银纳米碗、纳米笼与中空多孔纳米片的制备研究
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摘要
金、银纳米颗粒及其纳米壳层的一切特性及其应用,与其纳米颗粒的尺寸、形貌有很大的关系,特别是特殊结构(空心、碗状、笼状等),有可能实现特殊的性能。因此,对特殊形貌,特定尺寸金银纳米颗粒的制备研究显得尤为重要。
本文在综述了国内外纳米科技的研究进展和金属银空心孔洞纳米结构的研究现状的基础上,针对目前采用模板法制备的碗状及笼状结构,通常是多晶或无定形的缺陷,在方法上也有一定的局限性,本文提出了一种简单的化学沉积法,在不需要模板的情况下,通过控制反应前驱物形貌以及反应条件的方法,制备出了银纳米碗、纳米笼以及中空夹层银纳米片,对其形貌和结构进行了表征,并对这种结构的形成机理和影响因素进行了分析,为新的碗状、笼状及中空多孔结构的制备和应用提供了新的思路。本文主要内容及结论如下：
采用化学沉积法,以硝酸银为原料,甲醛作为还原剂,PVP为分散剂,在0℃下成功合成了内部空心表面呈大孔洞的粒径在80-150nm的碗状银纳米结构。研究了不同阶段的形貌和结构变化,探讨了氢氧化钠浓度、反应温度、还原剂浓度、PVP含量对最终形貌的影响规律。结果表明,通过控制氢氧化钠的浓度可以控制碗状结构的尺寸。不加PVP时也得到碗状结构,PVP在这个反应中主要起着分散剂的作用。还原生成的银原子在氧化银表面的沉积生长和反应中气体的生成释放是碗状结构形成的关键。通过紫外吸收光谱的分析,碗状结构的最大吸收峰位置在478nm,相比纳米粒子和纳米线发生了很大的红移,表明其具有更好的光学吸收性能。
在与碗状结构同等制备条件下,采用硼氢化钠为还原剂,得到了表面多孔内部空心的的笼状结构,粒径在100nm左右。温度、还原剂浓度、氢氧化钠浓度等反应条件,对笼状结构的形成有很大的影响,条件的改变,就会有环状、框架状、不规则粒子的生成,通过机理的分析,导致这些结构出现的原因是由于笼状结构生成的过程中,表面孔过大并且比较密集,使得笼的框架坍塌,就会得到环状或坍塌后的不规则粒子生成。
通过不同阶段的研究分析,再结合不同反应条件对产物的影响因素分析,得出碗状结构形成的机理是由以下几步组成的：1.Ag2O纳米小粒子的生成；2.Ag2O纳米小颗粒聚集成球形Ag2O粒子；3.Ag2O被还原成Ag；4.生成的Ag原子在Ag2O表面沉积生长和表面带小孔洞空心结构的逐渐形成；5.反应过程中气泡的释放促使表面大孔洞的形成,最终得到碗状结构。由于ostwald熟化效应,随着反应时间的增长,表面也表的更加的光滑平整。笼状结构的形成于碗状结构的不同之处在于第五步,反应过程中气体生成和释放的速率不一样促使最终粒子表面的孔洞不同。
以碗状结构和笼状结构的形成机理为基础,通过改变添加剂来改变前驱物的组成和结构,得到了片状的中空多孔片状银纳米结构,边长为1微米左右,厚度小于100nm。通过不同时间段的形貌和结构分析,我们初步推断了中空多孔银纳米片的形成机理。
It is well known that the properties of gold and silver nanostructures are strongly dependent on their size, morphology, and composition. Very recently, the synthesis of cavity-containing metal nanoparticles with reduced symmetry, such as nanobowls, nanocups and hollow nanospheres has attracted great attention, as it could have specific applications in optics, magnetics, catalysts, biosensors, microchip reactors. Therefore it's important to do research on the special appearance, specific size of gold and silver nanoparticles.
This paper reviews the progress of research on metallic silver nanostructure with hollow cavity at home and abroad. The nanobowl and nanocage obtained by template recently are often polycrystalline or amorphous, and the method is limited. This paper presents a simple chemical deposition method without any templates. In our work, we have developed a simple chemical deposition method for the preparation of silver nanobowl, nanocage and hollow porousnanoplate through controlling the reaction conditions and the morphology of precursor. Their morphology and structure were characterized. The mechanism and influence factors of the formation of these structures were discussed. This may provides a new ideas for the new preparation and application of reduced symmetric structure. In this paper, the content and conclusions are as follows:
Silver nanobowls with the diameter of 80-150 nm have been successfully synthesized in this paper at 0℃through chemical deposition method using silver nitrate as precursor, formaldehyde as reductant, and PVP as dispersing agent. The changes of morphology at different stages were characterized, and the effect of the sodium hydroxide concentration, reaction temperature, the reductant concentration, PVP content on the the final morphology were studied. Results show that, the deposition and growth of Ag reduced by formaldehyde on the surface of silver oxide and the formation of bubbles during the reactions are the key for the formation of bowllike structure. Moreover, the size of bowl particles can tuned by the concentration of sodium hydroxide. Bowllike structures were also obtained without PVP, which indicates that PVP only plays the main role of dispersant in this reaction. The UV/vis absorption spectra showed the maximum absorption peaks at 478 nm. Compared to nanoparticles and nanowires, it has red shift which show these structures has larger absorbtion region.
Based on the bowlike structure, we have synthesis 100nm cagelike structure with internal hollow and some holes on the surface, using sodium borohydride as reducing agent. The ring-shaped, frame, and irregular particles are present following the change of reaction conditions, such as temperature and the concentration of sodium hydroxide, etc. Through the mechanism analysis, these structures obtained are attributed to the collapse of the framework,the enlarge and merging of the holes on the surface during the formation of cagelike structure.
On the basis of the above results, the processes of bowlike nanoparticles can be possibly summarized:(i) formation of Ag2O nanocrystallites; (ii) spherical aggregation of primary Ag2O crystallites; (iii) reductive conversion of Ag2O to Ag; (iv) deposition of Ag atoms on Ag2O and formation of hollow structures with pinholes on the surface; (v) growth of the main pore on the surface caused by the releasing of bubbles and formation of the bowllike morphology. The smooth surface is due to the Ostwald ripening process as the reaction time proceeded. Compared to the bowllike structures, cagelike structures are different in the fifth step. The difference in the generating and releasing rate of bubbles lead to the diffence on the morphology of the particles.
Based on the formation mechanism of bowlike and cagelike structures, we have obtained hollow and porous silver nanosheets with a side length of 1 micrometer and thickness less than 100 nm by turning the composition of the precursor. Through the morphology and structure change at each step in the formation, we concluded the formation mechanism of these stuctures.
本文在综述了国内外纳米科技的研究进展和金属银空心孔洞纳米结构的研究现状的基础上,针对目前采用模板法制备的碗状及笼状结构,通常是多晶或无定形的缺陷,在方法上也有一定的局限性,本文提出了一种简单的化学沉积法,在不需要模板的情况下,通过控制反应前驱物形貌以及反应条件的方法,制备出了银纳米碗、纳米笼以及中空夹层银纳米片,对其形貌和结构进行了表征,并对这种结构的形成机理和影响因素进行了分析,为新的碗状、笼状及中空多孔结构的制备和应用提供了新的思路。本文主要内容及结论如下：
采用化学沉积法,以硝酸银为原料,甲醛作为还原剂,PVP为分散剂,在0℃下成功合成了内部空心表面呈大孔洞的粒径在80-150nm的碗状银纳米结构。研究了不同阶段的形貌和结构变化,探讨了氢氧化钠浓度、反应温度、还原剂浓度、PVP含量对最终形貌的影响规律。结果表明,通过控制氢氧化钠的浓度可以控制碗状结构的尺寸。不加PVP时也得到碗状结构,PVP在这个反应中主要起着分散剂的作用。还原生成的银原子在氧化银表面的沉积生长和反应中气体的生成释放是碗状结构形成的关键。通过紫外吸收光谱的分析,碗状结构的最大吸收峰位置在478nm,相比纳米粒子和纳米线发生了很大的红移,表明其具有更好的光学吸收性能。
在与碗状结构同等制备条件下,采用硼氢化钠为还原剂,得到了表面多孔内部空心的的笼状结构,粒径在100nm左右。温度、还原剂浓度、氢氧化钠浓度等反应条件,对笼状结构的形成有很大的影响,条件的改变,就会有环状、框架状、不规则粒子的生成,通过机理的分析,导致这些结构出现的原因是由于笼状结构生成的过程中,表面孔过大并且比较密集,使得笼的框架坍塌,就会得到环状或坍塌后的不规则粒子生成。
通过不同阶段的研究分析,再结合不同反应条件对产物的影响因素分析,得出碗状结构形成的机理是由以下几步组成的：1.Ag2O纳米小粒子的生成；2.Ag2O纳米小颗粒聚集成球形Ag2O粒子；3.Ag2O被还原成Ag；4.生成的Ag原子在Ag2O表面沉积生长和表面带小孔洞空心结构的逐渐形成；5.反应过程中气泡的释放促使表面大孔洞的形成,最终得到碗状结构。由于ostwald熟化效应,随着反应时间的增长,表面也表的更加的光滑平整。笼状结构的形成于碗状结构的不同之处在于第五步,反应过程中气体生成和释放的速率不一样促使最终粒子表面的孔洞不同。
以碗状结构和笼状结构的形成机理为基础,通过改变添加剂来改变前驱物的组成和结构,得到了片状的中空多孔片状银纳米结构,边长为1微米左右,厚度小于100nm。通过不同时间段的形貌和结构分析,我们初步推断了中空多孔银纳米片的形成机理。
It is well known that the properties of gold and silver nanostructures are strongly dependent on their size, morphology, and composition. Very recently, the synthesis of cavity-containing metal nanoparticles with reduced symmetry, such as nanobowls, nanocups and hollow nanospheres has attracted great attention, as it could have specific applications in optics, magnetics, catalysts, biosensors, microchip reactors. Therefore it's important to do research on the special appearance, specific size of gold and silver nanoparticles.
This paper reviews the progress of research on metallic silver nanostructure with hollow cavity at home and abroad. The nanobowl and nanocage obtained by template recently are often polycrystalline or amorphous, and the method is limited. This paper presents a simple chemical deposition method without any templates. In our work, we have developed a simple chemical deposition method for the preparation of silver nanobowl, nanocage and hollow porousnanoplate through controlling the reaction conditions and the morphology of precursor. Their morphology and structure were characterized. The mechanism and influence factors of the formation of these structures were discussed. This may provides a new ideas for the new preparation and application of reduced symmetric structure. In this paper, the content and conclusions are as follows:
Silver nanobowls with the diameter of 80-150 nm have been successfully synthesized in this paper at 0℃through chemical deposition method using silver nitrate as precursor, formaldehyde as reductant, and PVP as dispersing agent. The changes of morphology at different stages were characterized, and the effect of the sodium hydroxide concentration, reaction temperature, the reductant concentration, PVP content on the the final morphology were studied. Results show that, the deposition and growth of Ag reduced by formaldehyde on the surface of silver oxide and the formation of bubbles during the reactions are the key for the formation of bowllike structure. Moreover, the size of bowl particles can tuned by the concentration of sodium hydroxide. Bowllike structures were also obtained without PVP, which indicates that PVP only plays the main role of dispersant in this reaction. The UV/vis absorption spectra showed the maximum absorption peaks at 478 nm. Compared to nanoparticles and nanowires, it has red shift which show these structures has larger absorbtion region.
Based on the bowlike structure, we have synthesis 100nm cagelike structure with internal hollow and some holes on the surface, using sodium borohydride as reducing agent. The ring-shaped, frame, and irregular particles are present following the change of reaction conditions, such as temperature and the concentration of sodium hydroxide, etc. Through the mechanism analysis, these structures obtained are attributed to the collapse of the framework,the enlarge and merging of the holes on the surface during the formation of cagelike structure.
On the basis of the above results, the processes of bowlike nanoparticles can be possibly summarized:(i) formation of Ag2O nanocrystallites; (ii) spherical aggregation of primary Ag2O crystallites; (iii) reductive conversion of Ag2O to Ag; (iv) deposition of Ag atoms on Ag2O and formation of hollow structures with pinholes on the surface; (v) growth of the main pore on the surface caused by the releasing of bubbles and formation of the bowllike morphology. The smooth surface is due to the Ostwald ripening process as the reaction time proceeded. Compared to the bowllike structures, cagelike structures are different in the fifth step. The difference in the generating and releasing rate of bubbles lead to the diffence on the morphology of the particles.
Based on the formation mechanism of bowlike and cagelike structures, we have obtained hollow and porous silver nanosheets with a side length of 1 micrometer and thickness less than 100 nm by turning the composition of the precursor. Through the morphology and structure change at each step in the formation, we concluded the formation mechanism of these stuctures.
引文
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