调控金纳米花表面凸起的策略及其表面增强拉曼散射活性

引用本文: 冯瑞沁, 樊晔, 方云, 夏咏梅. 调控金纳米花表面凸起的策略及其表面增强拉曼散射活性[J]. 物理化学学报, 2024, 40(4): 230402. doi: 10.3866/PKU.WHXB202304020 shu

Citation: Ruiqin Feng, Ye Fan, Yun Fang, Yongmei Xia. Strategy for Regulating Surface Protrusion of Gold Nanoflowers and Their Surface-Enhanced Raman Scattering[J]. Acta Physico-Chimica Sinica, 2024, 40(4): 230402. doi: 10.3866/PKU.WHXB202304020 shu

调控金纳米花表面凸起的策略及其表面增强拉曼散射活性

冯瑞沁 ^1, ,
樊晔 ^1, ,
方云 ^{1,
,} ,
夏咏梅 ^{1,2,
,}

1.
江南大学化学与材料工程学院, 合成与生物胶体教育部重点实验室, 江苏无锡 214122;
2.
江南大学, 食品科学与技术国家重点实验室, 江苏无锡 214122

通讯作者: 方云,Email:yunfang@126.com; 夏咏梅,Email:ymxia@jiangnan.edu.cn

基金项目:
国家自然科学基金(21606107)资助项目

摘要: 以聚乙烯吡咯烷酮(PVP)与十二烷基硫酸钠(SDS)通过阳离子架桥形成的拟聚阴离子为软模板，通过改变PVP、SDS和纳米材料前驱体氯金酸(HAuCl₄)浓度以及反应时间等因素，调控还原产物金纳米花形貌及粒径。表面张力、电导率、毛细管电泳及Zeta电位等实验结果表明PVP-SDS-HAuCl₄形成新的拟聚阴离子，透射电子显微镜和X射线衍射结果表明SDS、PVP和HAuCl₄的较低浓度组合更易获得表面凸起丰富的金纳米花。PVP-SDS拟聚阴离子发挥了二级软模板作用，在PVP (50 g∙L⁻¹)-SDS (2 mmol∙L⁻¹)-HAuCl₄ (0.25 mmol∙L⁻¹)溶液中调控合成的金纳米花为{111}晶面为主的面心立方结构，其平均等效粒径为108 nm，且表面上密集分布约16.5 nm的凸起。该金纳米花有较强的表面增强拉曼散射(SERS)活性，探针分子罗丹明6G的SERS信号强度依赖于金纳米花的表面凸起形貌。该研究中金纳米花的SERS增强因子最高达6.71×10⁷，优于同类金纳米花的文献报道水平(10⁶)；尽管低于石墨负载的金纳米粒子(1×10⁸)或阳离子软模板合成的金纳米棒(5×10⁹)，但成功避免了基质干扰或阳离子强吸附使应用受限。

关键词:

English

Strategy for Regulating Surface Protrusion of Gold Nanoflowers and Their Surface-Enhanced Raman Scattering

Ruiqin Feng ^1, ,
Ye Fan ^1, ,
Yun Fang ^{1,
,} ,
Yongmei Xia ^{1,2,
,}

1.
The Key Laboratory of Synthetic and Biological Colloids(Ministry of Education), School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122, Jiangsu Province, China;
2.
State Key Laboratory of Food Science and Technology, Jiangnan University, Wuxi 214122, Jiangsu Province, China

Corresponding author: Yun Fang, ; Yongmei Xia,

Received Date: 07 April 2023
Accepted Date: 07 June 2023
Revised Date: 06 June 2023
Available Online: 16 June 2023
Fund Project:
The project was supported by the National Natural Science Foundation of China (21606107).

Abstract: Mixed solutions of polyvinylpyrrolidone (PVP) and sodium dodecyl sulfate (SDS) were investigated by capillary electrophoresis, together with other technologies, to confirm the formation of PVP-bound SDS micelles through cation-bridging association, which shows the nature of polyanions and the ability to exchange Na⁺ of SDS with environmental cations. Because additional water-soluble precursors of nanomaterials are capable of entering the cation-bridging layer of the PVP-SDS pseudo-polyanions, we speculate that the PVP chain and PVP-bound SDS micelles located on both sides of the precursor may act as a two-stage soft template to synthesize nanomaterials with unique morphologies. In this study, PVP-SDS pseudo-polyanions were used as soft templates to promote the growth of gold particles into gold nanoflowers (AuNFs). Tensiometry, conductometry, capillary electrophoresis, and zeta potential measurements confirmed the formation of the new PVP-SDS-HAuCl₄ pseudo-polyanions. Transmission electron microscopy, X-ray diffraction, and UV-Vis spectroscopy analyses showed that the AuNFs synthesized in the mixed solution of PVP (50 g·L⁻¹)-SDS (2 mmol·L⁻¹)-HAuCl₄ (0.25 mmol·L⁻¹) possessed a face-centered cubic structure with abundant {111} crystal plane, demonstrating an average equivalent diameter of 108 nm with rich nano-protrusion of approximately 16.5 nm on the surface of AuNFs. The mechanistic study shows that PVP mainly acts as an in situ reductant for HAuCl₄ in PVP-bound SDS micelles that simultaneously act as the primary template to govern the size of the primary gold crystals. In addition to continuously reducing HAuCl₄, PVP functions as a secondary template, leading to primary gold crystals in a finite space linked by the PVP chain through preferential adsorption, stacked, and grown into mature AuNFs. Finally, a lower HAuCl₄ concentration and an adequate reduction period are favorable in the aforementioned process dominated by the soft template rather than by the crystal growth rule of gold particles; thus, the reduction rate of HAuCl₄ and nucleation-growth competition of gold particles can be regulated. Therefore, the optimal combination of low concentrations of SDS, PVP, and HAuCl₄, together with an appropriate reduction period, would result in synergism between the reduction rate of HAuCl₄, crystal growth rule of gold particles, and stacking degree of the primary gold crystals. AuNFs show strong surface-enhanced Raman scattering (SERS) activity for the Raman probe molecule of rhodamine 6G, strongly depending on the nano-protrusion morphology of AuNFs. The highest SERS enhancement factor can reach 6.71×10⁷, which is superior to the reported level of the similar AuNFs (10⁶). Because the particle sizes and morphologies of AuNFs can be precisely regulated, this strategy is a facile aqueous one-pot method for the synthesis of nanomaterials under normal temperature and pressure, which eliminates carrier requirements or adsorption interference from cationic surfactants, and has the potential to further enhance the SERS activity of the nanomaterials.

Key words:

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沈阳化工大学材料科学与工程学院沈阳 110142

调控金纳米花表面凸起的策略及其表面增强拉曼散射活性

通讯作者: 方云,Email:yunfang@126.com; 夏咏梅,Email:ymxia@jiangnan.edu.cn

English

Strategy for Regulating Surface Protrusion of Gold Nanoflowers and Their Surface-Enhanced Raman Scattering

Corresponding author: Yun Fang, ; Yongmei Xia,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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中国化学会秘书处

调控金纳米花表面凸起的策略及其表面增强拉曼散射活性

通讯作者: 方云,Email:yunfang@126.com; 夏咏梅,Email:ymxia@jiangnan.edu.cn

English

Strategy for Regulating Surface Protrusion of Gold Nanoflowers and Their Surface-Enhanced Raman Scattering

Corresponding author: Yun Fang, ; Yongmei Xia,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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