表面技术2025，Vol.54Issue(13)：107-120,14.DOI:10.16490/j.cnki.issn.1001-3660.2025.13.010
真空退火对Zr-B-N/ZrO2多层复合涂层结构及性能的影响
Effect of Vacuum Annealing on Microstructure and Properties of Zr-B-N/ZrO2 Multilayered Coatings
摘要
Abstract
The nano-composite structure of Zr-B-N coatings,consisting of amorphous nanocrystals,provides advantages such as high hardness,high toughness,and excellent wear resistance.However,during high-temperature operation,the amorphous BN phases within the coatings are prone to oxidation and volatilization,leading to poor high-temperature thermal stability and oxidation resistance.This significantly restricts its application in high-temperature environments like high-efficiency machining and dry cutting.To overcome these limitations,a nano-multilayer structure is designed to integrate the superior hardness-toughness balance of Zr-B-N layers with the excellent thermal resistance of ZrO2 layers.Periodic deposition of ZrO2 layers into the Zr-B-N coating is implemented to enhance thermal stability.Vacuum annealing further improves the properties of Zr-B-N/ZrO2 multilayer composite coatings to systematically investigate the mechanisms of interfacial diffusion behavior,microstructure,mechanical properties,and tribological properties at high temperature. Zr-B-N/ZrO2 multilayer composite coatings are fabricated on YG 8 cemented carbide and single-crystal Si(100)substrates using composite magnetron sputtering technology.Vacuum annealing experiments are conducted at 500-800℃(<10‒3 Pa,1 h)in a vacuum tube furnace.The phase composition,micro-morphology,microstructure,mechanical properties,and tribological properties of the coatings are analyzed using XRD,FESEM,HRTEM,nanoindentation,high-load scratch testing,high-temperature tribometry,ultra-depth-of-field 3D microscopy,and white light interferometry. The Zr-B-N/ZrO2 multilayer composite coating primarily consists of the t-ZrO2 phase and fcc-ZrN phase.As the annealing temperature increases,the B content gradually decreases while the O content increases,accompanied by enhanced diffraction peak intensity of the t-ZrO2 phase,which shifts toward larger angles.When annealing at 600℃,the coating surface remains dense with an intact nano-multilayer structure,exhibiting maximum hardness and elastic modulus values of 32.75 GPa and 391.70 GPa,respectively.The corresponding bonding strength reaches 47.95 N,with a friction coefficient of 0.658 and a wear rate of 1.11×10‒5 mm3/(N·m).When the annealing temperature reaches 800℃,the O content decreases while the B content increases,with fcc-ZrO and hcp-ZrB2 phases precipitating in the coating.The friction coefficient(0.507)and wear rate(4.54×10‒6 mm3/(N·m))reach their lowest values,representing reductions of 43.29%and 69.97%,respectively,compared with the values before vacuum annealing.However,due to grain size growth,numerous microcracks form at grain boundaries.The formation of extensive cross-sectional microcrack channels enhances mutual diffusion between elements,leading to significant interfacial solubility and nearly complete collapse of the nano-multilayer structure.Edge dislocations in the Zr-B-N layer penetrate the interface and propagate into the ZrO2 layer.This interfacial degradation results in a notable reduction in adhesion between the coating and substrate,with hardness,elastic modulus,and bonding strength decreasing to their minimum values. Appropriate vacuum annealing can significantly influence coating properties.When annealing at 600℃,the coating exhibits optimal comprehensive performance.Although wear resistance improves after annealing at 800℃,the overall performance deteriorates substantially due to structural damage.关键词
复合磁控溅射/真空退火/纳米多层涂层/微观结构/力学性能/摩擦学性能Key words
hybrid magnetron sputtering/vacuum annealing/nano-multilayered coating/microstructure/mechanical property/tribological property分类
矿业与冶金引用本文复制引用
叶佳妮,马莉莎,张纪福,刘艳梅,曹凤婷,范其香,王铁钢..真空退火对Zr-B-N/ZrO2多层复合涂层结构及性能的影响[J].表面技术,2025,54(13):107-120,14.基金项目
中央引导地方科技发展资金(24ZYCGCG00520) （24ZYCGCG00520）
天津市自然科学基金项目(24JCYBJC00110) Funds for Central Guidance of Local Science and Technology Development(24ZYCGCG00520) （24JCYBJC00110）
Natural Science Foundation of Tianjin(24JCYBJC00110) （24JCYBJC00110）
