<110>织构铱涂层结构与性能研究
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摘要
难熔金属因其高温强度高，所以在航空航天领域有重要的应用价值。然而，难熔金属在高温环境下易被氧化形成多孔甚至挥发性氧化物，致使其服役的温度及寿命均受到极大限制。铂族金属具有优良的化学稳定性，尤其是铱(Ir)具有极低氧渗透率和氧化速率，成为难熔材料表面超高温抗氧化涂层的候选材料。本文采用双层辉光等离子表面冶金技术在难熔工件表面制备了Ir涂层，研究了基体和双辉工艺参数对Ir涂层组织结构的影响，分析了Ir涂层与基体界面形成过程，提出了Ir涂层<110>织构形成机制与涂层的生长机理。研究了双辉Ir涂层硬度、弹性模量、结合力和残余应力。研究了Ir涂层高温氧化烧蚀后形成微孔的机理。为了抑制微孔形成或使微孔能自愈合，对Ir涂层进行了掺Zr处理，研究了掺Zr对Ir涂层组织结构和性能的影响。
采用扫描显微镜、透射电镜和原子力显微镜观察表征了涂层的微观组织结构；采用X射线能谱仪、X射线光电子能谱仪和电子探针X射线显微分析仪检测了涂层成分；采用电子背散射衍射技术测定了涂层的微观织构、晶界取向差和晶粒尺寸；采用X射线衍射仪鉴定了涂层物相、晶粒尺寸、宏观织构和残余应力；采用纳米压痕仪测试涂层表面硬度和弹性模量；采用划痕仪测量涂层与基体间结合力；氩气保护条件下对涂层进行1400℃×1.5h高温热处理，评价涂层高温热稳定性。对涂层进行800℃~1000℃×1h氧化处理，采用耐驰热分析仪对Ir涂层进行差热和热重分析，评价涂层高温抗氧化性能。用氧-乙炔焰对涂层表面进行2000℃±100℃×35s烧蚀，评价涂层高温抗烧蚀性能。本文创新性的成果和结论如下：
（1）系统开展了双辉等离子体沉积Ir涂层的研究，提出了Ir涂层的<110>织构的形成机制。<110>织构的形成机制是沉积初期原子低迁移速率，(111)晶面晶粒易生长，以及在沉积过程中的沟道效应的溅射机制。由于双辉沉积技术具有反溅射特点，双辉Ir涂层的<110>织构的形成机制是沟道效应的溅射机制，沉积层受到高能量溅射粒子的反溅射。由于晶粒的溅射产额存在各向异性，<110>晶向晶粒的溅射率较小能保存下来并继续长大，而其它晶向晶粒由于其溅射率较大，生长受到抑制。
（2）提出了双辉<110>织构Ir涂层的生长模式，建立了Ir涂层界面形成过程模型，研究了双辉Ir涂层的生长机理。Ir涂层生长模式是以岛状生长，涂层的生长机理是在沉积初期涂层生长主要受晶粒形核速率控制，随着涂层继续沉积，涂层生长主要受晶粒生长速率控制。
（3）研究了高温真空热处理、高温氧化和高温烧蚀后Ir涂层产生微孔的形成机理。热处理后Ir涂层产生微孔的原因是涂层再结晶、涂层缺陷聚集和Kirkendall效应；高温氧化后涂层表面出现间隙是由于IrO3挥发所致；高温烧蚀后涂层产生的微孔来自于Ir氧化物的挥发和氧通过涂层晶界快速扩散至界面形成气态氧化物的逸出。
（4）提出了对Ir涂层掺Zr改性的新方案，通过Zr的氧化膨胀，对微纳米孔进行弥合，改善了其高温结构稳定性。掺低含量Zr的Ir涂层比高含量Zr的Ir涂层的高温稳定性要好。经过800℃氧化后，Ir-25at.%Zr涂层表面保持完整、无微孔；Ir-40at.%Zr涂层表面局部被氧化，出现大颗粒氧化物。经过1000℃氧化后，Ir-25at.%Zr涂层表面出现微裂纹、氧化物大颗粒和微孔，这是由于涂层Zr的分布不均匀导致。
Due to high specific strength at high temperature, it’s of viable significance to utilise refractorymetals in the field of aerospace application. However, the refractory metals are easily oxidized toform micropores, even to form volatile oxides in high-temperature environments, which results intheir service temperature and life being restricted extremely. Platinum group metals have anexcellent chemical compatibility and stability, especially, iridium (Ir) has extremely low oxygenpermeability and oxidation rate, which is one of the most promising candidates as super-hightemperature oxidation-resistant coating for refractory materials. In this dissertation, the Ir coatingand was prepared by double glow plasma surface metallurgy technology on the surface of refractorymetals. The main goal of this dissertation was to investigate the effect of substrates and depositionparameters on structure of the coating and analyze the formation processing of the interface betweenthe coating and the substrate, the formation mechanism of <110> texture of the coating and growthmechanism of the coating. It was to investigate the mechanical properties of the coating, such ashardness, elastic modulus, adhesive force and residual stress. It was to investigate the mechanism ofmicropore formation in the Ir coating after heat treatment, oxidation and ablation. In order to inhibitmicropore formation or micropores self-healing, the effect of doping Zr on structure andperformance of the Ir coating was investigated.
The microstructure and morphology of the coating were observed and characterized usingscanning electron microscopy, transmission electron microscopy and atomic force microscopy. Thechemical composition of the coating was examined by X-ray energy dispersive spectroscopy, X-rayphotoelectron spectroscopy and electron probe micro analyzer. The micro-texture, grainmisorientation angle and grain size of the Ir coating were determined by electron backscatterdiffraction technique. The phase identification, grian size, macro-texture and residual stress of thecoating were identified by X-ray diffraction. The hardness and the elastic modulus of the coatingwere estimated by nanoindentation instrument. The adhesive force of the coating was performedwith scratch tester. Ir coating were heat-treated at1400℃for90min in Ar atmosphere, to evaluatethe thermal stability of the coating. The Ir and Ir-Zr coatings were oxidized at800℃and1000℃for1h in air, meanwhile, the reaction heat and weight change of the Ir coating were measured using aNETZSCH thermal analyzer, to assess oxidation resistance of the coating. The ablation resistance ofthe coating was tested at2000℃±100℃for35s in an oxyacetylene flame. The main conclusions and innovative results of this dissertation are drawn as follows:
1. The research work of Ir coating by double glow plasma technology is systematicly carried out,we proposed the formation mechanism of <110> texture for Ir coating. The formation mechanism of<110> texture is that (110) grains easily grow over under the low mobility of adatoms at the begin ofthe deposition, and sputtering mechanism of channeling effect. Due to the anisotropy of sputteringyields for grains, the erosion of <110> crystal direction grains is smaller, which could result in theformation and growth of <110> texture grains. In contrast, the erosion of other crystal direction grainsis relatively large, which lead to the inhibited growth of other crystal direction grains.
2. We propose growth mode of Ir coating, develop a model of interface formation process of Ircoating and research the growth mechanism of the Ir coating. The growth mode of Ir coating followsisland growth model. The growth mechanism of the Ir coating is that the growth mode of the coatingis mainly controlled by the nucleation rate at the beginning of the deposition. With the depositionprocess, the growth of the coating is governed by the grain growth rate.
3. We reseach the formation mechanisms of the micropores on/in the Ir coating after hightemperature vacuum heat-treatment, oxidation and ablation. After heat treatment, the formationmechanism of micropores in the coating results from recrystallization of the coating, aggregation inthe development of birth defects in the coating and Kirkendall effect. After oxidation, lots of voidsand gaps are present on the surface of the coating due to the formation of volatile IrO3. After hightemperature ablation, the formation mechanism of the micropores on the surface of the coating is dueto volatile IrO3and O element diffusing quickly through intercrystalline boundaries to be oxidized toform gaseous MoO3.
4. We propose a new plan that Zr element is doped in the Ir coating. The Zr in the Ir coating isoxidized to make the micropore of the Ir coating self-heal. The volume expansion of Zr changed toZrO2imporves the high-temperature thermal stability of the coating. The thermal stability ofIr-25at.%Zr coating is better than that of Ir-40at.%Zr coating. After oxidation at800℃, the surface ofIr-25at.%Zr coating keeps integrity and no micropores are found. The surface of Ir-40at.%Zr coatingshows some oxidized portion, and presents large particles of oxides. After oxidation at1000℃, thesurface of Ir-25at.%Zr coating appears microcracks, abnormal large particles and less micropores dueto unhomogeneous distribution of Zr element in the coating.
采用扫描显微镜、透射电镜和原子力显微镜观察表征了涂层的微观组织结构；采用X射线能谱仪、X射线光电子能谱仪和电子探针X射线显微分析仪检测了涂层成分；采用电子背散射衍射技术测定了涂层的微观织构、晶界取向差和晶粒尺寸；采用X射线衍射仪鉴定了涂层物相、晶粒尺寸、宏观织构和残余应力；采用纳米压痕仪测试涂层表面硬度和弹性模量；采用划痕仪测量涂层与基体间结合力；氩气保护条件下对涂层进行1400℃×1.5h高温热处理，评价涂层高温热稳定性。对涂层进行800℃~1000℃×1h氧化处理，采用耐驰热分析仪对Ir涂层进行差热和热重分析，评价涂层高温抗氧化性能。用氧-乙炔焰对涂层表面进行2000℃±100℃×35s烧蚀，评价涂层高温抗烧蚀性能。本文创新性的成果和结论如下：
（1）系统开展了双辉等离子体沉积Ir涂层的研究，提出了Ir涂层的<110>织构的形成机制。<110>织构的形成机制是沉积初期原子低迁移速率，(111)晶面晶粒易生长，以及在沉积过程中的沟道效应的溅射机制。由于双辉沉积技术具有反溅射特点，双辉Ir涂层的<110>织构的形成机制是沟道效应的溅射机制，沉积层受到高能量溅射粒子的反溅射。由于晶粒的溅射产额存在各向异性，<110>晶向晶粒的溅射率较小能保存下来并继续长大，而其它晶向晶粒由于其溅射率较大，生长受到抑制。
（2）提出了双辉<110>织构Ir涂层的生长模式，建立了Ir涂层界面形成过程模型，研究了双辉Ir涂层的生长机理。Ir涂层生长模式是以岛状生长，涂层的生长机理是在沉积初期涂层生长主要受晶粒形核速率控制，随着涂层继续沉积，涂层生长主要受晶粒生长速率控制。
（3）研究了高温真空热处理、高温氧化和高温烧蚀后Ir涂层产生微孔的形成机理。热处理后Ir涂层产生微孔的原因是涂层再结晶、涂层缺陷聚集和Kirkendall效应；高温氧化后涂层表面出现间隙是由于IrO3挥发所致；高温烧蚀后涂层产生的微孔来自于Ir氧化物的挥发和氧通过涂层晶界快速扩散至界面形成气态氧化物的逸出。
（4）提出了对Ir涂层掺Zr改性的新方案，通过Zr的氧化膨胀，对微纳米孔进行弥合，改善了其高温结构稳定性。掺低含量Zr的Ir涂层比高含量Zr的Ir涂层的高温稳定性要好。经过800℃氧化后，Ir-25at.%Zr涂层表面保持完整、无微孔；Ir-40at.%Zr涂层表面局部被氧化，出现大颗粒氧化物。经过1000℃氧化后，Ir-25at.%Zr涂层表面出现微裂纹、氧化物大颗粒和微孔，这是由于涂层Zr的分布不均匀导致。
Due to high specific strength at high temperature, it’s of viable significance to utilise refractorymetals in the field of aerospace application. However, the refractory metals are easily oxidized toform micropores, even to form volatile oxides in high-temperature environments, which results intheir service temperature and life being restricted extremely. Platinum group metals have anexcellent chemical compatibility and stability, especially, iridium (Ir) has extremely low oxygenpermeability and oxidation rate, which is one of the most promising candidates as super-hightemperature oxidation-resistant coating for refractory materials. In this dissertation, the Ir coatingand was prepared by double glow plasma surface metallurgy technology on the surface of refractorymetals. The main goal of this dissertation was to investigate the effect of substrates and depositionparameters on structure of the coating and analyze the formation processing of the interface betweenthe coating and the substrate, the formation mechanism of <110> texture of the coating and growthmechanism of the coating. It was to investigate the mechanical properties of the coating, such ashardness, elastic modulus, adhesive force and residual stress. It was to investigate the mechanism ofmicropore formation in the Ir coating after heat treatment, oxidation and ablation. In order to inhibitmicropore formation or micropores self-healing, the effect of doping Zr on structure andperformance of the Ir coating was investigated.
The microstructure and morphology of the coating were observed and characterized usingscanning electron microscopy, transmission electron microscopy and atomic force microscopy. Thechemical composition of the coating was examined by X-ray energy dispersive spectroscopy, X-rayphotoelectron spectroscopy and electron probe micro analyzer. The micro-texture, grainmisorientation angle and grain size of the Ir coating were determined by electron backscatterdiffraction technique. The phase identification, grian size, macro-texture and residual stress of thecoating were identified by X-ray diffraction. The hardness and the elastic modulus of the coatingwere estimated by nanoindentation instrument. The adhesive force of the coating was performedwith scratch tester. Ir coating were heat-treated at1400℃for90min in Ar atmosphere, to evaluatethe thermal stability of the coating. The Ir and Ir-Zr coatings were oxidized at800℃and1000℃for1h in air, meanwhile, the reaction heat and weight change of the Ir coating were measured using aNETZSCH thermal analyzer, to assess oxidation resistance of the coating. The ablation resistance ofthe coating was tested at2000℃±100℃for35s in an oxyacetylene flame. The main conclusions and innovative results of this dissertation are drawn as follows:
1. The research work of Ir coating by double glow plasma technology is systematicly carried out,we proposed the formation mechanism of <110> texture for Ir coating. The formation mechanism of<110> texture is that (110) grains easily grow over under the low mobility of adatoms at the begin ofthe deposition, and sputtering mechanism of channeling effect. Due to the anisotropy of sputteringyields for grains, the erosion of <110> crystal direction grains is smaller, which could result in theformation and growth of <110> texture grains. In contrast, the erosion of other crystal direction grainsis relatively large, which lead to the inhibited growth of other crystal direction grains.
2. We propose growth mode of Ir coating, develop a model of interface formation process of Ircoating and research the growth mechanism of the Ir coating. The growth mode of Ir coating followsisland growth model. The growth mechanism of the Ir coating is that the growth mode of the coatingis mainly controlled by the nucleation rate at the beginning of the deposition. With the depositionprocess, the growth of the coating is governed by the grain growth rate.
3. We reseach the formation mechanisms of the micropores on/in the Ir coating after hightemperature vacuum heat-treatment, oxidation and ablation. After heat treatment, the formationmechanism of micropores in the coating results from recrystallization of the coating, aggregation inthe development of birth defects in the coating and Kirkendall effect. After oxidation, lots of voidsand gaps are present on the surface of the coating due to the formation of volatile IrO3. After hightemperature ablation, the formation mechanism of the micropores on the surface of the coating is dueto volatile IrO3and O element diffusing quickly through intercrystalline boundaries to be oxidized toform gaseous MoO3.
4. We propose a new plan that Zr element is doped in the Ir coating. The Zr in the Ir coating isoxidized to make the micropore of the Ir coating self-heal. The volume expansion of Zr changed toZrO2imporves the high-temperature thermal stability of the coating. The thermal stability ofIr-25at.%Zr coating is better than that of Ir-40at.%Zr coating. After oxidation at800℃, the surface ofIr-25at.%Zr coating keeps integrity and no micropores are found. The surface of Ir-40at.%Zr coatingshows some oxidized portion, and presents large particles of oxides. After oxidation at1000℃, thesurface of Ir-25at.%Zr coating appears microcracks, abnormal large particles and less micropores dueto unhomogeneous distribution of Zr element in the coating.
引文
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