Cu_2O/Ag微纳米结构的制备及其表面增强拉曼散射性能研究
摘要
由于表面增强拉曼散射（Surface-enhanced Raman Scattering，SERS）活性基底匮乏以及应用范围有限等问题，因此对SERS基底的研究十分必要。本论文开展了对半导体Cu2O，贵金属Ag及其复合物纳微米结构基底的SERS性能的研究。此研究不仅丰富了SERS活性基底的种类，也拓宽了SERS光谱技术的应用领域。主要研究内容包括：
1.用简单的水浴方法，在80℃条件下，以葡萄糖为还原剂，调节柠檬酸钠碳酸钠混合物浓度和反应时间，合成了一系列具有良好单分散性的不同形貌的Cu2O微/纳米颗粒。并且用较短时间获得了空心结构Cu2O纳米骨架，补充和改进了原位选择氧化刻蚀方法。
2.采用Cu2O化学模板方法制备了由纳米薄片组装而成的空心Ag纳米颗粒。稀硝酸的浓度对空心Ag纳米颗粒的合成起重要作用，随着混合物中酸浓度的增加Cu2O含量逐渐减少，而Ag含量逐渐增多，最后当加入的稀硝酸浓度达到2mM时，Cu2O基本消失，形成了表面粗糙的由纳米薄片组装而成的空心Ag纳米颗粒。与其他样品对比空心Ag纳米颗粒表现出最好的SERS能力，增强因子达到3.3×104。我们认为是空心结构和特殊的粗糙表面共同增加了“拉曼热点”和罗丹明B探针分子的吸附，因而使空心Ag纳米颗粒相对于其它样品呈现出更高的拉曼信号。此外，还对空心Ag纳米颗粒基底的灵敏度与均一性进行了测试，发现当罗丹明B浓度低到1×10-8M时仍可得到明显的拉曼峰，并且样品具有很好的均一性，其相对标准方差低于9.6%。这些特性对拉曼基底的实际应用是十分重要的。
3.采用原位还原方法，在截角八面体Cu2O和Cu2O纳米骨架上分别包覆Ag纳米粒子，制备了实心Ag-Cu2O复合物微米结构（Ag-Cu2O CMSs）和空心Cu2O/Ag复合物纳米骨架（Cu2O/Ag CNFs）。随着母液中AgNO3含量的提高，所得实心Ag-Cu2O CMSs和空心Cu2O/Ag CNFs中的Ag颗粒尺寸和在Cu2O表面包覆的密度均增大，并趋于包覆完整。在AgNO3用量为0.40mM时，两种复合微纳米结构中Ag颗粒在Cu2O表面包覆完整且均匀，两者之间是生长在一起，且此时Ag与Cu2O之间形成的有效肖特基结面积达到最大。
4.以原位还原方法制备的实心Ag-Cu2O CMSs和空心Cu2O/Ag CNFs复合微纳米结构为SERS基底，以罗丹明B为探针分子。对两种复合微纳米结构SERS性能进行研究，发现均具有随着AgNO3浓度的增加，产物的SERS性能先提高后降低规律。并且，在加入0.40mM的AgNO3时所制备实心Ag-Cu2O CMSs和空心Cu2O/Ag(2) CNFs均获得各自最优的拉曼增强特性。增强因子分别可达到7.8×104和1.8×105，其相对标准方差分别低于9.3%和2.88%，后者空心结构优于前者。并且都显著优于相同尺寸纯Ag纳米颗粒产生的SERS性能。
5.将空心Cu2O/Ag(2) CNFs复合微纳米结构获得显著增强SERS归因于：一方面，Cu2O/Ag(2) CNFs能吸附更多的目标分子，并在界面处产生了更多的拉曼热点；另一方面，Ag与Cu2O之间肖特基结的引入，除了金属Ag表面局域等离子体共振产生的放大的电磁场外，还在Ag纳米颗粒与Cu2O之间形成了较强电磁场。在这两部分放大的电磁场和“借SERS效应”的协同作用下，使更多的吸附在Cu2O/Ag(2) CNFs表面的探针分子的SERS性能得以增强。因而Cu2O/Ag(2) CNFs优于纯Ag纳米颗粒，表现出更好的SERS性质。
The lack of notable metal Surface-enhanced Raman scattering (SERS) substratelimits the breadth of practical applications. In this work, we had a study about Cu2Osemiconductor, Ag nanoparticle and Ag-Cu2O composite composite structure SERSsubstrate, which has an important and significance. The study enrichs the kinds ofthe SERS substrates, and also widen the application of SERS technique. The mainresearch works are listed as following:
1. We reported a simple solution-phase route for synthesis of Cu2O crystals withdifferent morphologies at temperature of80℃. In our system, the morphologicalevolution of Cu2O crystals has been investigated by using different amounts ofsodium citrate and sodium carbonate mixed solution, and then Cu2O nanoframes areobtained in relatively shorter time by stirring the resulting solution in air for about12hours at room temperature. The condition/theory for synthesis of Cu2O nanoframesand nanocages in our previous work is supplemented. Finally, the morphologicalevolution and the growth mechanism are also explored.
2. Uniform silver hollow nanoparticles assembled by nanosheets have beensynthesized by using Cu2O as chemical template at room temperature. It was foundthat the concentrations of acid were critical to the formation of perfect nanosheetassembled hollow silver nanoparticles. In the reaction system, the Ag+ions werereduced by Cu+ions released from Cu2O template. When the concentration of acidincreased to2mM, the Cu2O template dissolved completely, and perfect nanosheetassembled hollow silver nanoparticles were generated. The hollow silvernanoparticles show the optimum SERS properties with an enhancement factor of3.3×104. The relative standard deviation (RSD) of Raman intensity is lower than9.6%, which are important for practical assays. The reasons for the enhancement of theSERS performance are investigated in detail.
3. Ag-Cu2O composite microstructures (Ag-Cu2O CMSs) and hollow Cu2O/Agcomposite nanoframes (Cu2O/Ag CNFs) with tunable silver content have beensynthesized by directly deposited Ag onto Cu2O truncated octahedra/Cu2Onanoframes. Ag contents on the surface of Cu2O can be tuned through the variation ofthe concentration of AgNO3. When0.40mM AgNO3is used, Ag are uniformly andcompactly coated on Cu2O, and the effective coverage area of Ag on Cu2O isenhanced significantly.
4. When0.40mM AgNO3is used, the prepared Ag-Cu2O CMSs and Cu2O/AgCNFs show significantly improved SERS properties. Ag-Cu2O CMSs with anenhancement factor is7.8×104, the value of RSD for the sample is lower than9.3%;Cu2O/Ag CNFs with an enhancement factor is1.8×105, the value of RSD for thesample is lower than2.88%. Cu2O/Ag CNFs exhibit higher SERS signals thanAg-Cu2O CMSs, and then pure Ag.
5. The Cu2O/Ag (2) CNFs exhibits the highest SERS performance, this may bedue to (1) more Raman hot spots are introduced not only due to the Ag hot spots butalso the hot spots formed at the interface between Ag NPs and the Cu2O.(2) Underthe irradiation of a suitable laser, Cu2O/Ag CNFs cause charge transfer from Ag NPsto Cu2O nanoframes, which induce a larger electromagnetic field, except that A largeelectromagnetic field caused by localized surface plasmon resonance (LSPR) inducedby metal Ag. The adsorbed RB molecules are located in two part of enhancedelectromagnetic field and consequently exhibit a stronger Raman signal.
1.用简单的水浴方法，在80℃条件下，以葡萄糖为还原剂，调节柠檬酸钠碳酸钠混合物浓度和反应时间，合成了一系列具有良好单分散性的不同形貌的Cu2O微/纳米颗粒。并且用较短时间获得了空心结构Cu2O纳米骨架，补充和改进了原位选择氧化刻蚀方法。
2.采用Cu2O化学模板方法制备了由纳米薄片组装而成的空心Ag纳米颗粒。稀硝酸的浓度对空心Ag纳米颗粒的合成起重要作用，随着混合物中酸浓度的增加Cu2O含量逐渐减少，而Ag含量逐渐增多，最后当加入的稀硝酸浓度达到2mM时，Cu2O基本消失，形成了表面粗糙的由纳米薄片组装而成的空心Ag纳米颗粒。与其他样品对比空心Ag纳米颗粒表现出最好的SERS能力，增强因子达到3.3×104。我们认为是空心结构和特殊的粗糙表面共同增加了“拉曼热点”和罗丹明B探针分子的吸附，因而使空心Ag纳米颗粒相对于其它样品呈现出更高的拉曼信号。此外，还对空心Ag纳米颗粒基底的灵敏度与均一性进行了测试，发现当罗丹明B浓度低到1×10-8M时仍可得到明显的拉曼峰，并且样品具有很好的均一性，其相对标准方差低于9.6%。这些特性对拉曼基底的实际应用是十分重要的。
3.采用原位还原方法，在截角八面体Cu2O和Cu2O纳米骨架上分别包覆Ag纳米粒子，制备了实心Ag-Cu2O复合物微米结构（Ag-Cu2O CMSs）和空心Cu2O/Ag复合物纳米骨架（Cu2O/Ag CNFs）。随着母液中AgNO3含量的提高，所得实心Ag-Cu2O CMSs和空心Cu2O/Ag CNFs中的Ag颗粒尺寸和在Cu2O表面包覆的密度均增大，并趋于包覆完整。在AgNO3用量为0.40mM时，两种复合微纳米结构中Ag颗粒在Cu2O表面包覆完整且均匀，两者之间是生长在一起，且此时Ag与Cu2O之间形成的有效肖特基结面积达到最大。
4.以原位还原方法制备的实心Ag-Cu2O CMSs和空心Cu2O/Ag CNFs复合微纳米结构为SERS基底，以罗丹明B为探针分子。对两种复合微纳米结构SERS性能进行研究，发现均具有随着AgNO3浓度的增加，产物的SERS性能先提高后降低规律。并且，在加入0.40mM的AgNO3时所制备实心Ag-Cu2O CMSs和空心Cu2O/Ag(2) CNFs均获得各自最优的拉曼增强特性。增强因子分别可达到7.8×104和1.8×105，其相对标准方差分别低于9.3%和2.88%，后者空心结构优于前者。并且都显著优于相同尺寸纯Ag纳米颗粒产生的SERS性能。
5.将空心Cu2O/Ag(2) CNFs复合微纳米结构获得显著增强SERS归因于：一方面，Cu2O/Ag(2) CNFs能吸附更多的目标分子，并在界面处产生了更多的拉曼热点；另一方面，Ag与Cu2O之间肖特基结的引入，除了金属Ag表面局域等离子体共振产生的放大的电磁场外，还在Ag纳米颗粒与Cu2O之间形成了较强电磁场。在这两部分放大的电磁场和“借SERS效应”的协同作用下，使更多的吸附在Cu2O/Ag(2) CNFs表面的探针分子的SERS性能得以增强。因而Cu2O/Ag(2) CNFs优于纯Ag纳米颗粒，表现出更好的SERS性质。
The lack of notable metal Surface-enhanced Raman scattering (SERS) substratelimits the breadth of practical applications. In this work, we had a study about Cu2Osemiconductor, Ag nanoparticle and Ag-Cu2O composite composite structure SERSsubstrate, which has an important and significance. The study enrichs the kinds ofthe SERS substrates, and also widen the application of SERS technique. The mainresearch works are listed as following:
1. We reported a simple solution-phase route for synthesis of Cu2O crystals withdifferent morphologies at temperature of80℃. In our system, the morphologicalevolution of Cu2O crystals has been investigated by using different amounts ofsodium citrate and sodium carbonate mixed solution, and then Cu2O nanoframes areobtained in relatively shorter time by stirring the resulting solution in air for about12hours at room temperature. The condition/theory for synthesis of Cu2O nanoframesand nanocages in our previous work is supplemented. Finally, the morphologicalevolution and the growth mechanism are also explored.
2. Uniform silver hollow nanoparticles assembled by nanosheets have beensynthesized by using Cu2O as chemical template at room temperature. It was foundthat the concentrations of acid were critical to the formation of perfect nanosheetassembled hollow silver nanoparticles. In the reaction system, the Ag+ions werereduced by Cu+ions released from Cu2O template. When the concentration of acidincreased to2mM, the Cu2O template dissolved completely, and perfect nanosheetassembled hollow silver nanoparticles were generated. The hollow silvernanoparticles show the optimum SERS properties with an enhancement factor of3.3×104. The relative standard deviation (RSD) of Raman intensity is lower than9.6%, which are important for practical assays. The reasons for the enhancement of theSERS performance are investigated in detail.
3. Ag-Cu2O composite microstructures (Ag-Cu2O CMSs) and hollow Cu2O/Agcomposite nanoframes (Cu2O/Ag CNFs) with tunable silver content have beensynthesized by directly deposited Ag onto Cu2O truncated octahedra/Cu2Onanoframes. Ag contents on the surface of Cu2O can be tuned through the variation ofthe concentration of AgNO3. When0.40mM AgNO3is used, Ag are uniformly andcompactly coated on Cu2O, and the effective coverage area of Ag on Cu2O isenhanced significantly.
4. When0.40mM AgNO3is used, the prepared Ag-Cu2O CMSs and Cu2O/AgCNFs show significantly improved SERS properties. Ag-Cu2O CMSs with anenhancement factor is7.8×104, the value of RSD for the sample is lower than9.3%;Cu2O/Ag CNFs with an enhancement factor is1.8×105, the value of RSD for thesample is lower than2.88%. Cu2O/Ag CNFs exhibit higher SERS signals thanAg-Cu2O CMSs, and then pure Ag.
5. The Cu2O/Ag (2) CNFs exhibits the highest SERS performance, this may bedue to (1) more Raman hot spots are introduced not only due to the Ag hot spots butalso the hot spots formed at the interface between Ag NPs and the Cu2O.(2) Underthe irradiation of a suitable laser, Cu2O/Ag CNFs cause charge transfer from Ag NPsto Cu2O nanoframes, which induce a larger electromagnetic field, except that A largeelectromagnetic field caused by localized surface plasmon resonance (LSPR) inducedby metal Ag. The adsorbed RB molecules are located in two part of enhancedelectromagnetic field and consequently exhibit a stronger Raman signal.
引文
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