李玉阁,朱小鹏,吴彼,雷明凯.高功率调制脉冲磁控溅射沉积TiAlSiN纳米复合涂层对钛合金基体抗氧化性能的影响研究[J].表面技术,2020,49(12):220-227.
LI Yu-ge,ZHU Xiao-peng,WU Bi,LEI Ming-kai.Oxidation Resistance of TiAlSiN Nanocomposite Coatings on Titanium Alloy Prepared by Modulated Pulsed Power Magnetron Sputtering[J].Surface Technology,2020,49(12):220-227 |
| 高功率调制脉冲磁控溅射沉积TiAlSiN纳米复合涂层对钛合金基体抗氧化性能的影响研究 |
| Oxidation Resistance of TiAlSiN Nanocomposite Coatings on Titanium Alloy Prepared by Modulated Pulsed Power Magnetron Sputtering |
| 投稿时间：2020-06-10 修订日期：2020-07-10 |
| DOI：10.16490/j.cnki.issn.1001-3660.2020.12.025 |
| 中文关键词: TiAlSiN纳米复合涂层 高功率调制脉冲磁控溅射 钛合金 抗氧化 |
| 英文关键词:TiAlSiN nanocomposite coatings modulated pulsed power magnetron sputtering titanium alloy oxidation resistance |
| 基金项目:国家重点研发计划项目资助(2018YFA0704603);国家自然科学基金(51601029，U1508218);中央高校基本科研业务费(DUT19JC52) |
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| Author | Institution |
| LI Yu-ge | Surface Engineering Laboratory, School of Materials Science and Technology, Dalian University of Technology, Dalian 116024, China |
| ZHU Xiao-peng | Surface Engineering Laboratory, School of Materials Science and Technology, Dalian University of Technology, Dalian 116024, China |
| WU Bi | Surface Engineering Laboratory, School of Materials Science and Technology, Dalian University of Technology, Dalian 116024, China |
| LEI Ming-kai | Surface Engineering Laboratory, School of Materials Science and Technology, Dalian University of Technology, Dalian 116024, China |
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| 中文摘要: |
| 目的 研究Ti6Al4V基TiAlSiN涂层在800 ℃下的抗循环氧化性能。方法 采用高功率调制脉冲磁控溅射技术，通过调节N2/Ar的流量比fN2，在Ti6Al4V合金和Si(100)上沉积了一系列不同Si含量的TiAlSiN涂层。通过X射线衍射仪、扫描电子显微镜、电子探针、透射电镜和纳米压痕仪，表征了TiAlSiN涂层的成分、相组成、微结构和硬度，并通过X射线衍射仪和扫描电子显微镜，进一步对TiAlSiN涂层在800 ℃下循环氧化后的微观结构和形貌进行分析。结果 脉冲平均功率为2 kW时，fN2由10%增至30%，TiAlSiN涂层的Si含量(以原子数分数计)由6.1%增加至16.4%，涂层中Ti和Al含量则相应地降低。当fN2为10%时，TiAlSiN涂层呈现典型的X射线非晶结构特征，涂层中N含量(以原子数分数计)约为47%;当fN2为30%时，TiAlSiN涂层呈现TiAlN和非晶相的混合结构。TEM结果表明，涂层中TiAlN晶粒尺寸约为5 nm并均匀镶嵌在非晶相上。所有沉积于Si基底上的TiAlSiN涂层均具有相近的纳米硬度、弹性模量及残余应力，分别为17 GPa、225 GPa和–300 MPa。选取fN2为10%和25%，溅射具有不同氮含量和特征微结构的TiAlSiN涂层作为Ti6Al4V合金防护涂层，研究涂层的抗循环氧化性能。在800 ℃高温循环氧化70 h后，TiAlSiN涂层保护的合金样品较原始样品呈现更优异的抗氧化性能，且fN2为25%制备的高Si含量TiAlSiN涂层较fN2为10%制备的涂层具有更为优异的抗循环氧化性能。循环氧化后，TiAlSiN氧化层结构完整致密并呈现柱状晶特征，氧化层由上至下分别形成富α-Al2O3、a-TiO2及r-TiO2三层结构。结论 高Si含量的TiAlSiN涂层具有更低的氧化速率，涂层的纳米复合结构和低压缩应力是其抗循环氧化能力提高的主要原因。 |
| 英文摘要: |
| The work aims to study the oxidation behavior of the TiAlSiN nanocomposite coatings on the Ti6Al4V alloy at 800 ℃ by a cyclic oxidation test. A series of TiAlSiN coatings with different Si contents were deposited on the titanium alloy and Si(100) substrates through modulated pulsed power magnetron sputtering (MPPMS) by controlling the nitrogen/argon flow ratio fN2. The constituent, phase composition, microstructure and hardness of TiAlSiN were characterized by X-ray diffractometer, scanning electron microscope, electron probe, transmission electron microscope and nanoindenter, and the microstructure and morphology of TiAlSiN coating after cyclic oxidation test at 800 ℃ were analyzed with X-ray diffractometer and scanning electron microscope. When the average pulse power was 2 kW, fN2 increased from 10% to 30% and the Si content (by atomic weight fraction) increased from 6.1% to 16.4%, but the contents of Ti and Al decreased accordingly. When fN2 was 10%, the TiAlSiN coatings with the nitrogen content of about 47% were observed as x-ray amorphous structure. When fN2 increased up to 30%, the TiAlSiN coatings had the distinct TiAlN X-ray diffraction peak together with the amorphous phase. TEM indicated that the nanocrystalline grains in TiAlN coatings were about 5 nm and embedded in the amorphous matrix. All the TiAlSiN coatings deposited on Si substrate exhibited the similar nano-hardness, modulus and residual compressive stress of about 17 GPa, 225 GPa and -300 MPa. The TiAlSiN coatings with the distinguished nitrogen contents and characteristic microstructure were deposited under the fN2 of 10% and 25% and selected as the protective coatings to study the cyclic oxidation resistance. The TiAlSiN coatings had better oxidation resistance at a higher temperature of 800 ℃ for 70 h, compared with the original Ti6Al4V alloy. The coatings with high silicon contents under the fN2 of 25% exhibited the obviously better cyclic oxidation resistance than that deposited under the fN2 of 10%, and oxidation layers on the TiAlSiN coatings were composed of three sublayers, i.e. rich α-Al2O3, and a-TiO2 and r-TiO2 sublayers with the dense columnar structure from top to bottom. The TiAlSiN nanocomposite coatings with high silicon contents have lower oxidation rate, and the nanocomposite structure and low compressive stress are the main factors to improve the cyclic oxidation resistance of the coating. |
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