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同时测量纳米颗粒悬浊液粒度、密度及浓度的方法研究

ISSN号：1004-4957
期刊名称：分析测试学报
时间：2011
页码：1246-1251
分类：O657.5[理学—分析化学;理学—化学] TQ577.77[化学工程—精细化工]
作者机构：[1]上海理工大学颗粒与两相流测量所,上海200093
相关基金：国家自然科学基金资助项目（50706029,50836003,51076106）;上海市科委资助项目（10540501000）
相关项目：超声多方法融合测量变参数液固颗粒两相体系研究

关键词：超声, 两相流, 多参数, 颗粒粒度, 浓度和密度, ultrasound, two-phase flow, multi-parameter, particle size, concentration and density

中文摘要：

提出了一种基于超声检测同时测量纳米颗粒悬浊液的粒度、密度和浓度的方法。设计了一套高频宽带脉冲超声波检测系统，以纳米掺锑氧化锡（ATO）悬浊液为研究对象，结合脉冲回波技术，获得了频率为17～26MHz的声衰减谱。据此运用最优正则化方法求解粒度反演方程，得到纳米ATO颗粒的分布曲线，中位径为22．07nm，该值与离心沉降纳米分析仪测量结果较吻合，中位径偏差仅为0．1％。以相同的实验装置，采用多次回波技术，获得了质量分数分别为5％、10％、15％和20％的纳米ATO悬浊液多达12次的回波信号，经过进一步数据处理和声学理论计算得到该悬浊液的声阻抗、密度和浓度，密度和浓度的相对测量误差分别在0．6％和8％以内。该方法具有实验装置简单，耗时短，易实现在线测量的特点，可用于纳米颗粒的加工和制备过程中颗粒相粒度、密度和浓度的实时监测。

英文摘要：

A method for measuring particle size distribution, density and concentration of nanometer suspension was proposed, and the measurement apparatus and system was designed. Meanwhile, the pulse echo mode was adopted to measure the attenuation spectrum of nano-antimony tin oxide （ ATO ） suspension at high frequencies. A wide-band ultrasonic transducer with a center frequency of 25 MHz （V324-SU, OLYMPUS ） served as an emitter and a receiver simultaneously in the experiments. Then it can yield an ultrasonic spectrum over the frequency from 17 MHz to 26 MHz. The optimum regularization algorithm was applied to minimize the influence of ill-conditioned equation during the inversion of particle size distribution. The recovered median size D50 of nano-ATO was 22.07 nm which was in agreement with that of the sedimentation method with the error no more than 0. 1%. At the same time, the multiple reflection approach was employed to obtain the ultrasonic impedance of the nanometer suspension. Several groups of superb ultrasonic signals consisting of more than 12 pluse-echoes in each one, were acquired with the same ultrasonic transducer. The ultrasonic velocity, overall density and concentration of the aqueous ATO suspensions can be determined based on the mathematical derivation and acoustic theory. Experimental results showed that the error of density and concentration was within 0.6% and 8% , respectively. Due to its avantages of reliable principle, simple apparatus and time-saving, the proposed method could provide an online monitoring for the particle size, density and concentration of nano-particle materials during the processing and preparation.

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