肖垚,贺小燕,万涛,白秀琴.改性氧化铈/水性环氧复合涂层制备及防腐性能分析[J].表面技术,2024,53(14):96-105, 189.
XIAO Yao,HE Xiaoyan,WAN Tao,BAI Xiuqin.Preparation and Corrosion Resistance Analysis of Modified Cerium Oxide/Waterborne Epoxy Composite Coatings[J].Surface Technology,2024,53(14):96-105, 189 |
| 改性氧化铈/水性环氧复合涂层制备及防腐性能分析 |
| Preparation and Corrosion Resistance Analysis of Modified Cerium Oxide/Waterborne Epoxy Composite Coatings |
| 投稿时间：2023-08-24 修订日期：2023-12-29 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.14.008 |
| 中文关键词: 氧化铈 聚苯胺 水性环氧 复合涂层 防腐性能 |
| 英文关键词:cerium oxide polyaniline waterborne epoxy composite coatings corrosion resistance |
| 基金项目:湖北省自然科学基金创新发展联合基金重点项目(2022CFD029);2023 年湖北省重大攻关项目(JD)(2023BAA003) |
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| Author | Institution |
| XIAO Yao | Hubei Longzhong Laboratory, Hubei Xiangyang 441000, China;a.State Key Laboratory of Maritime Technology and Safety, b.School of Transportation and Logistics Engineering, Wuhan University of Technology, Wuhan 430063, China |
| HE Xiaoyan | Hubei Longzhong Laboratory, Hubei Xiangyang 441000, China;a.State Key Laboratory of Maritime Technology and Safety, b.School of Transportation and Logistics Engineering, Wuhan University of Technology, Wuhan 430063, China |
| WAN Tao | Hubei Swan Coatings Co., Ltd., Hubei Xiangyang 441000, China |
| BAI Xiuqin | Hubei Longzhong Laboratory, Hubei Xiangyang 441000, China;a.State Key Laboratory of Maritime Technology and Safety, b.School of Transportation and Logistics Engineering, Wuhan University of Technology, Wuhan 430063, China |
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| 中文摘要: |
| 目的 利用改性氧化铈掺杂水性环氧制备水性复合涂层，提高水性涂层的防腐性能。方法 通过硅烷偶联剂接枝纳米氧化铈(CeO2-K)，然后原位聚合聚苯胺(PANI)，合成了质量比为1︰1、4︰1、7︰1的聚苯胺/氧化铈复合颗粒(PA@CeO2(1︰1)、PA@CeO2(4︰1)及PA@CeO2(7︰1))，制备了硅烷改性氧化铈复合水性环氧涂层(CeO2-K/WEP)、PANI@CeO2复合水性环氧涂层(PA@CeO2(1︰1)/WEP、PA@CeO2(4︰1)/WEP及PA@CeO2(7︰1)/WEP);通过扫描电镜、吸水率试验、电化学测试、中性盐雾试验等探讨改性氧化铈/水性环氧复合涂层的防腐性能。结果 改性后CeO2-K颗粒间的团聚作用减弱，PA@CeO2复合粒子呈现“球状+纤维状”纳米复合结构。与水性环氧树脂涂层(WEP)相比，纳米复合涂层的致密性增强，PA@CeO2复合粒子的引入提高了CeO2与环氧树脂间的相容性，并增强了涂层与基体的结合力。PA@CeO2(4︰1)/WEP浸泡30 d后，在最低频率0.01 Hz下表现出最高的阻抗模值，是CeO2-K/WEP的2.4倍，比WEP提高了2个数量级。经过336 h的盐雾试验，WEP和CeO2-K/WEP出现了明显的锈蚀和剥落，而PA@CeO2/WEP涂层剥离区域未发生扩展，表现出更好的耐盐雾性能。结论 PA@CeO2/WEP复合涂层的防腐性能优于WEP和CeO2-K/WEP的，其中PA@CeO2(4︰1)/WEP复合涂层的性能最佳。 |
| 英文摘要: |
| The work aims to prepare waterborne composite coatings with modified cerium oxide nanoparticles to improve their corrosion resistance. The cerium oxide was modified by the coupling agent γ-Glycidoxypropyltrimethoxysilane (KH560) to obtain the silanized cerium oxide (CeO2-K), and then aniline was polymerized in-situ on the surface of CeO2-K particles to obtain the polyaniline/cerium oxide composite particles, with mass ratios of aniline to cerium oxide of 1∶1, 4∶1, 7∶1, respectively, and were named as PA@CeO2(1∶1), PA@CeO2(4∶1), and PA@CeO2(7∶1). CeO2-K composite waterborne epoxy coatings (CeO2-K/WEP) and PANI@CeO2 composite waterborne epoxy coatings (PA@CeO2(1:1)/WEP, PA@CeO2(4∶1)/WEP and PA@CeO2(7∶1)/WEP) were prepared. The structure and morphology of the modified nanoparticles were characterized by SEM, EDS, and FTIR. The SEM morphology analysis showed that the agglomeration of the CeO2-K particles was attenuated after modification, and the PA@CeO2 composite particles exhibited a 'spherical + fibrous' nanocomposite structure, and polyaniline was grafted and coated on the surface of CeO2-K particles. The EDS and FTIR analysis revealed that KH560 and polyaniline successfully grafted onto cerium oxide nanoparticles. The corrosion resistance of modified cerium oxide/waterborne epoxy composite coatings was investigated from different aspects including SEM morphology analysis from surfaces and cross sections, EDS analysis, and LSCM morphology analysis, scratch test, water absorption test, electrochemical test and neutral salt spray test. SEM and LSCM morphology analysis indicated that the nanocomposite coating exhibited enhanced densification without any discernible voids compared with waterborne epoxy coatings, indicating effective hole-filling by nanoparticles. The densification and impermeability of PA@CeO2(4∶1)/WEP coatings was further confirmed through a water absorption test, revealing its exceptionally low water penetration rate of 1.72%. Additionally, the scratch test results, with a grade of 0, indicated that PA@CeO2 added epoxy waterborne coatings exhibited superior bonding properties with the substrate. After 30 d of immersion, the bode plot of impedance spectrum revealed that PA@CeO2(4∶1)/WEP coatings exhibited the highest impedance modulus at the lowest frequency of 0.01 Hz. Remarkably, this impedance modulus was found to be 2.4 times greater than that of CeO2-K/WEP coatings and two orders of magnitude higher than WEP coatings. The equivalent circuit fitting analysis showed that the coating resistance of PA@CeO2(4∶1)/WEP coatings was consistently higher than that of the other nanocomposite coatings, and could still be stably maintained above 107 Ω.cm2 under long time immersion. The charge transfer resistance of nanocomposite coatings was much higher than that of WEP coatings, roughly 20 times higher than that of WEP coatings. After 336 h of salt spray test, both WEP and CeO2-K/WEP coatings exhibited noticeable corrosion and peeling. The peeling width at scratches of WEP coatings was the largest, and that of CeO2-K/WEP coatings was narrower than that of WEP coatings, which was about 6.5 mm. However, PA@CeO2/WEP coatings demonstrated the narrowest peeling width of 4 mm at the scratch, and the peeling area remained stable without expanding throughout the duration of the experiment. The aforementioned series of experimental results has demonstrated that PA@CeO2/WEP composite coatings exhibit optimal corrosion resistance performance compared with WEP and CeO2-K/WEP coatings. |
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