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Micro-reaction device and method for synthesizing cadmium selenide nano-crystal by using temperature gradient

A micro-reaction device and temperature gradient technology, applied in the field of micro-chemical machinery and nano-materials, can solve the problems of out-of-control, reduction, and poor precision in the growth process of nano-crystals, achieve large-scale preparation, flexible implementation methods, and improve yield and quality Effect

Inactive Publication Date: 2008-08-06
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

Among them, the organic solvothermal method in the flask synthesis device is a good example for the preparation of high-quality CdSe nanocrystals, but the whole reaction process has almost strict requirements on the reaction temperature, reaction time and the uniformity of the reaction materials, and the geometric amplification of the flask reaction device It will bring problems such as long control response time and poor precision, and it is difficult to ensure high consistency of reaction conditions
The effectiveness of high-temperature nucleation and low-temperature growth in controlling the reaction kinetics of nanocrystals has been widely verified. However, the lack of control accuracy and control response time of the flask device makes the determination of nucleation and growth temperatures difficult for different materials. large randomness
The application of micro-synthesis devices in the preparation of nanocrystals has effectively solved the control problem, but the existing micro-synthesis devices all use the same temperature for the nucleation and growth of nanocrystals, and the high temperature required for instantaneous nucleation makes the follow-up process of nanocrystals difficult. The growth process is out of control, which directly leads to the broadening of the size distribution of nanocrystals and the reduction of crystallization properties

Method used

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  • Micro-reaction device and method for synthesizing cadmium selenide nano-crystal by using temperature gradient
  • Micro-reaction device and method for synthesizing cadmium selenide nano-crystal by using temperature gradient

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Embodiment

[0034] (1) A mixture of 17.13mg CdO, 0.47ml oleic acid and 3.53ml octadecene was heated at 150°C for 1.5 hours to obtain a transparent solution as a Cd precursor; Se (52.67mg) was dissolved in 1.5ml tri-n-octylphosphine , the obtained transparent solution was diluted to 4 ml with octadecene and oleylamine to obtain the Se precursor. The two precursors were degassed at 100 °C for 1 hour and loaded into tightly sealed syringes;

[0035](3) Plastic hoses are used to connect the syringe, the convective micro-mixer and the polytetrafluoroethylene micro-pipe to ensure strict sealing. A polytetrafluoroethylene capillary with an inner diameter of 0.3 mm was used as the reaction microchannel. Using a tube-type electric furnace as a heat source, fix a stainless steel tube (inner diameter 1mm) along the axis of the tube-type furnace at a position close to the heating resistance wire in the tube-type furnace, and place another stainless steel tube of the same specification parallel to it...

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Abstract

The invention relates to a method for synthesizing cadmium selenide nanometer crystallite and a device for synthesizing cadmium selenide nanometer crystallite by the temperature gradient, the reaction system realizes regulating the temperature gradient by changing the relative distance between the high temperature stage and the low temperature stage or by selecting different thermal barrier material, optimizing the nucleation and the growth process by changing the temperature difference between the high temperature stage and the low temperature stage and the detention period in the two stages, and realizing a continuous preparation of the high quality cadmium selenide nanometer crystallite. The method and the device have the advantages that: (1) the realizing mode of the particle nucleation and the growth process of the micro-channel is flexible and reliable by adopting temperature gradient method, which can be extensively applied in a micro-reaction system and a capillary micro-reaction system, (2) the obtained nanocrystalline has a narrow distributing size and a good performance, (3) the high quality continuous synthesis of the various nanocrystalline can be realized, only need changing the species and the procedure parametric of the precursor, and the method and the device can be extensively applied to the solvent-thermal method for preparing various nanocrystalline.

Description

technical field [0001] The invention relates to a micro-synthesis device and method for controlling the nucleation and growth of cadmium selenide nanocrystals, the purpose of which is to realize the continuous preparation of high-performance cadmium selenide nanocrystals; the preparation of cadmium selenide nanocrystals by using the device has good stability, It has the characteristics of high product quality and flexible operation process; it belongs to the field of microchemical machinery and nanomaterials. Background technique [0002] The energy crisis and the deteriorating environmental problems have made miniaturization an important trend in the development of natural science and engineering technology. In particular, the development of nanomaterials and microelectromechanical systems has aroused great interest in small-scale and fast processes. The miniaturization of chemical / chemical machinery has significantly enhanced the heat transfer coefficient and mass transfer...

Claims

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Application Information

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IPC IPC(8): C30B29/48C30B11/00
Inventor 栾伟玲杨洪伟黄永范宁宁万真毛乐园涂善东
Owner EAST CHINA UNIV OF SCI & TECH
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