原子层沉积技术合成氧化铝薄膜包覆二硝酰胺铵

doi:10.15541/jim20130572

摘要/Abstract

摘要：

通过原子层沉积(ALD)技术以三甲基铝和水作为前驱体在二硝酰胺铵(ADN)表面沉积氧化铝包覆膜。分别采用扫描电子显微镜(SEM), X射线光电子能谱(XPS)对包覆后ADN的表面形貌、化学成分进行了分析, 通过蒸汽吸附分析仪(VSA)对包覆氧化铝薄膜的ADN样品进行了吸湿性测试, 并且对ADN表面氧化铝薄膜生成机理进行了探讨。结果表明: ALD氧化铝薄膜对ADN表面形成了完整的包覆, 薄膜厚度最高可达数百纳米。包覆有ALD氧化铝薄膜的ADN样品暴露在潮湿空气中48 h形貌不发生明显变化。在25℃, 湿度70%的环境条件下, VSA测得包覆200和400周期氧化铝薄膜的ADN吸湿率分别为40.99%和40.75%。以上研究结果表明, 尽管ALD氧化铝对ADN表面实现了完整包覆并在潮湿空气中维持了样品形貌, 被包覆的ADN样品吸湿性尚未获得明显改善。

关键词: 原子层沉积(ALD), 二硝酰胺铵(ADN), 氧化铝, 吸湿性

Abstract:

To deposit alumina thin films on ammonium dinitramide (ADN) by atomic layer deposition (ALD), trimethylaluminum and water were used as the precursors. The surface morphology and chemical compositions of the ALD alumina coated ADN were characterized by scanning electron microscope (SEM) and X-ray photoelectron spectroscope (XPS). The hygroscopic property of the ALD alumina coated ADN was studied by a vapor adsorption analyzer (VSA). The possible mechanism of ALD aluminafilm growth on the surface of ADN was discussed. The characterization results indicate that the ALD alumina film completely covers the surface of ADN. The thickness of the alumina film can reach hundreds of nanometers. After 48 h of air exposure, the shapes and topologies of the alumina coated ADN particles are maintained. The hygroscopicity of the ADN samples coated by 200 and 400 cycles of ALD alumina are 40.99% and 40.75%, respectively. Although the ALD alumina coating completely covers the surface of ADN and successfully maintains the shapes and topologies of ADN particles in a wet environment, the hygroscopicity of the ALD alumina coated ADN is not improved.

Key words: atomic layer deposition, ammonium dinitramide, alumina, hygroscopicity

中图分类号:

TN304
V512

龚婷, 秦利军, 严蕊, 胡岚, 姬月萍, 冯昊. 原子层沉积技术合成氧化铝薄膜包覆二硝酰胺铵[J]. 无机材料学报, 2014, 29(8): 869-874.

GONG Ting, QIN Li-Jun, YAN Rui, HU Lan, JI Yue-Ping, FENG Hao. Alumina Thin Film Coated Ammonium Dinitramide Fabricated by
Atomic Layer Deposition[J]. Journal of Inorganic Materials, 2014, 29(8): 869-874.

图/表 6

表1 AAO表面ALD氧化铝薄膜厚度

Table 1 ALD Al2O3 film thickness on AAO

ALD cycles	m₁/mg	m₂/mg	△m/mg	h/nm
200	10.9	14.3	3.4	20.0
400	10.6	16.8	6.2	40.7

图1 AAO表面沉积氧化锌薄膜ALD过程饱和曲线

Fig. 1 Saturation curve of ALD ZnO film growth on AAO

图2 未经表面修饰及经过200和400周期ALD氧化铝修饰后的ADN样品的XPS图谱

Fig. 2 XPS spectra of bare ADN and ADN coated by 200- and 400-cycle ALD A12O3 (a) Survey scan; (b) N1s; (c)Al2p

图3 未包覆的ADN颗粒(a)和经过400周期ALD氧化铝包覆处理并移除ADN后包覆膜(b~f)的SEM照片

Fig. 3 SEM images of uncoated ADN particles (a) and the 400-cycle ALD Al2O3 film deposited on ADN (b-f) in which the ADN substrate is removed

图4 未经包覆处理(a)与经过400周期ALD氧化铝包覆处理的(b)ADN在空气中放置48 h后样品形貌对比

Fig. 4 Comparison between uncoated (a) and 400-cycle ALD Al2O3 coated (b) ADN samples after 48-h air exposure

图5 25℃、未包覆与经过400周期ALD氧化铝包覆的ADN样品的等温吸湿曲线

Fig. 5 Isothermal hygroscopic curves of uncoated and 400- cycle ALD Al2O3 coated ADN at 25℃

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