_3的量大于其在硫酸盐中的溶解量,延长了带涂层材料的热腐蚀孕育期;Si和Y元素还能细化氧化物颗粒,使氧化层致密,SO_4~(2-)和O元素通过致密的氧化层扩散比较困难,从而很好地保护了合金基材,改善了Ti-Al-Cr涂层体系的抗热腐蚀性能。此外,Ti-60合金及Ti-Al-Cr-(Si,Y)涂层在75%Na_2SO_4+25%K_2SO_4中的腐蚀比在纯硫酸钠中剧烈。
热冲击实验中,900℃和950℃实验温度下,电弧离子镀沉积的Ti-48Al-12Cr涂层表现出良好的抗热冲击性能,分别经过80个和30个周期的热冲击的实验后,涂层并没有发生明显的剥落;而Ti-48Al-5Cr涂层在900℃和950℃两种温度的热冲击下,氧化层和涂层发生了大量的剥落,产生了失重的现象。这是由于5%Cr元素的加入增加了Ti-48Al涂层中TiO_2中氧离子空位浓度,使原子扩散系数增大,提高了生成TiO_2的速率,使生成的氧化层较厚,易发生剥落。而12%Cr的加入从热力学和动力学上促进了保护性Al_2O_3氧化膜的形成,并且生成的Al_2O_3薄膜较薄,提高了带涂层材料的抗热冲击性能。此外,热冲击实验加速了氧化膜的剥落和破坏,因此也加速了内氧化的发生和裂纹的扩展。
Ti-60与Ti-Al-Cr涂层之间的扩散实验表明扩散层的厚度与时间和温度两个因素相关,其中与温度的关系最为密切。在800℃、850℃和900℃,Ti-60与Ti-48Al-12Cr涂层之间的扩散层的生长是由扩散控制的,大致遵循抛物线规律。Ti-60与Ti-48Al-12Cr涂层之间扩散层的生长激活能为113.71kJ/mol。
Ti-60 alloy is a near-αhigh temperature titanium alloy belonging to Ti-Al-Zr-Mo-Si-Sn system.It can be used stably up to 600℃.However,when Ti-60 was used at high temperatures,oxidation and oxygen brittleness were the main reasons that affected heat stability of Ti-60 alloys.On the one hand,surface oxidation formed porous TiO_2 which had no protection;on the other hand,for titanium alloy had a good affinity towards oxygen at elevated temperatures in air,thereby oxygen penetrated into titanium alloys and formed oxygen-enriched layer which decreased the alloy's plasticity obviously. Thoese two factors severely limited the application of Ti-60 at high temperatures.Measures to improve one property often leaded to degradation of the other.Since oxidation attack was mainly limited to the outer region of a component,and mechanical properties were determined by the entire cross-section,hence,a promising approach to obtain both the best mechanical property and oxidation resistance was the use of surface modification technologies,particularly coating techniques.
This thesis mainly concerns on two aspects,one is the oxidation behavior of Ti-60,and the other aspect,high temperature properties,hot corrosion behaviors,thermal shock cycling behaviors of the Ti-Al-Cr coatings deposited by arc ion plating(AIP) and interaction between coatings and Ti-60 base alloy were also investigated.
The results showed that Ti-60 alloys followed positive effect rules of grain size at 650℃and 750℃,i.e.the smaller a grain size was,the lower oxidation rate was.The weight increased smallest for the Ti-60 alloy exposed at 600℃,slightly heavy at 700℃,and at 800℃destabilizing oxidation occurred.
The as-deposited coatings prepared in AIP grew in layer and the peak of XRD diffraction pattern was obviously widened.After vacuum annealing,the layered microstructure disappeared and the inner of coatings became much denser.The peak of XRD diffraction patterns became narrow.Annealed Ti-48Al(atomic fraction,%) coatings were composed ofγphase,Ti_3Al phase and TiAl_3 phase;the amount of Ti_3Al phase and TiAl_3 phase were small.Annealed Ti-48Al-12Cr(atomic fraction,%) coatings were composed ofγphase,Laves phase,Ti_3Al phase and TiAl_3 phase;the amount of TiAl_3 phase was larger than that in Ti-48Al coatings.
The oxide layer of Ti-48Al coatings and Ti-48Al-12Cr coatings remained intact and no spalling occurred in the process of isothermal oxidation and cycling oxidation at 800℃. Both of the two coatings could protect Ti-60 alloys effectively and keep a good binding force with matrixes at 800℃.In the process of oxidation at 900℃,Ti-48Al coatings spalled seriously,which could not protect Ti-60 matrix.While Ti-48Al-12Cr coatings formed lots of Al_2O_3 which could protect Ti-60 matrix effectively.This demonstrated that the addition of 12%Cr element could improve oxidation resistance of coatings effectively.
Ti-Al-Cr-(Si,Y) coatings prepared in AIP could keep Ti-60 matrix from corrosion effectively in sulfate at 800℃and 850℃.Ti-Al-Cr-Si and Ti-Al-Cr-Si-Y coatings had better hot corrosion resistance than Ti-Al-Cr coatings in sulfate due to Y element could promote Al_2O_3 to form on the surface of the coatings;this could form more Al_2O_3 on the surface of coatings than that dissolved in sulfate,extend the hot corrosion incubation period of coatings.Si and Y elements could also make oxidation particles thinner which made the oxide layer denser and thus SO_4~(2-) and O diffused through the dense oxide layer difficultly. Therefore,the Ti-Al-Cr-Si and Ti-Al-Cr-Si-Y coatings could protect Ti-60 matrix effectively and improve the hot corrosion resistance of Ti-Al-Cr coatings.In addition to that, Ti-60 alloys and Ti-Al-Cr(Si,Y) coatings experienced more serious corrosion in 75% Na_2SO_4+25%K_2SO_4(weight fraction,%) than in pure Na_2SO_4.
The AIP Ti-48Al-12Cr coatings provided excellent thermal shock protection on Ti-60 alloys at 900℃and 950℃.No obvious coatings spallings were found after 900℃/80 cycles and 950℃/30 cycles.While a large amount of coatings and oxidation layers were found to spall when Ti-48Al-5Cr coatings were thermal shocked at 900℃and 950℃,hence induced weight change curve descended.As 5%Cr was added into Ti-48Al coatings,it increased vacancies of oxygen in TiO_2;enhanced the atomic diffusion coefficient;promoted the growing rate of forming of TiO_2;oxide layers thicker and spalling occurred easily.12%Cr elements promoted the formation of Al_2O_3 oxidation layers in thermodynamics and kinetics points.Al_2O_3 was very thin and dense improved the thermal shock resistance of Ti-60 with coatings.Besides,thermal shock cycling experiments accelerated the oxides spalling and breakdown thereby they accelerated internal oxidation,crack forming and crack propagation.
Diffusion experience between Ti-60 and Ti-48Al-12Cr coatings showed the relationship between the thicknesses of diffusion layers with time and temperatures, especially with temperatures.At 800℃,850℃and 900℃,the growth of diffusion layer between Ti-60 and Ti-48Al-12Cr coatings was controlled by diffusion,which followed parabolic rule.Growth activation energy of the diffusion layers between Ti-60 and Ti-48Al-12Cr coating was 113.71kJ/mol.
引文
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