多功能纳米复合水凝胶与石墨烯纳米复合材料的制备及性能研究
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摘要
纳米复合水凝胶将纳米材料的优异性质与水凝胶本身独特的性能结合起来,使之性能协同或互补,形成单一材料所不具备的新的性能,在药物控制释放、催化剂、传感器及生物材料等领域都有很广泛的应用,因而备受关注。目前在合成上,一般需要先制备纳米材料然后再使其与单体共聚合,或者利用合成好的水凝胶作为反应场所来制备纳米复合材料。这样的合成需要多步反应,合成过程相对较复杂,也较难控制,因此,寻找新的简单有效的制备方法是目前亟待解决的一项重要课题。虽然新的纳米材料随着纳米技术的迅猛发展而层出不穷,但与之相对应的新的复合水凝胶种类则比较少,发展并合成新颖的纳米复合水凝胶具有重要的研究意义和应用前景。本论文正是基于上述考量,以合成新颖性质优异的纳米材料为基础,进而与智能水凝胶复合成具有多功能的新型复合材料。在调研大量文献的基础上,同时结合本课题组的优势,发展利用γ射线“一步”辐射等途径制备纳米复合水凝胶,并探索研究相关新材料在传感器、可控催化剂、微流体开关及加热源等方面的具体应用。本论文研究内容分述如下：
1.利用γ射线辐射技术“一步”合成PNIPAM/AuNPs复合水凝胶。在这个反应体系中,PNIPAM水凝胶与AuNPs同步形成。合成过程简单,易于控制。考察了单体浓度、吸收剂量以及Au3+浓度对复合水凝胶的光学与热学性能的影响。结果表明,随着单体浓度的增加,复合凝胶中的纳米颗粒粒径随之增大,吸收剂量与Au3+浓度可以有效的控制水凝胶的温敏性与AuNPs的含量。研究了PNIPAM/AuNPs复合水凝胶优异的催化性能、可重复性,以及其利用温度导致的相变对其催化活性的可控性。
2.发展Y射线辐射引发原位聚合制备了PNIP AM/GO复合水凝胶。复合水凝胶的颜色以及相变温度随着GO载入量的不同而不同。由于GO优异的光吸收能力,赋予复合水凝胶独特的光热性能,即通过近红外(NIR)激光照射可以远程控制其相变。基于NIR照射与否,这种相变是完全可逆的。GO的载入量以及光照时间可以用于控制光诱导温度的增长。利用PNIPAM/GO复合水凝胶优异的光热性能,成功的制备了一个微流体开关。
3.将PNIPAM水凝胶作为一个化学反应器,在其三维网络中合成铁氧化物纳米颗粒得到(?)NIPAM/Fe304纳米复合水凝胶,并对其进行了详细的表征。由于很多的科研工作者对PNIPAM/Fe3O4纳米复合水凝胶的磁性能予以特别的关注,而忽略了其黑色的水凝胶本身的光热性能。其优异的光热性能也是第一次得到了深入的研究。实验结果表明NIR激光照射可以很快的诱使PNIPAM/Fe3O4纳米复合水凝胶相变,而且这种相变可以通过激光照射与否进行控制,具有可逆性。辐照时间越长,水凝胶周围环境温度越高。基于PNIPAM/Fe3O4纳米复合水凝胶优异的光热与磁性性能,制备了一个磁控定点光加热源。
4采用丫射线辐照方法还原了水溶液中的GO,并利用X射线衍射、红外光谱等检测手段对其还原程度进行表征。如果在GO的水溶液中加入Au3+并进行辐照,经过表征证明Au3+也得到了还原并负载于还原氧化石墨烯上。在这里,Au3+的还原与GO的还原同步进行,并且复合材料中AuNP的粒径随着Au3+浓度的增加而增加。此外,考察了r-GO/AuNPs复合材料的催化性能。
Nanocomposite hydrogels combine the novel properties of nanoparticles with unique properties of hydrogels which lead to new functions originated from the synergic effect or complementary performance of components. Such nanocomposite hydrogels have attracted intensive interests in many fields such as controlled drug delivery, catalysis, sensors and biomaterials. Nowadays, the methods for preparing nanocomposite hydrogels require the mix pre-formed nanoparticles with a hydrogel precursor followed by gelation, or in situ synthesis of metal nanoparticles within polymeric network architectures. The dispersibility and the size of Au nanoparticles in hydrogels are difficult to be controlled by those multi-steps synthesis routes requiring the separate preparation of metal nanoparticles and hydrogels. With the fast development of technologies for synthesis and application of the nanocomposites, it is of great significance to search for a simple and effective method of preparing nanocomposite hydrogel. Herein, based on synthesis of multi-functional nanocomposite hydrogel and novel nanomaterials with unique properties, also combining the advantages of our research group, one-step y-irradiation was used as an effective method to synthesize nanocomposite hydrogel. Moreover, the potential applications for those nanocomposites in the sensor, catalysis, microvalve and heating source are also explored. More details are as follows:
1. Thermosensitive poly (N-isopropylacrylamide)/Au nanoparticles (PNIPAM/Au) nanocomposite hydrogels have been synthesized by in situ y-radiation-assisted polymerization. In this reaction, the PNIPAM hydrogels and the Au nanoparticles (NPs) are formed simultaneously, demonstrating an easy and straightforward synthetic strategy for the preparation of a uniform nanocomposite. The results suggest that increasing the monomer content during the preparation of nanocomposite materials can increase the sizes of Au nanoparticles. The effects of irradiation dose and concentration of HAUCI44H2O on the optical and thermal properties of the hydrogel have also been investigated. The PNIPAM/Au nanocomposite hydrogels can act as an excellent catalyst for the conversion of o-nitroaniline to1,2-benzenediamine, and catalytic activity of the composite hydrogel can be tuned by the volume transition of PNIPAM.
2. A photo-thermal sensitive PNIPAM/GO nanocomposite hydrogel have been synthesized by in situ y-irradiation-assisted polymerization. The colors and phase transition temperatures of PNIPAM/GO hydrogels change with different GO doping level. Due to the high optical absorbance of GO, the nanocomposite hydrogel shows excellent photo-thermal property where its phase transitions can be controlled remotely by the near-infrared (NIR) laser irradiation and is completely reversible via laser exposure or non exposure. With higher GO loading, the NIR-induced temperature of the nanocomposite hydrogel increases quicker than lower doping level and can be tunable effectively by irradiation time. The nanocomposite hydrogel with excellent photo-thermal property would have great application in biomedical, especially microfluidic device, which have been proved in our experiment as a remote microvalve to control the fluidic flow.
3. The PNIPAM hydrogels have been used as reactors for the synthesis of ferroferric oxid, and the excellent laser-induced photo-thermal property of PNIPAM/Fe3O4nanocomposite hydrogel which was ignored in the previous studies was investigated in the application of near-infrared (NIR) laser irradiation. The loading of Fe3O4nanoparticles in the hydrogel can be manipulated to get the desired remote heating on application of NIR laser exposure. The phase transition of the magnetic hydrogel was controlled easily by the laser exposure or non-exposure, and it was completely reversible. The laser-induced temperature was increased quickly with the irradiation time. Based on these excellent magnetic and photo-thermal properties, a valuable heating source with controlled warming position was fabricated.
4. A straightforward and facile method for reducing graphite oxide using y-irradiation is explored without using any photocatalysts or reducing agents. The obtained reduced graphene oxide (r-GO) is investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), and fourier transform infrared spectroscopy (FT-IR). Such unique approach not only triggers the deoxygenation reaction of graphite oxide (GO) in water, but also reduces the Au3+simultaneously under the same condition. Various spectroscopic and imaging techniques confirm that most of the chemical functional groups present on GO are removed by irradiation, and Au nanoparticles are deposited on r-GO sheets. The size of nanoparticles increases with increasing Au3+doping level. Moreover, the catalytic activity of the r-GO/Au nanocomposites was investigated.
1.利用γ射线辐射技术“一步”合成PNIPAM/AuNPs复合水凝胶。在这个反应体系中,PNIPAM水凝胶与AuNPs同步形成。合成过程简单,易于控制。考察了单体浓度、吸收剂量以及Au3+浓度对复合水凝胶的光学与热学性能的影响。结果表明,随着单体浓度的增加,复合凝胶中的纳米颗粒粒径随之增大,吸收剂量与Au3+浓度可以有效的控制水凝胶的温敏性与AuNPs的含量。研究了PNIPAM/AuNPs复合水凝胶优异的催化性能、可重复性,以及其利用温度导致的相变对其催化活性的可控性。
2.发展Y射线辐射引发原位聚合制备了PNIP AM/GO复合水凝胶。复合水凝胶的颜色以及相变温度随着GO载入量的不同而不同。由于GO优异的光吸收能力,赋予复合水凝胶独特的光热性能,即通过近红外(NIR)激光照射可以远程控制其相变。基于NIR照射与否,这种相变是完全可逆的。GO的载入量以及光照时间可以用于控制光诱导温度的增长。利用PNIPAM/GO复合水凝胶优异的光热性能,成功的制备了一个微流体开关。
3.将PNIPAM水凝胶作为一个化学反应器,在其三维网络中合成铁氧化物纳米颗粒得到(?)NIPAM/Fe304纳米复合水凝胶,并对其进行了详细的表征。由于很多的科研工作者对PNIPAM/Fe3O4纳米复合水凝胶的磁性能予以特别的关注,而忽略了其黑色的水凝胶本身的光热性能。其优异的光热性能也是第一次得到了深入的研究。实验结果表明NIR激光照射可以很快的诱使PNIPAM/Fe3O4纳米复合水凝胶相变,而且这种相变可以通过激光照射与否进行控制,具有可逆性。辐照时间越长,水凝胶周围环境温度越高。基于PNIPAM/Fe3O4纳米复合水凝胶优异的光热与磁性性能,制备了一个磁控定点光加热源。
4采用丫射线辐照方法还原了水溶液中的GO,并利用X射线衍射、红外光谱等检测手段对其还原程度进行表征。如果在GO的水溶液中加入Au3+并进行辐照,经过表征证明Au3+也得到了还原并负载于还原氧化石墨烯上。在这里,Au3+的还原与GO的还原同步进行,并且复合材料中AuNP的粒径随着Au3+浓度的增加而增加。此外,考察了r-GO/AuNPs复合材料的催化性能。
Nanocomposite hydrogels combine the novel properties of nanoparticles with unique properties of hydrogels which lead to new functions originated from the synergic effect or complementary performance of components. Such nanocomposite hydrogels have attracted intensive interests in many fields such as controlled drug delivery, catalysis, sensors and biomaterials. Nowadays, the methods for preparing nanocomposite hydrogels require the mix pre-formed nanoparticles with a hydrogel precursor followed by gelation, or in situ synthesis of metal nanoparticles within polymeric network architectures. The dispersibility and the size of Au nanoparticles in hydrogels are difficult to be controlled by those multi-steps synthesis routes requiring the separate preparation of metal nanoparticles and hydrogels. With the fast development of technologies for synthesis and application of the nanocomposites, it is of great significance to search for a simple and effective method of preparing nanocomposite hydrogel. Herein, based on synthesis of multi-functional nanocomposite hydrogel and novel nanomaterials with unique properties, also combining the advantages of our research group, one-step y-irradiation was used as an effective method to synthesize nanocomposite hydrogel. Moreover, the potential applications for those nanocomposites in the sensor, catalysis, microvalve and heating source are also explored. More details are as follows:
1. Thermosensitive poly (N-isopropylacrylamide)/Au nanoparticles (PNIPAM/Au) nanocomposite hydrogels have been synthesized by in situ y-radiation-assisted polymerization. In this reaction, the PNIPAM hydrogels and the Au nanoparticles (NPs) are formed simultaneously, demonstrating an easy and straightforward synthetic strategy for the preparation of a uniform nanocomposite. The results suggest that increasing the monomer content during the preparation of nanocomposite materials can increase the sizes of Au nanoparticles. The effects of irradiation dose and concentration of HAUCI44H2O on the optical and thermal properties of the hydrogel have also been investigated. The PNIPAM/Au nanocomposite hydrogels can act as an excellent catalyst for the conversion of o-nitroaniline to1,2-benzenediamine, and catalytic activity of the composite hydrogel can be tuned by the volume transition of PNIPAM.
2. A photo-thermal sensitive PNIPAM/GO nanocomposite hydrogel have been synthesized by in situ y-irradiation-assisted polymerization. The colors and phase transition temperatures of PNIPAM/GO hydrogels change with different GO doping level. Due to the high optical absorbance of GO, the nanocomposite hydrogel shows excellent photo-thermal property where its phase transitions can be controlled remotely by the near-infrared (NIR) laser irradiation and is completely reversible via laser exposure or non exposure. With higher GO loading, the NIR-induced temperature of the nanocomposite hydrogel increases quicker than lower doping level and can be tunable effectively by irradiation time. The nanocomposite hydrogel with excellent photo-thermal property would have great application in biomedical, especially microfluidic device, which have been proved in our experiment as a remote microvalve to control the fluidic flow.
3. The PNIPAM hydrogels have been used as reactors for the synthesis of ferroferric oxid, and the excellent laser-induced photo-thermal property of PNIPAM/Fe3O4nanocomposite hydrogel which was ignored in the previous studies was investigated in the application of near-infrared (NIR) laser irradiation. The loading of Fe3O4nanoparticles in the hydrogel can be manipulated to get the desired remote heating on application of NIR laser exposure. The phase transition of the magnetic hydrogel was controlled easily by the laser exposure or non-exposure, and it was completely reversible. The laser-induced temperature was increased quickly with the irradiation time. Based on these excellent magnetic and photo-thermal properties, a valuable heating source with controlled warming position was fabricated.
4. A straightforward and facile method for reducing graphite oxide using y-irradiation is explored without using any photocatalysts or reducing agents. The obtained reduced graphene oxide (r-GO) is investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), and fourier transform infrared spectroscopy (FT-IR). Such unique approach not only triggers the deoxygenation reaction of graphite oxide (GO) in water, but also reduces the Au3+simultaneously under the same condition. Various spectroscopic and imaging techniques confirm that most of the chemical functional groups present on GO are removed by irradiation, and Au nanoparticles are deposited on r-GO sheets. The size of nanoparticles increases with increasing Au3+doping level. Moreover, the catalytic activity of the r-GO/Au nanocomposites was investigated.
引文
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