纳米微晶纤维素/金属/电介质杂化材料的制备与性能研究
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摘要
以纳米微晶纤维素，纳米金属及二氧化硅等电介质组成的杂化结构材料是一类正在兴起的新型材料。通过高压均质法制备分散性好的纳米微晶纤维素，再以其为模板诱导使正硅酸乙酯(TEOS)在水解过程形成棒状物杂化物，该杂化物经过高温煅烧可以得到晶须状的碳化硅。以改性的二氧化硅为和聚苯乙烯微球为基，表面包覆或负载纳米银，以及将荧光染料包覆于电介质二氧化硅中可以得到不同功能化的杂化物，此类杂化物可以实现金属银和荧光物染料的多功能化特性。因而此类杂合材料被广泛应用于聚合物基的增强、抗菌、表面增强拉曼散射、生物医学等领域。本文报道了纳米微晶纤维素及碳化硅晶须的制备、并制备了Ag/SiO2、Ag/CNC、Ag/PS纳米结构杂化物及荧光物染料掺杂二氧化硅的杂合物，并讨论了聚合物基增强、抗菌、表面增强拉曼散射荧光标记等性能。全文共分五章。
第一章概述纳米杂合物结构材料的研究意义和目的、常用的制备方法、基本性质、应用领域以及本论文研究的意义、主要内容和创新。
第二章以物理机械法(高压均质的方法)制备了纳米微晶纤维素，并用相同的方法细化了低熔点的玻璃粉，并探讨了不同均质时间对纤维素及玻璃粉粒径等影响。所得到纳米微晶纤维素为棒状，分散性较好，同样该方法得到的玻璃粉粒径比均质前明显减小，分散性更好。另外还对均质后的玻璃粉的烧结温度和软化温度进行了研究，研究表明玻璃粉的粒径越小，其烧结温度和软化温度越低。
第三章用纳米微晶纤维素为模板及诱导剂，可以使TEOS在水解过程形成棒状的杂合物，该杂合物经过高温煅烧可合成晶须状的碳化硅，并对碳化硅的形貌和结构进行了表征。进一步将碳化硅晶须应用于聚苯乙烯基树脂的增强，碳化硅晶须增强的树脂力学性能有明显改善，相比于普通的聚苯乙烯，其中拉伸强度增加到原来的3倍，缺口冲击强度增加到8倍左右。通过CNC合成的SiC晶须显示了在聚合物基等领域的潜在的应用前景。
第四章以改性的二氧化硅微纳球为载体，Fe3+为催化剂，DMF为还原剂制备了表面包覆好的Ag/SiO2杂化物，并探讨了有无催化剂和不同的反应温度对纳米银负载物的影响。将银纳米粒子包覆的杂合物应用于抗菌测试，展现除了优异的抗菌性能。另将荧光染料掺杂于改性的二氧化硅纳米球，得到的纳米杂合物大小均一，粒径在50～80nm之间，分散性好。荧光测试实验表明该杂合物仍保留原始荧光单体的性能，但荧光单体泄露可以明显改善，进一步应用于生物标记，发现在细胞中有明显的纳米荧光杂合物颗粒。
第五章以制备了单分散性好的聚苯乙烯微球，并以聚苯乙烯微球和纳米微晶纤维素为基质，通过在PS微球表面吸附不同电荷，将Ag+还原为纳米银负载于聚苯乙烯表面上。该Ag/PS复合物应用于SERS增强实验，发现MB(亚甲基)的拉曼信号可以明显地提高。另外通过简单的方法超声还原法制备了纳米银负载纳米微晶纤维素杂合物，发现随着超声反应时间的增加，纳米银粒子不断地生长，超声反应60min时，CNC表面的纳米银大小均一，无明显团聚现象，但是超声时间80min时，纳米银变得更大，而且大小不均一。进一步应用抗菌实验，表明超声反应60min时，所得到纳米银负载的CNC杂合物具有较好的抗菌效果，该杂合物可应用于抗菌，生物医学等研究领域。
The cellulose nanocrystals (CNC), nano-metals hybrid and silica dielectric compositestructure nanomaterials are an emerging class of new materials. Dispersibility cellulosenanocrystal is prepared by a high pressure homogenizer. Then the CNC as a template inducessilica rods hybrids during the TEOS (Tetracethyl orthosilicate) hydrolysis process. The siliconcarbide whisker can be obtained by high temperature calcination for hybrids. The modifiedsilica and polystyrene microspheres as the matrix, the surface coats or deposits nano-silver,and the fluorescent dyes can be coated on the dielectric silica spheres. The hybrids have thedifferent functions, such as the multifunctional characteristics of metallic silver and themultifunctional characteristics of the fluorescent dyes. Therefore such hybrid materials arewidely used in the polymer matrix enhanced, antimicrobial, surface-enhanced Ramanscattering and biomedical field. This study reports that cellulose nanocrystals, silicon carbidewhiskers, nano-structure of hybrids hybrids (Ag/SiO2,Ag/CNC and Ag/PS) and fluorescentmaterial dye-doped silica hybrid compounds are prepared. The properities of polymerreinforce, fluorescently labeled performance, surface-enhanced Raman and antimicrobial arealso discussed. The paper is divided into five chapters.
In the first chapter, the overview research significance and purpose of the hybrids structuralmaterials are given. And the commonly used preparation method, basic properties, applicationareas, our study thesis, main content and innovation are given.
In the second chapter, the CNC is prepared by physical and mechanical method (highpressure homogenization method), and refinement of the low melting point glass powder arealso obtained by the same way. We discuss different homogenization time for effectingcellulose and glass powder particle size. The preparation CNC has a rod like and a gooddispersibility. And the particle diameter of glass powder reduces before than homogeneoussignificantly by the same method. After high homogeneous, the sintering temperature andsoftening of the glass powder are also studied. The result showes that the smaller the particlesize of the glass powder, the sintering temperature and the softening temperature is lower.
In the third chapter, the cellulose nanocrystals as a template and inducers can form rod like hybrid materials during the TEOS hydrolysis process. The silicon carbide is obtainedhigh-temperature calcination the hybrid materials. We also test the silicon carbide whiskestructure by XRD, TEM, FTIR and so on. The silicon carbide whisker is applied polystyreneresin reinforced. And compared to ordinary polystyrene, the mechanical properties of siliconcarbide whisker-reinforced resin is significant improvement which the tensile strengthincreased by3times, notched impact strength increased by about8times. It shows that thesynthesis SiC whiskers have broad application prospects in polymer-based areas.
In the fourth chapter, the modified silica as matrix, Fe3+as catalyst and DMF as a reducingagent, we prepare high dispersion Ag/SiO2hybrids. The catalyst and the reaction temperaturealso discussed for Ag nanoparticles deposited. The silver nanoparticles coating SiO2is usedin antibacterial test, and it also showes excellent antibacterial properties. Another fluorescentdye doping in the modified SiO2nanospheres is synthesized. The nanocomposites have gooddispersion, uniform size and the particle size between50～80nm. The fluorescence testexperiments show that the nanocomposites still retain the performance of the originalfluorescent and fluorescent leak can be significantly improved. We find that the cells have thedye doping silica nanocomposites when the nanocomposites are applied to cell label.
In the fifth chapter, we prepare monodisperse polystyrene microspheres. And the obtainedPS spheres as a matrix, the nanocrystalline silver deposite different charges in PSmicrospheres surface. The Ag/PS composites are used in SERS enhancement experiments andit can improve MB’s Raman signals. In addition, by the simple ultrasound method, we canobtain nano-silver deposited CNC surface. It find that the growth of nano-silver particlesincrease with ultrasonic reaction time. With ultrasonic reaction60min, the uniform size of thenano-silver can deposit CNC surface. When ultrasonic time is80min, nano silver becomeslarger, and nano silver is obvious agglomeration and uneven in size. Further application ofantibacterial experiments, the nanosilver deposited CNC composites show good antibacterialeffect. And this material can be applied to antibacterial and biomedical research field.
第一章概述纳米杂合物结构材料的研究意义和目的、常用的制备方法、基本性质、应用领域以及本论文研究的意义、主要内容和创新。
第二章以物理机械法(高压均质的方法)制备了纳米微晶纤维素，并用相同的方法细化了低熔点的玻璃粉，并探讨了不同均质时间对纤维素及玻璃粉粒径等影响。所得到纳米微晶纤维素为棒状，分散性较好，同样该方法得到的玻璃粉粒径比均质前明显减小，分散性更好。另外还对均质后的玻璃粉的烧结温度和软化温度进行了研究，研究表明玻璃粉的粒径越小，其烧结温度和软化温度越低。
第三章用纳米微晶纤维素为模板及诱导剂，可以使TEOS在水解过程形成棒状的杂合物，该杂合物经过高温煅烧可合成晶须状的碳化硅，并对碳化硅的形貌和结构进行了表征。进一步将碳化硅晶须应用于聚苯乙烯基树脂的增强，碳化硅晶须增强的树脂力学性能有明显改善，相比于普通的聚苯乙烯，其中拉伸强度增加到原来的3倍，缺口冲击强度增加到8倍左右。通过CNC合成的SiC晶须显示了在聚合物基等领域的潜在的应用前景。
第四章以改性的二氧化硅微纳球为载体，Fe3+为催化剂，DMF为还原剂制备了表面包覆好的Ag/SiO2杂化物，并探讨了有无催化剂和不同的反应温度对纳米银负载物的影响。将银纳米粒子包覆的杂合物应用于抗菌测试，展现除了优异的抗菌性能。另将荧光染料掺杂于改性的二氧化硅纳米球，得到的纳米杂合物大小均一，粒径在50～80nm之间，分散性好。荧光测试实验表明该杂合物仍保留原始荧光单体的性能，但荧光单体泄露可以明显改善，进一步应用于生物标记，发现在细胞中有明显的纳米荧光杂合物颗粒。
第五章以制备了单分散性好的聚苯乙烯微球，并以聚苯乙烯微球和纳米微晶纤维素为基质，通过在PS微球表面吸附不同电荷，将Ag+还原为纳米银负载于聚苯乙烯表面上。该Ag/PS复合物应用于SERS增强实验，发现MB(亚甲基)的拉曼信号可以明显地提高。另外通过简单的方法超声还原法制备了纳米银负载纳米微晶纤维素杂合物，发现随着超声反应时间的增加，纳米银粒子不断地生长，超声反应60min时，CNC表面的纳米银大小均一，无明显团聚现象，但是超声时间80min时，纳米银变得更大，而且大小不均一。进一步应用抗菌实验，表明超声反应60min时，所得到纳米银负载的CNC杂合物具有较好的抗菌效果，该杂合物可应用于抗菌，生物医学等研究领域。
The cellulose nanocrystals (CNC), nano-metals hybrid and silica dielectric compositestructure nanomaterials are an emerging class of new materials. Dispersibility cellulosenanocrystal is prepared by a high pressure homogenizer. Then the CNC as a template inducessilica rods hybrids during the TEOS (Tetracethyl orthosilicate) hydrolysis process. The siliconcarbide whisker can be obtained by high temperature calcination for hybrids. The modifiedsilica and polystyrene microspheres as the matrix, the surface coats or deposits nano-silver,and the fluorescent dyes can be coated on the dielectric silica spheres. The hybrids have thedifferent functions, such as the multifunctional characteristics of metallic silver and themultifunctional characteristics of the fluorescent dyes. Therefore such hybrid materials arewidely used in the polymer matrix enhanced, antimicrobial, surface-enhanced Ramanscattering and biomedical field. This study reports that cellulose nanocrystals, silicon carbidewhiskers, nano-structure of hybrids hybrids (Ag/SiO2,Ag/CNC and Ag/PS) and fluorescentmaterial dye-doped silica hybrid compounds are prepared. The properities of polymerreinforce, fluorescently labeled performance, surface-enhanced Raman and antimicrobial arealso discussed. The paper is divided into five chapters.
In the first chapter, the overview research significance and purpose of the hybrids structuralmaterials are given. And the commonly used preparation method, basic properties, applicationareas, our study thesis, main content and innovation are given.
In the second chapter, the CNC is prepared by physical and mechanical method (highpressure homogenization method), and refinement of the low melting point glass powder arealso obtained by the same way. We discuss different homogenization time for effectingcellulose and glass powder particle size. The preparation CNC has a rod like and a gooddispersibility. And the particle diameter of glass powder reduces before than homogeneoussignificantly by the same method. After high homogeneous, the sintering temperature andsoftening of the glass powder are also studied. The result showes that the smaller the particlesize of the glass powder, the sintering temperature and the softening temperature is lower.
In the third chapter, the cellulose nanocrystals as a template and inducers can form rod like hybrid materials during the TEOS hydrolysis process. The silicon carbide is obtainedhigh-temperature calcination the hybrid materials. We also test the silicon carbide whiskestructure by XRD, TEM, FTIR and so on. The silicon carbide whisker is applied polystyreneresin reinforced. And compared to ordinary polystyrene, the mechanical properties of siliconcarbide whisker-reinforced resin is significant improvement which the tensile strengthincreased by3times, notched impact strength increased by about8times. It shows that thesynthesis SiC whiskers have broad application prospects in polymer-based areas.
In the fourth chapter, the modified silica as matrix, Fe3+as catalyst and DMF as a reducingagent, we prepare high dispersion Ag/SiO2hybrids. The catalyst and the reaction temperaturealso discussed for Ag nanoparticles deposited. The silver nanoparticles coating SiO2is usedin antibacterial test, and it also showes excellent antibacterial properties. Another fluorescentdye doping in the modified SiO2nanospheres is synthesized. The nanocomposites have gooddispersion, uniform size and the particle size between50～80nm. The fluorescence testexperiments show that the nanocomposites still retain the performance of the originalfluorescent and fluorescent leak can be significantly improved. We find that the cells have thedye doping silica nanocomposites when the nanocomposites are applied to cell label.
In the fifth chapter, we prepare monodisperse polystyrene microspheres. And the obtainedPS spheres as a matrix, the nanocrystalline silver deposite different charges in PSmicrospheres surface. The Ag/PS composites are used in SERS enhancement experiments andit can improve MB’s Raman signals. In addition, by the simple ultrasound method, we canobtain nano-silver deposited CNC surface. It find that the growth of nano-silver particlesincrease with ultrasonic reaction time. With ultrasonic reaction60min, the uniform size of thenano-silver can deposit CNC surface. When ultrasonic time is80min, nano silver becomeslarger, and nano silver is obvious agglomeration and uneven in size. Further application ofantibacterial experiments, the nanosilver deposited CNC composites show good antibacterialeffect. And this material can be applied to antibacterial and biomedical research field.
引文
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