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高质量、大尺寸的磷化铟量子点(InP quantum dots)的制备对其在生物荧光标记等领域的应用有重大的意义.提出一种持续注射法合成InPZnS/ZnS核壳结构量子点.首先将磷化锌和硫酸反应生成的磷化氢持续注入高温铟前体溶液中,并在反应开始加入适量的锌和硫前体,可制得合金结构的InPZnS核,其量子产率达9%.该方法无需加锌回流处理,可直接升温包覆ZnS壳层,成功制备出发光波长至680 nm且量子产率接近50%的InPZnS/ZnS核壳结构量子点.同时系统地研究了反应物配比对量子点粒径的影响规律,结果表明:通过调控反应物配比可合成不同粒径的InP量子点,其光谱范围几乎可覆盖整个可见光区,甚至到近红外区.通过吸收光谱、荧光光谱、透射电子显微镜、X射线衍射仪和X射线能谱仪考察了所制备量子点的光学特性和形貌结构.最后,采用其它磷前体探究了此方法的通用性,通过注射泵将三(二乙氨基)膦持续注入到高温铟前体溶液中,同样制备出较大尺寸的InP量子点,其发光波长至710 nm.
The preparation of high-quality, large-size InP quantum dots is of great significance for its application in the field of bioluminescence labeling, etc. A continuous injection method for the synthesis of InPZnS / ZnS core-shell quantum dots is proposed The phosphine generated by the reaction between zinc phosphide and sulfuric acid is continuously injected into the high-temperature indium precursor solution, and an appropriate amount of zinc and sulfur precursors are added at the beginning of the reaction to produce an InPZnS alloy with an alloy structure with a quantum yield of 9% The method can directly heat up the ZnS shell without adding zinc reflow and successfully prepare the InPZnS / ZnS core-shell quantum dots with an emission wavelength of 680 nm and a quantum yield close to 50% .At the same time, The results show that the InP quantum dots with different particle sizes can be synthesized by adjusting the ratio of reactants, and the spectral range can cover almost the entire visible light region and even the near infrared region.By the absorption spectra, Fluorescence spectroscopy, transmission electron microscopy, X-ray diffraction and X-ray energy dispersive spectroscopy were used to investigate the optical properties and morphology of the prepared quantum dots.Finally, the versatility of this method was explored by using other phosphorus precursors, Tris (diethylamino) phosphine continuous injection to a high temperature the indium precursor solution, prepared in the same InP quantum dots of larger size, the emission wavelength to 710 nm.