铁氧化物/贵金属复合材料的制备及其SERS效应研究
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摘要
随着纳米技术的迅速发展,磁性铁氧化物微纳结构因其独特的物化性能,在化学传感、生物技术／生物医学、环境治理、磁流体和数据存储等方面有着广泛的应用前景。其中,Fe3O4作为一种具有高磁饱和强度和低生物毒性的铁氧化物,在生物技术和生物医学领域具有独特的应用优势。而贵金属(Au、Ag)纳米粒子在激发光的作用下会产生独特的局域表面等离子体共振效应,这一发现有力地促进了表面增强拉曼光谱(SERS)技术的发展,使拉曼光谱在超高灵敏度检测方面取得了长足的进步,推动拉曼光谱成为迄今很少的,可达到单分子检测水平的技术。若将磁性纳米粒子的快速分离与靶向作用和贵金属纳米粒子的SERS效应有机结合,则可以实现二者功能的互补和优化,在利用磁示踪目标分析物的同时,还可以对其组分进行实时的检测分析。本文在此前提下,围绕铁氧化物、铁氧化物/贵金属复合材料的制备、表征及其在有机染料分子检测与处理等方面开展了一系列的工作,其主要内容如下：
一、在油酸的存在下,基于简单的溶剂热反应一步合成了粒径均一的a-Fe2O3介孔超结构(～2μm)。采用XRD、Raman、SEM、TEM、FT-IR、TG-DSC和N2等温吸附-脱附测试手段对获得样品的结构和形貌进行了表征。结果表明：由大量纳米尺度的颗粒通过稀疏组装而成的a-Fe2O3超结构不仅拥有较大的比表面积(78.3m2/g),还具有大量的介孔结构。研究了反应时间、表面活性剂及其用量、前躯体的量对样品结构、结晶性、形貌和尺寸的影响。基于上述的实验调查和分析,重点讨论了a-Fe2O3介孔超结构的形成机制以及随着反应时间的延长而出现的相转变(Fe3O4-a-Fe2O3-γ-Fe2O3),并给出了合理的解释。室温下,a-Fe2O3介孔超结构的磁饱和强度高达28.9emu/g,剩磁和矫顽力接近于零,呈现出少有的超顺磁行为。零场冷-场冷(ZFC-FC)测试证实：该材料在158K出现超顺磁转变温度一截止温度(TB),进一步证实了室温下α-Fe2O3介孔超结构的超顺磁行为。
二、以前期获得的Fe3O4纳米粒子,Fe3O4微球为磁性载体,以贵金属纳米颗粒(Au、Ag)为负载对象,通过简单的液相自组装和进一步生长,先后获得了Fe3O4/Au、Fe3O4/Ag复合纳米结构和具有不同负载浓度的Fe3O4@Au复合微球；UV-vis和磁性测试表明上述复合结构不但继承了贵金属所具有的局域表面等离子体共振吸收性能,而且还保留了良好的磁响应行为。以罗丹明(R6G)、对巯基吡啶(4-Mpy)分子为例,以正常分散的贵金属纳米粒子为参照,利用磁诱导调整聚集状态的理念,调整了复合结构的聚集状态,并研究了相应的SERS效应；证实了磁诱导的复合结构团聚体不仅富集了吸附的探针分子,而且提供了更多的活性"hot spots",其SERS效果有明显的改善。尤其是具有良好结构形貌的Fe3O4@Au复合微球,可作为今后开展特定生物组织、细胞的追踪和分析工作的良好选材。
三、采用一种简单、高效的化学液相方法合成了具有良好水溶性的Au纳米颗粒负载的Fe3O4@C光磁复合结构。通过改变Au纳米颗粒的加入量或进一步生长,可以有效的调节Au纳米颗粒的负载浓度(0.95%-5.93%, Au的原子百分数)。获得的复合结构对于废水中常见的染料分子表现出优异的SERS敏感性和催化降解能力。三种染料分子R6G、结晶紫(CV)和亚甲基蓝(MS)的SERS信号强度,随着Au的负载量的增加而提高。此外,催化实验表明：高负载量(5.93%)的Fe3O4@C@Au复合结构具有优秀的催化降解反应速率常数(0.331min-1),在10min内即可以实现MB溶液(1.0×10-5M)降解率高达98%,并且可以多次循环使用。上述结果表明Au负载的Fe3O4@C复合结构对于废水处理有一定的实际意义。
With the development of nanotechnology, iron oxide micro/nanostructures have displayed wide applications in chemical sensor, biotechnology/biomedicine, environmental treatment, magnetic fluids and data store due to their unique physicochemical properties. Especially, Fe3O4nanoparticles (NPs), which possess high saturation magnetization, low toxicity and good biocompatibility, have been comprehensively studied for a range of applications in biotechnology and biomedicine. Likewise, noble metal (Au, Ag) NPs can produce unique local surface plasmon resonance effect under the action of laser, which effectively improves the development of surface enhanced Raman spectroscopy (SERS). Nowadays, SERS technology has realized extreme sensitive detection and unwonted single molecular detection. It is easy to see that combination of magnetic NPs with noble metal NPs would endow possibilities for the development of interesting advanced composites as a result of bring together rapid separation, target and unique SERS effect. Not only can so advanced composites tract targeted analyte, also analyze them in time. In this dissertation, we reported some iron oxides and iron oxide/noble metal composites, mainly investigated their application in SERS detection and treatment of organic dyes. The main contents are included:
1. Uniform mesoporous hematite superstructures (～2μm) have been obtained via an oleic acid-assisted one-pot solvothermal route. The as-obtained products were characterized by XRD, XPS, Raman, SEM, TEM, FT-IR, TG-DSC and N2absorption-desorption isotherm. These results indicate that hematite superstructures self-assembled by using large number of NPs have high surface area (78.3m2/g) and mesoporous structures. Some factors (reaction time, surfactant, the amount of surfactant and precursor) influencing the phase, crystallinity and morphology of the products were systematically investigated. Based on the experimental investigation and analysis, we mainly discussed the formation mechanism of mesoporous hematite superstructures, phase transition (magnetite-hematite-maghemite) induced by reaction time and gave a proper explaination. The magnetic study reveals a surprising phenomenon that the mesoporous. hematite superstructures exhibit a unique superparamagnetic behavior with a high saturation magnetization (28.9 emu/g) at room temperature, which is seldom reported thus far for. hematite micro/nanostructures. The Zero field cooled-field cooled (ZFC-FC) measurement verified the existence of superparamagnetic blocking temperature (Tb=158K), which further approves the superparamagnetic behavior of the mesoporous superstructures at room temperature.
2. Fe3O4/Au, Fe3O4Ag and Fe3O4@Au composites with different Au content were obtained by phase-liquid assembly of Au, Ag NPs and further growth on Fe3O4supports. UV-visible absorption spectroscopy and magnetic measurements demonstrate not only do the obtained composites inherit local surface plasmon resonance effect of noble metal NPs, also keep excellent magnetic response behavior. Taking Rhodamine6G (R6G),4-mercaptopyridine (4-Mpy) model molecules for example and normal dispersed Au, Ag NPs for reference, a magnetic-induced idea was introduced to adjust aggregated states of above-mentioned composites and research their SERS performances. It indicates that magnetic-induced aggregated states of composites concentrate the adsorbed probe molecules, and create more "hot spots", which cause superior SERS performances. Especially, Fe3O4@Au composite microspheres with well-defined structures can be considered as candidates for track and analysis of special tissue and cell.
3. Water-dispersive Au-loaded Fe3O4@C composite microspheres were controllably synthesized by a simple and efficient chemical liquid-phase route. The amount of Au loading can be effectively tuned (0.95%-5.93%atomic percent) by altering the feeding amounts of solution Au NPs or further growth. The obtained Au-loaded Fe3O4@C composites exhibit both superior SERS sensitivity and catalytic degradation activity for organic dyes. The SERS signal intensity of R6G, crystal violet (CV) and methylene blue (MB) distinctly enhance with the increase of Au loading. Furthermore, the catalytic experiments of the Fe3O4@C@Au composite microspheres with a5.93%of Au loading demonstrate that the model organic dye of MB solution (1.0×10-5M) could be degraded within10min and the catalytic activity could be recovered without sharp activity loss in six runs, which indicate their superior catalytic degradation efficiency (98%) and rate (0.331min-1). These results indicate that Au-loaded Fe3O4@C composite microspheres could be served as promising materials in wastewater treatment.
一、在油酸的存在下,基于简单的溶剂热反应一步合成了粒径均一的a-Fe2O3介孔超结构(～2μm)。采用XRD、Raman、SEM、TEM、FT-IR、TG-DSC和N2等温吸附-脱附测试手段对获得样品的结构和形貌进行了表征。结果表明：由大量纳米尺度的颗粒通过稀疏组装而成的a-Fe2O3超结构不仅拥有较大的比表面积(78.3m2/g),还具有大量的介孔结构。研究了反应时间、表面活性剂及其用量、前躯体的量对样品结构、结晶性、形貌和尺寸的影响。基于上述的实验调查和分析,重点讨论了a-Fe2O3介孔超结构的形成机制以及随着反应时间的延长而出现的相转变(Fe3O4-a-Fe2O3-γ-Fe2O3),并给出了合理的解释。室温下,a-Fe2O3介孔超结构的磁饱和强度高达28.9emu/g,剩磁和矫顽力接近于零,呈现出少有的超顺磁行为。零场冷-场冷(ZFC-FC)测试证实：该材料在158K出现超顺磁转变温度一截止温度(TB),进一步证实了室温下α-Fe2O3介孔超结构的超顺磁行为。
二、以前期获得的Fe3O4纳米粒子,Fe3O4微球为磁性载体,以贵金属纳米颗粒(Au、Ag)为负载对象,通过简单的液相自组装和进一步生长,先后获得了Fe3O4/Au、Fe3O4/Ag复合纳米结构和具有不同负载浓度的Fe3O4@Au复合微球；UV-vis和磁性测试表明上述复合结构不但继承了贵金属所具有的局域表面等离子体共振吸收性能,而且还保留了良好的磁响应行为。以罗丹明(R6G)、对巯基吡啶(4-Mpy)分子为例,以正常分散的贵金属纳米粒子为参照,利用磁诱导调整聚集状态的理念,调整了复合结构的聚集状态,并研究了相应的SERS效应；证实了磁诱导的复合结构团聚体不仅富集了吸附的探针分子,而且提供了更多的活性"hot spots",其SERS效果有明显的改善。尤其是具有良好结构形貌的Fe3O4@Au复合微球,可作为今后开展特定生物组织、细胞的追踪和分析工作的良好选材。
三、采用一种简单、高效的化学液相方法合成了具有良好水溶性的Au纳米颗粒负载的Fe3O4@C光磁复合结构。通过改变Au纳米颗粒的加入量或进一步生长,可以有效的调节Au纳米颗粒的负载浓度(0.95%-5.93%, Au的原子百分数)。获得的复合结构对于废水中常见的染料分子表现出优异的SERS敏感性和催化降解能力。三种染料分子R6G、结晶紫(CV)和亚甲基蓝(MS)的SERS信号强度,随着Au的负载量的增加而提高。此外,催化实验表明：高负载量(5.93%)的Fe3O4@C@Au复合结构具有优秀的催化降解反应速率常数(0.331min-1),在10min内即可以实现MB溶液(1.0×10-5M)降解率高达98%,并且可以多次循环使用。上述结果表明Au负载的Fe3O4@C复合结构对于废水处理有一定的实际意义。
With the development of nanotechnology, iron oxide micro/nanostructures have displayed wide applications in chemical sensor, biotechnology/biomedicine, environmental treatment, magnetic fluids and data store due to their unique physicochemical properties. Especially, Fe3O4nanoparticles (NPs), which possess high saturation magnetization, low toxicity and good biocompatibility, have been comprehensively studied for a range of applications in biotechnology and biomedicine. Likewise, noble metal (Au, Ag) NPs can produce unique local surface plasmon resonance effect under the action of laser, which effectively improves the development of surface enhanced Raman spectroscopy (SERS). Nowadays, SERS technology has realized extreme sensitive detection and unwonted single molecular detection. It is easy to see that combination of magnetic NPs with noble metal NPs would endow possibilities for the development of interesting advanced composites as a result of bring together rapid separation, target and unique SERS effect. Not only can so advanced composites tract targeted analyte, also analyze them in time. In this dissertation, we reported some iron oxides and iron oxide/noble metal composites, mainly investigated their application in SERS detection and treatment of organic dyes. The main contents are included:
1. Uniform mesoporous hematite superstructures (～2μm) have been obtained via an oleic acid-assisted one-pot solvothermal route. The as-obtained products were characterized by XRD, XPS, Raman, SEM, TEM, FT-IR, TG-DSC and N2absorption-desorption isotherm. These results indicate that hematite superstructures self-assembled by using large number of NPs have high surface area (78.3m2/g) and mesoporous structures. Some factors (reaction time, surfactant, the amount of surfactant and precursor) influencing the phase, crystallinity and morphology of the products were systematically investigated. Based on the experimental investigation and analysis, we mainly discussed the formation mechanism of mesoporous hematite superstructures, phase transition (magnetite-hematite-maghemite) induced by reaction time and gave a proper explaination. The magnetic study reveals a surprising phenomenon that the mesoporous. hematite superstructures exhibit a unique superparamagnetic behavior with a high saturation magnetization (28.9 emu/g) at room temperature, which is seldom reported thus far for. hematite micro/nanostructures. The Zero field cooled-field cooled (ZFC-FC) measurement verified the existence of superparamagnetic blocking temperature (Tb=158K), which further approves the superparamagnetic behavior of the mesoporous superstructures at room temperature.
2. Fe3O4/Au, Fe3O4Ag and Fe3O4@Au composites with different Au content were obtained by phase-liquid assembly of Au, Ag NPs and further growth on Fe3O4supports. UV-visible absorption spectroscopy and magnetic measurements demonstrate not only do the obtained composites inherit local surface plasmon resonance effect of noble metal NPs, also keep excellent magnetic response behavior. Taking Rhodamine6G (R6G),4-mercaptopyridine (4-Mpy) model molecules for example and normal dispersed Au, Ag NPs for reference, a magnetic-induced idea was introduced to adjust aggregated states of above-mentioned composites and research their SERS performances. It indicates that magnetic-induced aggregated states of composites concentrate the adsorbed probe molecules, and create more "hot spots", which cause superior SERS performances. Especially, Fe3O4@Au composite microspheres with well-defined structures can be considered as candidates for track and analysis of special tissue and cell.
3. Water-dispersive Au-loaded Fe3O4@C composite microspheres were controllably synthesized by a simple and efficient chemical liquid-phase route. The amount of Au loading can be effectively tuned (0.95%-5.93%atomic percent) by altering the feeding amounts of solution Au NPs or further growth. The obtained Au-loaded Fe3O4@C composites exhibit both superior SERS sensitivity and catalytic degradation activity for organic dyes. The SERS signal intensity of R6G, crystal violet (CV) and methylene blue (MB) distinctly enhance with the increase of Au loading. Furthermore, the catalytic experiments of the Fe3O4@C@Au composite microspheres with a5.93%of Au loading demonstrate that the model organic dye of MB solution (1.0×10-5M) could be degraded within10min and the catalytic activity could be recovered without sharp activity loss in six runs, which indicate their superior catalytic degradation efficiency (98%) and rate (0.331min-1). These results indicate that Au-loaded Fe3O4@C composite microspheres could be served as promising materials in wastewater treatment.
引文
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