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报道了一种采用同轴静电纺丝法制备的表面增强Raman散射(SERS)活性衬底,用于微量环境污染物的快速检测.采用醋酸纤维素(CA)/丙酮-二甲基乙酰胺溶液作为前驱液分散银纳米立方体,利用丙酮促进银颗粒适度团聚,采用同轴静电纺丝法制备了大面积银立方体/CA纳米纤维.由于团聚态银纳米立方体之间的等离子体耦合作用,复合薄膜具有优异的SERS活性,是单分散态的银立方体/CA纳米纤维SERS灵敏度的4倍,实现了0.1 nmol/L的对巯基苯胺以及10 nmol/L的甲基对硫磷农药的SERS检测,SERS信号强度偏差小于12％.“,”Cellulose acetate (CA) nanofibers were embedded with aggregated silver-nanocubes (AgNCs) by a coaxial electrospinning method. AgNCs were dispersed with CA and acetone-dimethylacetamide (DMAc) as a precursor solution, and AgNCs aggregation was induced with acetone. The nanofibers have a remarkable surface-enhanced Raman scattering (SERS) activity due to the strong plasmon coupling between neighboring AgNCs, which is 4 times of the monomeric-AgNC/CA sample. As a result, 0.1 nmol/L p-aminothiophenol (p-ATP) and 10 nmol/L methyl parathion can be identified, respectively. The nanofibers generate large-area homogeneous SERS signals with a relative signal deviation of less than 12％ over 1 mm×1 mm area due to the homogeneous adsorption of target molecules. It is thus indicated that aggregated-AgNCs/CA nanofibers have a promising potential in SERS-based detection of organic pollutants in aqueous solutions.