Chemical Synthesis of ZnO Nanocrystals

Y. Wu, A. Tok, F. Boey, X. Zeng, X. Zhang
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引用次数: 2

Abstract

Nano-crystalline ZnO particles were synthesized using alcoholic solutions of zinc acetate dihydrate through a colloidal process. Five types of capping agents: 3-aminopropyl trimethoxysilane (Am), tetraethyl orthosilicate (TEOS), mercaptosuccinic acid (Ms), 3-mercaptopropyl trimethoxysilane (Mp) and polyvinylpyrrolidone (Pv) were added at the first ZnO precipitation time (1stPPT) to limit the particle growth. The first three capping agents effectively capped the ZnO nanoparticles and limited the growth of the particles, while the last two capping agents caused agglomeration or larger clusters in the solutions. Particles synthesized were in the size range of 10nm to 30nm after capping, and grew to 60nm and 100nm in 3 weeks and 6 weeks respectively during storage at ambient conditions. Refluxing time was found to only affect the 1stPPT time. Washing by methanol and water and slow drying are very important in converting Zn(OH)2into ZnO. XRD analyses revealed that single crystal ZnO nanoparticles were achieved with crystal size 53-55nm. Photoluminescence (PL) spectra showed high intensity in UV emission and very low intensity in the visible emission, which indicates a good surface morphology of the ZnO nanoparticles with little surface defect. Optical absorption spectra showed absorption at wavelength of 380nm from the uncapped ZnO, corresponding to the band-gap of bulk ZnO. While capped ZnO absorbed at shorter wavelength (350nm) indicating a much smaller particle size.
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氧化锌纳米晶的化学合成
以二水乙酸锌醇溶液为原料,采用胶体法制备了纳米晶氧化锌颗粒。在第一次ZnO沉淀时间(1stPPT)加入5种封盖剂:3-氨基丙基三甲氧基硅烷(Am)、正硅酸四乙酯(TEOS)、巯基琥珀酸(Ms)、3-巯基丙基三甲氧基硅烷(Mp)和聚乙烯吡罗烷酮(Pv)来限制颗粒的生长。前3种封盖剂有效封盖ZnO纳米颗粒,限制了颗粒的生长,而后2种封盖剂在溶液中导致团聚或更大的团簇。封盖后合成的颗粒尺寸范围为10nm ~ 30nm,在常温条件下储存3周和6周后分别生长到60nm和100nm。返流时间仅影响第1次ppt时间。在将Zn(OH)2转化为ZnO的过程中,甲醇和水的洗涤和缓慢干燥是非常重要的。XRD分析表明,制备得到了晶粒尺寸为53 ~ 55nm的ZnO纳米单晶。光致发光(PL)光谱显示紫外发射强度高,可见光发射强度极低,表明ZnO纳米颗粒表面形貌良好,表面缺陷小。光学吸收光谱显示,未封顶ZnO在380nm波长处被吸收,与体ZnO的带隙相对应。而封顶ZnO吸收波长较短(350nm),表明粒径小得多。
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