CN100557091C - A kind of micro-reaction device and method of utilizing the thermograde synthesizing cadmium selenide nano-crystal - Google Patents
A kind of micro-reaction device and method of utilizing the thermograde synthesizing cadmium selenide nano-crystal Download PDFInfo
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- CN100557091C CN100557091C CNB2007100479181A CN200710047918A CN100557091C CN 100557091 C CN100557091 C CN 100557091C CN B2007100479181 A CNB2007100479181 A CN B2007100479181A CN 200710047918 A CN200710047918 A CN 200710047918A CN 100557091 C CN100557091 C CN 100557091C
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Abstract
The present invention relates to a kind ofly carry out the little synthetic method and apparatus of cadmium selenide nano-crystal by thermograde.Reactive system is by changing high temperature section and the relative distance of low-temperature zone or the regulation and control of selecting different thermal boundary material realization thermogrades for use.Change the temperature difference of high temperature section and low-temperature zone and, realize the continuous preparation of high quality cadmium selenide nano-crystal in two sections the residence time realization forming core and the optimization of process of growth.This invention embodies following advantage: (1) temperature gradient method make particle forming core and process of growth in the microchannel implementation flexibly, reliable, be widely used in little reactive system of chip and the little reactive system of kapillary; (2) the nanocrystalline narrow size distribution that obtains, and have good performance; (3) can realize that multiple nanocrystalline high quality is synthetic continuously.Only need change presoma kind and process parameter, the present invention can be widely used in multiple nanocrystalline solvent-thermal method preparation.
Description
Technical field
The present invention relates to a kind of little synthesizer and method of controlling cadmium selenide nano-crystal forming core and growth, purpose is to realize the continuous preparation of high-performance cadmium selenide nano-crystal; This utilizes this device preparation cadmium selenide nano-crystal to have characteristics such as good stability, quality product height, operating process be flexible; Belong to little chemical machinery and field of nanometer material technology.
Background technology
The continuous deterioration of energy dilemma and environmental problem makes microminiaturization become the important trend of natural science and engineering development, and especially the development of nano material and microelectromechanical systems causes that the investigator is to the very big interest of small scale with quick process.The microminiaturization of chemistry/chemical machinery is significantly strengthened heat transfer coefficient and mass-transfer performance, is applied to chemical reaction process and can directly causes reaction conversion ratio, optionally significantly improve.In addition, little chemistry/chemical machinery institute inherent scale effect simple in structure, no, control accurate and safe and reliable etc. have to name a person for a particular job traditional chemical reaction process is produced revolutionary impact.
Nano material has the characteristics such as mechanics, optics, magnetics, calorifics and chemistry that are different from conventional material.Nano material and nanotechnology will be created an a whole new world for the mankind, bring human a large amount of mysterious variation.In nano material, the semiconductor nanocrystal of zero dimension reveals unique magnetic and luminescent properties, and wherein CdSe is nanocrystalline because its fluorescence scope that covers whole visible region more causes materials chemistry man's very big interest.At present its applied research in fields such as laser, solar cell, photodiode, biomarkers is also made a breakthrough.
The nanocrystalline preparation of high quality is used prerequisite with fundamental research as nano material, is just becoming the hot issue of physics, chemistry, material and Related Research Domain.Chemical synthesis process has advantages such as raw material is various, flexibility of operation good, product convenient post-treatment.Wherein in the flask synthesizer, carry out the good examples that organic solvent hydrothermal method is the nanocrystalline preparation of high quality CdSe, but entire reaction course is close to harshness to the requirement of temperature of reaction, reaction times and reaction mass homogeneity, and how much amplifications of flask reaction unit will bring the control response time long, problems such as low precision, and be difficult to guarantee the height consistence of reaction conditions.High temperature forming core and the low-temperature epitaxy validity in nanocrystalline reaction kinetics control is extensively verified, yet the deficiency of flask device at aspects such as control accuracy and control response times makes the definite of forming core and growth temperature show bigger randomness to differing materials.The application of little synthesizer in nanocrystalline preparation effectively solved control problem, but existing little synthesizer all adopts identical temperature to carry out nanocrystalline forming core and growth, the required high temperature of instantaneous forming core makes nanocrystalline subsequent growth process out of control, directly causes the broadening of nanocrystalline distribution of sizes and the reduction of crystal property.
Summary of the invention
The objective of the invention is to develop the little synthesizer and the method for the control nanocrystalline forming core of CdSe and growth, with realize nanocrystalline synthetic in the accurate control of forming core and process of growth, thereby the nanocrystalline continuous preparation of realization high quality.
The present invention is achieved by the following technical solutions:
A kind of micro-reaction device that utilizes the thermograde synthesizing cadmium selenide nano-crystal, it is characterized in that, described device comprises to sample system, micro mixer, reactive system and collection container, liquid storage container 1 links to each other with micro-injection pump 2 and constitutes the sample system that gives, and converges back access micro mixer 3 by the outlet conduit of micro-injection pump 2 for the sample system by two groups; Reactive system comprises an electric tube furnace 11, a stainless steel tube 12a is along the electric tube furnace axis direction, be fixed in the stove near the resistive heater place, another root stainless steel tube 12b is parallel with 12a to be placed near furnace axis line place, vertical range between two stainless steel pipes is greater than 0 and less than the stove radius, there are 13 sealings of two heat insulations at electric tube furnace 11 two ends, a micro-tube 8 is entered in the stainless steel tube 12a by high temperature section import 4, lay to high temperature section along stainless steel tube 12a and to export 5 places, export 5 places in low-temperature zone import 6 enters stainless steel tube 12b by high temperature section, lay to low-temperature zone outlet 10 along rust steel pipe 12b; The part that micro-tube 8 is positioned at stainless steel tube 12a is a high temperature section, the part that micro-tube 8 is positioned at stainless steel tube 12b is a low-temperature zone, by high temperature section outlet 5 parts to low-temperature zone import 6 is transition section, wherein, high temperature section is 1: 5～1: 35 with the length ratio of low-temperature zone, at the middle part of the stainless steel tube at high temperature section and low-temperature zone place, respectively offer an aperture and insert micro thermocouple 7; Micro mixer 3 links to each other with reactive system by the high temperature section import 4 that is positioned on the micro-tube 8, and collection container 14 links to each other with reactive system by low-temperature zone outlet 10; Wherein, the internal diameter of described micro-tube is 0.2～0.5mm.
This installs further improved plan: in the reactive system of above-mentioned micro-reaction device, be provided with thermofin 9 between stainless steel tube 12a and 12b.
The present invention also provides a kind of CdSe of preparation nanocrystalline method:
A kind of described micro-reaction device of claim 1 that uses prepares the nanocrystalline method of CdSe, it is characterized in that described method is following steps:
1) presoma of configuration Se and Cd: with 17.13mg CdO, the heating under 150 ℃ of 0.47ml oleic acid, the mixture of 3.53ml octadecylene obtained clear solution as the Cd presoma in 1.5 hours; 52.67mg Se is dissolved in the 1.5ml tri-n-octyl phosphine, and the clear solution that obtains uses octadecylene and oleyl amine to be diluted to 4ml and obtains the Se presoma;
Import for the sample system by two groups respectively the presoma of Se and Cd, after switching interface converges, enter the convection current micro mixer;
2) start electric tube furnace, slowly heat up, when treating that the variation of micro thermocouple reading in 10min is no more than 0.5 ℃, start syringe pump and begin to react, mixed uniformly reactant enters reactive system;
3) temperature of adjusting tube furnace, making the high-temperature zone temperature is 285 ℃, the cold zone temperature is 230 ℃～264 ℃;
4) reactant enters low-temperature region through transition section after by high temperature section, carries out product at last and collects, and it is nanocrystalline to obtain required CdSe.
Key problem in technology of the present invention is to realize controlled temperature range at the heating component of little synthesizer, use two kinds of different temperature sections for the nanocrystalline forming core requirement different of CdSe with process of growth, and obtain effective control of forming core and process of growth in the residence time of two warm areas by changing forming core and growth temperature and reactant, realize singly disperseing, nanocrystalline continuous synthesizing of CdSe of high-crystallinity.
This synthetic method and apparatus has following characteristics:
(1) the reinforcement convection type realization response presoma in whole synthesizer uses between microvoid is seen figure one in the high efficient mixed of low flow conditions.
(2) Se and Cd presoma are respectively by importing for the sample system, after converging, switching interface enters the convection current micro mixer, mixed uniformly reactant enters heating region, after stopping certain hour, high temperature section enters low-temperature region through transition section, micro-tube conduct heat efficiently make effusive product at internal cooling in short-term to room temperature, carry out product at last and collect.
The tetrafluoroethylene microtubule can show stability preferably when (3) temperature of reaction was lower than 285 ℃, and higher temperature of reaction need realize in high-temp-resistant micro pipelines such as quartz, stainless steel.Micro-tube places heat conductivility supporting tube preferably, and the internal diameter of supporting tube needs suitable with the micro-tube internal diameter, with the planeness of micro-tube behind the assurance stringing.In the corresponding position perforate of high and low temperature supporting tube surface, respectively as micro-tube in the outlet of high temperature section and the import of low-temperature zone.
(4) come the realization response thing in the adjustment of the different warm area residence time by changing high-temperature zone and the length of cold zone micro-tube, raw material is mixed and the influence of reactant residence time distribution in passage with the variation of avoiding flow velocity.The length of high-temperature zone micro-tube will guarantee that material is lower than 3s in the residence time of this section, and the micro-tube length of cold zone is by required reaction times respective change.
(5) hot spots of micro-tube is divided into two zones, between can separate (also can be filled in the middle of two supporting tubes) with thermofin 9 with lagging material, change two-part temperature head, the transition in thermofin of two warm areas by the thickness of adjusting thermofin; In same temperature province, guarantee the homogeneous, stable in temperature field.Select for use the good material of heat-proof quality as thermofin, can guarantee in thin thermal insulation layer, to obtain the big temperature difference.
(6) product that obtains is characterized, can be by the relatively more definite best forming core of product performance and the temperature and time of growth.
Beneficial effect
This little synthesizer is realized stable, controlled different warm areas at heating region, and the adjustment of the temperature and time by forming core and growth realizes effective control of nanocrystalline building-up process, the output and the quality of raising product.The implementation of temperature range flexibly, reliably among the present invention, both can be at the heating region etching groove of chip microreactor, with air or other lagging material as thermofin, also the hot spots of microreactor can be placed two kinds of different heating mediums to heat, to realize wider temperature variation.This invention extensively is adapted to nanocrystalline solvent process for thermosynthesizing, can realize that by adjusting reaction parameter multiple nanocrystalline height is controlled and synthetic continuously; Simultaneously, the operating method of the increase of Bing Hang micro-tube number and operation continuously all helps nanocrystalline mass preparation also can satisfy the needs of flexible production.
Description of drawings
The nanocrystalline structure diagram of CdSe is synthesized in the little reaction of Fig. 1 thermograde;
Wherein, 1-liquid storage container; The 2-micro-injection pump; The 3-micro mixer; The import of 4-high temperature section; The outlet of 5-high temperature section; The import of 6-low-temperature zone; The 7-micro thermocouple; 8-micro-tube (internal diameter 0.2～0.5mm); The 9-thermofin; The outlet of 10-low-temperature zone; The 11-electric tube furnace; 12a-high temperature section stainless steel supporting tube, 12b-low-temperature zone stainless steel supporting tube; The 13-heat insulation; The 14-collection container;
Absorption that the CdSe of Fig. 2 temperature gradient method and constant temperature method preparation is nanocrystalline and fluorescence spectrum are relatively;
The nanocrystalline absorption spectrum of Fig. 3 CdSe is with the variation of the high temperature section residence time;
The nanocrystalline absorption spectrum of Fig. 4 CdSe is with the variation of the low-temperature zone residence time;
Under Fig. 5 (a) condition of different temperatures and (b) the nanocrystalline absorption spectrum of synthetic CdSe is relatively under the constant temperature;
The typical high-resolution-ration transmission electric-lens photo that Fig. 6 CdSe is nanocrystalline.
Embodiment
The present invention is further elaborated below by embodiment, but do not limit protection scope of the present invention.
Embodiment:
(1) with 17.13mg CdO, the heating under 150 ℃ of 0.47ml oleic acid, the mixture of 3.53ml octadecylene obtained clear solution as the Cd presoma in 1.5 hours; Se (52.67mg) is dissolved in the 1.5ml tri-n-octyl phosphine, and the clear solution that obtains uses octadecylene and oleyl amine to be diluted to 4ml and obtains the Se presoma.In the syringe of the strict seal of packing into after two kinds of presomas outgased 1 hour under 100 ℃;
(3) connect with plastic hose between syringe, convection current micro mixer and the tetrafluoroethylene micro-tube, guarantee strict seal.Use internal diameter as the polytetrafluoroethylene capillary of 0.3mm as the reaction micro-tube.With electric tube furnace as thermal source, a stainless steel tube (internal diameter 1mm) is fixed in the position of close resistive heater in the tube furnace along the axis direction of tube furnace, the parallel with it position that places near the tube furnace axle center of another root same size stainless steel tube utilizes the interior atmospheric thermal insulation of stove to form different temperature ranges on two stainless steel tubes.Polytetrafluoroethylene capillary is support with the stainless steel tube, advance a segment distance along the high temperature stainless steel pipe after, enter low-temperature region by transition section, and along this place's stainless steel tube stringing.In the process of the test, the micro-tube length of high temperature section is 1cm-7cm, the length of low-temperature zone changes between 5cm and 35cm, realize that by changing two parallel distances that support stainless steel tube the control of the high temperature and the low-temperature zone temperature difference is (in this example, the high-temperature zone is fixed as 285 ℃, and the cold zone temperature changes between 230 ℃ and 264 ℃).The adiabatic cotton strict seal is used at the tube furnace two ends; The variation of micro thermocouple with real-time monitor temperature inserted in the stainless steel pipe surface perforate.Open tube furnace, slowly heat up (5 ℃ of per minutes), treat that the stable back of furnace temperature (variation of micro thermocouple reading in 10min is no more than 0.5 ℃) starts syringe pump and begins to react;
(4) temperature of adjusting tube furnace is so that the high-temperature zone reaches 285 ℃ of preset values.
(5) sample of exit collection absorbs with fluorescence spectrum and tests.Find that by test with nanocrystalline the comparing of use steady temperature synthetic CdSe, the nanocrystalline absorption peak and the fluorescence spectra of the little reaction method preparation of alternating temperature significantly narrow down (Fig. 2), show that high temperature forming core and low-temperature epitaxy help the improvement of nanocrystalline distribution of sizes.Reactant produces material impact in the residence time of high temperature section to nanocrystalline performance, and along with the prolongation of the high temperature section residence time, the increase earlier of the granule density of CdSe reduces then gradually in the product, and maximum (Fig. 3) occurs at the 1.2s place; Product fluorescence half width at half maximum minimum value occurs at the 2.4s place.Be accompanied by nanocrystalline prolongation in the low-temperature zone residence time, concentration phenomenon (Fig. 4) appears in the distribution of sizes of product, occurs Ostwald ripening subsequently, causes distribution of sizes to broaden.
(6) by changing high temperature and low temperature parallel distance capillaceous, use native system can realize the temperature difference (when temperature end is 285 ℃) of 55 ℃ of high temperature and low-temperature zone, by changing the temperature value of cold zone, can realize the nanocrystalline continuous production (Fig. 5, Fig. 6) of high quality CdSe of serial size, and compare with constant temperature is synthetic, the little reaction method of alternating temperature obtains nanocrystallinely has a narrower absorption peak (Fig. 5).
Claims (3)
1, a kind of micro-reaction device that utilizes the thermograde synthesizing cadmium selenide nano-crystal, it is characterized in that, described device comprises to sample system, micro mixer, reactive system and collection container, liquid storage container (1) links to each other with micro-injection pump (2) and constitutes the sample system that gives, and converges back access micro mixer (3) by the outlet conduit of micro-injection pump (2) for the sample system by two groups; Reactive system comprises an electric tube furnace (11), a stainless steel tube (12a) is along the electric tube furnace axis direction, be fixed in the stove near the resistive heater place, another root stainless steel tube (12b) is parallel with (12a) to be placed near furnace axis line place, vertical range between two stainless steel pipes is greater than 0 and less than the stove radius, there is two heat insulations (13) sealing at electric tube furnace (11) two ends, a micro-tube (8) is entered in the stainless steel tube (12a) by high temperature section import (4), lay to high temperature section outlet (5) along stainless steel tube (12a) and to locate, locate in low-temperature zone import (6) enters stainless steel tube (12b) by high temperature section outlet (5), lay to low-temperature zone outlet (10) along stainless steel tube (12b); The part that micro-tube (8) is positioned at stainless steel tube (12a) is a high temperature section, the part that micro-tube (8) is positioned at stainless steel tube (12b) is a low-temperature zone, by high temperature section outlet (5) to the part of low-temperature zone import (6) is transition section, wherein, high temperature section is 1: 5～1: 35 with the length ratio of low-temperature zone, at the middle part of the stainless steel tube at high temperature section and low-temperature zone place, respectively offer an aperture and insert micro thermocouple (7); Micro mixer (3) links to each other with reactive system by the high temperature section import (4) that is positioned on the micro-tube (8), and collection container (14) links to each other with reactive system by low-temperature zone outlet (10), and wherein, the internal diameter of described micro-tube is 0.2～0.5mm.
2, the micro-reaction device that utilizes the thermograde synthesizing cadmium selenide nano-crystal as claimed in claim 1 is characterized in that, described stainless steel tube (12a) and (12b) between be provided with thermofin (9).
3, a kind of described micro-reaction device of claim 1 that uses prepares the nanocrystalline method of CdSe, it is characterized in that described method is following steps:
1) presoma of configuration Se and Cd:
With 17.13mg CdO, the heating under 150 ℃ of 0.47ml oleic acid, the mixture of 3.53ml octadecylene obtained clear solution as the Cd presoma in 1.5 hours; 52.67mg Se is dissolved in the 1.5ml tri-n-octyl phosphine, and the clear solution that obtains uses octadecylene and oleyl amine to be diluted to 4ml and obtains the Se presoma;
Import for the sample system by two groups respectively the presoma of Se and Cd, after switching interface converges, enter the convection current micro mixer;
2) start electric tube furnace, slowly heat up, when treating that the variation of micro thermocouple reading in 10min is no more than 0.5 ℃, start syringe pump and begin to react, mixed uniformly reactant enters reactive system;
3) temperature of adjusting tube furnace, making the high-temperature zone temperature is 285 ℃, the cold zone temperature is 230 ℃～264 ℃;
4) reactant enters low-temperature region through transition section after by high temperature section, carries out product at last and collects, and it is nanocrystalline to obtain required CdSe.
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| KR101078050B1 (en) * | 2008-10-27 | 2011-10-31 | 한국기계연구원 | apparatus and method for producing quantum dot |
| KR101147840B1 (en) | 2008-10-27 | 2012-05-21 | 한국기계연구원 | apparatus and method for producing quantum dot having multiple heating area |
| CN101618308B (en) * | 2009-06-09 | 2011-12-21 | 宋玉军 | Microfluid reactor based nano-particle preparation and particle controlled preparation process |
| US9493351B2 (en) * | 2011-12-07 | 2016-11-15 | East China University Of Science And Technology | Methods of producing cadmium selenide multi-pod nanocrystals |
| CN102765704A (en) * | 2012-07-31 | 2012-11-07 | 上海交通大学 | Preparation method of tin-doped lead selenide nanoparticle |
| CN104638034B (en) * | 2015-02-13 | 2016-09-07 | 中国科学院重庆绿色智能技术研究院 | A kind of flexible thin-film solar cell |
| CN107675251B (en) * | 2017-09-28 | 2019-07-16 | 哈尔滨工业大学 | A kind of gas-phase synthesizing method of high-purity cadmium selenide polycrystalline material |
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