石英晶体微天平电学参数获取及在物理吸附上的应用
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摘要
石英晶体微天平(QCM)是一种新型的高灵敏度质量传感器,具有精度高、稳定性好、体积小以及结构简单等优点,能在纳米尺度上精确测量质量、粘度和剪切模量等物理参量,被广泛地应用于电化学、生物医学、有机化学、分析化学和物理学等领域。本论文详细地论述了QCM的基本原理、理论模型、电路实现、网络分析仪测量以及其在物理吸附方面的应用。文中介绍了负载物理属性对测量结果的影响的模拟计算,讲述了基于频率、电阻及耗散因子的QCM数据采集系统的软硬件设计,给出了网络分析仪技术用在QCM测量上的实现方案,并在固体表面的大分子的物理吸附方面取得了很有意义的研究成果。
本研究工作的主要创新点在于:
1)基于QCM的力学模型和电学模型开展了一系列关于QCM电学响应的模拟计算。计算结果给出了膜的粘弹性和溶液属性对QCM测量结果的影响,指出了液相中QCM作为质量传感器所带来的测量偏差。
2)分析了QCM驱动电路的重点和难点,给出了一种能测量耗散因子和串联电阻以及串联谐振频率的QCM驱动电路的实现方案。针对QCM对温度稳定性的苛刻要求设计出了一套智能温度控制系统,温度稳定度极高。
3)针对此QCM驱动电路,设计出了一套基于USB2.0接口的高速数据采集系统。采用了高速和高精度模数转换技术以及等精度频率测量技术,拥有两路模拟通道,可以同时采集两路QCM模拟数据以便做差分运算和比较分析。对外接口简单,使用方便,具有较高的科研价值和商业价值。
4)设计了一套基于网络分析仪的QCM参数测量系统,给出了详细的硬件和软件实现方案,能够方便地获取各种负载环境下晶体各次谐波所对应的QCM电学参数,并通过实验验证了此系统的有效性。此系统功能强大,可测参数多,晶体能工作在很高的能量耗散环境中,可与通用的QCM互补使用。
5)用QCM开展了金表面上聚(N-异丙基丙烯酰胺)(PNIPAM)的物理吸附实验,结果表明PNIPAM的结构强烈地影响着其在固体表面上的物理吸附。伸张状态下的吸附动力学受分子向吸附底层的扩散所影响,吸附时间常数受溶液的浓度和温度的影响较大。塌缩状态下PNIPAM的吸附时间常数基本上不依赖于温度和浓度。浓度在0-100ppm的范围内,伸张状态下的PNIPAM只在金表面形成单层吸附膜。而当聚合物转变到塌缩态时,同样的底层上会形成多层膜。
Quartz Crystal Microbalance (QCM) is a new type of micro-mass sensor which allows accurate measurements of mass, viscosity and shear modulus on nano-scale. It has been used widely in many fields, such as electrochemistry, biomedicine, organic chemistry, analytical chemistry, physics, etc, because of its high precision, good stability, small size and simple structure. In this thesis, we extensively discussed the basic principle, theoretical model, driving and interface circuit, measurement of network analyzer, application on physisorption of QCM. We presented the simulating calculation about the influence of physical properties on measurable results. The design of hardware and software of the data-acquisition system of QCM was introduced. The implementation of network analyzer on QCM measurements was proposed. Also we got some interesting results about the physisorption of macromolecule on solid surface.
In our research, we did something new as follows:
1) Based on the mechanical and electrical model we carried out a series of simulation on the electrical response of QCM. The result shows that the viscoelastic properties of adsorption films and solution have a large impact on the measurable result of QCM. We calculated the determinate errors which were brought by the solution when quartz acted as the mass sensor.
2) We analysed the important and difficult points of the driving circuit of QCM and proposed a new design of driving circuit which can measure frequency, resistance and dissipation. An intellectual temperature controllable system was designed to satisfy the rigorous demand of temperature stability.
3) We designed a high speed data-acquisition circuit of QCM with USB2.0 interface. It adopts the technique of high speed and high precision A/D converter and frequency measurement with equal-precision. It has two analog channels and can be used in many scientific and commercial fields.
4) We built a system in order to determine the parameters of QCM based on network analyzer. It can measure the electrical parameters of QCM at different harmonics. It can work under extremely lossy circumstances and can be used together with the general QCM apparatus.
5) We carried out the experiments of physisorption of PNIPAM on gold surface by QCM. The results suggest that the adsorption of PNIPAM is strongly influenced by the conformation of the polymer. The adsorption kinetics in the swollen state is governed by molecular diffusion to the adsorption substrate; the adsorption time constant depends strongly on concentration and temperature. The time constant for PNIPAM in the collapsed state is nearly temperature- and concentration-independent. In the concentration range below 100 ppm in weight, only a monolayer of PNIPAM in the swollen state can form on the gold electrode surface of QCM. As the polymer transforms to the collapsed state, multilayer PNIPAM forms on the same substrate.
本研究工作的主要创新点在于:
1)基于QCM的力学模型和电学模型开展了一系列关于QCM电学响应的模拟计算。计算结果给出了膜的粘弹性和溶液属性对QCM测量结果的影响,指出了液相中QCM作为质量传感器所带来的测量偏差。
2)分析了QCM驱动电路的重点和难点,给出了一种能测量耗散因子和串联电阻以及串联谐振频率的QCM驱动电路的实现方案。针对QCM对温度稳定性的苛刻要求设计出了一套智能温度控制系统,温度稳定度极高。
3)针对此QCM驱动电路,设计出了一套基于USB2.0接口的高速数据采集系统。采用了高速和高精度模数转换技术以及等精度频率测量技术,拥有两路模拟通道,可以同时采集两路QCM模拟数据以便做差分运算和比较分析。对外接口简单,使用方便,具有较高的科研价值和商业价值。
4)设计了一套基于网络分析仪的QCM参数测量系统,给出了详细的硬件和软件实现方案,能够方便地获取各种负载环境下晶体各次谐波所对应的QCM电学参数,并通过实验验证了此系统的有效性。此系统功能强大,可测参数多,晶体能工作在很高的能量耗散环境中,可与通用的QCM互补使用。
5)用QCM开展了金表面上聚(N-异丙基丙烯酰胺)(PNIPAM)的物理吸附实验,结果表明PNIPAM的结构强烈地影响着其在固体表面上的物理吸附。伸张状态下的吸附动力学受分子向吸附底层的扩散所影响,吸附时间常数受溶液的浓度和温度的影响较大。塌缩状态下PNIPAM的吸附时间常数基本上不依赖于温度和浓度。浓度在0-100ppm的范围内,伸张状态下的PNIPAM只在金表面形成单层吸附膜。而当聚合物转变到塌缩态时,同样的底层上会形成多层膜。
Quartz Crystal Microbalance (QCM) is a new type of micro-mass sensor which allows accurate measurements of mass, viscosity and shear modulus on nano-scale. It has been used widely in many fields, such as electrochemistry, biomedicine, organic chemistry, analytical chemistry, physics, etc, because of its high precision, good stability, small size and simple structure. In this thesis, we extensively discussed the basic principle, theoretical model, driving and interface circuit, measurement of network analyzer, application on physisorption of QCM. We presented the simulating calculation about the influence of physical properties on measurable results. The design of hardware and software of the data-acquisition system of QCM was introduced. The implementation of network analyzer on QCM measurements was proposed. Also we got some interesting results about the physisorption of macromolecule on solid surface.
In our research, we did something new as follows:
1) Based on the mechanical and electrical model we carried out a series of simulation on the electrical response of QCM. The result shows that the viscoelastic properties of adsorption films and solution have a large impact on the measurable result of QCM. We calculated the determinate errors which were brought by the solution when quartz acted as the mass sensor.
2) We analysed the important and difficult points of the driving circuit of QCM and proposed a new design of driving circuit which can measure frequency, resistance and dissipation. An intellectual temperature controllable system was designed to satisfy the rigorous demand of temperature stability.
3) We designed a high speed data-acquisition circuit of QCM with USB2.0 interface. It adopts the technique of high speed and high precision A/D converter and frequency measurement with equal-precision. It has two analog channels and can be used in many scientific and commercial fields.
4) We built a system in order to determine the parameters of QCM based on network analyzer. It can measure the electrical parameters of QCM at different harmonics. It can work under extremely lossy circumstances and can be used together with the general QCM apparatus.
5) We carried out the experiments of physisorption of PNIPAM on gold surface by QCM. The results suggest that the adsorption of PNIPAM is strongly influenced by the conformation of the polymer. The adsorption kinetics in the swollen state is governed by molecular diffusion to the adsorption substrate; the adsorption time constant depends strongly on concentration and temperature. The time constant for PNIPAM in the collapsed state is nearly temperature- and concentration-independent. In the concentration range below 100 ppm in weight, only a monolayer of PNIPAM in the swollen state can form on the gold electrode surface of QCM. As the polymer transforms to the collapsed state, multilayer PNIPAM forms on the same substrate.
引文
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