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磁控溅射WO₃纳米颗粒的合成——2-氯乙基乙基硫醚和甲基膦酸二甲酯的降解

Synthesis of magnetron sputtered WO₃ nanoparticles-degradation of 2-chloroethyl ethyl sulfide and dimethyl methyl phosphonate.

作者信息

Verma Monu, Chandra Ramesh, Gupta Vinod Kumar

机构信息

Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667, India; Institute Instrumentation Centre, Indian Institute of Technology Roorkee, Roorkee 247667, India.

Institute Instrumentation Centre, Indian Institute of Technology Roorkee, Roorkee 247667, India.

出版信息

J Colloid Interface Sci. 2015 Sep 1;453:60-68. doi: 10.1016/j.jcis.2015.04.039. Epub 2015 Apr 22.

DOI:10.1016/j.jcis.2015.04.039
PMID:25965433
Abstract

In the present study, tungsten oxide nanoparticles were synthesized using DC magnetron sputtering and investigated their potential for decontamination of 2-chloroethyl ethyl sulfide (CEES) and dimethyl methyl phosphonate (DMMP). The tungsten oxide nanoparticles were characterized by Powder XRD, FE-SEM, EDS, TEM, TGA, N2-BET and FT-IR techniques. The XRD patterns of as-deposited and post annealed tungsten oxide nanoparticles reveal that the crystallite size of detected monoclinic phase WO3 nanoparticle was increased with increasing annealing temperatures. The phase and increase in particles size of WO3 nanoparticles were also confirmed by Raman and TEM analyses. The obtained surface area (∼63-33 m(2)/g) of magnetron sputtered WO3 nanoparticles was found to be enhanced significantly as compared to reported surface area of WO3 nanoparticles synthesis by various techniques. The study of degradation reactions of CEES and DMMP on the surface of obtained nanoparticles was carried out by using GC and GC-MS techniques. The decontamination reactions were found to be pseudo first order steady state with rate constant (k) and half life values 0.143-0.109 h(-1) and 4.82-6.49 h for CEES and 0.018-0.010 h(-1) and 36.87-66.65 h for DMMP, respectively. The FT-IR data reveal the role of hydrolysis reactions in the decontamination of CEES as well as DMMP.

摘要

在本研究中,采用直流磁控溅射法合成了氧化钨纳米颗粒,并研究了其对2-氯乙基乙基硫醚(CEES)和甲基膦酸二甲酯(DMMP)的去污潜力。通过粉末XRD、场发射扫描电子显微镜(FE-SEM)、能谱仪(EDS)、透射电子显微镜(TEM)、热重分析仪(TGA)、N2-比表面积分析仪(N2-BET)和傅里叶变换红外光谱仪(FT-IR)技术对氧化钨纳米颗粒进行了表征。沉积态和退火后的氧化钨纳米颗粒的XRD图谱表明,随着退火温度的升高,检测到的单斜相WO3纳米颗粒的微晶尺寸增大。拉曼光谱和TEM分析也证实了WO3纳米颗粒的相和粒径增加。与通过各种技术合成的WO3纳米颗粒的报道表面积相比,发现磁控溅射WO3纳米颗粒的表面积(约63-33 m(2)/g)显著提高。利用气相色谱(GC)和气相色谱-质谱联用(GC-MS)技术对CEES和DMMP在所得纳米颗粒表面的降解反应进行了研究。发现去污反应为准一级稳态反应,CEES的速率常数(k)和半衰期分别为0.143-0.109 h(-1)和4.82-6.49 h,DMMP的速率常数(k)和半衰期分别为0.018-0.010 h(-1)和36.87-66.65 h。FT-IR数据揭示了水解反应在CEES和DMMP去污中的作用。

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