以锌(II)希夫碱配合物为前驱体热分解法制备ZnO纳米颗粒及表征

IF 3.5 Q2 CHEMISTRY, MULTIDISCIPLINARY Chemical Methodologies Pub Date : 2019-09-01 DOI:10.33945/SAMI/CHEMM.2019.5.6
A. D. Khalaji
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引用次数: 3

摘要

本文以ZnBr2和希夫碱配体(pma-ba)2en为原料,在甲醇溶液中以1:1的摩尔比,利用超声波辅助浴法制备了纳米尺寸的单核四面体锌(II)配合物,其通式为Zn((pma-ba)2en)Br2.2H2O, (pma-ba)2en=N,Nⅱ-二{(参氨基)苄基}乙二胺。采用元素分析(CHN)、傅里叶变换红外光谱(FT-IR)、x射线粉末衍射(XRD)和扫描电子显微镜(SEM)对锌(II)希夫碱配合物进行了表征。同时,研究了该配合物在室温至780℃氩气氛下的热稳定性。热重分析表明锌(II)配合物的分解分为三个阶段。分解结束时,剩余部分为ZnO。用XRD证实了热分解后ZnO的制备。配合物的XRD谱图表明,尖锐的晶峰表明配合物的晶相。根据Scherrer公式,计算出配合物的纳米尺寸的平均尺寸>200 nm,并通过SEM图像证实了这一点。此外,将锌(II)希夫碱配合物在550℃下热分解3 h,得到ZnO纳米颗粒。XRD结果表明,ZnO产品具有良好的结晶度,无杂质。计算得到ZnO纳米颗粒的平均尺寸<50 nm。
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Preparation and Characterization of ZnO Nanoparticles via Thermal Decomposition from Zinc(II) Schiff Base Complex as New Precursor
In this paper,nano-sized of mononuclear tetrahedral zinc(II) complex with the general formula of Zn((pma-ba)2en)Br2.2H2O, (pma-ba)2en=N,N¢-bis{(paramethylamino)benzylidene}ethylenediamine, was synthesized by ultrasonic bath assisted from the reaction of ZnBr2 and Schiff base ligand (pma-ba)2en in molar ratio 1:1 in methanol solution. The zinc(II) Schiff base complex characterized by elemental analyses (CHN), Fourier transformed infra-red (FT-IR) spectroscopy, X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). Also, thermal stability of the complex was studied from room temperature to 780 °C under argon atmosphere. TGA shows three stages for decomposition of the zinc(II) complex. At the end of decomposition, the remainder part is ZnO. The preparation of ZnO at the end of thermal decomposition confirmed with XRD. The XRD pattern of complex has shown that the sharp crystalline peaks indicating the crystalline phase in complex. By Scherrer’s formula, the average size of the nano-sizes of the complex was calculated >200 nm, that confirmed by SEM image. In addition, ZnO nanoparticles were obtained by thermal decomposition of zinc(II) Schiff base complex at 550 °C for 3 h. XRD result that the good crystallinity for zinc(II) oxide with no impurity observed in the ZnO product. The average size of the nanoparticles of the ZnO was calculated <50 nm.
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来源期刊
Chemical Methodologies
Chemical Methodologies CHEMISTRY, MULTIDISCIPLINARY-
CiteScore
3.10
自引率
1.80%
发文量
8
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