硅酸盐学报

06Ni9DR合金钢用SiC-Al₂O₃-玻璃复合涂层的高温氧化防护性能及其机理

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杨启宝 ¹^,² , 桑绍柏 ¹^,² , 李亚伟 ¹^,² , 杨富云 ¹^,² , 朱天彬 ¹^,² , 王恒 ¹^,²

硅酸盐学报 | 研究论文 2026,54(1): 216-224

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硅酸盐学报 |研究论文 2026 , 54 (1) : 216 -224

06Ni9DR合金钢用SiC-Al₂O₃-玻璃复合涂层的高温氧化防护性能及其机理

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杨启宝¹^,², 桑绍柏¹^,², 李亚伟¹^,², 杨富云¹^,², 朱天彬¹^,², 王恒¹^,²

作者信息

^1．武汉科技大学先进耐火材料全国重点实验室，武汉 430081

^2．武汉科技大学高温材料与炉衬技术国家地方联合工程研究中心，武汉 430081

通讯作者:

桑绍柏（1979—），男，博士，教授。

作者简介:

杨启宝（1999—），男，博士研究生。

Protection Performance and Mechanism of SiC-Al₂O₃-Glass Composite Coating against High Temperature Oxidation of 06Ni9DR Alloy Steel

Qibao YANG¹^,², Shaobai SANG¹^,², Yawei LI¹^,², Fuyun YANG¹^,², Tianbin ZHU¹^,², Heng WANG¹^,²

Affiliations

^1.State Key Laboratory of Advanced Refractories, Wuhan University of Science and Technology, Wuhan 430081, China

^2.National-provincial Joint Engineering Research Center of High Temperature Materials and Lining Technology, Wuhan University of Science and Technology, Wuhan 430081, China

Corresponding Author:

SANG Shaobai (1979-), male, Ph.D., Professor. E-mail: sangshaobai@126.com

YANG Qibao (1999-), male, Doctoral candidate. E-mail: 2783665132@qq.com

出版时间: 2026-01-20 doi: 10.14062/j.issn.0454-5648.20250259

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摘要

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针对06Ni9DR合金钢在轧制前序加热环节中氧化严重的问题，本工作制备了4种不同SiC含量的SiC-Al₂O₃-玻璃复合涂层，测试了涂层在不同时间的防护性能并揭示了SiC在氧化防护中的作用机制。结果表明，在1200 ℃氧化10 min后，4种复合涂层均达到96%以上的优异防护效果。随着氧化时间延长至180 min，低SiC比例复合涂层因SiC氧化带来的“发泡”效应，导致氧化防护率降至40.9%；相比之下，高SiC比例复合涂层因液相含量减少导致“发泡”效应明显减弱，涂层内部仍保留平均孔径约为2.7 μm的微孔结构，可以最大限度发挥SiC的“耗氧”机制，最终保持了96.1%的氧化防护效果，并能有效改善镍合金钢加热后的表面质量。

关键词

镍合金钢 / 氧化防护 / 碳化硅 / 消耗氧气 / 发泡衰减 / 扩散路径

Abstract

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Introduction

06Ni9DR alloy steel has become a core material for LNG storage and transportation equipment due to its excellent low-temperature toughness (down to -196 ℃) and low thermal expansion properties. The 06Ni9DR alloy steel is heated at 1100-1250 ℃ before hot rolling. However, there are severe oxidation and difficulties in removing the oxide skin, which leads to increased processing costs. The protective coating method has become one of the main means of high-temperature oxidation protection for alloy steels due to its simple preparation process, wide applicability and freedom from shape and size limitations. In the previous stage, a reaction-sintered Al₂O₃-glass composite coating with 73.6% protection after oxidization at 1200 ℃ for 3 h was prepared by our team. The addition of SiC to deplete the oxygen inside the coating is expected to improve oxidation protection. It is worth noting that when there is liquid phase in the coating at high temperature, the SiC will act as foaming and leave pores in it, which will become the oxygen diffusion channel. Therefore, in this work, SiC-Al₂O₃-glass composite coatings with different silicon carbide contents were prepared, and the effect of silicon carbide content on the oxidation protection and its mechanism were revealed.

Methods

The crystal structure of the coating samples after heat treatment was by power X-ray diffraction using a diffractometer (10°-90°, X' pert pro, PHILIPS, Netherlands). The XRD spectra were recorded at 40 mA and 40 kV using Cu K_α radiation (λ=0.1542 nm). The apparent porosity (AP) and bulk density (BD) of the coating samples were measured by Archimedes drainage method. The microstructure and element analysis of the coating samples and steels with coatings were evaluated by using field emission scanning electron microscopy (SEM, EVO-10, ZEISS, Germany), equipped with an X-ray energy dispersive spectrometer (EDS, Xplose30, Oxford, Britain) at 16 kV. The average pore size inside the coating was counted by Image Pro Plus 6.0. The mass loss rate (β) of GC steels with coatings after oxidation test was referred to the Chinese industry standard for the determination and calculation method for oxidation burning loss of slab (YB/T 4773-2019). The pore size distributions and average pore diameter of coatings samples after heat treatment for 3 h were measured by mercury piezometer (5 nm-800 μm, AUTOPORE V9620, Micromeritics Instruments, America).

Results and discussion

The composition of the physical phase showed that the SiC in the composite coatings could continuously oxidize to generate the square quartz phase, and the amount of generation increased with the content of SiC and the heat treatment duration. The average pore size of all coating samples after 10 min of oxidation was only about 2.5 μm. The number of macropores in the composite coatings with low SiC content increased significantly, and the average pore size also increased to 30.6 μm with the oxidation duration. The average pore size decreased with the SiC content in the composite coatings after heat treatment for 180 min. The excellent oxidation protection was observed for all steels with coatings after oxidation for 10 min, which was more than 96%. The oxidation protection ratio of the composite coating with the low SiC content decreased to 40.9% for 180 min, and the oxidation protection ratio of the composite coating with the high SiC content remained almost unchanged, up to 96.1%.

Conclusions

The main conclusions of this paper are summarized as following. The mechanism of "foaming attenuation" in composite coatings with low SiC content was revealed. There was a high content of liquid phase in it. During the oxidation process, the oxidation products of SiC, such as CO and CO₂, will be wrapped by the liquid phase. The amounts of gases wrapped inside the coating increased with the oxidation duration, resulting in a significant "foaming" phenomenon in the coating and the formation of large-size pore channels, which significantly reduced the oxidation protection. The mechanism of "oxygen depletion enhancement" in composite coatings with high SiC content was also revealed. The liquid phase content in composite coatings with high SiC content was low, and the generation of square quartz from the oxidation of SiC increased the viscosity of the liquid phase. The foaming effect of SiC was inhibited, resulting in the formation of a microporous structure with an average pore size of about 2.7 μm, effectively extending the oxygen diffusion path. At the same time, the oxygen in the diffusion process will be continuously consumed by the SiC in the composite coating, so that the excellent oxidation protection was provided at 1200 ℃ for different oxidation durations.

Key words

nickel alloy steel / oxidation protection / silicon carbide / oxygen-consuming / foaming attenuation / diffusion path

引用本文

杨启宝, 桑绍柏, 李亚伟, 杨富云, 朱天彬, 王恒. 06Ni9DR合金钢用SiC-Al₂O₃-玻璃复合涂层的高温氧化防护性能及其机理. 硅酸盐学报, 2026 , 54 (1) : 216 -224 . DOI: 10.14062/j.issn.0454-5648.20250259

Qibao YANG, Shaobai SANG, Yawei LI, Fuyun YANG, Tianbin ZHU, Heng WANG. Protection Performance and Mechanism of SiC-Al₂O₃-Glass Composite Coating against High Temperature Oxidation of 06Ni9DR Alloy Steel[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (1) : 216 -224 . DOI: 10.14062/j.issn.0454-5648.20250259

基金

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湖北省自然科学基金创新群体项目(2024AFA022)

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2026年第54卷第1期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250259

接收时间：2025-04-10
首发时间：2026-10-27
出版时间：2026-01-20

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收稿日期：2025-04-10
修回日期：2025-04-26

基金

湖北省自然科学基金创新群体项目(2024AFA022)

作者信息

^1．武汉科技大学先进耐火材料全国重点实验室，武汉 430081

^2．武汉科技大学高温材料与炉衬技术国家地方联合工程研究中心，武汉 430081

通讯作者:

桑绍柏（1979—），男，博士，教授。

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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