基于后向动态光散射的高浓度纳米颗粒粒径测量技术的研究
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摘要
作为21世纪的重要学科之一，纳米技术为材料科学带来了广泛而深刻的变革。我国在2006年2月9日公布的国家中长期科技发展规划纲要中，已把“纳米技术研究”列为4个重大科学研究计划之一。纳米颗粒的粒度检测是纳米技术中极其重要的一个方面，特别是近年来随着纳米技术广泛应用于制药、生物、电子、光电子、能源、催化和陶瓷等领域，各行业对纳米颗粒粒径的测量和监控要求也越来越严格，其发展水平已成为当前衡量一个国家纳米科技水平以及在这方面综合实力的重要标志之一。较之先进国家，我国在纳米颗粒的粒度测量技术及仪器方面尚有不小的差距，尤其是在高浓度纳米颗粒的粒径测量方面差距更大。
动态光散射技术是目前应用最广泛的纳米颗粒粒径测量技术，但传统的动态光散射法一般只适用于稀溶液的测量。本文针对高浓度下的纳米颗粒粒径测量这一技术难点，提出了基于后向动态光散射的高浓度纳米颗粒粒径测量方法，以及基于现代功率谱估计的动态光散射频谱测量法。
本论文的主要研究内容包括：
一．研究了传统动态光散射法测量纳米颗粒悬浮液时其浓度受限的诸多因素，提出了当检测高浓度纳米颗粒的粒径时，应首先着眼于消除散射光的多重散射效应，并针对这一难点分析了国内外研究的现状，最后研发了基于后向动态光散射的高浓度纳米颗粒粒径测量装置。
二．从麦克斯韦方程组出发推导了基于信号涨落的散射光场一般方程的表达式，针对颗粒布朗运动的统计特性，研究了散射光强涨落的表征方法，建立了与涨落有关的颗粒粒径信息表达式。
三.利用颗粒运动的特征函数的概念，并认为基于粒子运动模型的散射光谱与粒子运动的特征函数是一时空双重傅立叶变换，进而建立了散射光场谱密度与颗粒粒径的联系。
四．研究了动态光散射频谱测量技术的发展及其存在的问题，提出了一种新的基于现代功率谱估计的动态光散射频谱测量方法。从光电倍增管计数统计特性出发，根据Wiener-Khintchine定理，将时域自相关函数转换为频域的功率谱密度，得到了散射光强的谱密度表达式；根据FFT，利用现代功率谱估计中的自回归（AR）模型，实现了动态光散射信号功率谱密度的估计；最后通过计算信号自相关矩阵的秩得到AR模型中的阶数p，从而解决了在应用中由于待测颗粒粒径未知而无法确定阶数p的问题。
五．根据本文研制的高浓度纳米颗粒粒径测量系统，分别采用时域相关光谱方法和频域谱密度测量法进行了相应的实验，并与传统光子相关光谱测量法进行了比较和分析。
六．本文还对实际应用中与测量相关的一些问题进行了讨论，包括：光源的偏振态变化对测量结果的影响，采样时间的间隔对测量结果的影响，以及传统动态光散射系统的最佳检测孔径等问题。
As one of the important subjects in the21st century, nanotechnology has broughtmaterials science extensive and profound changes. Our country has identified"nanotechnology research" as one of the four major scientific research programs in theoutline of development planning, which was announced in medium and long-termNational Science and Technology in9th Feb.2006. Nanoparticle sizing is extremelyimportant in nano-technology. Especially in recent years, with the nano-technologywidely used in pharmaceutical, biotechnology, electronics, optoelectronics, energy,catalytic and ceramic and other fields, the requirements of various industries for themeasurement and monitoring of nanoparticle are increasingly stringent. And itsdevelopment level has become a standard to measure the level of a NationalNanotechnology and overall strength in this area. Compared with advanced countries,Our country has a distance in the nanoparticle sizing techniques and equipment,particularly in the measurement of nano-particle size in concentrated dispersion.
Dynamic light scattering (DLS) technique is the most widely used nano-particlesizing technique currently. However, the traditional dynamic light scattering method isgenerally applied only to the measurement in dilute dispersion. In this paper, a methodwas proposed to solve the difficulty of the measurement of nanoparticle in concentrateddispersion, which was based on backscattering dynamic light, as well as themeasurement by dynamic light scattering spectrum based on the modern powerspectrum estimation.
The main researches are as following:
The factors, which limit the measurement by traditional DLS in concentrateddispersion, are studied. It was proposed that the focus should be first put on theelimination of the multiple scattering effect, when measuring the nanoparticle inconcentrated dispersion. And a review on research status at home and abroad wasanalyzed for this difficulty. Finally the method and equipment for nanoparticle sizingbased on backscattering dynamic light in concentrated dispersion was developed.
Starting from the Maxwell's equations, the expressions of the general equation ofthe scattered light based on the fluctuation of the signal were derived. According to thestatistical properties of particles with Brownian motion, the characterization method ofthe intensity fluctuation of scattering light was studied, and the expressions of the particle size related to the fluctuation of the signal were set up.
The relationship between the particle size and the spectrum density of scatteredlight field was set up, using the characteristic function of particle movement and that itis a double Fourier transform in time and space between the scattering spectra based onthe model of the movement of particle and characteristic function of movement.
The development and existence of the problems of dynamic light scatteringspectrum measurement technique were studied. A new method was proposed based onthe modern power spectrum estimation. From the counting statistical characteristics ofthe Photomultiplier tubes, the spectral density expression of the intensity of scatteringlight was deduced by converting the time-domain auto-correlation function to frequencydomain power spectral density according to Wiener-Khintchine theorem; The powerspectral density estimation of the dynamic scattering light was implemented by the useof autoregressive (AR) model of modern power spectrum estimation with FFT; Finallythe problem that the number of p-order could not be determined because of theunknown particle size in application was resolved by calculating the rank of the matrixof signal auto-correlation.
The measurement system for nanoparticle sizing in concentrated dispersion wasdeveloped based on backscattering dynamic light scattering, which includes: preparationof test nanoparticle dispersion, optical system (the selection of light source, the incidentand scattering optical path), the devices for signal detecting and treatment (the digitalcorrelator and photon counter were used separately based on two methods of signalanalysis). The experiments were carried out by correlation spectroscopy in time-domainand spectral density in frequency domain separately, and the results were compared andanalyzed with the measurements using traditional photon correlation spectroscopy.
A number of problems about the practical application of measurement werediscussed, which includes: The impact of the measurement result from the changes ofthe Polarization of light source; the change in measurement results led by the samplingtime, as well as the problem of the best detection aperture in traditional dynamic lightscattering system.
动态光散射技术是目前应用最广泛的纳米颗粒粒径测量技术，但传统的动态光散射法一般只适用于稀溶液的测量。本文针对高浓度下的纳米颗粒粒径测量这一技术难点，提出了基于后向动态光散射的高浓度纳米颗粒粒径测量方法，以及基于现代功率谱估计的动态光散射频谱测量法。
本论文的主要研究内容包括：
一．研究了传统动态光散射法测量纳米颗粒悬浮液时其浓度受限的诸多因素，提出了当检测高浓度纳米颗粒的粒径时，应首先着眼于消除散射光的多重散射效应，并针对这一难点分析了国内外研究的现状，最后研发了基于后向动态光散射的高浓度纳米颗粒粒径测量装置。
二．从麦克斯韦方程组出发推导了基于信号涨落的散射光场一般方程的表达式，针对颗粒布朗运动的统计特性，研究了散射光强涨落的表征方法，建立了与涨落有关的颗粒粒径信息表达式。
三.利用颗粒运动的特征函数的概念，并认为基于粒子运动模型的散射光谱与粒子运动的特征函数是一时空双重傅立叶变换，进而建立了散射光场谱密度与颗粒粒径的联系。
四．研究了动态光散射频谱测量技术的发展及其存在的问题，提出了一种新的基于现代功率谱估计的动态光散射频谱测量方法。从光电倍增管计数统计特性出发，根据Wiener-Khintchine定理，将时域自相关函数转换为频域的功率谱密度，得到了散射光强的谱密度表达式；根据FFT，利用现代功率谱估计中的自回归（AR）模型，实现了动态光散射信号功率谱密度的估计；最后通过计算信号自相关矩阵的秩得到AR模型中的阶数p，从而解决了在应用中由于待测颗粒粒径未知而无法确定阶数p的问题。
五．根据本文研制的高浓度纳米颗粒粒径测量系统，分别采用时域相关光谱方法和频域谱密度测量法进行了相应的实验，并与传统光子相关光谱测量法进行了比较和分析。
六．本文还对实际应用中与测量相关的一些问题进行了讨论，包括：光源的偏振态变化对测量结果的影响，采样时间的间隔对测量结果的影响，以及传统动态光散射系统的最佳检测孔径等问题。
As one of the important subjects in the21st century, nanotechnology has broughtmaterials science extensive and profound changes. Our country has identified"nanotechnology research" as one of the four major scientific research programs in theoutline of development planning, which was announced in medium and long-termNational Science and Technology in9th Feb.2006. Nanoparticle sizing is extremelyimportant in nano-technology. Especially in recent years, with the nano-technologywidely used in pharmaceutical, biotechnology, electronics, optoelectronics, energy,catalytic and ceramic and other fields, the requirements of various industries for themeasurement and monitoring of nanoparticle are increasingly stringent. And itsdevelopment level has become a standard to measure the level of a NationalNanotechnology and overall strength in this area. Compared with advanced countries,Our country has a distance in the nanoparticle sizing techniques and equipment,particularly in the measurement of nano-particle size in concentrated dispersion.
Dynamic light scattering (DLS) technique is the most widely used nano-particlesizing technique currently. However, the traditional dynamic light scattering method isgenerally applied only to the measurement in dilute dispersion. In this paper, a methodwas proposed to solve the difficulty of the measurement of nanoparticle in concentrateddispersion, which was based on backscattering dynamic light, as well as themeasurement by dynamic light scattering spectrum based on the modern powerspectrum estimation.
The main researches are as following:
The factors, which limit the measurement by traditional DLS in concentrateddispersion, are studied. It was proposed that the focus should be first put on theelimination of the multiple scattering effect, when measuring the nanoparticle inconcentrated dispersion. And a review on research status at home and abroad wasanalyzed for this difficulty. Finally the method and equipment for nanoparticle sizingbased on backscattering dynamic light in concentrated dispersion was developed.
Starting from the Maxwell's equations, the expressions of the general equation ofthe scattered light based on the fluctuation of the signal were derived. According to thestatistical properties of particles with Brownian motion, the characterization method ofthe intensity fluctuation of scattering light was studied, and the expressions of the particle size related to the fluctuation of the signal were set up.
The relationship between the particle size and the spectrum density of scatteredlight field was set up, using the characteristic function of particle movement and that itis a double Fourier transform in time and space between the scattering spectra based onthe model of the movement of particle and characteristic function of movement.
The development and existence of the problems of dynamic light scatteringspectrum measurement technique were studied. A new method was proposed based onthe modern power spectrum estimation. From the counting statistical characteristics ofthe Photomultiplier tubes, the spectral density expression of the intensity of scatteringlight was deduced by converting the time-domain auto-correlation function to frequencydomain power spectral density according to Wiener-Khintchine theorem; The powerspectral density estimation of the dynamic scattering light was implemented by the useof autoregressive (AR) model of modern power spectrum estimation with FFT; Finallythe problem that the number of p-order could not be determined because of theunknown particle size in application was resolved by calculating the rank of the matrixof signal auto-correlation.
The measurement system for nanoparticle sizing in concentrated dispersion wasdeveloped based on backscattering dynamic light scattering, which includes: preparationof test nanoparticle dispersion, optical system (the selection of light source, the incidentand scattering optical path), the devices for signal detecting and treatment (the digitalcorrelator and photon counter were used separately based on two methods of signalanalysis). The experiments were carried out by correlation spectroscopy in time-domainand spectral density in frequency domain separately, and the results were compared andanalyzed with the measurements using traditional photon correlation spectroscopy.
A number of problems about the practical application of measurement werediscussed, which includes: The impact of the measurement result from the changes ofthe Polarization of light source; the change in measurement results led by the samplingtime, as well as the problem of the best detection aperture in traditional dynamic lightscattering system.
引文
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