微胶囊的微流体数字化制备技术及配套器件制作工艺研究
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摘要
随着微胶囊技术的迅速发展和学科交叉,微胶囊的应用领域不断扩展,对微胶囊产品的品质提出了越来越高的要求。虽然目前制备微胶囊的方法很多,但有效地减小微胶囊的粒径和粒径分布、提高制备过程的可控性等问题,仍是微胶囊控释等应用实践的关键问题。为此需要很好的解决微胶囊的成粒方式、微量流体驱动方式和核心成粒器件的设计与制作等问题。
微流体数字化技术在基本概念上和理论上有原创性,实现了微量流体在微流体器件中的脉冲流动,为建立与信息、能量传输及固体运动数字化有等同意义的物质传输数字化开辟了道路。本论文以微流体数字化技术为研究基础的,以数字化制备单分散的乳液和微胶囊为研究导向,在微量流体驱动基础理论的研究、乳液和微胶囊数字化制备实验、及以新型微流体器件工艺与装备的研制等方面取得了以下成果:
提出了基于微流体数字化技术的规整单分散双重乳液和微胶囊的制备方法,进行了这两种微颗粒的连续序列和编码序列制备实验,制作了(O_1/W/O_2)型双重乳液、包覆液体芯材的微胶囊和包覆固体芯材的微胶囊;该方法实现了双重乳液和微胶囊制备时序的节拍化和制备粒径的系列规整化,提高了微颗粒制备过程的可控性和颗粒粒径的单分散性。
总结了内构变径型微喷嘴中数字化微喷射过程的影响因素,在此基础上通过实验设计出微喷射稳定性图;设计了流体示踪实验,观测并研究了内构变径型微喷嘴内微喷射发生的过程;在实验观测的基础上,总结和归纳了内构变径微喷嘴内数字化微喷射过程的特征和实现的必要条件,提出了惯性力—弹性力—黏性力交替作用的数字化瞬态喷射过程的模型;应用类声学的办法对所建立的模型进行数理分析,由此对微喷射稳定性提出理论上的指导意见,解决了实践中的高黏度液体稳定喷射的问题。
提出了一种新的基于玻璃微管道热流变拉伸成型原理的二维玻璃微流体器件制作工艺。使用该工艺方法制作了玻璃三通微管道,储液池在拉制的过程中同时成型;三通微管道截面呈圆形或无柄哑铃形,表面张力成形的三根微管道壁面具有较高的质量且光滑连接,因此三通管道结点处无内棱角和死腔;该三通微管道制作工艺成本低廉,工艺过程安全简单;在该工艺成熟的基础上,设计了玻璃三通微管道拉制仪,制备了支路内径不同的三通微管道;以三通微管道制备工艺为基础,设计了微流体管道网络装配工艺,制作了三种基本的微管道网络。
将三通微管道工艺改进,制作了三通嵌合微喷嘴,并设计了以此种微喷嘴为核心的微喷射装置。以此装置为平台进行了微胶囊数字化制备实验,所制备微胶囊的有效载量得到提高。
提出了符合微流体数字化技术驱动要求的直列微孔径多喷嘴制作工艺。使用此直列微喷嘴进行了初步的微喷射实验和微胶囊制备实验,实验中微喷射和微胶囊的制备效率显著提高。
Along with the rapid development of the microcapsules technology and discipline-crossing, the application fields of microcapsules keep expanding, and the quality requirement of microcapsules has become higher and higher. Although there are a lot of methods for microcapsules preparation, in practical fields of controlled-releasing, there are some bottlenecks such as better controlling of the preparing process, reducing the particle size and reducing its distribution. Therefore problems in method of particle formation, designing and fabrication of the core microfluidic components and method for driving microfluid should be well solved.
There are some creative theories in the digitalization of microfluids technology, which exploits the field of the digital matter transportation, equaled with the digital information, the digital energy transmission or solid movement. Pulsating flow of microfluid has been realized in the microfluidic components by using the technology. The research foundation of this paper is the digitalization of microfluids technology, and the research directions are the digital preparation of monodispersed emulsions and microcapsules. The creative achievements on the theoretic research of microcfluid driving, the designing of the method and equipment for fabricating novel microfluidic components, and the digital preparation of emulsions and microcapsules are described as follow.
A new method of preparing monodisperse double emulsions and microcapsules is proposed on the basis of digitalization of microfluids technology. Double emulsions of type (O_1/W/O_2) and microcapsules with both liquid and solid core have been prepared. The rhythm of the preparing process could be either sequential or encoded, therefore the process was provided with a digitalized and volume controllable character. The number of particles could be counted and controlled, and the size distribution of the micro-droplets was narrow.
The influencing factors of digital micro-jetting of the inner diameter changing micropipette were summarized, and the stability diagram of micro-jetting which based on the summarizing was designed. On the basis of the diagram, the quantitative index of stability for digital micro-jetting was proposed. The process of micro-jetting occurred in the micropipette was observed, which based on the experiments of fluid trace. After the induction of the features of micro-jetting, the author put forward the model of the micro-jetting. It was found that the inertial force, elastic force and viscous force act in the micropipette in turn. On the basis of the model, method of mathematical analysis similar with acoustics was used to analyze the flow field in the micropipette. Therefore the theoretic opinion for improving stability of micro-jetting could be obtained by the analyzing, and practical problems of stable micro-jetting of high-viscosity liquid had been solved.
A new Non-IC method for fabricating two-dimensional vitreous microfluidic components is proposed, which is based on the theory of hot rheologic deformation. In the drawing process, reservoirs which connect the microchannels with conical pipes formed. The cross sections of the microchannels are round or dumbbell with no handle, and the walls of the three microchannels connect smoothly in the joint, so there is no dead volume. High quality surface of the microchannels are obtained due to the surface tension. The process has characteristics of low cost, simple manipulation and safe process. On the basis of the prodess, puller for fabricating such three-way microchannels with equal or unequal inner diameter was designed. Method for fabricating microchannel networks was also designed, and three basic microchannel networks had been made.
After the technological improvement, the three-way micropipette embedded with another micropipette was designed. Micro-jetting equipment taking the compound micropipette as the core was fabricated, and then followed with experiment of microencapsulation. The effective content of the prepared microcapsules improved obviously.
This paper also provides a new method for fabricating in-line multi-micropipettes, which is compatible with digitalization of microfluids technology. Experiments of micro-jetting and microcapsules preparation were carried out by using the micropipettes. The results showed that the efficiency of the micro-jetting and microcapsules preparation improved obviously.
微流体数字化技术在基本概念上和理论上有原创性,实现了微量流体在微流体器件中的脉冲流动,为建立与信息、能量传输及固体运动数字化有等同意义的物质传输数字化开辟了道路。本论文以微流体数字化技术为研究基础的,以数字化制备单分散的乳液和微胶囊为研究导向,在微量流体驱动基础理论的研究、乳液和微胶囊数字化制备实验、及以新型微流体器件工艺与装备的研制等方面取得了以下成果:
提出了基于微流体数字化技术的规整单分散双重乳液和微胶囊的制备方法,进行了这两种微颗粒的连续序列和编码序列制备实验,制作了(O_1/W/O_2)型双重乳液、包覆液体芯材的微胶囊和包覆固体芯材的微胶囊;该方法实现了双重乳液和微胶囊制备时序的节拍化和制备粒径的系列规整化,提高了微颗粒制备过程的可控性和颗粒粒径的单分散性。
总结了内构变径型微喷嘴中数字化微喷射过程的影响因素,在此基础上通过实验设计出微喷射稳定性图;设计了流体示踪实验,观测并研究了内构变径型微喷嘴内微喷射发生的过程;在实验观测的基础上,总结和归纳了内构变径微喷嘴内数字化微喷射过程的特征和实现的必要条件,提出了惯性力—弹性力—黏性力交替作用的数字化瞬态喷射过程的模型;应用类声学的办法对所建立的模型进行数理分析,由此对微喷射稳定性提出理论上的指导意见,解决了实践中的高黏度液体稳定喷射的问题。
提出了一种新的基于玻璃微管道热流变拉伸成型原理的二维玻璃微流体器件制作工艺。使用该工艺方法制作了玻璃三通微管道,储液池在拉制的过程中同时成型;三通微管道截面呈圆形或无柄哑铃形,表面张力成形的三根微管道壁面具有较高的质量且光滑连接,因此三通管道结点处无内棱角和死腔;该三通微管道制作工艺成本低廉,工艺过程安全简单;在该工艺成熟的基础上,设计了玻璃三通微管道拉制仪,制备了支路内径不同的三通微管道;以三通微管道制备工艺为基础,设计了微流体管道网络装配工艺,制作了三种基本的微管道网络。
将三通微管道工艺改进,制作了三通嵌合微喷嘴,并设计了以此种微喷嘴为核心的微喷射装置。以此装置为平台进行了微胶囊数字化制备实验,所制备微胶囊的有效载量得到提高。
提出了符合微流体数字化技术驱动要求的直列微孔径多喷嘴制作工艺。使用此直列微喷嘴进行了初步的微喷射实验和微胶囊制备实验,实验中微喷射和微胶囊的制备效率显著提高。
Along with the rapid development of the microcapsules technology and discipline-crossing, the application fields of microcapsules keep expanding, and the quality requirement of microcapsules has become higher and higher. Although there are a lot of methods for microcapsules preparation, in practical fields of controlled-releasing, there are some bottlenecks such as better controlling of the preparing process, reducing the particle size and reducing its distribution. Therefore problems in method of particle formation, designing and fabrication of the core microfluidic components and method for driving microfluid should be well solved.
There are some creative theories in the digitalization of microfluids technology, which exploits the field of the digital matter transportation, equaled with the digital information, the digital energy transmission or solid movement. Pulsating flow of microfluid has been realized in the microfluidic components by using the technology. The research foundation of this paper is the digitalization of microfluids technology, and the research directions are the digital preparation of monodispersed emulsions and microcapsules. The creative achievements on the theoretic research of microcfluid driving, the designing of the method and equipment for fabricating novel microfluidic components, and the digital preparation of emulsions and microcapsules are described as follow.
A new method of preparing monodisperse double emulsions and microcapsules is proposed on the basis of digitalization of microfluids technology. Double emulsions of type (O_1/W/O_2) and microcapsules with both liquid and solid core have been prepared. The rhythm of the preparing process could be either sequential or encoded, therefore the process was provided with a digitalized and volume controllable character. The number of particles could be counted and controlled, and the size distribution of the micro-droplets was narrow.
The influencing factors of digital micro-jetting of the inner diameter changing micropipette were summarized, and the stability diagram of micro-jetting which based on the summarizing was designed. On the basis of the diagram, the quantitative index of stability for digital micro-jetting was proposed. The process of micro-jetting occurred in the micropipette was observed, which based on the experiments of fluid trace. After the induction of the features of micro-jetting, the author put forward the model of the micro-jetting. It was found that the inertial force, elastic force and viscous force act in the micropipette in turn. On the basis of the model, method of mathematical analysis similar with acoustics was used to analyze the flow field in the micropipette. Therefore the theoretic opinion for improving stability of micro-jetting could be obtained by the analyzing, and practical problems of stable micro-jetting of high-viscosity liquid had been solved.
A new Non-IC method for fabricating two-dimensional vitreous microfluidic components is proposed, which is based on the theory of hot rheologic deformation. In the drawing process, reservoirs which connect the microchannels with conical pipes formed. The cross sections of the microchannels are round or dumbbell with no handle, and the walls of the three microchannels connect smoothly in the joint, so there is no dead volume. High quality surface of the microchannels are obtained due to the surface tension. The process has characteristics of low cost, simple manipulation and safe process. On the basis of the prodess, puller for fabricating such three-way microchannels with equal or unequal inner diameter was designed. Method for fabricating microchannel networks was also designed, and three basic microchannel networks had been made.
After the technological improvement, the three-way micropipette embedded with another micropipette was designed. Micro-jetting equipment taking the compound micropipette as the core was fabricated, and then followed with experiment of microencapsulation. The effective content of the prepared microcapsules improved obviously.
This paper also provides a new method for fabricating in-line multi-micropipettes, which is compatible with digitalization of microfluids technology. Experiments of micro-jetting and microcapsules preparation were carried out by using the micropipettes. The results showed that the efficiency of the micro-jetting and microcapsules preparation improved obviously.
引文
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