目的 针对超黏粉体在原子层沉积（Atomic Layer Deposition,ALD）表面改性过程中存在的团聚严重、解聚困难、气-固传质阻力大及反应不完全等问题,开发声共振过程强化ALD技术,以克服传统ALD工艺在超黏粉体表面改性存在的局限,实现超黏粉体材料表面高质量、高均匀性薄膜的ALD可控制备。方法 开发一种基于声共振混合装置的声共振过程强化ALD反应器,匹配共振频率实现宏观流体混合与声场微观分散的协同作用。利用该反应器在纳米氧化硅（SiO2）粉体表面沉积了氧化铝（Al2O3）薄膜,并在高黏性硼（B）粉表面制备金属钼（Mo）改性层。采用X射线光电子能谱（XPS）、X射线衍射（XRD）、电子显微镜等技术分析粉末表面改性层元素组成及形貌特征。结果 在SiO2粉体表面成功制备了纳米级Al2O3包覆层,160循环样品包覆层平均厚度约4.1 nm;在高黏性硼粉表面制备了纳米级Mo包覆层,3循环样品包覆层平均厚度约7 nm,不同粉体材料表面所得各类ALD 包覆层结构完整,厚度分布均匀,且包覆层厚度可纳米级精确调控。结论 本研究首次将声共振过程强化引入ALD反应过程,成功在高团聚粉体材料表面实现了纳米级包覆层的均匀可控制备。证实了声共振过程强化ALD技术能够有效解聚高团聚性粉体、显著提升气相沉积过程中的气-固传质效率,为ALD技术在高表面能、易团聚粉体材料上的高效、精准表面修饰提供了创新性方法与路径。
Abstract
Regarding the issues of high agglomeration, difficulty in deagglomeration, high gas-solid mass transfer resistance, and incomplete reactions encountered during the surface modification of ultra-adhesive powders via Atomic Layer Deposition (ALD), the work aims to develop a resonant acoustic enhanced ALD reactor based on the resonant acoustic mixing device. This ALD reactor effectively promotes the efficient deagglomeration and uniform dispersion of ultra-adhesive powders through the synergistic effects of macroscopic fluid mixing and acoustic field microscopic dispersion, overcoming the limitations of conventional ALD processes in surface modification of ultra-adhesive powders and achieving controllable ALD fabrication of high-quality, highly uniform thin films on the surfaces of ultra-adhesive powder materials.
The fundamental process research was conducted on the reactor. Alumina (Al2O3) films were deposited on nano-silica (SiO2) powder surfaces and molybdenum (Mo) modified layers were prepared on ultra-adhesive boron (B) powder surfaces. Techniques such as X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and electron microscopy were employed to analyze the elemental composition and morphological characteristics of the modified layers on the powder surfaces.
Nanoscale Al2O3 coating layers were successfully prepared on the surface of SiO2 powders, with an average thickness of approximately 4.1 nm after 160 cycles. On the surfaces of ultra-adhesive boron powders, nanoscale Mo coating layers were fabricated, with an average thickness of approximately 7 nm after 3 cycles. The resulting ALD coating layers on different powder materials featured intact structures, uniform thickness distribution, and precise controllability at the nanoscale. The characterization results indicated that the various ALD coating layers deposited on different ultra-adhesive powder materials were structurally complete, uniformly distributed in thickness, and precisely controllable at the nanoscale.
This work introduces resonant acoustic technology into the ALD reaction process for the first time, successfully achieving uniform and controlled preparation of nanoscale coating layers on ultra-adhesive powder materials. It demonstrates that the resonant acoustic process-intensified ALD technology can effectively deagglomerate ultra-adhesive powders, significantly improve gas-solid mass transfer efficiency during vapor deposition, and provides an innovative method and pathway for the efficient and precise surface modification of high-surface-energy, easily agglomerated powder materials with ALD technology.
关键词
原子层沉积 /
声共振 /
过程强化 /
粉体材料 /
解聚 /
表面改性
Key words
atomic layer deposition /
resonant acoustic /
process intensification /
powder materials /
deagglomeration /
surface modification
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