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Porous Silicon을 이용한 폭발물 탐지

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Author(s)
김범석
Issued Date
2006
Abstract
Detection of nitroaromatic compounds is desirable since there are approximately 120 million unexploded land mines worldwide. Detection of nitroaromatic compound based on adsorption into polymers has been reported. Chemo-selective polymers on SAW(surface acoustic wave) device, cyclic voltammetry using gold micro-electrode covered with non-volatile electrolyte, and organic polymer has been previously reported to detect TNT vapor.
In this study very sensitive detection of TNT (2,4,6-trinitrotoluene), DNT (2,4-dinitrotoluene), NB (nitrobenzene), and PA (picric acid) has been achieved in gas phase with porous silicon films using photoluminescence quenching of the silicon crystallites as a trans- duction mode. Porous silicon films are electrochemically etched from crystalline silicon wafers in an aqueous solution of hydrofluoric acid. We used two types of PSi for detection of nitroaromatic compounds. One is the freshly etched PSi and the other is hydrosilylated PSi.
First, fresh porous silicon synthesized from the electrochemical etching Detection of nitroaromatic compounds is desirable since there are approximately 120 million unexploded land mines worldwide. Detection of nitroaromatic compound based on adsorption into polymers has been reported. Chemo-selective polymers on SAW(surface acoustic wave) device, cyclic voltammetry using gold micro-electrode covered with non-volatile electrolyte, and organic polymer has been previously reported to detect TNT vapor.
In this study very sensitive detection of TNT (2,4,6-trinitrotoluene), DNT (2,4-dinitrotoluene), NB (nitrobenzene), and PA (picric acid) has been achieved in gas phase with porous silicon films using photoluminescence quenching of the silicon crystallites as a trans- duction mode. Porous silicon films are electrochemically etched from crystalline silicon wafers in an aqueous solution of hydrofluoric acid. We used two types of PSi for detection of nitroaromatic compounds. One is the freshly etched PSi and the other is hydrosilylated PSi.
First, fresh porous silicon synthesized from the electrochemical etching described above exhibits strong photoluminescence(PL) at the wavelength around 720 nm. The intensity of PL from the freshly etched porous silicon is decreased upon the exposure of the vapor of NB, DNT, TNT or PA. Flow rate of analyte-saturated air is about 5 L/min. After 30 minute, the percentage of quenching PL is 37%, 45% and 40% in the case of DNT-saturated air (vapor pressure = 200 ppb at 25?C), TNT-saturated air (vapor pressure = 4 ppb at 25?C) and PA-saturated air, respectively. It is interesting to report that 38% of quenching PL for nitrobenzene was observed just in 50 seconds.
Secondly, hydrosilylation of PSi has been also investigated with methylvinyltetraphenylsilole(MVTPS). It is observed that the intensity of emission from porous silicon was decreased after hydrosilylation. The detection of nitroaromatic compounds has been achieved using surface-derivatized porous silicon with methylvinyltetraphenylsilole. Hydrosilylated PSi shows the PL at 660 nm, which exhibits the blue-shift of the wavelength compared to fresh PSi. The percentage of quenching PL of hydrosilylated PSi after exposure to nitroaromatic compounds for 30 min is 47% for DNT-saturated air, 63% for TNT-saturated air, and 52% for PA-saturated air, respectively. The percentage of quenching PL with nitrobenzene-saturated air is about 45% in 50 seconds. The detection limit on time for the analyte-saturated air is 1 sec. for NB, 1 min. for DNT, and 15 sec. for TNT, respectively.
The mechanism of quenching PL is attributed to the electron transfer quenching of quantum-sized nano-crystallites in the porous silicon matrix to analyte. We also observed the chemical oxidation of porous silicon by the nitroaromatics that leads to an irreversible response at long exposure times (>5min).
Partially reversible detection mode for nitroaromatic compounds was observed.
Consequently, it has been shown that porous silicon is a versatile substrate for chemical sensing with a large surface area and highly sensitive transduction modes.
Alternative Title
Detection of Explosives Based on Porous Silicon
Alternative Author(s)
Kim, Bum seok
Affiliation
조선대학교 대학원
Department
일반대학원 화학과
Advisor
조성동, 손홍래
Awarded Date
2006-02
Table Of Contents
Abstract = 1
Ⅰ.Introduction = 4
Ⅱ.Experimental Section = 6
1.Sample preparation = 6
2.Photoluminescence measurement = 8
3.Infrared spectroscopic measurement = 9
4.Preparation of gas and nitroaromatic compounds = 9
5.Synthesis of methylvinyltetraphenylsilole (MVTPS) = 10
5.1 Synthesis of methylchlorosilole = 10
5.2 Synthesis of methylvinyltetraphenylsilole(MVPTS) = 12
6.PSi 표면의 hydrosilylation = 14
Ⅲ.Results and Discussion = 18
1.Emission characteristics of PSi depending on current density & etch time = 18
2.Photoluminescence quenching by nitroaromatic compounds = 20
2-1.Mechanism of reversible quenching of photoluminescence = 20
2-2.Fresh PSi(50 mA/15 min) 칩을 이용한 폭발물 탐지 = 20
2-3.Fresh PSi(300 mA/5 min) 칩을 이용한 폭발물 탐지 = 24
2-4.Hydrosilylated PSi 칩을 이용한 폭발물 탐지 = 29
Ⅳ.Device Fabrication = 37
1.Semiconductor sensor = 37
2.Fabrication of photoluminescent porous silicon chip as sensors = 37
Ⅴ.Conclusion = 41
Ⅵ.References = 43
Degree
Master
Publisher
조선대학교 대학원
Citation
김범석. (2006). Porous Silicon을 이용한 폭발물 탐지.
Type
Dissertation
URI
https://oak.chosun.ac.kr/handle/2020.oak/6067
http://chosun.dcollection.net/common/orgView/200000232727
Appears in Collections:
General Graduate School > 3. Theses(Master)
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