壳聚糖共价接枝碳纳米管复合材料的制备及性能研究
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摘要
碳纳米管/壳聚糖复合材料是一种具有生物和光电双重性能的复合材料。壳聚糖具有良好的生物相容性、可降解性及低毒性,在生物领域具有广泛的应用。将壳聚糖与碳纳米管制备成复合材料,不仅有望利用生物大分子的亲水性来改善碳纳米管的分散性,更有可能赋予碳纳米管某些生物学的性质,为碳纳米管在生物医学领域的应用提供了途径。
通过壳聚糖共价接枝在碳纳米管表面的方法制备一种新型的碳纳米管/壳聚糖复合材料。通过红外光谱分析,证明了壳聚糖与碳纳米管之间通过共价键连接。紫外光谱分析表明碳纳米管在265 nm处出现吸收峰,且吸收峰的强度与碳纳米管的浓度成正比,满足Lambert-Beer定律。透射电子显微镜表明壳聚糖共价接枝碳纳米管为芯-皮结构,碳纳米管被厚厚的一层聚合物链包裹。热失重分析为碳纳米管表面接枝壳聚糖提供了定量的分析。共价接枝方法提高了碳纳米管与壳聚糖两相之间的结合力,使碳纳米管在一些稀的有机弱酸(甲酸、苯甲酸、乙酸等)中产生了稳定的分散性。
为了表征壳聚糖共价接枝碳纳米管复合材料的电化学性质,我们用电化学沉积的方法对其沉积到金电极表面。扫描电子显微镜显示接枝产物在电极表面为多孔结构,与壳聚糖非共价修饰碳纳米管不同。所制备的壳聚糖共价接枝碳纳米管修饰电极对过氧化氢有良好的电催化能力,因此可以应用于氧化类的生物传感器。作为一个例子,葡萄糖氧化酶通过戊二醛交联法固定于修饰电极表面,构筑成葡萄糖生物传感器。由于接枝产物的特殊结构,电极表面与葡萄糖氧化酶活性中心之间的电子传递更加容易。与壳聚糖非共价修饰的碳纳米管相比,壳聚糖共价接枝修饰碳纳米管的生物传感器具有更高的响应电流、更宽的线性响应范围。
将壳聚糖共价接枝碳纳米管分散于聚乙烯醇基体中进行静电纺丝,得平均直径为232±85 nm的电纺纤维。拉曼光谱证明的纤维中碳纳米管的存在,并且吸收峰的强度与碳纳米管的浓度有关。扫描电子显微镜观察了壳聚糖共价接枝碳纳米管/聚乙烯醇电纺纤维的微观形貌,并与壳聚糖非共价修饰碳纳米管/聚乙烯醇电纺纤维进行比较,结果表明该电纺纤维具有更均匀的直径分布,说明壳聚糖共价接枝碳纳米管在聚乙烯醇中具有良好可纺性。此外由于该电纺纤维具有高的比表面积,它的电化学性能也很好,有望在生物传感器等领域得到的应用。
Carbon nanotubes/chitosan (CNT/CS) composite has biologic and optoelectronic function. Based on attractive biocompatibility, biodegradability and non-toxicity of CS, many researchers explored the possibility of CS as platforms in biological field. CNT/CS composites not only are hopeful to improve the dispersibility and solubility of CNT by the hydrophilicity of biopolymer, but also could endue some biologic ability for CNT that can provide an approach for the application of CNT.
A novel Chitosan-grafted multiwalled carbon nanotubes (CS-g-MWCNT) was prepared through covalently grafting a biocompatible polymer CS onto the surfaces of MWCNT. On the basis of Fourier transform infrared spectroscopy (FT-IR), we can conclude that the CS was covalently grafted onto MWCNT. Ultraviolet-visible spectroscopy (UV-vis) shows a sharp absorption peak in about 265 nm appeared which can be attributed to the characteristic absorption of MWCNT. Interestingly, the observed absorption peak in CS-g-MWCNT solution depends on the solution concentrations in a linear fashion, obeying the Lambert-Beer’s law. A core-shell nanostructure can be observed by transmission electron microscopy (TEM), indicating that the nanotubes were coated with polymer chains. Thermogravimetry analysis (TGA) data furnish quantitative information on the degree of functionalization. The covalent modification overcomes the issues of poor interfacial bonding and results in stable dispersibility of MWCNT in some diluted organic acid (formic, benzoic, acetic, etc.).
The electrochemical properties of the CS-g-MWCNT were characterized by an electrodeposition method that involves depositing it on an Au electrode. The porous microstructure of the CS-g-MWCNT modified electrode was observed by scanning electron microscopy (SEM) which is contrast to the non-covalent modification of MWCNTs with CS (CS/MWCNT). The excellent electrocatalytic ability of the CS-g-MWCNT modified electrode towards hydrogen peroxide is applicable to the development of oxidase-based amperometric biosensors. As an example, an amperometric glucose biosensor based on the enzyme electrode with CS-g-MWCNT modified electrode was fabricated. The glucose oxidase (GOD) was cross-linked and immobilized on the electrode surface by the use of glutaraldehyde. The electron could transfer more easily between electrode surface and bioactive center of GOD because of the special structure of CS-g-MWCNT. The CS-g-MWCNT biosensor has higher sensitivity and wider linear response range than the CS/MWCNT biosensor.
The CS-g-MWCNT in poly(vinyl alcohol) (PVA) matrix was electrospun into nanofibers with a mean diameter of 232±85 nm. Raman spectroscopy shows the existence of MWCNT and the absorption peak in CS-g-MWCNT/PVA electrospun nanofibers depends on the concentrations of CS-g-MWCNT. Scanning electron microscopy (SEM) was used to characterize the morphologies of the CS-g-MWCNT nanofibers and the results show that the CS-g-MWCNT/PVA nanofibers have uniform diameter distribution in contrast to CS/MWCNT/PVA nanofibers. The excellent electrochemical properties of the CS-g-MWCNT/PVA nanofibers attribute to high surface/volume ratio which is applicable to the development of biosensors.
通过壳聚糖共价接枝在碳纳米管表面的方法制备一种新型的碳纳米管/壳聚糖复合材料。通过红外光谱分析,证明了壳聚糖与碳纳米管之间通过共价键连接。紫外光谱分析表明碳纳米管在265 nm处出现吸收峰,且吸收峰的强度与碳纳米管的浓度成正比,满足Lambert-Beer定律。透射电子显微镜表明壳聚糖共价接枝碳纳米管为芯-皮结构,碳纳米管被厚厚的一层聚合物链包裹。热失重分析为碳纳米管表面接枝壳聚糖提供了定量的分析。共价接枝方法提高了碳纳米管与壳聚糖两相之间的结合力,使碳纳米管在一些稀的有机弱酸(甲酸、苯甲酸、乙酸等)中产生了稳定的分散性。
为了表征壳聚糖共价接枝碳纳米管复合材料的电化学性质,我们用电化学沉积的方法对其沉积到金电极表面。扫描电子显微镜显示接枝产物在电极表面为多孔结构,与壳聚糖非共价修饰碳纳米管不同。所制备的壳聚糖共价接枝碳纳米管修饰电极对过氧化氢有良好的电催化能力,因此可以应用于氧化类的生物传感器。作为一个例子,葡萄糖氧化酶通过戊二醛交联法固定于修饰电极表面,构筑成葡萄糖生物传感器。由于接枝产物的特殊结构,电极表面与葡萄糖氧化酶活性中心之间的电子传递更加容易。与壳聚糖非共价修饰的碳纳米管相比,壳聚糖共价接枝修饰碳纳米管的生物传感器具有更高的响应电流、更宽的线性响应范围。
将壳聚糖共价接枝碳纳米管分散于聚乙烯醇基体中进行静电纺丝,得平均直径为232±85 nm的电纺纤维。拉曼光谱证明的纤维中碳纳米管的存在,并且吸收峰的强度与碳纳米管的浓度有关。扫描电子显微镜观察了壳聚糖共价接枝碳纳米管/聚乙烯醇电纺纤维的微观形貌,并与壳聚糖非共价修饰碳纳米管/聚乙烯醇电纺纤维进行比较,结果表明该电纺纤维具有更均匀的直径分布,说明壳聚糖共价接枝碳纳米管在聚乙烯醇中具有良好可纺性。此外由于该电纺纤维具有高的比表面积,它的电化学性能也很好,有望在生物传感器等领域得到的应用。
Carbon nanotubes/chitosan (CNT/CS) composite has biologic and optoelectronic function. Based on attractive biocompatibility, biodegradability and non-toxicity of CS, many researchers explored the possibility of CS as platforms in biological field. CNT/CS composites not only are hopeful to improve the dispersibility and solubility of CNT by the hydrophilicity of biopolymer, but also could endue some biologic ability for CNT that can provide an approach for the application of CNT.
A novel Chitosan-grafted multiwalled carbon nanotubes (CS-g-MWCNT) was prepared through covalently grafting a biocompatible polymer CS onto the surfaces of MWCNT. On the basis of Fourier transform infrared spectroscopy (FT-IR), we can conclude that the CS was covalently grafted onto MWCNT. Ultraviolet-visible spectroscopy (UV-vis) shows a sharp absorption peak in about 265 nm appeared which can be attributed to the characteristic absorption of MWCNT. Interestingly, the observed absorption peak in CS-g-MWCNT solution depends on the solution concentrations in a linear fashion, obeying the Lambert-Beer’s law. A core-shell nanostructure can be observed by transmission electron microscopy (TEM), indicating that the nanotubes were coated with polymer chains. Thermogravimetry analysis (TGA) data furnish quantitative information on the degree of functionalization. The covalent modification overcomes the issues of poor interfacial bonding and results in stable dispersibility of MWCNT in some diluted organic acid (formic, benzoic, acetic, etc.).
The electrochemical properties of the CS-g-MWCNT were characterized by an electrodeposition method that involves depositing it on an Au electrode. The porous microstructure of the CS-g-MWCNT modified electrode was observed by scanning electron microscopy (SEM) which is contrast to the non-covalent modification of MWCNTs with CS (CS/MWCNT). The excellent electrocatalytic ability of the CS-g-MWCNT modified electrode towards hydrogen peroxide is applicable to the development of oxidase-based amperometric biosensors. As an example, an amperometric glucose biosensor based on the enzyme electrode with CS-g-MWCNT modified electrode was fabricated. The glucose oxidase (GOD) was cross-linked and immobilized on the electrode surface by the use of glutaraldehyde. The electron could transfer more easily between electrode surface and bioactive center of GOD because of the special structure of CS-g-MWCNT. The CS-g-MWCNT biosensor has higher sensitivity and wider linear response range than the CS/MWCNT biosensor.
The CS-g-MWCNT in poly(vinyl alcohol) (PVA) matrix was electrospun into nanofibers with a mean diameter of 232±85 nm. Raman spectroscopy shows the existence of MWCNT and the absorption peak in CS-g-MWCNT/PVA electrospun nanofibers depends on the concentrations of CS-g-MWCNT. Scanning electron microscopy (SEM) was used to characterize the morphologies of the CS-g-MWCNT nanofibers and the results show that the CS-g-MWCNT/PVA nanofibers have uniform diameter distribution in contrast to CS/MWCNT/PVA nanofibers. The excellent electrochemical properties of the CS-g-MWCNT/PVA nanofibers attribute to high surface/volume ratio which is applicable to the development of biosensors.
引文
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