3Y-TZP/LZAS微晶玻璃功能梯度涂层的微观结构与性能

doi:10.15541/jim20160206

摘要/Abstract

摘要：

为了提高钢基体微晶玻璃涂层的韧性, 在Q235钢基体上采用涂搪法制备了钇稳定四方相氧化锆/Li₂O- ZnO-Al₂O₃-SiO₂ (3Y-TZP/LZAS) 微晶玻璃功能梯度涂层。采用XRD、SEM分析了梯度涂层的物相组成和微观结构, 采用压痕法测试并计算了涂层的显微硬度和断裂韧性, 通过粘接-拉伸法测试了涂层的结合强度。结果表明, 3Y-TZP/LZAS微晶玻璃功能梯度涂层各层之间的界面结合紧密; 涂层与钢基体依靠玻璃中的SiO₂与铁的氧化物发生界面反应形成牢固的结合, 反应产物为Fe₂SiO₄和FeSiO₃; 涂层的显微硬度和断裂韧性沿涂层厚度方向逐渐增大, 涂层韧性提高是表面残余压应力增韧、3Y-TZP相变及3Y-TZP的颗粒增韧共同作用的结果; 梯度涂层与Q235的结合强度达16.3 MPa。热震实验表明, 梯度涂层在300℃下经历30余次热循环, 表现出较好的抗热震性能。

关键词: 功能梯度涂层, 微晶玻璃, 涂搪法, 微观结构

Abstract:

In order to improve toughness of glass-ceramic coatings, 3mol% yattria-tetragonal zirconia polycrystal/Li₂O-ZnO-Al₂O₃-SiO₂(3Y-TZP/LZAS) glass-ceramic functionally gradient coatings on Q235 steel substrate were prepared by slurry method. Phase constitution and microstructure of samples were examined by XRD and SEM, respectively. Their micro-hardness and fracture toughness were measured by indentation method. And their bonding strength of the coatings was also investigated by pulling test. Resulting data indicate that the seamless interfaces among toughening coatings, LZAS transition layer and substrate are obtained. SiO₂ in the LZAS glass reacts with iron oxides at interfacial region forming Fe₂SiO₄ and FeSiO₃, which causes tight interface bind between gradient coatings and steel substrate. Micro-hardness and fracture toughness from inner substrate to top surface on the section of the coatings increase gradually. Residual compressive stress toughening, 3Y-TZP particles toughening and 3Y-TZP transformation toughening are the dominant factors for improving fracture toughness of the gradient coatings. Bonding strength of the coatings is up to 16.3 MPa. The gradient coatings withstand more than 30 thermal cycles at 300℃, demonstrating their excellent thermal sock resistance.

Key words: functionally gradient coating, glass-ceramic, slurry method, microstructure

中图分类号:

TG174

龚伟, 李华, 周黎明, 白朝中, 王恩泽. 3Y-TZP/LZAS微晶玻璃功能梯度涂层的微观结构与性能[J]. 无机材料学报, 2017, 32(1): 63-68.

GONG Wei, LI Hua, ZHOU Li-Ming, BAI Cao-Zhong, WANG En-Ze. Microstructure and Properties of 3Y-TZP/LZAS Glass-ceramic Functionally Gradient Coatings[J]. Journal of Inorganic Materials, 2017, 32(1): 63-68.

图/表 10

图1 3Y-TZP/LZAS梯度涂层的制备工艺流程

Fig. 1 Flow chart for preparing 3Y-TZP/LZAS gradient coatings by slurry method

图2 LZAS微晶玻璃的粘度与温度的关系

Fig. 2 Relationship between viscosity of LZAS glass ceramic and temperature

图3 不同温度下LZAS微晶玻璃与Q235的润湿结果

Fig. 3 Wettability of LZAS glass ceramic with Q235 steel at different temperatures(a) 690℃, 88.9°; (b) 720℃, 68.3°; (c) 750℃, 35.6°; (d) 780℃, 15.9°

图4 3Y-TZP/LZAS微晶玻璃梯度涂层的涂烧制度

Fig. 4 Firing schedule for the 3Y-TZP/LZAS gradient coatings

图5 3Y-TZP/LZAS梯度涂层顶层的XRD图谱

Fig. 5 XRD pattern of the top surface of 3Y-TZP/LZAS gradient coatings

图6 3Y-TZP/LZAS微晶玻璃梯度涂层截面组织形貌

Fig. 6 Section morphology of the 3Y-TZP/LZAS gradient coatings

图7 Q235与LZAS微晶玻璃界面区域的组织形貌

Fig. 7 Interface morphology of Q235-LZAS glass-ceramic

图8 Q235-LZAS微晶玻璃界面处的X射线衍射图谱

Fig. 8 XRD pattern of the interface between LZAS glass ceramic and Q235 steel

表1 梯度涂层各层的显微硬度与断裂韧性值

Table 1 Micro-hardness and fracture toughness of different layer for the 3Y-TZP/LZAS gradient coatings

Layer	Micro-hardness H_v/GPa	Fracture toughness K_IC/(MPa•m^1/2)
Transition layer	2.43	0.62
1st toughening layer	3.24	1.32
2nd toughening layer	3.78	1.94
3rd toughening layer	4.53	2.12
4th toughening layer	5.11	2.83

图9 涂层截面的压痕形貌

Fig. 9 Optical images of Vickers indentation on the section of coatings(a) Transition layer; (b) The 1st toughening layer; (c) The 2nd toughening layer; (d) The 3rd toughening layer; (e) The 4th toughening layer

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