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纸基爆炸物检测基底的制备及可视化应用研究
王冲
学位类型硕士
导师窦新存
2017-05-27
学位授予单位中国科学院大学
学位授予地点北京
学位专业材料物理与化学
关键词爆炸物检测 表面增强拉曼散射 化学比色法 纸基 机器视觉
摘要

随着恐怖主义对公共安全的威胁,爆炸物检测受到国际反恐领域的高度关注。纸基材料由于其低廉的成本及柔性可擦拭检测的优势,是一种优良的检测平台。在爆炸物检测领域中,科研工作者们将纸基材料与其它技术相结合,制备了越来越多的小型化、智能化的爆炸物纸基检测芯片,极大地降低了爆炸物检测的成本,使爆炸物检测实现小型化、低成本和高精度成为可能。表面增强拉曼散射(SERS)检测具有灵敏度高、指纹识别、易实现便携式检测等特点,已成为重要的定性分析方法,将纸基材料与SERS 技术结合,利用具有良好SERS 增强效应的贵金属纳米粒子负载在纸基材料上,可以制备出超灵敏的、可擦拭检测的柔性SERS 活性基底,实现爆炸物的痕量检测。化学比色法是一种采样简单、可靠性高、性能优异的经典的检测方法。通过开发特异性检测试剂,以纸基材料擦拭取样,在纸基材料上快速的完成显色反应,可实现爆炸物的快速可视化检测。配合特异性检测试剂,开发多通道爆炸物检测纸基反应芯片,利用机器视觉分析不同反应区域的颜色变化,可实现爆炸物的智能化检测。本论文从研制基于纸基材料的爆炸物检测基底入手,配合不同的检测技术,完成对爆炸物的准确快速检测。研究进展分为如下三个部分:1、滤纸负载的银纳米三角片SERS 基底的构建及检测应用研究——制备超灵敏纸基SERS 基底。由于纳米片的边缘和尖端具有强的电磁增强“热点”,可以显著增强表面增强拉曼散射活性。我们使用N,N-二甲基甲酰胺(DMF)并辅助聚乙烯吡咯烷酮(PVP)还原AgNO3 制备了具有锋利边缘的银纳米三角片(厚度20 nm)。通过将银纳米三角片负载在滤纸上,得到了具有良好活性与重现性的柔性SERS 基底,并检测到了浓度低至10-8 M的超痕量的对巯基苯胺(PATP)。通过有限元方法模拟了不同厚度(10-80nm)的银纳米三角片、不同形状的银纳米片(四边形、六边形)以及银纳米棒、纳米立方块、纳米球的等离子体共振特征,证明了锋利的边缘与尖端确实会增强SERS 活性。实验与理论结果都证实了在滤纸上制造的空隙对增强整体SERS 活性起到了很大的作用。此外,滤纸负载银纳米三角片SERS 基底可以灵敏且选择性检测10-6 M 的痕量的制式爆炸物苦味酸(PA)。2、基于化学比色法的爆炸物特异性显色反应研究及在滤纸上的可视化检测——实现在纸基材料上的爆炸物可视化检测。本工作利用化学比色原理,研究了多种制式爆炸物与非制式爆炸物的特异性显色反应,其中包括硝基芳香类、硝胺与硝酸酯类、硝酸盐类、铵盐类、氯酸盐类、过氧化物类、糖类、尿素类、硫磺等多种单体爆炸物及易制爆物;滤纸是实验室常见纸张,具有良好的亲水性及一定的储液能力,并具备柔性擦拭的特点;因此,我们开发了多组可在滤纸基底上显色的爆炸物检测试剂,以滤纸为显色基底,通过擦拭取样,在纸上快速的完成显色反应,实现纸基材料上对爆炸物的快速可视化检测。3、基于多通道爆炸物检测纸基芯片的机器视觉智能化分析仪的研制——实现爆炸物的智能化检测。本工作基于化学比色原理的特异性检测试剂,设计了一种多通道爆炸物检测纸基反应芯片,可作为多组特异性检测试剂的反应平台。基于纸基芯片利用机器视觉分析原理开发了一款手持式爆炸物分析仪,该分析仪使用Android操作系统,通过纸基芯片特定区域反应前后颜色的RGB值变化进行智能化识别分析,可检测多种制式与非制式爆炸物,并可以准确报出类别。其检测范围基本涵盖了我国暴恐案件中出现的大多数爆炸物;同时,我们开发了智能化APP,可方便快速的进行分析数据库扩容及二次开发。

其他摘要

The threat of terrorism attacks is the greatest challenge to homeland security and social stability, and the field of international against-terrorism has paid great attention to the detection of explosives. Based on the advantages of low cost and flexible, paper materials have developed to an excellent substrate for explosive detection. Furthermore, more and more miniaturization, intelligent explosives detection paper base chip are prepared by combining paper-based materials with other technologies, which not only greatly reduced the cost but also improved the accuracy in explosives detection.The surface enhanced Raman scattering (SERS) based detection is a surface-sensitive technique providing the specific structural and vibrational fingerprints of the interested analytes, which makes SERS serve as one of the most powerful tools for qualitative analysis. A flexible SERS substrate with good activity and reproducibility was obtained by combining with paper-based materials. Colorimetric is an excellent classical detection method because of its simple sample, high reliability. Then development specificity detection reagent for explosives, made paper to wipe sampling for color reaction substrate, will reduce the test cost, improve the testing efficiency and accuracy. Fabrication paper-based chips for explosives detection, which can realize the miniaturization of explosives detection platform and intelligent.To realize accurately rapid detection of explosives, my graduation thesis focused on developing explosive detection based on paper-based material substrate with different detection technologies. The research progress can be divided into three parts as follows:1. Silver nanotriangles-loaded filter paper for ultrasensitive SERS detection application benefited by interspacing of sharp edges.The strongly enhanced electromagnetic “hotspots” from the edges and tips of nanoplates are highly preferred to significantly promote the surface enhanced Raman scattering (SERS) activity. Here, Ag nanotriangles with a sharp edge of 20 nm were prepared by the reduction of AgNO3 using N,N-Dimethylformamide with the assistance of Polyvinyl pyrrolidone. By loading Ag nanotriangles onto the filter paper, a flexible SERS substrate with good activity and reproducibility was obtained and the ultratrace detection of 4-aminothiophenol with a concentration as low as 10-8 M was achieved. The sharp edges and tips could boost SERS activity was proved by the finite element method modeling of the plasmonic properties of Ag nanotriangles with different edge thicknesses (10 - 80 nm), Ag nanosheets with different tip acutances (squares and hexagons) together with Ag nanorods, nanocubes and nanospheres. The experimental and theoretical results confirmed that the interspacing created by filter paper plays an important role in enhancing the overall SERS activity. Furthermore, it is shown that the present silver nanotriangles-loaded filter paper SERS substrate can be employed to sensitive and selective detecting ultratrace military explosives picric acid of 10?6 M.2. The explosive detection reagent development and its colorimetric application.Due to the simple and high reliability, colorimetric has developed to an excellent classical detection method. Herein we developed some specificity detection reagents for general explosives and homemade explosives, including TNT, DNT, PA, RDX, HMX, PETN, nitrate, ammonium salt, chlorate, peroxide, sugar, urea, sulphur, etc. Filter paper with good hydrophilicity and the ability to reservoir, and the characteristics of flexible wipe, which make the filter paper to be color reaction substrate. The paper base material on visual detection of explosives could be realized through wiping samples.3. Based on the colorimetric paper-based chip for the development of handheld explosives analyzer.We designed a handheld explosives analyzer on the basis of the colorimetric. The analyzer integrates multiple sets of specificity detection reagent and could analyze the characteristics of a variety of general and homemade explosives. And the analyzer can accurately read out the category of explosives. The testing scope covers the basic critical cases of all occurrences of explosives. Based on the Android operating system, developing a smart APP can facilitate the rapid expansion, database analysis and secondary development.

文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/4977
专题环境科学与技术研究室
作者单位中国科学院新疆理化技术研究所
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王冲. 纸基爆炸物检测基底的制备及可视化应用研究[D]. 北京. 中国科学院大学,2017.
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