Spray-anti-solvent crystallization method for preparing doped aluminum powder composite microspheres

doi:10.11949/0438-1157.20231397

Abstract

Abstract:

Nano-aluminum powder is widely used in the field of energetic composite materials as a high-energy additive. However, the preparation of high sphericity aluminum powder doped composite microspheres is faced with a series of challenges. In this paper, a spray-crystallization method for the preparation of composite functional microspheres formed by nano-aluminum powder and organic molecules was explored by using the method of spray and anti-solvent crystallization. Through the self-designed internal mixing three-flow air atomization nozzle, the precursor liquid is atomized into liquid droplets. After receiving in the anti-solvent receiving bath, the solvent and anti-solvent rapidly mutual diffusion and mass transfer process occur. The energetic molecular simulation sucrose octaacetate (SOA) is precipitated in the droplet, the aluminum powder is wrapped in it, and the aluminum powder doped composite microspheres are obtained after washing and drying. In this paper, by adjusting suitable conditions such as atomization, solvent and anti-solvent, additives, etc., the phenomenon of low sphericity and agglomeration of the composite microspheres after drying was successfully solved. Finally, the doped aluminum powder microsphere composite material with narrow particle size distribution, uniform morphology, good dispersion, sphericity and high compactness was prepared.

Key words: crystallization, polymeric additives, doped, sucrose octaacetate, nano-aluminum, composite microspheres

摘要：

纳米铝粉作为高能添加剂广泛应用于含能复合材料领域。然而，制备高球形度铝粉掺杂的复合微球却面临着一系列挑战。采用喷雾与反溶剂结晶相结合的方法，探索了一种制备纳米铝粉与有机分子形成复合功能微球的喷射-结晶途径。通过自主设计的内混三流式空气雾化喷嘴，将前驱液雾化成液滴，反溶剂接收浴接收后，溶剂与反溶剂发生快速的相互扩散和传质过程，含能分子模拟物蔗糖八乙酸酯（SOA）在液滴内部析出，将铝粉包裹在内，洗涤干燥后得到铝粉掺杂的复合微球。通过调控合适的雾化、溶剂与反溶剂、添加剂等条件，成功解决了干燥后复合微球球形度低、微球之间相互团聚等现象，最终制备出粒径分布窄、形貌均一、分散性较好、球形度和密实度较高的掺杂铝粉的微球复合材料。

关键词: 结晶, 聚合物添加剂, 掺杂, 蔗糖八乙酸酯, 纳米铝粉, 复合微球

CLC Number:

O 636.1

Jing LIU, Wenbo YANG, Yingdi LYU, Shengyang TAO. Spray-anti-solvent crystallization method for preparing doped aluminum powder composite microspheres[J]. CIESC Journal, 2024, 75(4): 1724-1734.

刘静, 杨文博, 吕英迪, 陶胜洋. 喷雾-反溶剂结晶法制备掺杂铝粉的复合微球[J]. 化工学报, 2024, 75(4): 1724-1734.

Figures/Tables 13

Fig.1 Spray-antisolvent receiver and nozzle structure

Fig.2 Schematic diagram of preparation of doped aluminum powder composite microspheres

Table 1 Atomization conditions of internal mixing three-stream air atomizing nozzle

序号	气压/mbar	液压/mbar	气液比	D₅₀/μm
1	1600	100	32	62.514
2	1700	100	34	60.144
3	1800	100	36	56.609
4	1900	100	38	54.237
5	2000	100	40	49.848
6	1800	90	40	50.781

Fig.3 Optical images of the droplets at different time

Fig.4 SEM image of composite microspheres

Fig.5 Characterization of droplets and composite microspheres with petroleum ether and toluene as antisolvent

Fig.6 Optical microscopy photos and particle size distribution of the original droplet received by different antisolvents

Fig.7 SEM image of composite microspheres

Fig.8 SEM of composite microspheres

Fig.9 SEM images of surface and section and corresponding energy spectra of composite microspheres

Fig.10 TGA of composite microspheres when PVP∶PEG=1∶1

Fig.11 Analysis and characterization results

Fig.12 Schematic diagram of molecular structure

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