原子层沉积氧化铝包覆羰基铁粉的抗腐蚀性及吸波性能

doi:10.15541/jim20160558

摘要/Abstract

摘要：

为了提高羰基铁粉的抗腐蚀能力及改善其电磁性能, 以TMA和H₂O为前驱体, 利用原子层沉积(ALD)方法对羰基铁粉进行表面包覆改性, 在羰基铁粉表面包覆不同厚度的氧化铝。通过扫描电镜(SEM)、透射电镜(TEM)、综合热分析仪(TGA)、红外光谱(FTIR)和矢量网络分析仪等技术手段系统分析了改性前后羰基铁粉性能指标。结果表明, 通过ALD方法可在羰基铁粉表面生长纳米级别具有良好保型的氧化铝薄膜, 形成了极佳的羰基铁/氧化铝壳层结构复合材料。与原样品相比, 包覆改性后的羰基铁粉热稳定性与抗腐蚀性有极大的提高, 且随着包覆厚度的增加, 抗氧化能力增强, 最大抗氧化温度可超过550℃。同时羰基铁粉包覆氧化铝后, 其介电常数明显减小, 磁导率变化相对较小, 改善了原羰基铁粉的电磁参数与吸波性能。

关键词: 原子层沉积, 羰基铁粉, 氧化铝, 吸波材料, 抗腐蚀性

Abstract:

To improve the corrosion resistant capability and electromagnetic performance of carbonyl iron powders (CIPs), alumina thin films were coated on carbonyl iron powder by atomic layer deposition (ALD) using trimethylaluminum and water as precursors. Original and modified carbonyl iron powder was characterized comprehensively via scanning electron microscope (SEM), transmission electron microscope (TEM), thermogravimetric analyzer (TGA), Fourier Transform infrared spectroscope (FTIR), and vector network analyzer. The results indicated that nano-alumina films were conformably grown on the surface of carbonyl iron powders via ALD, forming an excellent core-shell CIP/alumina structure. Compared to the original sample, thermal stability and corrosion resistance of the modified carbonyl iron powders were greatly improved. Antioxidation capability of CIPs was found enhanced with the increase of alumina coating thickness, and the maximum antioxidation temperature can exceed 550℃. It was also found that the complex permittivity of core-shell CIP/alumina decreased greatly while the complex permeability was almost the same. Therefore, the electromagnetic parameters and microwave absorption properties of the modified CIPs was also improved.

Key words: atomic layer deposition, carbonyl iron powder, alumina, wave absorbing materials, corrosion resistant

中图分类号:

TB33

刘彦峰, 李磊削, 王韫宇, 李昌烽. 原子层沉积氧化铝包覆羰基铁粉的抗腐蚀性及吸波性能[J]. 无机材料学报, 2017, 32(7): 751-757.

LIU Yan-Feng, LI Lei-Xiao, WANG Yun-Yu, LI Chang-Feng. Corrosion Resistance and Wave Absorbing Property of Carbonyl Iron Powder Coating with Alumina by Atomic Layer Deposition[J]. Journal of Inorganic Materials, 2017, 32(7): 751-757.

图/表 9

图1 原子层沉积过程反应脉冲示意图

Fig. 1 Schematic diagram of reaction pulse during ALD

图2 CIP(a)和CIP/Al2O3(b)的扫描电镜照片; (c~h) CIP/Al2O3的透射电镜照片及能谱图

Fig. 2 SEM images of CIP(a) and CIP/Al2O3(b); (c-h) TEM and EDS of CIP/Al2O3

图3 CIP和CIP/Al2O3复合材料红外光谱图

Fig. 3 FTIR spectra of (a) CIP and (b) CIP/Al2O3

图4 不同ALD循环包覆的CIP /Al2O3复合材料中氧化铝的质量分数

Fig. 4 Mass fraction of alumina in CIP/Al2O3 composites after different cycles of ALD deposition

图5 CIP和CIP/Al2O3复合材料的热重曲线

Fig. 5 TG curves of CIP and CIP/Al2O3

图6 CIP和 CIP/Al2O3在0.2mol/L HCl腐蚀试验

Fig. 6 The corrosion test of CIP and CIP /Al2O3 in 0.2 mol/L HCl(a) 2 min; (b) 20 min; (c) 15 h

图7 CIP和CIP/Al2O3与石蜡混合物的复介电常数与磁导率随频率的变化

Fig. 7 Complex permittivity and permeability relative to the frequency for paraffin mixture of CIP and CIP /Al2O3

图8 CIP和CIP/Al2O3与石蜡混合物的反射损耗频率的变化(2.5 mm)

Fig. 8 Microwave reflection loss of paraffin mixture for CIP and CIP /Al2O3 (2.5 mm)

图9 CIP(a)和CIP/Al2O3(b)复合材料对电磁波吸收作用示意图

Fig. 9 Schematic diagram of electromagnetic wave absorption of CIP (a) and CIP/Al2O3 composites (b)

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